DE1211922B - Aid for filler retention in papermaking - Google Patents

Aid for filler retention in papermaking

Info

Publication number
DE1211922B
DE1211922B DEF34651A DEF0034651A DE1211922B DE 1211922 B DE1211922 B DE 1211922B DE F34651 A DEF34651 A DE F34651A DE F0034651 A DEF0034651 A DE F0034651A DE 1211922 B DE1211922 B DE 1211922B
Authority
DE
Germany
Prior art keywords
papermaking
aid
epichlorohydrin
viscosity
filler retention
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.)
Granted
Application number
DEF34651A
Other languages
German (de)
Other versions
DE1211922C2 (en
Inventor
Dr Wolfgang Lehmann
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Bayer AG
Original Assignee
Bayer AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority to NL281756D priority Critical patent/NL281756A/xx
Priority to BE620936D priority patent/BE620936A/xx
Priority to NL203939D priority patent/NL203939A/xx
Priority to DE1961F0034651 priority patent/DE1211922C2/en
Application filed by Bayer AG filed Critical Bayer AG
Priority to CH834962A priority patent/CH422502A/en
Priority to AT574262A priority patent/AT247706B/en
Priority to FR905992A priority patent/FR1330510A/en
Priority to GB3019362A priority patent/GB964065A/en
Publication of DE1211922B publication Critical patent/DE1211922B/en
Application granted granted Critical
Publication of DE1211922C2 publication Critical patent/DE1211922C2/en
Expired legal-status Critical Current

Links

Classifications

    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03Non-macromolecular organic compounds
    • D21H17/05Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/07Nitrogen-containing compounds
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20Macromolecular organic compounds
    • D21H17/33Synthetic macromolecular compounds
    • D21H17/46Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/54Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen

Description

BUNDESREPUBLIK DEUTSCHLAND Int. CL: D21dFEDERAL REPUBLIC OF GERMANY Int. CL: D21d

D 21h
DEUTSCHES 4fflTW> PATENTAMT
D 21h
GERMAN 4fflTW> PATENT OFFICE

Deutsche Kl.: 55 c-3/10 German class: 55 c -3/10

AUSLEGESCHRIFTEDITORIAL

Aktenzeichen: F 34651VI b/55 c
1211 922 Anmeldetag: 9. August 1961
File number: F 34651VI b / 55 c
1211 922 Filing date: August 9, 1961

Auslegetag: 3. März 1966Opening day: March 3, 1966

Hilfsmittel für die Füllstoffretention bei derAid for filler retention in

Gegenstand der vorliegenden Erfindung ist die PapierherstellungThe present invention relates to papermaking

Verwendung von Produkten, die durch Umsetzung
von 0,8 bis 0,95 Mol Epichlorhydrin bzw. a-Dichlorhydrin mit 1 Mol eines Di- oder Polyamins, dessen Anmelder:
Use of products made by implementation
from 0.8 to 0.95 mol of epichlorohydrin or a-dichlorohydrin with 1 mol of a di- or polyamine, the applicant of which:

Aminogruppen durch mindestens 3 Kohlenstoffatome 5 Farbenfabriken Bayer Aktiengesellschaft,
getrennt sind, in einem Verdünnungsmittel, Vorzugs- Leverkusen
Amino groups with at least 3 carbon atoms 5 Farbenfabriken Bayer Aktiengesellschaft,
are separated, in a diluent, preferred Leverkusen

weise in Wasser, hergestellt sind, als Hilfsmittel fürwise in water, made as an aid for

die Füllstoffretention bei der Papierherstellung. Als Erfinder benannt:filler retention in papermaking. Named as inventor:

Als Di- bzw. Polyamine, die den erfindungsgemäß ^ „, 1f T . T ,As di- or polyamines, which according to the invention ^ ", 1f T. T ,

zu verwendenden Umsetzungsprodukten zugrunde io Dr. Wolfgang Lehmann, Leverkusen
liegen, seien beispielsweise genannt Trimethylen- _
conversion products to be used based on io Dr. Wolfgang Lehmann, Leverkusen
are, for example, trimethylene _

diamin, Tetramethylendiamin, Hexamethylendiamin, *diamine, tetramethylene diamine, hexamethylene diamine, *

