US3473948A - Method of improving resin finished textiles - Google Patents

Method of improving resin finished textiles Download PDF

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US3473948A
US3473948A US583062A US3473948DA US3473948A US 3473948 A US3473948 A US 3473948A US 583062 A US583062 A US 583062A US 3473948D A US3473948D A US 3473948DA US 3473948 A US3473948 A US 3473948A
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resin
acid
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fabric
textile
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John Dean Turner
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Burlington Industries Inc
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/39Aldehyde resins; Ketone resins; Polyacetals
    • D06M15/423Amino-aldehyde resins
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/20Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
    • Y10T442/273Coating or impregnation provides wear or abrasion resistance

Definitions

  • Improved resin-finished cellulosic textiles with increased abrasion resistance are produced by (a) subjecting resin-treated textiles, which have been treated with a cross-linking agent and at least partially cured, to a hydrolyzing step in an aqueous bath with a strong organic or mineral acid in the presence of an alkali metal, alkaline earth metal, or ammonium salt electrolyte and (b) immediately thereafter neutralizing the fabric.
  • the present invention resides in the process of subjecting a resin-treated textile, which is at least partially cured, to a hydrolyzing step by immersing the textile in an aqueous bath containing a strong organic or mineral acid and also containing an alkali metal salt electrolyte, an alkaline earth metal salt electrolyte, or an ammonium salt electrolyte, and thereafter neutralizing and washing the textile.
  • Suitable cellulosic or cellulose-containing textiles were described above and include, but are not to be limited to, cotton, rayon, linen and blends of these fibers with other natural and synthetic fibers.
  • the present invention contemplates a fabric containing at least 20 percent of cellulosic fibers.
  • Suitable resins for cross-linking agents were described above. Any of the conventional curing resins or reactants which are used for the treatment of cellulosic textiles to give durable surface effects, e.g., permanent press, washwear or the like, may be used herein. This includes, for example, the methylolated derivatives of various nitrogencontaining compounds such as urea, N,N-'ethylene urea, propylene urea, aminotriazines such as melamines and substituted melamines, triazones and urons. Combinations of these materials, for example, a mixture of polymethylolated triazine and polymethylolated ethylene urea, may also be employed.
  • the amount of reactant or resin which is applied to the fabric according to the invention may be widely varied and will depend on other operating factors, e.g., the fabric construction, reactant employed and the properties described in the ultimate product. However, the amount will generally be in the range of about 220% solids add-on based on the weight of the fabric although amounts outside this range may also be employed.
  • the resin and the cross-linking agent are applied in the usual manner and at least partially cured prior to the hydrolyzing step.
  • the hydrolysis may be conducted as either a continuous process or a batch process with the fabric in open width or in rope form.
  • the hydrolyzing bath may contain 0.01 to 15% w./v. of the acid, and preferably 2 to 5% w./v. of the acid; and from 5% w./v. up to the saturation point of the electrolyte salt, and preferably 15 to 25% w./v. of the electrolyte salt.
  • the hydrolyzing acid is a strong organic or mineral acid.
  • Typical examples, which should not be construed to limit the invention thereto, of such an acid are hydrochloric acid, nitric acid, chloric acid, hydrobromic acid, hydroiodic acid, perchloric acid, sulfuric acid, trichloroacetic acid, dichloroacetic acid, monobromoacetic acid, alpha-chloropropionic acid, malonic acid, formic acid, oxalic acid, thiocyanoacetic acid, lactic acid and cyanoacetic acid.
  • electrolyte is defined by the Condensed Chemical Dictionary, 6th edition, as a substance which disassociates into ions when in a solution or a fused state and it will then conduct an electric current.
  • electrolytes which are salts of alkali metals, alkaline earth metals, or ammonium salts.
  • Suitable salts for the present invention include sodium chloride, sodium hydrogen phosphates, sodium nitrate, potassium chloride, sodium sulphate, calcium chloride, magnesium chloride, ammonium chloride, potassium nitrate, potassium ferricyanide, potassium bromide, etc.
  • the above listing is by way of exemplification only and is not to be construed to limit the present invention in any way.
  • the preferred neutralizing agent is a weak alkaline compound, for example, ammonia, sodium carbonate or sodium bicarbonate.
  • the neutralization may be accomplished by a variety of ways, such as immersing the fabric in a neutralizing bath, spraying the fabric with a solution of the neutralizing compound, subjecting the fabric to the action of vapors of the neutralizing agent, etc.
  • the preferred method of neutralization is by immersing the fabric in a bath containing the neutralizing agent.
  • the bath temperature may vary over a wide temperature range, i.e. 40 F.180 F., but preferably is approximately room temperature.
  • the bath concentration and temperature and the duration of the treatment determine the degree of acid neutralization.
  • the duration of the treatment will be of /2 to 2 minutes although the treatment time may vary from A to 30 minutes in length. Generally, treatment times of over 5 minutes may be used but are not practical from an economic standpoint.
  • the bath concentration may vary from quite weak, e.g., w./v., up to quite concentrated solutions, e.g., 15% w./v.
  • the neutralization bath preferably contains about 5 to w./v. of the neutralizing agent.
