CN106893065A - A kind of fixation aqueous polyurethane dispersion, preparation method and applications - Google Patents
A kind of fixation aqueous polyurethane dispersion, preparation method and applications Download PDFInfo
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- CN106893065A CN106893065A CN201510967560.9A CN201510967560A CN106893065A CN 106893065 A CN106893065 A CN 106893065A CN 201510967560 A CN201510967560 A CN 201510967560A CN 106893065 A CN106893065 A CN 106893065A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
- C08G18/4837—Polyethers containing oxyethylene units and other oxyalkylene units
- C08G18/4845—Polyethers containing oxyethylene units and other oxyalkylene units containing oxypropylene or higher oxyalkylene end groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/008—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated using reactive dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/66—Natural or regenerated cellulose using reactive dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
Abstract
The invention discloses a kind of fixation aqueous polyurethane dispersion, preparation method and applications.A kind of preparation method of fixation aqueous polyurethane dispersion, including step 1：Polymerisation is carried out by polyisocyanates and oligomer polyol and small molecule dihydroxylic alcohols, base polyurethane prepolymer for use as is obtained；Step 2：In a solvent, base polyurethane prepolymer for use as and crosslinking agent are carried out into cross-linking reaction, obtains cross-linked polyurethane；Step 3：By cross-linked polyurethane and deionized water, dispersion and emulsion is carried out, obtain cross-linked polyurethane dispersion；Step 4：Cross-linked polyurethane dispersion and diamines are carried out into chain extending reaction, the cross-linked polyurethane after chain extension is obtained；Step 5：Cross-linked polyurethane after chain extension and Amino End Group silane coupler are carried out into end capping reaction, fixation aqueous polyurethane dispersion is obtained.Preparation method process is simple of the invention, energy consumption are low, obtained product filming performance is good, fixing property is good, be suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of fixation aqueous polyurethane dispersion, preparation method and applications.
Background technology
Due to containing the water soluble groups such as sulfonic group or carboxylic acid group in many commonly-used dye molecule, they
Dyefastness, particularly color fastness to washing are poor, and the adhesion with fabric is poor, need fixation to post-process.Gu
Toner can form insoluble salt with dye molecule, reduce dye solubility, improve water-fast and wet fastness；
Film can be formed on dyestuff as special adhesive, prevent dyestuff from being contacted with water：Can also with dyestuff and
Active group reacts on fiber, forms covalent bond and produces stronger affinity, so as to reach fixation effect
Really.
Aqueous polyurethane (WPU) has extensive compatibility in field of textiles, can be used as pigment printing
Low-temperature adhesive, non-woven fabric adhesive, laminating adhesive, textile sizing agent, introduce specific groups
WPU can be made into finishing agent of water resistant oil resistant antistatic etc..WPU as textile dye-Fixing agents, with green
Environmental protection, good gas permeability, improve fabric flexibility, be remarkably improved rub resistance of fabric etc. its
The incomparable advantage of his color fixing agent.Its mechanism of action is to stick to dye molecule surface to form film, and
Can be reacted with active group on dyestuff and fiber, so as to improve the crock fastness of fabric.With WPU
Adhesive has turned into study hotspot for weaving fixation post-finishing agent.
Aqueous polyurethane is divided into ionic and nonionic according to whether dispersion ion is powered, and ionic
Aqueous polyurethane can be divided into anionic, cationic and two again according to the powered property in polyurethane backbone
Property ionic.Positive electricity is carried on the molecule segment of cation aqueous polyurethane, to hydrophobic polyester, fabric
Fiber has good wellability, at the same it is insensitive to the hardness of water, therefore it is in weaving, papermaking, coating
It is with a wide range of applications Deng field.
CN101914857A discloses a kind of preparation method of reactive polyurethane film-forming color fixing agent, by low
Polymers polyalcohol and polyisocyanates reaction prepare base polyurethane prepolymer for use as, through chain extending reaction, quaterisation,
Ethylenediamine chain extension, introduce 3- NCO propyl-triethoxysilicane coupling agents, last acetic acid on the rocks and
Deionized water emulsification is obtained.It is in preparation process that the operation of performed polymer quaternization is more complicated, use
Iodomethane or epoxychloropropane etc. be unstable or noxious material, and with the silane coupled of isocyanate groups
Agent block, it is relatively costly, and emulsification after product stability it is poor.Therefore, process is simple, energy consumption are found
It is low, obtained product filming performance is good, fixing property is good, be suitable for the polyurethane film-forming of industrialized production
The preparation method of color fixing agent is the technical problem for being badly in need of solving at present.