1,3-Diaminobutan, 2-Oxy-l,3-diaminopropan, Dipro- die Retentionswirkung sich mit der Steigerung der1,3-diaminobutane, 2-oxy-l, 3-diaminopropane, dipro- the retention effect increases with the increase in

pylentriamin, Dioxydipropylentriamin der Formel Viskosität erhöht und daß zur Erzielung einer gutenpylenetriamine, dioxydipropylenetriamine of the formula increases viscosity and that to achieve good

H N γη rwrnmrH νηγη rwnwru ktw 15 Retentionswirkung die Viskosität einer 15%igen H2N-CH2-CH(OH)CH2NHCh2-CH(OH)CH2NH2. Lösung mindestens 1OcP230, die Viskosität einerHN γη rwrnmrH νηγη rwnwru ktw 15 R etenti onswerkung the viscosity of a 15% H 2 N-CH 2 -CH (OH) CH 2 NHCh 2 -CH (OH) CH 2 NH 2 . Solution at least 1OcP 230 , the viscosity of a

Tetrapropylenpentamin, Ν,Ν'-Diaminopropyl-tetra- 25°/oigen Lösung mindestens 40 cP2So und die Vis-Tetrapropylenpentamine, Ν, Ν'-Diaminopropyl-tetra- 25% solution at least 40 cP 2S o and the Vis-

methylendiamin der Formel kosität einer 35°/oigen Lösung mindestens 160 cP25omethylenediamine of the formula viscosity of a 35% solution at least 160 cP 25 o

H N crw ϊ MHCrw ϊ xrmrw ϊ \rw betragen sollte. Eine ausreichende Lagerstabilität derH N crw ϊ MHCrw ϊ xrmrw ϊ \ rw should be. Sufficient storage stability of the

H2N-(CH2)3NH(CH2)4NH(CH2)3NH2, ao die Umsetzungsprodukte enthaltenden Lösungen,H 2 N- (CH 2 ) 3 NH (CH 2 ) 4 NH (CH 2 ) 3 NH 2 , ao solutions containing the reaction products,

1,6,11-Triamino-n-undecan der Formel d. h. eine Lagerstabilität, die sich bei Raumtempera-1,6,11-triamino-n-undecane of the formula d. H. a storage stability that increases at room temperature

tur au^ min(3estens 1 Jahr erstreckt, ist dann gegeben, wenn das produ]jtj das aus einer probe der wäßrigenextends tur au ^ m i n (3estens 1 year, is then added when the p rodu] tj j the robe of a p of the aqueous

I Lösung bei Zusatz der doppelten Menge an 5O°/oigerI solution with the addition of twice the amount of 50%

2 25 Kalilauge ausgefällt ist, sich in Wasser innerhalb 2 25 potassium hydroxide solution has precipitated out in water within

besonders bewährt haben sich die Umsetzungs- einer Stunde wieder auflöst. Wünscht man die Lagerprodukte, denen γ, /-Diaminopropylalkylamine der Stabilität zu verbessern, so ist die Menge an EpiFormel chlorhydrin bzw. «-Dichlorhydrin innerhalb des an-The implementation times of one hour have proven to be particularly effective. If you want the storage products, which γ, / -Diaminopropylalkylamine to improve the stability, then the amount of EpiFormel chlorohydrin or «-dichlorohydrin is within the other

H xrrR . m rw xr rw πι γη mm gegebenen Bereichs möglichst niedrig zu halten;H xrrR. to keep m rw xr rw πι γη mm given range as low as possible;

- 2 - - : 2 - 2 - 30 wünscht man die Viskosität zu steigern, so ist die- 2 - -: 2 - 2 - 30 if you want to increase the viscosity, it is

Ι,, ι Menge an Epichlorhydrin bzw. «-DichlorhydrinΙ ,, ι amount of epichlorohydrin or «-dichlorohydrin

^ innerhalb des angegebenen Bereichs möglichst hoch^ as high as possible within the specified range

wie z. B. γ,/-Diaminopropyl-methylamin und γ,γ'- zuhalten.such as B. γ, / -diaminopropyl-methylamine and γ, γ'- to keep .