  • the fabric is preferably washed with water to remove any residual traces of neutralizing agent or neutralizing acid.
  • Any of the conventional washing operations commonly used in the textile art may be utilized, e.g., immersion or spraying.
  • a film-forming additive and/ or lubricating agent to the textile.
  • Such materials may be added before and/or after the hydrolyzing step of the present invention, and the resulting resin-finished cellulose textile generally has abrasion resistance exceeding that produced by either step alone.
  • Acrylic resins have been commonly used as such film-forming additives and lanolinbased lubricating agents, such as Bi-Chem Softener LLS,
  • the lubricating agent which is a mixture of lanolin and polyethylene emulsions, may be used as the lubricating agent.
  • the acrylic resin is used before and after the acid hydrolysis step.
  • the temperature and the time of the hydrolysis will depend upon the particular fabric involved and the results desired. Generally, temperatures in the order of to 210 F. may be used and more preferably temperatures of to 200 F. may be used. Generally, times in excess of five minutes are uneconomical and times less than one-fourth of a minute do not allow suflicient hydrolization to occur. Therefore, the time of the hydrolyzing step will generally be from one-fourth to five minutes, and most preferably from one-half to three minutes.
  • the hydrolyzing step process of the present invention readily lends itself to the production of fibers which may be permanently pleated or shaped.
  • the cellulose textile may be treated with the resin and the cross-linking agent. and partially cured.
  • the partially cured fabric is then hydrolyzed to produce a resin-finished cellulose textile with improved abrasion resistance which may be subsequently permanently pleated or shaped.
  • any alkali metal salt, alkaline earth metal salt, or ammonium salt electrolyte may be used according to the present invention
  • preferred salts are those of the hydrolyzing acid utilized.
  • the hydrolyzing acid is hydrochloric acid and the electrolyte salt is sodium chloride. It is necessary that the electrolyte salts be neutral or slightly acid. Buffering compounds, such as sodium carbonate, should be avoided.
  • the electrolyte salt cation will be an alkali metal cation, an alkaline earth metal cation, or an ammonium cation, while the electrolyte salt anion will be a strong organic acid or mineral acid anion, and preferably is the anion corresponding to the anion of the hydrolyzing acid.
  • the resin-treated cellulose fabric may optionally be pre-wetted before the hydrolyzing step.
  • the pre-wetting may, for example, be effected by passing the fabric through an aqueous bath which may optionally contain minor amounts of a conventional wetting agent.
  • w./v. means weight percent by volume, that is, weight percent based on the total volume of solution, and W and F represent warp and fill, respectively.
  • the resin-treated fabric was passed through a first aqueous bath containing the hydrochloric acid and the sodium chloride, then through a neutralizing aqueous bath containing 2% w./v. of sodium carbonate, and thereafter through an aqueous washing bath, and dried at F.
  • Concentrations are defined as grams per liter, e.g., 30% means 300 grams of reagent per r. 4 Concentrated hydrochloric acid, approximately 37%.
  • Example 10 11 12 13 14 NaCl 15 15 20 HCl 0.5 0.5 0.5 0 5 0 5 Temp., F 140 140 140 140 140 140 140 Time (rnin.)-.- 3 Tear Strength (W/F) 1. 8/1. 4 2 6/2 4 1. 6/1. 3 1 8/1 5 1 8/1 6 Crease Resistance (W +F), Dry 248 290 252 2 Crease Resistance (W+F), Wet 267 285 273 258 264 Stoll-Flex Abrasion, Warp 118 376 91 132 155 Stoll-Flex Abrasion, F111. 419 545 333 629 360 Weight (ozJsq. yd.) 8. 8. 53 8. 37 8. 31 8. 33
  • Example X 20 20 25 25 x 0.5 0. 5 0. 5 0.5 X 200 200 200 200 X 1 /2 1 TABLE 8 Fabric: 100% Cotton, Army Twill; Pretreatment: 25% Resin 183, 4.5% Catalyst 43, 4% Rhoplex K-3, Dry at 200 F. for 3 minutes; Cure at 320 F. for 10 minutes.
  • Example 15 15 20 20 20 20 20 20 X X 5 0 0. 5 0. 5 0. 5 X X 140 140 170 170 170 X X 3 1 1 2 2 X X Aftertreatment:
  • Rhoplex K3 4 X 4 X 4 X X 4 Bi-Chem Softener LLS 2 X 2 X 2 X X 2 Catalyst 43 X X X X Tear Strength:
  • Warp 1 261 281 202 145 277 189 80 82 Fill 1, 870 966 696 359 962 416 491 384 Weight (oz./sq. yd.) 8. 46 8. 33 8. 43 8.36 8. 48 8. 46 8. 43 8. 41
  • Example TABLE 10 Fabric 100% Cotton Broadcloth; Pretreatment: 25% Resin HK, 4.5% Catalyst 43, Dry at 200 F. for 3 minutes; Cure at 320 F. for 10 minutes.
