CA1100250A - Composition for forming an intumescent material - Google Patents
Composition for forming an intumescent materialInfo
- Publication number
- CA1100250A CA1100250A CA296,240A CA296240A CA1100250A CA 1100250 A CA1100250 A CA 1100250A CA 296240 A CA296240 A CA 296240A CA 1100250 A CA1100250 A CA 1100250A
- Authority
- CA
- Canada
- Prior art keywords
- weight
- parts
- resin
- water
- cross
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 36
- 239000000463 material Substances 0.000 title claims abstract description 34
- 229920005989 resin Polymers 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 18
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 11
- 239000004640 Melamine resin Substances 0.000 claims abstract description 10
- 229920002689 polyvinyl acetate Polymers 0.000 claims abstract description 10
- 239000011118 polyvinyl acetate Substances 0.000 claims abstract description 10
- 239000004254 Ammonium phosphate Substances 0.000 claims abstract description 8
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims abstract description 8
- 235000019289 ammonium phosphates Nutrition 0.000 claims abstract description 8
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002657 fibrous material Substances 0.000 claims abstract description 8
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 4
- 239000008259 solid foam Substances 0.000 claims abstract 4
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims description 6
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 4
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims description 3
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical group [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 3
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 3
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims description 3
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 3
- 239000006012 monoammonium phosphate Substances 0.000 claims description 3
- 239000011398 Portland cement Substances 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004568 cement Substances 0.000 claims description 2
- 238000004132 cross linking Methods 0.000 claims description 2
- 230000001427 coherent effect Effects 0.000 claims 1
- 238000005336 cracking Methods 0.000 abstract description 3
- 150000002440 hydroxy compounds Chemical class 0.000 abstract description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Inorganic materials [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 8
- 239000011507 gypsum plaster Substances 0.000 description 8
- 230000032683 aging Effects 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 4
- 230000009970 fire resistant effect Effects 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 3
- 229920000915 polyvinyl chloride Polymers 0.000 description 3
- 239000004800 polyvinyl chloride Substances 0.000 description 3
- 239000000565 sealant Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011093 chipboard Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- -1 methylol groups Chemical group 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000011120 plywood Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
- C09D5/185—Intumescent paints
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08L61/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/14—Macromolecular materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S521/00—Synthetic resins or natural rubbers -- part of the class 520 series
- Y10S521/907—Nonurethane flameproofed cellular product
Abstract
ABSTRACT
The invention provides a composition for forming an intumescent material which upon heating decomposes into gas and a solid foam residue, comprising: a water-dispersible melamine formaldehyde resin which when cured is hydrophobic; a setting agent which hardens in the presence of water thereby to cause the composition to set; a cross-linking agent for curing the resin, the cross-linking agent being a polyamido compound; an ammonium phosphate; polyvinyl acetate; a solid poly-hydroxy compound; and reinforcing fibrous material.
To form the intumescent material, the composition is caused to set and the melamine resin is cured. The intumescent material has improved anti-cracking properties.
The invention provides a composition for forming an intumescent material which upon heating decomposes into gas and a solid foam residue, comprising: a water-dispersible melamine formaldehyde resin which when cured is hydrophobic; a setting agent which hardens in the presence of water thereby to cause the composition to set; a cross-linking agent for curing the resin, the cross-linking agent being a polyamido compound; an ammonium phosphate; polyvinyl acetate; a solid poly-hydroxy compound; and reinforcing fibrous material.
To form the intumescent material, the composition is caused to set and the melamine resin is cured. The intumescent material has improved anti-cracking properties.
Description
The present invention relates to.a composition for forming an intumescent material. The intumescent material when exposed to heat swells (i.e. intumesces) and in the intumesced state is capable of acting as a fire-resistant barrier or sealant.
Intumescent material has been used to provide a fire-resistant barrier or sealant in gaps e.g. between a door and adjacent structure, e.g. the jamb, and between a window and an adjacent structure, e.g. the window frame.