Diaminopropyl-butylamin, zugrunde liegen. Die in dem nachfolgenden Beispiel angegebenenDiaminopropyl-butylamine, are based. The ones given in the example below

Zur Herstellung der erfindungsgemäß zu verwen- 35 Prozentzahlen sind Gewichtsprozente, bezogen aufTo produce the percentages to be used according to the invention, percentages by weight are based on

denden Produkte geht man zweckmäßig so vor, daß die im Papierstoff enthaltene Festsubstanz,It is advisable to proceed in such a way that the solid substance contained in the paper stock,

man die Umsetzung der Reaktionskomponenten in _ .the implementation of the reaction components in _.

dem Verdünnungsmittel bei Temperaturen zwischen Beispielthe diluent at temperatures between example

20 und 70° C vornimmt. Die Konzentration der Re- Einem in üblicher Weise bereiteten Papierbrei20 and 70 ° C. The concentration of the paper pulp prepared in the usual way

aktionspartner liegt zweckmäßig zwischen 20 und 40 vom Mahlgrad 23° Schopper-Riegler setzt manAction partner is expediently between 20 and 40 of the grinding degree 23 ° Schopper-Riegler one sets

60 Gewichtsprozent. Es empfiehlt sich, die Umsetzung 0,25 % eines der in der nachfolgenden Tabelle unter60 percent by weight. It is recommended that the implementation 0.25% of one of the in the table below

bei einer Konzentration von etwa 40% zu beginnen Ibis 7 angeführten Umsetzungsprodukte, 20% Titan-to begin at a concentration of about 40% Ibis 7 listed reaction products, 20% titanium

und sie nach Erreichen einer Viskosität von etwa 50 dioxyd und 5% eines handelsüblichen rosarotenand after reaching a viscosity of about 50 dioxide and 5% of a commercially available pink-red

bis 100 cP durch Verdünnen mit dem benutzten organischen Pigments zu. Man erhält dann eine her-up to 100 cP by diluting with the organic pigment used. You then get a her-

Lösungsmittel bei einer Konzentration von 15 bis 45 vorragende Füllstoffretention.Solvent at a concentration of 15 to 45 excellent filler retention.

30 % zu Ende zu führen. Die hervorragende Wirkung der unter 1 bis 7 an-30% to complete. The excellent effect of the items 1 to 7

Wie groß der Unterschuß an Epichlorhydrin bzw. geführten erfindungsgemäßen UmsetzungsprodukteHow large the deficit of epichlorohydrin or led reaction products according to the invention

a-Dichlorhydrin zu wählen ist, hängt ab von der Art gegenüber der Wirkung der Umsetzungsprodukte,a-dichlorohydrin is to be chosen, depends on the type against the effect of the reaction products,

des in Betracht gezogenen Amins, von der ge- für deren Herstellung auf 1 Mol Di- oder Polyaminof the amine under consideration, of the amount used for their preparation to 1 mole of di- or polyamine

wünschten Lagerstabilität und Viskosität der zu ver- 50 mehr als 1 Mol Epichlorhydrin bzw. a-DichlorhydrinDesired storage stability and viscosity of the 50 more than 1 mol epichlorohydrin or α-dichlorohydrin

wendenden Lösung sowie von der gewünschten Höhe eingesetzt war, ist aus der nachfolgenden Tabelleturning solution as well as of the desired height was used, is from the table below

der Retentionswirkung. Hierzu ist zu bemerken, daß ersichtlich:the retention effect. It should be noted that:

Mol Epichlorhydrin
auf 1 Mol
Amin
Moles of epichlorohydrin
to 1 mole
Amine

°/o Titandioxyd im
Papier
° / o titanium dioxide im
paper

Farbe des PapiersColor of the paper

;■, y'-Diaminopropylmethylamin ; ■, y'-diaminopropylmethylamine

;>, /-Diaminopropylbutylamin ;>, / -Diaminopropylbutylamine

Dipropylentriamin Dipropylenetriamine

Dioxydipropylentriamin Dioxydipropylenetriamine

Ν,Ν'-Diaminopropyl-tetramethylendiaminΝ, Ν'-diaminopropyl-tetramethylenediamine

Tetrapropylenpentamin ' Tetrapropylene pentamine '

1,6,11-Triamino-n-undecan 1,6,11-triamino-n-undecane

7, y'-Diaminopropylmethylamin 7, γ'-diaminopropylmethylamine

Tetraäthylenpentamin Tetraethylene pentamine

0,87
0,94
0,88
0,93
0,85
0,82
0,83
3,00
1,60
0.87
0.94
0.88
0.93
0.85
0.82
0.83
3.00
1.60