  • Warp 1. O 0.9 0.9 0. 9 0. 9 1. 0. 9 0. 9 0. 6 Fill 1.0 1.0 0.9 0.9 0.8 1.0 0.9 0.9 0.6 Crease Resistance:
  • Rhoplex K-3 1 1 1 1 1 1 1 1 1 1 1 1 1 X Bi-Chem Softener PE 00110. 2 2 2 2 2 2 2 2 2 X Catalyst 43 K; V; ya V2 56 X Tear Strength:
  • Rhoplex K-3 2 2 2 2 2 X 2 Bi-Chem Softener PE Gone. 2 2 2 2 X 2 Crystal 43 V X V Tear Strength:
  • Rhoplex K-3 Dry 200 F. for 3 minutes; Cure 320 F. for minutes
  • Warp 257 248 277 532 296 351 454 343 537 370 Fill 1, 118 738 763 1, 500+ 1, 500+ 631 1,056 815 1, 034 1, 315
  • Example Sodium Nitrate l Dried 3 minutes at 200 F. and cured 3 minutes at 325 F.
  • EXAMPLE 102 This example relates to an illustration of the improved moisture regain obtained by the present invention.
  • the textile product of Example 53 was tested for moisture regain, according to ASTM Test D629-59A, and compared with the resinated control textile of Example 69.
  • the test results were as follows:
  • a process of producing resin-treated cellulosic textiles comprising applying a resin to a cellulosic textile, and at least partially curing the resin on the textile 'by means of a cross-linking agent, the improvement comprising (a) hydrolyzing the partially cured resintreated textile in an aqueous bath containing a strong acid and a neutral or only slightly acid electrolyte salt selected from the group consisting of alkali metal, alkaline earth metal and ammonium salt electrolytes, the concentration of the electrolyte salt being at least 5% w./v. and the concentration of the acid being 0.01 to 15% w./v., and (b) thereafter neutralizing and washing the hydrolyzed resin-treated textile, whereby the textile has increased abrasion resistance and other improved textile properties.

Description

3,473,948 METHOD OF IMPROVEWG RESIN FINISHED TEXTILES .Iohn Dean Turner, Greensboro, N.C., assignor to Burlington Industries, Inc., Greensboro, N.C., a corporation of Delaware No Drawing. Filed Sept. 29, 1966, Ser. No. 583,062 Int. Cl. B4411 1/20, l/44 US. Cl. 117-621 8 Claims ABSTRACT OF THE DISCLOSURE This invention relates to improved resin-finished textiles and the method of making the same. More specifically it relates to resin-finished textile materials with improved abrasion resistance and the method of making the same.
BACKGROUND OF THE INVENTION Cellulose fiber-containing textiles such as cotton, rayon, linen and blends of these fibers have long been used in making garments. In recent years a number of various methods have been developed for treating such textile fabrics to impart desirable crease resistance, and also to impart permanent press characteristics to the textile fabrics. The majority of these methods involve the use of thermosetting resins. The use of thermosetting resinfinished textiles containing cellulosic fibers, such as cotton, regenerated cellulose (rayon) and blends thereof with other natural and/or synthetic fibers, has become much more widespread.
Typical patents relating to resin-finished cellulosic textiles are Hurwitz, US. Patent 2,950,553; Warnock et al., US. Patent 2,974,432 and Getchell, US. Patent 3,166,- 765, the disclosures of which are hereby incorporated by reference.
The copending application of Tomasino and Smith, application No. 521,443, filed Jan. 18, 1966 and assigned to the assignee of the present invention, is likewise directed to a process for resin-finishing cellulosic textile with curable resins or reactants for the purpose of obtaining durable finish or surface effects. The disclosure of this application is also incorporated herein by reference.
OBJECT S OF THE INVENTION It is an object of this invention to provide novel, improved resin-finished cellulosic textiles. It is a further object of the invention to provide resin-finished cellulosic textiles with improved abrasion resistance. It is another object of this invention to provide resin-finished cellulosic textiles with approved abrasion resistance, tear strength, handle, moisture regain and soil resistance. Yet another object of this invention is to provide a process for the production of resin-finished cellulosic textiles with improved abrasion resistance. A further object of this invention is to provide a process for the production of resin-finished cellulosic textiles With improved abrasion resistance, tear strength, handle, moisture regain and soil resistance.
Still further objects and the entire scope of applicability of the present invention will become apparent from the detailed description given hereinafter; it should be understood, however, that the detailed description and specific examples, while indicating preferred embodiments of the invention, are given by way of illustration only, since various changes or modifications within the scope of the te States Patent 3,473,948 Patented Oct. 21, 1969 invention will become apparent to those skilled in the art from this detailed description.
SUMMARY OF THE INVENTION Improved resin-finished cellulosic textiles with increased abrasion resistance are produced by (a) subjecting resin-treated textiles, which have been treated with a cross-linking agent and at least partially cured, to a hydrolyzing step in an aqueous bath with a strong organic or mineral acid in the presence of an alkali metal, alkaline earth metal, or ammonium salt electrolyte and (b) immediately thereafter neutralizing the fabric.