In British Patent No. 1,529,054 there is proposed intumescent materials comprising urea formaldehyde resin constituents, the intumescent material swelling when exposed - to heat and in the intumesced state being capable of acting as a fire-resistant barrier or sealant between adjacent structures. It is proposed in that Patent to have the intumescent material retained in a holder for securing to one of the structures. The material may be put into the holder in the form of a paste or slurry which is allowed to set in the holder. Alternatively, instead of applying the material into the holder, the material may be applied into a gap between the structures or onto a surface of one of the structures and then allowed to set. After setting the intumescent material dries out and ages. It has been found that there was a tendency for the intumescent material to crack during setting, drying or ageing.
.
Intumescent material has been used to provide a fire-resistant barrier or sealant in gaps e.g. between a door and adjacent structure, e.g. the jamb, and between a window and an adjacent structure, e.g. the window frame.
In British Patent No. 1,529,054 there is proposed intumescent materials comprising urea formaldehyde resin constituents, the intumescent material swelling when exposed - to heat and in the intumesced state being capable of acting as a fire-resistant barrier or sealant between adjacent structures. It is proposed in that Patent to have the intumescent material retained in a holder for securing to one of the structures. The material may be put into the holder in the form of a paste or slurry which is allowed to set in the holder. Alternatively, instead of applying the material into the holder, the material may be applied into a gap between the structures or onto a surface of one of the structures and then allowed to set. After setting the intumescent material dries out and ages. It has been found that there was a tendency for the intumescent material to crack during setting, drying or ageing.
.
2 ~
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, , It is ~elievcd that tlle crac]~ing is duc in thc main to the urea formaldchyde content of the intumcscent ; material. The resin is hydrophilic to an appreciable extent when cured and we believe that evaporation oi ~ater temporarily held by the cured resin gave rise to the cracking.
An object of the invention is to enable cracl~ing - of the intl~lescent material after application to be reduced.
.
- 10 Accordingly, the present invention provides a composition for forming an intumescent material which upon heating decomposes into gas and a so]id foam residue, comprising: a water-dispersible melamine Iorm~.ldehyde resin which when cured is hydrophobic; a setting agent which hardens in the presence of water t~leréby to cause the composition to set; a cross-linking agent for curing the resin, the cross-linking agent being a polyamido compound; an am.monium phosphate; pol~irl~-]
acetate; a solid polyhydroxy compound; and reinforciIlg fibrous material.
The invention further provides an intumescent material formed from the composition according to the invention, by curing of the melamine formaldehyde resin and hardening of the setting agent in the presence of water to cause the composition to set.
It will be appreciated that the intumesccnt materia] according to the invention necd not contain ~ (and ordinarily would not contain) any urea formaldellyde - resin constitllent.
`~ ' , The mel~line resin in the eoplposition prcferal)ly eithcr lS in powdcr form or is in thc form oI a liquid ~ having a solids content ol at lcast 75% by weight.
0 The setting agent may be calcium sulphate hemi-hydrate (plaster of Paris), Portland cement or high alumina cement or a mixture of such agents.
The cross-linking agent is provided in order to promote satisfactory curing of the resin and serves for cross-linking with the methylol groups on the resin molecules.
The cross-linking agent may be one or more polyamido compounds such as dicyandiamide and/or guanidine. Either of these .~
cross-linking agents will also serve to enhance the degree of intumescence of the material when exposed to head.
The ammonium phosphate, which is preferably monoammonium phosphate, in admixture with the melamine resin serves as the main source of the intumescence of the material.
The fibrous reinforcing material may be wood flour, hammer milled glass fibres or disintegrated nylon fibres.
The solid polyhydro~y compound may be pentaerythritol or a sugar.
In general it is preferred that the amounts of the various ingredients in a composition according to the invention (and the amount of water added thereto when forming an intumescent material) vary by no more than + 10%~ niore preferably no more than + 5%~ from the basic proportions given in the Table belo-~.
. ~ i -.
T~hle `~.' Ingredient Basic relative proportions ~Ielami~le formaldehyde resin Ammoni~n phosphate Cross-linking agent Pentaerylthritol (or othersolid poly-hydroxy compound) Plaster of Paris Polyvinyl acetate 25 Fibrous reinforcing agent 20 Water s _ The composition according to the invention preferably comprises: 90 to 110 parts by ~eight of the water-dispersible melamine resin; 90 to 110 parts by weight of the setting agent; 45 to 55 parts by weight of the cross-linking agent; 90 to 110 parts by weight of the ammonium phosphate; 3.6 to 4.4 parts by weight of the polyvinyl acetate; 18 to 22 parts by weight of the solid polyhydroxy compound and 4.5 tG 5.5 parts by weight of the reinforcing fibrous material; these parts by weight being based on a total of 250 parts by weight of the melamine resin, the setting agent and the cross-linkin~ agent.