14,2
14,0
13,6
13,8
13,5
12,5
12,4
8,0
11,0
14.2
14.0
13.6
13.8
13.5
12.5
12.4
8.0
11.0

tiefrosarotdeep pink

tiefrosarotdeep pink

tiefrosarotdeep pink

tiefrosarotdeep pink

tiefrosarotdeep pink

tiefrosarotdeep pink

tiefrosarotdeep pink

schwachrosarotpale pink

schwachrosarotpale pink

Die Herstellung der erfindungsgemäß zu verwendenden Umsetzungsprodukte sei nachstehend an Hand der Herstellung eines Umsetzungsproduktes aus Epichlorhydrin und y, /-Diaminopropyl-methylamin näher erläutert:The preparation of the reaction products to be used according to the invention will be explained in more detail below with reference to the preparation of a reaction product from epichlorohydrin and γ, / -diaminopropyl-methylamine:

Eine Lösung von 145 g γ, y'-Diaminopropylmethylamin (1 Mol) in 362 ml Wasser wird innerhalb 1 Stunde bei 30° C unter Rühren und unter Kühlen mit 80,5 g Epichlorhydrin (0,87 Mol) versetzt. Dann erhöht man die Temperatur des Reaktionsgemisches innerhalb 1Zs Stunde auf 40° C und rührt die Mischung bei dieser Temperatur noch so lange, bis die Viskosität auf etwa 7OcP angestiegen ist; dies ist nach etwa 80 Minuten der Fall. Hierauf setzt man dem Reaktionsgemisch 145 ml Wasser zu; dadurch sinkt die Viskosität auf ungefähr 40 cP. Nunmehr erwärmt man die Mischung bei 40° C so lange, bis die Viskosität der Lösung auf etwa 120 cP angestiegen ist. Diese Viskosität ist erreicht nach etwa 2V2 Stunden, gerechnet von der Zugabe der 145 ml Wasser, bzw. nach 4 Stunden, gerechnet von dem Ende der Zugabe des Epichlorhydrins. Abschließend fügt man zu der Lösung noch 171 ml Wasser hinzu. Die so bereitete Lösung enthält 25°/o des Umsetzungsproduktes aus Epichlorhydrin und 3>,/-Diaminopropylmethylamin und besitzt eine Viskosität von 145 cP bei 25° C.80.5 g of epichlorohydrin (0.87 mol) are added to a solution of 145 g of γ, γ'-diaminopropylmethylamine (1 mol) in 362 ml of water at 30 ° C., while stirring and with cooling, over the course of 1 hour. The temperature of the reaction mixture is then increased to 40 ° C. in the course of 1 hour and the mixture is stirred at this temperature until the viscosity has risen to about 70 cP; this is the case after about 80 minutes. Then 145 ml of water are added to the reaction mixture; this reduces the viscosity to around 40 cP. The mixture is now heated at 40 ° C. until the viscosity of the solution has risen to about 120 cP. This viscosity is reached after about 2/2 hours, calculated from the addition of the 145 ml of water, or after 4 hours, calculated from the end of the addition of the epichlorohydrin. Finally, 171 ml of water are added to the solution. The solution prepared in this way contains 25% of the reaction product of epichlorohydrin and 3>, / - diaminopropylmethylamine and has a viscosity of 145 cP at 25 ° C.

Ein Produkt mit praktisch gleichen Eigenschaften erhält man, wenn man an Stelle von 0,87 Mol Epichlorhydrin 0,9 Mol a-Dichlorhydrin zum Einsatz bringt. Die Bildung des Umsetzungsproduktes erfolgt in diesem Fall langsamer, kann jedoch gewünschtenfalls durch Zusatz von Kaliumhydroxyd oder Natriumhydroxyd in Mengen bis zu 0,9 Mol wesentlich beschleunigt werden.A product with practically the same properties is obtained if instead of 0.87 mol of epichlorohydrin 0.9 mol of a-dichlorohydrin is used. The conversion product is formed in this case more slowly, but can if desired by adding potassium hydroxide or sodium hydroxide can be significantly accelerated in amounts up to 0.9 mol.