DESCRIPTION OF THE INVENTION The present invention resides in the process of subjecting a resin-treated textile, which is at least partially cured, to a hydrolyzing step by immersing the textile in an aqueous bath containing a strong organic or mineral acid and also containing an alkali metal salt electrolyte, an alkaline earth metal salt electrolyte, or an ammonium salt electrolyte, and thereafter neutralizing and washing the textile.
Suitable cellulosic or cellulose-containing textiles were described above and include, but are not to be limited to, cotton, rayon, linen and blends of these fibers with other natural and synthetic fibers. The present invention contemplates a fabric containing at least 20 percent of cellulosic fibers.
Suitable resins for cross-linking agents were described above. Any of the conventional curing resins or reactants which are used for the treatment of cellulosic textiles to give durable surface effects, e.g., permanent press, washwear or the like, may be used herein. This includes, for example, the methylolated derivatives of various nitrogencontaining compounds such as urea, N,N-'ethylene urea, propylene urea, aminotriazines such as melamines and substituted melamines, triazones and urons. Combinations of these materials, for example, a mixture of polymethylolated triazine and polymethylolated ethylene urea, may also be employed.
The amount of reactant or resin which is applied to the fabric according to the invention may be widely varied and will depend on other operating factors, e.g., the fabric construction, reactant employed and the properties described in the ultimate product. However, the amount will generally be in the range of about 220% solids add-on based on the weight of the fabric although amounts outside this range may also be employed.
The resin and the cross-linking agent are applied in the usual manner and at least partially cured prior to the hydrolyzing step.
The hydrolysis may be conducted as either a continuous process or a batch process with the fabric in open width or in rope form. The hydrolyzing bath may contain 0.01 to 15% w./v. of the acid, and preferably 2 to 5% w./v. of the acid; and from 5% w./v. up to the saturation point of the electrolyte salt, and preferably 15 to 25% w./v. of the electrolyte salt.
The hydrolyzing acid is a strong organic or mineral acid. Typical examples, which should not be construed to limit the invention thereto, of such an acid are hydrochloric acid, nitric acid, chloric acid, hydrobromic acid, hydroiodic acid, perchloric acid, sulfuric acid, trichloroacetic acid, dichloroacetic acid, monobromoacetic acid, alpha-chloropropionic acid, malonic acid, formic acid, oxalic acid, thiocyanoacetic acid, lactic acid and cyanoacetic acid.
The term electrolyte is defined by the Condensed Chemical Dictionary, 6th edition, as a substance which disassociates into ions when in a solution or a fused state and it will then conduct an electric current. This invention contemplates the use of electrolytes which are salts of alkali metals, alkaline earth metals, or ammonium salts. Suitable salts for the present invention, for example, include sodium chloride, sodium hydrogen phosphates, sodium nitrate, potassium chloride, sodium sulphate, calcium chloride, magnesium chloride, ammonium chloride, potassium nitrate, potassium ferricyanide, potassium bromide, etc. The above listing is by way of exemplification only and is not to be construed to limit the present invention in any way.
After the hydrolysis step, the textile fabric is immediately neutralized and washed. The preferred neutralizing agent is a weak alkaline compound, for example, ammonia, sodium carbonate or sodium bicarbonate. The neutralization may be accomplished by a variety of ways, such as immersing the fabric in a neutralizing bath, spraying the fabric with a solution of the neutralizing compound, subjecting the fabric to the action of vapors of the neutralizing agent, etc. The preferred method of neutralization is by immersing the fabric in a bath containing the neutralizing agent. The bath temperature may vary over a wide temperature range, i.e. 40 F.180 F., but preferably is approximately room temperature. The bath concentration and temperature and the duration of the treatment determine the degree of acid neutralization. Preferably, the duration of the treatment will be of /2 to 2 minutes although the treatment time may vary from A to 30 minutes in length. Generally, treatment times of over 5 minutes may be used but are not practical from an economic standpoint. The bath concentration may vary from quite weak, e.g., w./v., up to quite concentrated solutions, e.g., 15% w./v. The neutralization bath preferably contains about 5 to w./v. of the neutralizing agent.
After the neutralization, the fabric is preferably washed with water to remove any residual traces of neutralizing agent or neutralizing acid. Any of the conventional washing operations commonly used in the textile art may be utilized, e.g., immersion or spraying.
In the production of certain resin-finished cellulose textiles, depending upon the particular resin, cross-linking agents, and cellulosic textile involved, it may be advantageous to incorporate minor amountse.g., 0.001 to 3% w./v.of a wetting agent. Almost any conventional wetting agent commonly used in the textile art may be utilized, for example, adducts of sorbitol and propylene oxide or ethylene oxide.
One of the common techniques known to the art for improving the abrasion resistance of cellulose textiles has been the application of a film-forming additive and/ or lubricating agent to the textile. Such materials may be added before and/or after the hydrolyzing step of the present invention, and the resulting resin-finished cellulose textile generally has abrasion resistance exceeding that produced by either step alone. Acrylic resins have been commonly used as such film-forming additives and lanolinbased lubricating agents, such as Bi-Chem Softener LLS,
which is a mixture of lanolin and polyethylene emulsions, may be used as the lubricating agent. Preferably the acrylic resin is used before and after the acid hydrolysis step.