The preferred composition described above is preferably a~nixed with 56 to 69 parts by ~Yeight of water pcr 100 parts by weight of the mc1~mine resin in prcparing ' ~
;~ - 5 -..... ~ - .
.
5~ ``
the i.l~t;lullescellt mat;erial accordi.ng to l;llc invention.
Tllc i.ntulllcsccnt materi.a:L accordin~ to the inventi.on preferably comprises: 90 to 110 parts by weight of the . melamine resin; the resin i.ncluding cross~linking residues being derived from 45 to 55 parts by weight .
. of the polyamido compound; 90 to 110 parts by weight of . the setting agent; 90 to 110 parts by weight of the . ammonil~n phosphate; 3.6 to 4.4 parts by weight of the . 10 pol~inyl acetate; 18 to 22 parts by weight of the solid polyhydroxy compound; 4.5 to 5.5 parts by weight of the reinforcing fibrous material; and 56 to 69 parts by weight of . ~ water; these parts by weight being based on a to~l of 250 parts by weight of the melamine resin and the setting agent.
The invention is illustrated by the following examples.
I Ex~mple 1 : . The following composition is made as a dry powder suitable for stocking by intermixing the following constituents in a dry powder state:
. . Melamine formaldehyde resin powder 3800 g .. Monoammonium phosphate 4200 g .~
:: Dicyandiamide 2000 g Pentaerythritol . 800 g Plaster of Paris 1100 g . Water dispersible polyvinyl acetate . I !powder 150 g 'Woodflour (passing through 90 mesh) 25 g The plaster ol' Paris is of the killd whi.cl-l exhibits high expansion during setting.
.~ .
~:.
~ I llOG2:;0 ``
~ 'atcr (2400 g) :is intermixed with the above dry composition imlllediately before it is to be put into a holder strip. The mixture thus formed is a s]urry which can be pumped into the holder if tubular. rl'he holder is loaded quickly with the slurry because of the setting action of the plaster of Paris which begins as soon as the water has been added. In tests carried out up to the present, the slurry mixture is allowed to stand in the holder for 2 days at room temperature, the holder if tubular thereafter being slotted along one face by a milling cutter to expose the mixture, which is there-after matured at 40C for 24 hours. The holder containing the mixture is then ready for application as a ~ire-resistant seal.
A water absorption test carried out on the matured mixture showed it to increase in weight by about 7% after a 24 hour immersion. It is therefore advisable to waterproof the mixture as soon as the standing and maturing periods are complete in order to improve the shelf and service life of the fire-resistant seal produced. Waterproofing can be effected by coating the matured mixture or material in th~ holder with polyurethane resin.
The intumescent material with the composition set out above and as a layer of 8 mm wide x 4 mm thick l I
and 1 metre long exhibited no cracking when examined 1 year after being put in the holder to mature.
` S A~' `~ ``\ :
The holder is prererably of mctal of high thermal conductivity such as aluminium, but may bc Or rigid plastics .
~ such as rigid P~C or ABS.
. . . . .
To make a wet mlx ready for lmmedlate lntermlxlng with additional water to form a paste or slurry for immediate loading into a holder, the polyvinylacetate powder in the foregoing composition may be replaced by 300 g of a vinyl resin emulsion (50,~ solids).
The foregoing composition can be adapted to the production of a plaster of Paris mix, for application, when made into a paste, to gaps round the jambs and lintel of a door and to surface areas generally, where intumescence under conflagration conditions is advantageous. To this end ordinary plaster of Paris as used by builders is used in the composition, and the proportion of plaster of Paris is as high as is consistent with an acceptable degree of intumescence. This modification of the invention is illustrated by Example 2 below.
Example 2 A first mix is prepared consisting of:-Plaster of Paris 4800 g ~- Dicyandiamide 2000 g .