Claims (1)

Patentanspruch:Claim: Verwendung von Produkten, die durch Umsetzung von 0,8 bis 0,95 Mol Epichlorhydrin bzw. a-Dichlorhydrin mit lMol eines Di- oder Polyamine, dessen Aminogruppen durch mindestens 3 Kohlenstoffatome getrennt sind, in einem Verdünnungsmittel, vorzugsweise in Wasser, hergestellt worden sind, als Hilfsmittel für die Füllstoffretention bei der Papierherstellung.Use of products made by reacting 0.8 to 0.95 moles of epichlorohydrin or a-dichlorohydrin with 1 mol of a di- or Polyamines, the amino groups of which are separated by at least 3 carbon atoms, in one Diluents, preferably in water, have been prepared as an aid to filler retention in papermaking. In Betracht gezogene Druckschriften: Deutsche Patentschrift Nr. 731030.Documents considered: German Patent No. 731030. 609 510/233 2.66 © Bundesdruckerei Berlin609 510/233 2.66 © Bundesdruckerei Berlin
DE1961F0034651 1961-08-09 1961-08-09 Aid for filler retention in papermaking Expired DE1211922C2 (en)

Priority Applications (8)

Application Number Priority Date Filing Date Title
NL281756D NL281756A (en) 1961-08-09
BE620936D BE620936A (en) 1961-08-09
NL203939D NL203939A (en) 1961-08-09
DE1961F0034651 DE1211922C2 (en) 1961-08-09 1961-08-09 Aid for filler retention in papermaking
CH834962A CH422502A (en) 1961-08-09 1962-07-11 Process for increasing filler retention in paper stock
AT574262A AT247706B (en) 1961-08-09 1962-07-16 Process for increasing filler retention in paper stock
FR905992A FR1330510A (en) 1961-08-09 1962-08-03 Process for increasing the retention of fillers in pulp
GB3019362A GB964065A (en) 1961-08-09 1962-08-07 Process for increasing the filler-retention of paper

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE1961F0034651 DE1211922C2 (en) 1961-08-09 1961-08-09 Aid for filler retention in papermaking

Publications (2)

Publication Number Publication Date
DE1211922B true DE1211922B (en) 1966-03-03
DE1211922C2 DE1211922C2 (en) 1973-05-10

Family

ID=7095651

Family Applications (1)

Application Number Title Priority Date Filing Date
DE1961F0034651 Expired DE1211922C2 (en) 1961-08-09 1961-08-09 Aid for filler retention in papermaking

Country Status (6)

Country Link
AT (1) AT247706B (en)
BE (1) BE620936A (en)
CH (1) CH422502A (en)
DE (1) DE1211922C2 (en)
GB (1) GB964065A (en)
NL (2) NL203939A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1771814B1 (en) * 1968-07-16 1972-08-31 Bayer Ag Use of aids for paper production
DE3446282A1 (en) * 1984-01-03 1985-07-11 Sandoz-Patent-GmbH, 7850 Lörrach Dyeing process
US4718918A (en) * 1984-01-03 1988-01-12 Sandoz Ltd. Treatment of textile materials to improve the fastness of dyeings made thereon and polymers useful therefor

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1264943B (en) * 1964-01-18 1968-03-28 Bayer Ag Paper auxiliaries

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE731030C (en) * 1939-02-02 1943-02-02 Ig Farbenindustrie Ag Process for the production of soluble nitrogen-containing condensation products that can be converted into insoluble, hard products by self-condensation

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE731030C (en) * 1939-02-02 1943-02-02 Ig Farbenindustrie Ag Process for the production of soluble nitrogen-containing condensation products that can be converted into insoluble, hard products by self-condensation

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1771814B1 (en) * 1968-07-16 1972-08-31 Bayer Ag Use of aids for paper production
DE3446282A1 (en) * 1984-01-03 1985-07-11 Sandoz-Patent-GmbH, 7850 Lörrach Dyeing process
US4718918A (en) * 1984-01-03 1988-01-12 Sandoz Ltd. Treatment of textile materials to improve the fastness of dyeings made thereon and polymers useful therefor

Also Published As

Publication number Publication date
CH422502A (en) 1966-10-15
BE620936A (en)
NL203939A (en)
NL281756A (en)
GB964065A (en) 1964-07-15
DE1211922C2 (en) 1973-05-10
AT247706B (en) 1966-06-27

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