The temperature and the time of the hydrolysis will depend upon the particular fabric involved and the results desired. Generally, temperatures in the order of to 210 F. may be used and more preferably temperatures of to 200 F. may be used. Generally, times in excess of five minutes are uneconomical and times less than one-fourth of a minute do not allow suflicient hydrolization to occur. Therefore, the time of the hydrolyzing step will generally be from one-fourth to five minutes, and most preferably from one-half to three minutes.
The hydrolyzing step process of the present invention readily lends itself to the production of fibers which may be permanently pleated or shaped. The cellulose textile may be treated with the resin and the cross-linking agent. and partially cured. The partially cured fabric is then hydrolyzed to produce a resin-finished cellulose textile with improved abrasion resistance which may be subsequently permanently pleated or shaped.
Other properties of the resin-treated cellulose textiles of this invention are improved in addition to the abrasion resistance. For example, tear strength, handle, moisture regain and soil resistance generally show a marked improvement as compared to ordinarily treated cellulose textiles.
Although any alkali metal salt, alkaline earth metal salt, or ammonium salt electrolyte may be used according to the present invention, preferred salts are those of the hydrolyzing acid utilized. Most preferably, the hydrolyzing acid is hydrochloric acid and the electrolyte salt is sodium chloride. It is necessary that the electrolyte salts be neutral or slightly acid. Buffering compounds, such as sodium carbonate, should be avoided. The electrolyte salt cation will be an alkali metal cation, an alkaline earth metal cation, or an ammonium cation, while the electrolyte salt anion will be a strong organic acid or mineral acid anion, and preferably is the anion corresponding to the anion of the hydrolyzing acid.
The resin-treated cellulose fabric may optionally be pre-wetted before the hydrolyzing step. The pre-wetting may, for example, be effected by passing the fabric through an aqueous bath which may optionally contain minor amounts of a conventional wetting agent.
When used in this specification, the expression w./v. means weight percent by volume, that is, weight percent based on the total volume of solution, and W and F represent warp and fill, respectively.
In the following examples, the resin-treated fabric was passed through a first aqueous bath containing the hydrochloric acid and the sodium chloride, then through a neutralizing aqueous bath containing 2% w./v. of sodium carbonate, and thereafter through an aqueous washing bath, and dried at F.
TABLE 1 Fabric: 100% Cotton, Army Twill; Treatment: 30% Resin 183, 6% Catalyst 43, Dry at 200 F. for 3 minutes; Cure at 340 F. for 6 minutes.
Example Temp, F 140 140 140 l Time (min.) 2 5 2 5 l Tear Strength (W/F) 1. 5/0. 9 1. 5/1. 1 1. 8/1. 5 1. 8/1. 4 1. 4/0. 9
Crease Resistance (W-l-F), Dry 256 254 248 244 261 Crease Resistance (W+F), Wet 283 277 274 275 277 Stoll Flex Abrasion, Warp 41 67 144 120 to Stoll Flex Abl'aSlOIl, Fill 269 300 504 490 235 Weight (ozJsq. yd.) 8.28 8. 28 8.38 8. 20 8. 33 Edge Abrasion:
5 min 4 4 5 5 7 min 3 3 4 4 i 9 min 2 1 3 4 l 1 Dihydroxydimethylol ethylene urea, by Sun Chemical Company. 2 Zinc nitrate solution, by Bi-C hem, Burlington Industries, Inc.
lite
Concentrations are defined as grams per liter, e.g., 30% means 300 grams of reagent per r. 4 Concentrated hydrochloric acid, approximately 37%.
y; lb. head load, 2 lbs. tension.
TABLE 2 Fabric: 75% Cotton/25% Polyester Twill; Pretreatment: 30% Resin 183, 6% Catalyst, Dry 3 minutes at 200 F.; Cure 6 minutes at 340 F.
Example 6 7 8 9 25 25 0. 5 140 140 Time (min.) 5 15 Tear Strength (W/F) 1. 9/2. 2 1. 6/1. 6 1. 9/1. 9 3. 4/4. 5 Crease Resistance (W-i-F), Dry-.. 263 270 277 179 Crease Resistance (W-i-F), Wet. 272 281 283 198 Stoll-Flex Abrasion, Warp. 1, 500 518 451 1, 246
Stoll-Flex Abrasion, Fill Weight (oz/sq. yd.)
Resin treated, but no hydrolysis. 2 Control, no resin no hydrolysis.
TABLE 3 Fabric: 100% Cotton, Army Twill; Pretreatment: 25% Bi-Chem BE, 1 Dry 3 minutes at 200 F.; 5% Catalyst 43, Cure 6 minutes at 340 F.