Pentaerythritol 800 g Water-dispersible polyvinyl acetate powder 150 g Wood flour (passing through 90 mesh) 250 g A second mix is prepared consisting of:-iIonoammonium phosphate ~200 g Melaminc lormaldellyde resin powder 380() g, ,, ~ ,, - ~3 - ' ~ 2S~ ;-:.
Equal parts by wcight of thc first and secon(lmixes arc admixed together and watcr is added to make a trowcllable paste which can be applied to surface areas g~nelally and becomes an int~nescent material.
An example of a suitable holder is shown in the accompanying drawing which is a cross-sectional view of - the holder.
The holder shown in the drawing is in the form of a strip 1 of uniform cross-section defining two grooves each loaded with intumescent material 2. The holder 1 has slots forming the mouths of the grooves.
A fire test was carried out using a sealïng device consisting of the holder shown in the drawing containing intumescent material prepared and loaded into the holder as described in the Example 1 above. The holder was formed of aluminium. The test is described below.
The fire test was primarlly a test for fire resistance on a wooden door according to British Standard 476; Part 8: 1972, Item 7. The door consisted of chipboard faced with plywood covered by PVC (polyvinyl chloride). The door was a two part swing door intended for hospital use. The door was located in a doorway, the top edge and the side edges of the doorway being fitted with fire barrier material. At the mceting stile down the middle of the two parts of the door, the sealing device according to the invention, was fittcd, the scaling dcvice being located in a groove in onc of _ 9 _ 25~
the door ~arts with its slots facing thc othcr door part.
A comb~stion chambcr behind the door contained ~as jets directed across the inside door face. The jets were lit and the temperature rose to about 800C
in 30 minutes and was held at about 850C for a further 30 minutes.
~ After 10 to 15 minutes from the start up there was a heat surge and the recorded temperature rose to about 950C. This was ascribed to the exothermic reaction as the inside PVC facing on the door was combusted.
At the end of the test run, that is 60 minutes from starting up the outside of the door and the sealin the stile was intact. Thus the intumescent material had complied with the test requirements.
The heating was continued for another 10 minutes to see whether any breakdown would take place At 3 - 5 minutes of extra time the door itse~f started to buckle .
~ at the bottom of the meeting stile, some smoke started .-; to seep out at that place.
Thus, the sealing device, according to the invention started to fail only after the door itself had failed.
Sealing devices as described above were also subjected to accelerated ageing tests to determine the thickness of intumesced material kno~ as "puff" formed ; after various amounts of accelerated ageing.
The results of the tests were as follows:
before ageing 20 mm puff .~
' , 11~1~25~
. after a~eing equatecl Wit}l one year 19 mm puff after ageing equatcd with five years 25 mm puff after ageing equated with eight years 23 mm puff.
~he thickness of the puff was measured in the . direction normal to the width of the slots in the holders.
.
,,, .
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:
:
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.
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.
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, , It is ~elievcd that tlle crac]~ing is duc in thc main to the urea formaldchyde content of the intumcscent ; material. The resin is hydrophilic to an appreciable extent when cured and we believe that evaporation oi ~ater temporarily held by the cured resin gave rise to the cracking.
An object of the invention is to enable cracl~ing - of the intl~lescent material after application to be reduced.
.
- 10 Accordingly, the present invention provides a composition for forming an intumescent material which upon heating decomposes into gas and a so]id foam residue, comprising: a water-dispersible melamine Iorm~.ldehyde resin which when cured is hydrophobic; a setting agent which hardens in the presence of water t~leréby to cause the composition to set; a cross-linking agent for curing the resin, the cross-linking agent being a polyamido compound; an am.monium phosphate; pol~irl~-]
acetate; a solid polyhydroxy compound; and reinforciIlg fibrous material.
The invention further provides an intumescent material formed from the composition according to the invention, by curing of the melamine formaldehyde resin and hardening of the setting agent in the presence of water to cause the composition to set.
It will be appreciated that the intumesccnt materia] according to the invention necd not contain ~ (and ordinarily would not contain) any urea formaldellyde - resin constitllent.