The content of the invention
The technical problems to be solved by the invention are to overcome polyurethane film-forming color fixing agent in the prior art
Preparation method operation it is more complicated, production cost is higher, product stability is poor, be not suitable for industrialization
Production etc. defect and provide a kind of fixation aqueous polyurethane dispersion, preparation method and applications.This
The preparation method process is simple of invention, energy consumption are low, obtained product filming performance is good, fixing property is good,
It is suitable for industrialized production.
The invention provides a kind of preparation method of fixation aqueous polyurethane dispersion, it includes following step
Suddenly：
Step 1：Polymerisation is carried out by polyisocyanates and oligomer polyol and small molecule dihydroxylic alcohols,
Base polyurethane prepolymer for use as is obtained；
Step 2：In a solvent, the base polyurethane prepolymer for use as step 1 being obtained carries out being crosslinked instead with crosslinking agent
Should, obtain cross-linked polyurethane；
Step 3：The cross-linked polyurethane and deionized water that step 2 is obtained, carry out dispersion and emulsion, obtain
Cross-linked polyurethane dispersion；
Step 4：The cross-linked polyurethane dispersion that step 3 is obtained carries out chain extending reaction with diamines, obtains
Cross-linked polyurethane after chain extension；
Step 5：Cross-linked polyurethane after the chain extension that step 4 is obtained is carried out with Amino End Group silane coupler
End capping reaction, obtains fixation aqueous polyurethane dispersion.
In step 1, described polyisocyanates can be polyisocyanates conventional in the art, preferably
Toluene di-isocyanate(TDI), hexamethylene diisocyanate, IPDI (IPDI) and 4,
One or more in 4 '-dicyclohexyl methyl hydride diisocyanate (HMDI).
In step 1, described oligomer polyol can be oligomer polyol conventional in the art,
It is preferred that polyoxypropylene dihydroxylic alcohols, polyoxyethylene dihydroxylic alcohols, polytetramethylene glycol and polyadipate diethyl two
One or more in alcohol ester ether.40~200 milligrams of the preferred hydroxyl value of described polyoxypropylene dihydroxylic alcohols
KOH/ grams, acid number is not more than 0.2 milligram KOH/ grams.The preferred hydroxyl value 40 of described polyoxyethylene dihydroxylic alcohols~
200 milligrams KOH/ grams, acid number is not more than 0.2 milligram KOH/ grams.Described polytetramethylene glycol is excellent
40~200 milligrams KOH/ grams of hydroxyl value is selected, acid number is not more than 0.2 milligram KOH/ grams.It is described to gather oneself two
40~200 milligrams KOH/ grams of the preferred hydroxyl value of acid diethylene glycol ester ether, acid number is 0.1~1.2 milligram of KOH/
Gram.
In step 1, the mass ratio of the cross-linked polyurethane after described oligomer polyol and described chain extension
Value preferably 0.1~0.8, further preferred 0.34~0.60, such as 0.43,0.46 or 0.48.
In step 1, the mass values of the cross-linked polyurethane after described polyisocyanates and described chain extension
It is preferred that 0.1~0.8, further preferred 0.25~0.56, such as 0.38,0.41 or 0.46.
In step 1, described small molecule dihydroxylic alcohols can be small molecule dihydroxylic alcohols conventional in the art,
It is preferred that one or more in ethylene glycol, 1,3-PD, BDO and 1,6- hexylene glycol.
In step 1, cross-linked polyurethane after the quality of described small molecule dihydroxylic alcohols and described chain extension
Mass values preferably 0.01~0.06, further preferred 0.018~0.043, such as 0.025 or 0.02.
In step 1, in described polyisocyanates and described oligomer polyol and small molecule dihydroxylic alcohols
The molar ratio of hydroxyl preferably 1.1~5, further preferred 1.5~4, such as 2.48 or 3.