Example 10 11 12 13 14 NaCl 15 15 20 HCl 0.5 0.5 0.5 0 5 0 5 Temp., F 140 140 140 140 140 Time (rnin.)-.- 3 Tear Strength (W/F) 1. 8/1. 4 2 6/2 4 1. 6/1. 3 1 8/1 5 1 8/1 6 Crease Resistance (W +F), Dry 248 290 252 2 Crease Resistance (W+F), Wet 267 285 273 258 264 Stoll-Flex Abrasion, Warp 118 376 91 132 155 Stoll-Flex Abrasion, F111. 419 545 333 629 360 Weight (ozJsq. yd.) 8. 8. 53 8. 37 8. 31 8. 33
1 Dihydroxydimethylol ethylene urea, by Bl-Chem, Burlington Industries, Inc.
TABLE 4.EFFECT OF PREWETTING BEFORE HYDROLYSIS Fabric: Cotton, Army Twill; Pretreatment: 25% Resin 183, 5% Catlyst 43, Dry at 250 F. for 3 minutes; Cure at 340 F. for 6 minutes.
Example Prewet before hydrolysis Yes No Yes No Yes No X X 15 15 20 20 25 25 X X 0.5 0.5 0.5 0.5 0.5 0.5 X X 140 140 140 140 140 140 X X 2 2 2 2 2 2 X X 4 4 4 4 4 4 X 4 2 2 2 2 2 2 X 2 Catalyst 43. 0. 5 0. 5 0. 5 0 5 0. 5 0. 5 X 0. 5 Tear Strength (W/F 2. 2/1. 8 2. 0/1. 7 4 0/1 6 2. 3/2. 0 2. 2/ 1. 8 2. 3/1. 7 1. 5/1. 0 1. 8/2 Crease Resistance:
(W-i-F) Dry- 319 306 311 311 321 326 286 29. 9 (W-i-F) Wet 299 298 300 302 317 313 280 297 Stoll Flex Abrasion:
W 118 78 83 201 132 49 66 638 446 401 455 729 486 265 352 Weight (oz. sq. y 8. 46 8. 50 8. 48 8. 52 8. 53 8. 70 8. 53 8. 64
1 Rohm and Hass, Rhoplex K-3 acrylic (U.S. Pat. 3,157,562) 1 Bi-Chem, Burlington Industries, Inc., Lanolin Base.
TABLE 5 Fabric: 100% All Cotton, Yard Stick (Mooresville Fabric); Pretreatment: 25% Resin 183, 4.5% Catalyst 43, Dry at 250 F. for 3 minutes; Cure at 320 F. for 10 minutes.
Example NaCl 20 20 20 20 25 25 25 25 X HCl 0.5 0.5 0 5 0.5 0.5 0 5 0.5 0.5 X Temp., F. 140 170 140 140 170 170 X Time (min.) 1 2 1 2 1 2 1 2 X Aitertreatment:
K-3 Acrylic 4 4 4 4 4 4 4 4 4 Bi-Chern softener LLS 2 2 2 2 2 2 2 2 2 Catalyst 43 1 1 1 1 1 1 1 1 1 Tear Strength:
arp-.- 1.8 1.9 1.7 1.9 2.1 1.8 1.8 1.2 F 0.8 7.7 8.5 7.2 0.7 0.7 0.8 0.6 Crease Resistance:
+F), Dry 317 316 306 309 315 316 304 320 (W-l-F) Wet 291 296 277 278 287 296 283 271 Stoll Flex Abrasion:
Warp 14 26 30 35 44 117 20 32 13 6 10 10 22 18 23 8 12 6 3. 38 3. 35 3. 39 3.33 3.40 3.35 3.32 3. 39
TABLE 6 Fabric: 100% Cotton, Army Twill; Pretreatment: As Indicated. Dry 3 minutes at 200 F., Cure minutes at 320 F.
Example Resin 15 2O 25 25 25 Catalyst 43 2. 7 2. 7 3. 6 3. 6 4. 5 4. 5 4. 5 4. 5 NaCl 20 20 20 20 20 20 20 20 0 5 0.5 0.5 0.5 0 25 1 2 3 140 140 140 140 140 140 140 140 2 2 2 2 2 2 4 X 4 X 4 4 4 4 2 X 2 X 2 2 2 2 05 X 0.5 X 0.5 0.5 0.5 0.5
Warp 2. 8 1. 8 2. 0 2. 4 3. 7 3. 5 3. 7 3. 9 24 1.6 1.8 2.6 2.8 3.2 2.9 3.6 Crease Resistance:
(W-l-F) Dry 306 248 303 245 311 309 307 288 (W+F), Wet 286 270 292 269 301 304 299 302 Stoll Flex Abrasion:
Warp 240 110 116 110 160 199 325 512 Fill. l, 125 389 647 363 688 737 727 1, 218 Weight (oz./sq. yd.) 8.14 8.08 8.32 8. 32 8.32 8. 8.31 8.26
TABLE 7 Fabric: 100% Cotton, Yarn Stick; Pretreatment: 25% Resin 183, 4.5% Catalyst 43, Dry at 200 F. for 3 minutes; Cure at 320 F. for 10 minutes.
Example X 20 20 25 25 x 0.5 0. 5 0. 5 0.5 X 200 200 200 200 X 1 /2 1 TABLE 8 Fabric: 100% Cotton, Army Twill; Pretreatment: 25% Resin 183, 4.5% Catalyst 43, 4% Rhoplex K-3, Dry at 200 F. for 3 minutes; Cure at 320 F. for 10 minutes.