`~ ' , The mel~line resin in the eoplposition prcferal)ly eithcr lS in powdcr form or is in thc form oI a liquid ~ having a solids content ol at lcast 75% by weight.
0 The setting agent may be calcium sulphate hemi-hydrate (plaster of Paris), Portland cement or high alumina cement or a mixture of such agents.
The cross-linking agent is provided in order to promote satisfactory curing of the resin and serves for cross-linking with the methylol groups on the resin molecules.
The cross-linking agent may be one or more polyamido compounds such as dicyandiamide and/or guanidine. Either of these .~
cross-linking agents will also serve to enhance the degree of intumescence of the material when exposed to head.
The ammonium phosphate, which is preferably monoammonium phosphate, in admixture with the melamine resin serves as the main source of the intumescence of the material.
The fibrous reinforcing material may be wood flour, hammer milled glass fibres or disintegrated nylon fibres.
The solid polyhydro~y compound may be pentaerythritol or a sugar.
In general it is preferred that the amounts of the various ingredients in a composition according to the invention (and the amount of water added thereto when forming an intumescent material) vary by no more than + 10%~ niore preferably no more than + 5%~ from the basic proportions given in the Table belo-~.
. ~ i -.
T~hle `~.' Ingredient Basic relative proportions ~Ielami~le formaldehyde resin Ammoni~n phosphate Cross-linking agent Pentaerylthritol (or othersolid poly-hydroxy compound) Plaster of Paris Polyvinyl acetate 25 Fibrous reinforcing agent 20 Water s _ The composition according to the invention preferably comprises: 90 to 110 parts by ~eight of the water-dispersible melamine resin; 90 to 110 parts by weight of the setting agent; 45 to 55 parts by weight of the cross-linking agent; 90 to 110 parts by weight of the ammonium phosphate; 3.6 to 4.4 parts by weight of the polyvinyl acetate; 18 to 22 parts by weight of the solid polyhydroxy compound and 4.5 tG 5.5 parts by weight of the reinforcing fibrous material; these parts by weight being based on a total of 250 parts by weight of the melamine resin, the setting agent and the cross-linkin~ agent.
The preferred composition described above is preferably a~nixed with 56 to 69 parts by ~Yeight of water pcr 100 parts by weight of the mc1~mine resin in prcparing ' ~
;~ - 5 -..... ~ - .
.
5~ ``
the i.l~t;lullescellt mat;erial accordi.ng to l;llc invention.
Tllc i.ntulllcsccnt materi.a:L accordin~ to the inventi.on preferably comprises: 90 to 110 parts by weight of the . melamine resin; the resin i.ncluding cross~linking residues being derived from 45 to 55 parts by weight .
. of the polyamido compound; 90 to 110 parts by weight of . the setting agent; 90 to 110 parts by weight of the . ammonil~n phosphate; 3.6 to 4.4 parts by weight of the . 10 pol~inyl acetate; 18 to 22 parts by weight of the solid polyhydroxy compound; 4.5 to 5.5 parts by weight of the reinforcing fibrous material; and 56 to 69 parts by weight of . ~ water; these parts by weight being based on a to~l of 250 parts by weight of the melamine resin and the setting agent.
The invention is illustrated by the following examples.
I Ex~mple 1 : . The following composition is made as a dry powder suitable for stocking by intermixing the following constituents in a dry powder state:
. . Melamine formaldehyde resin powder 3800 g .. Monoammonium phosphate 4200 g .~
:: Dicyandiamide 2000 g Pentaerythritol . 800 g Plaster of Paris 1100 g . Water dispersible polyvinyl acetate . I !powder 150 g 'Woodflour (passing through 90 mesh) 25 g The plaster ol' Paris is of the killd whi.cl-l exhibits high expansion during setting.
.~ .
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~ I llOG2:;0 ``
~ 'atcr (2400 g) :is intermixed with the above dry composition imlllediately before it is to be put into a holder strip. The mixture thus formed is a s]urry which can be pumped into the holder if tubular. rl'he holder is loaded quickly with the slurry because of the setting action of the plaster of Paris which begins as soon as the water has been added. In tests carried out up to the present, the slurry mixture is allowed to stand in the holder for 2 days at room temperature, the holder if tubular thereafter being slotted along one face by a milling cutter to expose the mixture, which is there-after matured at 40C for 24 hours. The holder containing the mixture is then ready for application as a ~ire-resistant seal.