In step 1, the temperature of described polymerisation can be the ordinary temperature of such reaction in this area,
Particularly preferred 50 DEG C~100 DEG C, further preferred 70 DEG C~85 DEG C, such as 75 DEG C~85 DEG C in the present invention
Or 70 DEG C~80 DEG C.
In step 1, the time of described polymerisation can be supervised using this area routine monitoring method
Survey, typically with di-n-butylamine-hydrochloric acid method titration system NCO content, to reach preset value as reaction end,
Preferably 1 hour~5 hours, further preferred 2 hours~3 hours time of described polymerisation.
Step 1 is preferably carried out under conditions of initiator presence, and described initiator can be in this area
The normal starter of the type of polymerization, particularly preferred dibutyl tin laurate in the present invention.Described
The mass values preferably 0~0.0050 (not including 0) of the cross-linked polyurethane after initiator and described chain extension,
Further preferred 0.00034~0.0026, such as 0.00056 or 0.0019.
In step 2, described crosslinking agent can be the common cross-linking agent of such cross-linking reaction in this area,
It is preferred that trimethylolpropane, trimethylolpropane polyglycol ether (TM, 423 milligrams of KOH/ of hydroxyl value
Gram, 0.1~1.2 milligram KOH/ grams of acid number), one or more in triethanolamine and diethylenetriamine.
In step 2, the mass ratio of the cross-linked polyurethane after the quality of described crosslinking agent and described chain extension
Value preferably 0.02~0.10, further preferred 0.035~0.091, such as 0.0448,0.0492 or 0.051.
In step 2, the temperature of described cross-linking reaction can be the routine of such cross-linking reaction in this area
Temperature, particularly preferred 50 DEG C~100 DEG C, further preferred 60 DEG C~70 DEG C in the present invention.
In step 2, the time of described cross-linking reaction can be supervised using this area routine monitoring method
Survey, typically with di-n-butylamine-hydrochloric acid method titration system NCO content, to reach preset value as reaction end,
Preferably 2 hours~6 hours, such as 4 hours time of described cross-linking reaction.
In step 3, described solvent can be the Conventional solvents of such dispersion and emulsion reaction in this area,
Particularly preferred ketones solvent and/or ether solvent, the preferred acetone of described ketones solvent in the present invention；It is described
The preferred tetrahydrofuran of ether solvent.
In step 3, the mass values of the cross-linked polyurethane after described solvent and described chain extension are preferred
0.30~1.2, further preferred 0.40~1.08, such as 0.52,0.56 or 0.57.
In step 3, the solid content preferably 15%~45% of described cross-linked polyurethane dispersion, further
It is preferred that 18%~40%, such as 23%, 24% or 27%.
In step 3, the temperature of described dispersion and emulsion can be such dispersion and emulsion reaction in this area
Ordinary temperature, particularly preferred 0 DEG C~50 DEG C, further preferred 0 DEG C~20 DEG C in the present invention.
In step 3, the time of described dispersion and emulsion can be supervised using this area routine monitoring method
Survey, preferably 1 hour~2 hours time that described dispersion and emulsion reacts.
In step 3, described dispersion and emulsion is carried out preferably under conditions of stirring, the speed of described stirring
Preferably 1000 revs/min~1500 revs/min of degree.
In step 4, described diamines can be the conventional diamines of such chain extending reaction in this area, this hair
One or more in bright in particularly preferred ethylenediamine, piperazine, diethanol amine and N methyldiethanol amine.
In step 4, the mass values of the cross-linked polyurethane after described diamines and described chain extension are preferred
0.01~0.10, further preferred 0.03~0.07, such as 0.05 or 0.06.
In step 4, described diamines preferably uses two amine aqueous solutions, the quality of described two amine aqueous solutions
Concentration preferably 35%~45%, such as 40%, described mass concentration refers to that the quality of diamines accounts for two aqueous amines
The percentage of solution gross mass.
In step 4, described chain extending reaction is preferably carried out under agitation, the speed of described stirring
It is preferred that 500 revs/min~1000 revs/min.
In step 4, the temperature of described chain extending reaction can be the routine of such chain extending reaction in this area
Temperature, particularly preferred 0 DEG C~50 DEG C, further preferred 0 DEG C~20 DEG C in the present invention.