Example 15 15 20 20 20 20 X X 5 0 0. 5 0. 5 0. 5 X X 140 140 170 170 170 170 X X 3 1 1 2 2 X X Aftertreatment:
Rhoplex K3 4 X 4 X 4 X X 4 Bi-Chem Softener LLS 2 X 2 X 2 X X 2 Catalyst 43 X X X X Tear Strength:
Warp 3.2 2.0 2.2 1 7 2.3 2 0 1.9 1.8 ill 2.8 2.0 1.9 15 2.1 1.8 1.5 1.5 Crease Resistance:
Dry 291 7 322 317 318 310 321 323 (W+F), Wet 302 294 306 294 303 301 290 305 Stoll Flex Abrasion:
Warp 1, 261 281 202 145 277 189 80 82 Fill 1, 870 966 696 359 962 416 491 384 Weight (oz./sq. yd.) 8. 46 8. 33 8. 43 8.36 8. 48 8. 46 8. 43 8. 41
TABLE 9 Fabric: 100% Cotton Broadcloth; Pretreatment: 25% Resin HR, 4. 5% Catalyst 43, Dry at 200 F. for 3 minutes; Cure at 320 F. for 10 minutes.
Example TABLE 10 Fabric: 100% Cotton Broadcloth; Pretreatment: 25% Resin HK, 4.5% Catalyst 43, Dry at 200 F. for 3 minutes; Cure at 320 F. for 10 minutes.
Example No.01 25 25 25 25 20 20 20 20 X HCI 3 3 3 3 3 3 3 3 X Temp., F 170 170 170 170 170 170 170 170 X Time (min) l 2 3 5 1 2 3 5 X Aitertreatment:
Rhoplex K-3 3 3 3 3 3 3 3 3 3 Bi-Chem Softener LLS 2 2 2 2 2 2 2 2 2 Catalyst 43 V, Tear Strength:
Warp 1. O 0.9 0.9 0. 9 0. 9 1. 0. 9 0. 9 0. 6 Fill 1.0 1.0 0.9 0.9 0.8 1.0 0.9 0.9 0.6 Crease Resistance:
W+F) Dry 283 271 26 256 208 271 254 326 (W+F) Wet 278 270 266 252 283 268 276 268 304 Stoll Flex Abrasion:
Warp 140 223 194 202 97 275 173 205 13 226 135 129 146 96 91 139 200 21 TABLE 11 Fabric: 100% Cotton Broadcloth (4.20 oz./sq. yd.); Pretreatment: 25% Resin 183, 4.5% Catalyst 43, 3.0% Acrylic K-3, Dry 3 minutes at 200 F.; Cure minutes at 320 F.
Example Pie-Wet Yes Y Yes Yes X X NaCl 15 20 20 20 20 20 X X H01 5 5 3 3 3 3 3 3 X X Temp., F 140 140 140 140 140 140 140 140 X X Time (min) 3 1 1 1 2 2 3 3 X X Aftertreatment:
Rhoplex K-3 1 1 1 1 1 1 1 1 1 X Bi-Chem Softener PE 00110. 2 2 2 2 2 2 2 2 2 X Catalyst 43 K; V; ya V2 56 X Tear Strength:
(W-l-F), Dry 308 317 317 305 283 293 299 299 311 314 (H-F). Wet 283 298 301 277 261 273 285 305 305 278 Stoll Flex Abrasion:
Warp 176 115 392 525 122 181 271 16 31 Fill 152 64 86 282 243 306 106 180 35 52 A polyethylene emulsion, manufactured by Bi-Chem Company, Division of Burlingflustries.
Table 12 Feb ric: Dacron/35% Cotton Cross Dyed; Pretreatment: 30% Resin 183, 5.5% Catalyst 43, 2% Rhoplex K-3, Dry 200 F. for 3 minutes; Cure 320 F. for 10 minutes.
Example Pre-Wet Yes X X NaCl. 20 20 20 20 X X Cl 3 3 3 3 X X Temp F. 140 140 X X Time (min.) 1 2 3 X X Aitertreatment:
Rhoplex K-3 2 2 2 2 X 2 Bi-Chem Softener PE Gone. 2 2 2 2 X 2 Crystal 43 V X V Tear Strength:
Warp 7. 5 7. 7 7. 5 7. 6 5. 5 7. 6 Fill 5. 4 5. 9 5. 9 5. 9 3. 4 5. 0 Crease Resistance:
(W+F), Dry- 320 322 322 322 328 (W+F), Wet 315 307 316 306 303 312 Press Abrasion (Class) 3 3 4 3 1 2 TABLE 13.-EFFECT OF ALKALINE EARTH METAL ELECTROLYTE SALTS Fabric: 100% Cotton, Army Twill, 8.0 ozJsq. yd.; Pretreatment: 25% Resin 183, 4.5% Catalyst 43,
Rhoplex K-3, Dry 200 F. for 3 minutes; Cure 320 F. for minutes Example CBClg (anhydrous) 10 0 0 0 0 MgClz 611 0 0 0 0 0 0 10 20 30 40 H01 (36 3 3 3 3 3 3 3 3 3 Time (min)... 1 1 1 1 1 1 1 1 1 Temperature, 140 140 140 140 140 140 140 140 140 Aitertreatment: l
Rhoplex K-3 5 5 5 5 5 5 5 5 5 2 Bi-Ohem Softener PE 2 2 2 2 2 2 2 2 2 5 Ammonium Chloride- 34 M 54 4 34 $4 $4 $4 )4 Tear Strength:
Warp 3. 2 3. 5 3. 4 4. 0 3. 8 3. 5 3. 5 3.5 3. 8 3. 9 ill 3. 4 3. 4 3. 3 4. 6 3. 6 3. 6 3. 5 3. 7 4. 2 4. 1 Crease Resistance:
Dry 313 309 311 299 306 312 302 300 287 315 W 300 299 301 294 311 302 300 300 296 290 Stoll-Flex Abrasion:
Warp 257 248 277 532 296 351 454 343 537 370 Fill 1, 118 738 763 1, 500+ 1, 500+ 631 1,056 815 1, 034 1, 315
l Dried 3 minutes at 200 F. and cured 3 minutes at 325 F.