A water absorption test carried out on the matured mixture showed it to increase in weight by about 7% after a 24 hour immersion. It is therefore advisable to waterproof the mixture as soon as the standing and maturing periods are complete in order to improve the shelf and service life of the fire-resistant seal produced. Waterproofing can be effected by coating the matured mixture or material in th~ holder with polyurethane resin.
The intumescent material with the composition set out above and as a layer of 8 mm wide x 4 mm thick l I
and 1 metre long exhibited no cracking when examined 1 year after being put in the holder to mature.
` S A~' `~ ``\ :
The holder is prererably of mctal of high thermal conductivity such as aluminium, but may bc Or rigid plastics .
~ such as rigid P~C or ABS.
. . . . .
To make a wet mlx ready for lmmedlate lntermlxlng with additional water to form a paste or slurry for immediate loading into a holder, the polyvinylacetate powder in the foregoing composition may be replaced by 300 g of a vinyl resin emulsion (50,~ solids).
The foregoing composition can be adapted to the production of a plaster of Paris mix, for application, when made into a paste, to gaps round the jambs and lintel of a door and to surface areas generally, where intumescence under conflagration conditions is advantageous. To this end ordinary plaster of Paris as used by builders is used in the composition, and the proportion of plaster of Paris is as high as is consistent with an acceptable degree of intumescence. This modification of the invention is illustrated by Example 2 below.
Example 2 A first mix is prepared consisting of:-Plaster of Paris 4800 g ~- Dicyandiamide 2000 g .
Pentaerythritol 800 g Water-dispersible polyvinyl acetate powder 150 g Wood flour (passing through 90 mesh) 250 g A second mix is prepared consisting of:-iIonoammonium phosphate ~200 g Melaminc lormaldellyde resin powder 380() g, ,, ~ ,, - ~3 - ' ~ 2S~ ;-:.
Equal parts by wcight of thc first and secon(lmixes arc admixed together and watcr is added to make a trowcllable paste which can be applied to surface areas g~nelally and becomes an int~nescent material.
An example of a suitable holder is shown in the accompanying drawing which is a cross-sectional view of - the holder.
The holder shown in the drawing is in the form of a strip 1 of uniform cross-section defining two grooves each loaded with intumescent material 2. The holder 1 has slots forming the mouths of the grooves.
A fire test was carried out using a sealïng device consisting of the holder shown in the drawing containing intumescent material prepared and loaded into the holder as described in the Example 1 above. The holder was formed of aluminium. The test is described below.
The fire test was primarlly a test for fire resistance on a wooden door according to British Standard 476; Part 8: 1972, Item 7. The door consisted of chipboard faced with plywood covered by PVC (polyvinyl chloride). The door was a two part swing door intended for hospital use. The door was located in a doorway, the top edge and the side edges of the doorway being fitted with fire barrier material. At the mceting stile down the middle of the two parts of the door, the sealing device according to the invention, was fittcd, the scaling dcvice being located in a groove in onc of _ 9 _ 25~
the door ~arts with its slots facing thc othcr door part.
A comb~stion chambcr behind the door contained ~as jets directed across the inside door face. The jets were lit and the temperature rose to about 800C
in 30 minutes and was held at about 850C for a further 30 minutes.
~ After 10 to 15 minutes from the start up there was a heat surge and the recorded temperature rose to about 950C. This was ascribed to the exothermic reaction as the inside PVC facing on the door was combusted.
At the end of the test run, that is 60 minutes from starting up the outside of the door and the sealin the stile was intact. Thus the intumescent material had complied with the test requirements.
The heating was continued for another 10 minutes to see whether any breakdown would take place At 3 - 5 minutes of extra time the door itse~f started to buckle .
~ at the bottom of the meeting stile, some smoke started .-; to seep out at that place.
Thus, the sealing device, according to the invention started to fail only after the door itself had failed.
Sealing devices as described above were also subjected to accelerated ageing tests to determine the thickness of intumesced material kno~ as "puff" formed ; after various amounts of accelerated ageing.