In step 4, the time of described chain extending reaction can be supervised using this area routine monitoring method
Survey, typically with di-n-butylamine-hydrochloric acid method titration system NCO content, to reach preset value as reaction end,
Preferably 0.5 hour~1.5 hours, such as 1 hour time of described chain extending reaction.
In step 5, the preferred Amino End Group Silane coupling agent KH550 of described Amino End Group silane coupler.
In step 5, the matter of the cross-linked polyurethane after described Amino End Group silane coupler and described chain extension
Amount ratio preferably 0.03~0.10, further preferred 0.039~0.081, such as 0.035,0.057 or 0.070.
In step 5, the temperature of described end capping reaction can be the routine of such end capping reaction in this area
Temperature, particularly preferred 10 DEG C~50 DEG C in the present invention, further preferred 35 DEG C~50 DEG C, such as 35 DEG C~
45 DEG C or 40 DEG C~50 DEG C.
In step 5, the time of described end capping reaction can be supervised using this area routine monitoring method
Survey, preferably 0.5 hour~2.5 hours, such as 1 hour time of described end capping reaction.
Present invention also offers fixation aqueous polyurethane dispersion obtained in above-mentioned preparation method.
Present invention also offers described fixation aqueous polyurethane dispersion as color fixing agent application.
Without prejudice to the field on the basis of common sense, above-mentioned each optimum condition, can be combined, and obtain final product this
Invent each preferred embodiments.
Agents useful for same of the present invention and raw material are commercially available.
In the present invention, described room temperature refers to environment temperature, is 10 DEG C~35 DEG C.
Positive effect of the invention is：Reaction process is simple, can be significantly reduced compared with quaterisation
Energy consumption；The silane containing isocyano is not used in reaction, the stability of reactor product is greatly improved；This product
Contain reactive silicon hydroxyl (SiOH) in product structure, can with the active group of dyestuff on fabric (such as hydroxyl,
Amino etc.) dehydration is carried out in drying process, chemical bond is formed, contribute to fixing of dye；
Product of the present invention also has excellent filming performance simultaneously, can form one layer of firm guarantor in fabric face
Cuticula is further up to fixation purpose.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but is not therefore limited the present invention to
Among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, according to normal
Rule method and condition, or selected according to catalogue.
In following embodiments, raw materials used material is commercially available.
Embodiment 1
A kind of preparation of fixation aqueous polyurethane dispersion, it is obtained by following steps：
From polyethenoxy ether dihydroxylic alcohols (PPG1000,112 milligrams KOH/ grams of hydroxyl value, acid number 0.1
KOH/ grams of milligram) 50 grams, 2.7 grams of BDO, IPDI (IPDI) 44
Gram, be added to above-mentioned raw materials equipped with reflux condensing tube, thermometer by 0.1 gram of dibutyl tin laurate,
In the 500mL four-hole boiling flasks of mixer, electric jacket heats 80 ± 5 DEG C, reacts 2 hours, and poly- ammonia is obtained
Ester performed polymer, adds 5.31 grams of triethanolamine, and 60 grams of acetone, 65 ± 5 DEG C of temperature is reacted 4 hours,
Less than 20 degree plus 270 grams of deionized water are cooled to, 1000 revs/min of rotating speed is adjusted, emulsification must consolidate for 1 hour
Containing the cross-linked polyurethane dispersion for 23%, below 20 DEG C of temperature control in system be added dropwise mass concentration be 40%
14.44 grams of the diethanol amine aqueous solution (described mass concentration refers to that the quality of diethanol amine accounts for diethanol
The percentage of amine aqueous solution gross mass), 500 revs/min of rotating speed is adjusted, react 1 hour, it is warming up to 40 DEG C
4.20 grams of Silane coupling agent KH550s are added, 40 ± 5 DEG C are reacted 1 hour, and vacuum extracts acetone out must be consolidated and contain
The fixation aqueous polyurethane dispersion of amount about 30%.