TABLE 14.EFFECT OF AMMONIUM CATION AND NITRATE ANION Fabric: 100% Cotton, Army Twill, 8.0 oz./sq. yd.; Pretreatment: 25% Resin 183, 4.0% Catalyst 43, 5% Rhoplex K-3, Dry 200 F. for 3 minutes; Cure 320 F. for 10 minutes.
Example Sodium Nitrate l Dried 3 minutes at 200 F. and cured 3 minutes at 325 F.
EXAMPLE 102 This example relates to an illustration of the improved moisture regain obtained by the present invention. The textile product of Example 53 was tested for moisture regain, according to ASTM Test D629-59A, and compared with the resinated control textile of Example 69. The test results were as follows:
Moisture regain Percent Resinated control (of Ex. 69) 3.4 Resinated acid hydrolysis (of Ex. 53) 4.9 Percent improvement 44 EXAMPLE 103 This example relates to an illustration of the improved soil resistance of the textiles of the present invention. The textile produced according of Example 82 was tested for soil resistance by the 3-M Test and compared with the resinated control textile of Example 85. The test produced the following results:
o 30 a a Obviously many modifications and variations of the present invention are possible in the light of the above teachings. It is therefore to be understood that within the scope of the appended claims the invention may be practiced otherwise than as specifically described.
What we claim is:
1. In a process of producing resin-treated cellulosic textiles comprising applying a resin to a cellulosic textile, and at least partially curing the resin on the textile 'by means of a cross-linking agent, the improvement comprising (a) hydrolyzing the partially cured resintreated textile in an aqueous bath containing a strong acid and a neutral or only slightly acid electrolyte salt selected from the group consisting of alkali metal, alkaline earth metal and ammonium salt electrolytes, the concentration of the electrolyte salt being at least 5% w./v. and the concentration of the acid being 0.01 to 15% w./v., and (b) thereafter neutralizing and washing the hydrolyzed resin-treated textile, whereby the textile has increased abrasion resistance and other improved textile properties.
2. The process as claimed in claim 1 wherein the electrolytic salt is a salt of said acid.
3. The process as claimed in claim 1 wherein 0.1 to 30 percent by weight of an acrylic resin and 0.1 to 10 percent by weight of a lubricating agent are applied to the resin-treated cellulose textile.
4. The process as claimed in claim 3 wherein said acrylic resin and said lubricating agent are applied to the 13 resin-treated cellulose textile before and after the hydrolyzing step.
5. The process as claimed in claim 1 wherein the resin-treated cellulose textile is pre-Wetted prior to the hydrolyzing step.
6. The process as claimed in claim 1 wherein the hydrolyzed resin-treated textile is neutralized by immersion in an aqueous bath containing a weak alkaline compound.
7. The process as claimed in claim 6 wherein the concentration of the weak alkaline compound in the neutralized bath is 0.01 to 10 percent w./v.
8. The process of claim 1 wherein the acid is hydrochloric acid, the salt is sodium chloride and the hydrolyzed resin-treated textile is neutralized by impregnating same with an aqueous solution of sodium carbonate, followed by washing with water and drying.
References Cited UNITED STATES PATENTS 1/1951 Fluck 117-143 X 2/1958 Sumner et a1 117140 X 8/1960 Hurwitz 117139.4 X 10/1960 Buck et a1 1l7139.4 X 7/1961 Miles et a1. 11762.1 X 10/ 1961 Sumner et al 117140 11/1961 Burkitt.
6/ 1964 Getchell 1l7--139.4 X 3/1968 Cotton 1l7-139.4
WILLIAM D. MARTIN, Primary Examiner 15 H. J. GWINNELL, Assistant Examiner US. Cl. X.R.
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US2823142A (en) * 1954-10-20 1958-02-11 Chicopee Mfg Corp Soft durable nonwoven fabric
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US10407597B2 (en) * 2009-10-08 2019-09-10 Johns Manville Binder composition
US10954421B2 (en) 2009-10-08 2021-03-23 Johns Manville Binder composition
US11685848B2 (en) 2009-10-08 2023-06-27 Johns Manville Binder composition

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