The results of the tests were as follows:
before ageing 20 mm puff .~
' , 11~1~25~
. after a~eing equatecl Wit}l one year 19 mm puff after ageing equatcd with five years 25 mm puff after ageing equated with eight years 23 mm puff.
~he thickness of the puff was measured in the . direction normal to the width of the slots in the holders.
.
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.
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.
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Claims (8)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A composition for forming an intumescent material which upon heating decomposes into gas and a solid foam residue, comprising: a water-dispersible melamine formaldehyde resin which when cured is hydrophobic; an inorganic hydrophilic setting agent which hardens in the presence of water thereby to cause the composition to set;
a cross-linking agent for curing the resin, the cross-linking agent being at least one of dicyandiamide and guanidine; an ammonium phosphate; polyvinyl acetate; a solid polyhydroxy compound; and reinforcing fibrous material.
a cross-linking agent for curing the resin, the cross-linking agent being at least one of dicyandiamide and guanidine; an ammonium phosphate; polyvinyl acetate; a solid polyhydroxy compound; and reinforcing fibrous material.
2. A composition according to claim 1, wherein the water-dispersible melamine formaldehyde resin has a solids content of at least 75% by weight.
3. A composition according to claim 1, wherein the ammonium phosphate is monoammonium phosphate.
4. A composition according to claim 1, wherein the setting agent comprises at least one of: calcium sulphate hemi-hydrate, Portland cement and high alumina cement.
5. A composition according to claim 1, in the form of a dry powder.
6. A composition according to claim 1, comprising:
90 to 110 parts by weight of the water-dispersible melamine resin; 90 to 110 parts by weight of the setting agent;
45 to 55 parts by weight of the cross-linking agent; 90 to 110 parts by weight of the ammonium phosphate; 3.6 to 4.4 parts by weight of the polyvinyl acetate; 18 to 22 parts by weight of the solid polyhydroxy compound and 4.5 to 5.5 parts by weight of the reinforcing fibrous material; these parts by weight being based on a total of 250 parts by weight of the melamine resin, the setting agent and the cross-linking agent.
90 to 110 parts by weight of the water-dispersible melamine resin; 90 to 110 parts by weight of the setting agent;
45 to 55 parts by weight of the cross-linking agent; 90 to 110 parts by weight of the ammonium phosphate; 3.6 to 4.4 parts by weight of the polyvinyl acetate; 18 to 22 parts by weight of the solid polyhydroxy compound and 4.5 to 5.5 parts by weight of the reinforcing fibrous material; these parts by weight being based on a total of 250 parts by weight of the melamine resin, the setting agent and the cross-linking agent.
7. An intumescent material which upon heating decomposes into gas and a solid foam residue, comprising: a cured hydro-phobic melamine formaldehyde resin cross-linked by residues of a polyamido compound of at least one of dicyandiamide and guanidine, the resin upon heating decomposing into gas and a solid foam residue, the resin having been water-dispersible prior to curing; a water-hardened setting agent which renders the intumescent material coherent; an ammonium phosphate; polyvinyl acetate; and reinforcing fibrous material.
8. An intumescent material according to claim 7, comprising:
90 to 110 parts by weight of the melamine resin; the resin including cross-linking residues being derived from 45 to 55 parts by weight of the polyamido compound; 90 to 110 parts by weight of the setting agent; 90 to 110 parts by weight of the ammonium phosphate; 3.6 to 4.4 parts by weight of the polyvinyl acetate; 18 to 22 parts by weight of the solid polyhydroxy compound; and 4.5 to 5.5 parts by weight of the reinforcing fibrous material; these parts by weight being based on a total of 250 parts by weight of the melamine resin and the setting agent.