Embodiment 2
A kind of preparation of fixation aqueous polyurethane dispersion, it is obtained by following steps：
From APEO dihydroxylic alcohols (PEG1000,112 milligrams KOH/ grams of hydroxyl value, acid number 0.15
KOH/ grams of milligram) 50 grams, 1.86 grams of ethylene glycol, 40.3 grams of hexamethylene diisocyanate, February
0.2 gram of dilaurylate, above-mentioned raw materials is added to equipped with reflux condensing tube, thermometer, mixer
In 500mL four-hole boiling flasks, electric jacket heats 80 ± 5 DEG C, reacts 3 hours, and base polyurethane prepolymer for use as is obtained,
5.36 grams of trimethylolpropane is added, 60 grams of acetone, 65 ± 5 DEG C of temperature is reacted 4 hours, is cooled to
Less than 20 DEG C plus 390 grams of deionized water, adjust 1000 revs/min of rotating speed, and emulsification must consolidate containing being 18% for 1 hour
Cross-linked polyurethane dispersion, below 20 DEG C of temperature control in system be added dropwise mass concentration be 40% piperazine
(described mass concentration refers to that the quality of piperazine accounts for two piperazine aqueous solution gross masses to 18.60 grams of the aqueous solution
Percentage), 500 revs/min of regulation rotating speed reacts 1 hour, is warming up to 40 DEG C of additions, 6 grams of silane couplers
KH550,40 ± 5 DEG C are reacted 1 hour, and vacuum is extracted acetone out and obtains solid content and is about 20% fixation with aqueous
Dispersions of polyurethanes.
Embodiment 3
A kind of preparation of fixation aqueous polyurethane dispersion, it is obtained by following steps：
From polytetramethylene glycol (PTMEG1000,112 milligrams KOH/ grams of hydroxyl value, acid number 0.05
KOH/ grams of milligram) 50 grams, 1,6- 3.54 grams of hexylene glycol, toluene di-isocyanate(TDI) (TDI) 20.9
Gram, above-mentioned raw materials are added to equipped with reflux condensing tube, thermometer, the 500mL four-hole boiling flasks of mixer
In, electric jacket heats 85 ± 5 DEG C, reacts 3 hours, and base polyurethane prepolymer for use as is obtained, and adds trihydroxy methyl third
Alkoxy polyalkylene glycol ether (TM, 423 milligrams KOH/ grams of hydroxyl value, 0.1~1.2 milligram KOH/ grams of acid number)
7.56 grams, 90 grams of tetrahydrofuran, 65 ± 5 DEG C of temperature is reacted 4 hours, is cooled to less than 0 degree plus is gone
130 grams of ionized water, adjusts 1000 revs/min of rotating speed, and emulsification must consolidate containing the poly- ammonia of crosslinking for 27% for 1 hour
Ester dispersion, to the ethylenediamine solution 1.8 that dropwise addition mass concentration in system is 40% below 0 DEG C of temperature control
Gram (described mass concentration refers to that the quality of ethylenediamine accounts for the percentage of ethylenediamine solution gross mass),
500 revs/min of regulation rotating speed reacts 1 hour, is warming up to 40 DEG C of additions, 2.87 grams of Silane coupling agent KH550s,
45 ± 5 DEG C are reacted 1 hour, and vacuum is extracted tetrahydrofuran out and obtains solid content and is about the aqueous poly- ammonia of 40% fixation
Ester dispersion.
Embodiment 4
A kind of preparation of fixation aqueous polyurethane dispersion, it is obtained by following steps：
From 50 grams of polytetramethylene glycol (PTMEG1000,112 milligrams KOH/ grams of hydroxyl value), 1,
2.7 grams of 4- butanediols, 4,83.8 grams of 4 '-dicyclohexyl methyl hydride diisocyanate (HMDI), two bays
0.05 gram of sour dibutyl tin, above-mentioned raw materials is added to equipped with reflux condensing tube, thermometer, mixer
In 500mL four-hole boiling flasks, electric jacket heats 75 ± 5 DEG C, reacts 2 hours, and base polyurethane prepolymer for use as is obtained,
5.15 grams of diethylenetriamine is added, 60 grams of acetone, 65 ± 5 DEG C of temperature is reacted 4 hours, is cooled to 0
Degree is following plus 160 grams of deionized water, adjusts 1000 revs/min of rotating speed, and emulsification must consolidate that to contain be 40% for 1 hour
Cross-linked polyurethane dispersion, below 0 DEG C of temperature control in system be added dropwise mass concentration be 40% ethylenediamine
(described mass concentration refers to that the quality of ethylenediamine accounts for ethylenediamine solution gross mass to 20.7 grams of the aqueous solution
Percentage), 500 revs/min of regulation rotating speed reacts 1 hour, is warming up to 40 DEG C, adds 12 grams of silane idols
Connection agent KH550,45 ± 5 DEG C are reacted 1 hour, obtain the fixation aqueous polyurethane that solid content is about 50%
Dispersion.