90 to 110 parts by weight of the melamine resin; the resin including cross-linking residues being derived from 45 to 55 parts by weight of the polyamido compound; 90 to 110 parts by weight of the setting agent; 90 to 110 parts by weight of the ammonium phosphate; 3.6 to 4.4 parts by weight of the polyvinyl acetate; 18 to 22 parts by weight of the solid polyhydroxy compound; and 4.5 to 5.5 parts by weight of the reinforcing fibrous material; these parts by weight being based on a total of 250 parts by weight of the melamine resin and the setting agent.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB4653/77A GB1601131A (en) | 1977-02-04 | 1977-02-04 | Composition for forming an intumescent material |
| GB4653/77 | 1977-02-04 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1100250A true CA1100250A (en) | 1981-04-28 |
Family
ID=9781264
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA296,240A Expired CA1100250A (en) | 1977-02-04 | 1978-02-03 | Composition for forming an intumescent material |
Country Status (3)
| Country | Link |
|---|---|
| US (1) | US4210725A (en) |
| CA (1) | CA1100250A (en) |
| GB (1) | GB1601131A (en) |
Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4269944A (en) * | 1978-02-02 | 1981-05-26 | Dixon International Limited | Composition for forming an intumescent material |
| US4645782A (en) * | 1981-02-16 | 1987-02-24 | Dixon International Limited | Putty or mastic |
| US4487862A (en) * | 1982-03-12 | 1984-12-11 | Nissan Motor Company, Limited | Thermosetting resin composition for injection molding and article formed by using the composition |
| CA1227311A (en) * | 1982-10-04 | 1987-09-29 | Tessa Malcolm-Brown | Protection of expanded material and other flammable materials of low compression strength from fire, especially in structural bearings |
| CA1224579A (en) * | 1983-08-23 | 1987-07-21 | Dixon International Limited | Intumescent material |
| GB2147301B (en) * | 1983-10-07 | 1987-05-13 | Dixon International Ltd | Intumescent rubber composition |
| GB8419040D0 (en) * | 1984-07-26 | 1984-08-30 | Dixon International Ltd | Adhesive/cement |
| DE3511864A1 (en) * | 1985-04-01 | 1986-10-09 | Kontron Elektronik | COORDINATE MEASURING DEVICE |
| GB8519654D0 (en) * | 1985-08-05 | 1985-09-11 | Shell Int Research | Insulation material |
| US4774268A (en) * | 1987-01-27 | 1988-09-27 | Dr. Wolman Gmbh | Process for the preparation of flame resistant polyurethane compositions |
| DE19861030A1 (en) * | 1998-11-10 | 2000-05-11 | Permatex Gmbh | Powder composition for the production of aqueous coating compositions |
| US6747074B1 (en) | 1999-03-26 | 2004-06-08 | 3M Innovative Properties Company | Intumescent fire sealing composition |
| US6822033B2 (en) | 2001-11-19 | 2004-11-23 | United States Gypsum Company | Compositions and methods for treating set gypsum |
| US8070895B2 (en) | 2007-02-12 | 2011-12-06 | United States Gypsum Company | Water resistant cementitious article and method for preparing same |
| US8329308B2 (en) | 2009-03-31 | 2012-12-11 | United States Gypsum Company | Cementitious article and method for preparing the same |
| CN103571287A (en) * | 2013-10-25 | 2014-02-12 | 安徽工贸职业技术学院 | Fire-retardant coating |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2566964A (en) * | 1948-04-24 | 1951-09-04 | United States Gypsum Co | Fire-retardant paints |
| US2684953A (en) * | 1952-03-29 | 1954-07-27 | Dow Chemical Co | Intumescent coating composition and an article of manufacture thereof |
| US3037951A (en) * | 1959-07-21 | 1962-06-05 | Moore Benjamin & Co | Intumescing, water resistant fire retardant compositions comprising at least one water-insoluble metal metaphosphate, a polypentaerythritol, and a water insoluble aminoplast resin |
| US4013599A (en) * | 1973-03-28 | 1977-03-22 | Hoechst Aktiengesellschaft | Fire-retardant coating composition comprising etherified and non-etherified amino-formaldehyde resin |
| US4043950A (en) * | 1973-08-27 | 1977-08-23 | Wilmsen Hans | Process for the manufacture of plastic foams and flame-proofing foams characterized by the use of a carrier foam |
-
1977
- 1977-02-04 GB GB4653/77A patent/GB1601131A/en not_active Expired
-
1978
- 1978-02-02 US US05/874,513 patent/US4210725A/en not_active Expired - Lifetime
- 1978-02-03 CA CA296,240A patent/CA1100250A/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| GB1601131A (en) | 1981-10-28 |
| US4210725A (en) | 1980-07-01 |
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