Embodiment 5
A kind of preparation of fixation aqueous polyurethane dispersion, it is obtained by following steps：
From 50 grams of polydiethylene glycol adipate ether (112 milligrams KOH/ grams of hydroxyl value), 1,3- the third two
2.3 grams of alcohol, 53.3 grams of IPDI (IPDI), 0.3 gram of dibutyl tin laurate,
Above-mentioned raw materials are added to equipped with reflux condensing tube, thermometer, in the 500mL four-hole boiling flasks of mixer,
Electric jacket heats 75 ± 5 DEG C, reacts 2 hours, and base polyurethane prepolymer for use as is obtained, and adds diethylenetriamine 5.15
Gram, 60 grams of tetrahydrofuran, 65 ± 5 DEG C of temperature is reacted 4 hours, is cooled to less than 20 degree plus deionization
290 grams of water, adjusts 1000 revs/min of rotating speed, and emulsification must consolidate containing the cross-linked polyurethane point for 24% for 1 hour
A prose style free from parallelism, to 10 grams of (institutes of ethylenediamine solution that dropwise addition mass concentration in system is 40% below 20 DEG C of temperature control
The mass concentration stated refers to that the quality of ethylenediamine accounts for the percentage of ethylenediamine solution gross mass), regulation turns
500 revs/min of speed is reacted 1 hour, is warming up to 40 DEG C, adds 8 grams of Silane coupling agent KH550s, 45 ± 5 DEG C
Reaction 1 hour, vacuum is extracted tetrahydrofuran out and obtains solid content and be about 30% fixation and disperseed with aqueous polyurethane
Body.
Carry out the side of film forming fixing finish to fabric with aqueous polyurethane dispersion using fixation of the invention
Method is, by product of the present invention and water with mass ratio (3~15)：100 prepare.At ambient temperature, two
Leaching two is rolled, and (described pick-up rate refers to fabric through the liquid carrying rate after mangle, meter to pick-up rate 70~100%
It is that fabric weighs × 100% before (fabric weight before fabric weight-mangle after mangle)/mangle to calculate formula), 80~
110 DEG C dry 2~4 minutes, then solidify 2~4 minutes at 120-140 DEG C.
In drying process, the active group in silicone hydroxyl (SiOH) and dyestuff in this product structure is (such as
Hydroxyl, amino etc.) dehydration is carried out, chemical bond is formed, while also being formed on dye for fabrics surface
One layer of firm diaphragm, increases the dyeing firmness of fabric, improves wash durability.
Reactive dye are carried out film forming fixing finish by application experiment example 1, and product of the present invention is with water with quality
Than 1：20 prepare housekeeping liquid, and the bafta of reactive dyeing is entered by foregoing fixing finish method
Row fixing finish.Sample test results are shown in Table 1.
Application experiment example 2, film forming fixing finish, product of the present invention are carried out to pigment printing：Pigment printing paste：
Thickener (sodium alginate)：Water quality ratio=20：5：1.5：100, thickener and water are first tuned into paste
Shape, is subsequently adding this product, is eventually adding mill base.
Stamp, dries 2~5 minutes by then 90~110 DEG C at ambient temperature, at 120~140 DEG C,
Solidification 2~5 minutes.Sample test results are shown in Table 2.
Application experiment example 3, according to GB/T 6753.3-1986 standard test emulsion intercalation methods.By from
Scheming Accelerated subsidence experimental simulation bin stability.Emulsion is put in centrifuge tube, with 3000 revs/min
Whether rotating speed centrifugal sedimentation 15 minutes, observation emulsion is layered.If without precipitation, it is believed that mechanically stable
Property it is good, have the stable storing phase of 6 months.Sample test results are shown in Table 3.
Table 1
Table 2
Table 3
| Laboratory sample | After centrifugation 15 minutes |
| Embodiment 1 | Without precipitation |
| Embodiment 2 | Without precipitation |
| Embodiment 3 | Without precipitation |
| Embodiment 4 | Without precipitation |
| Embodiment 5 | Without precipitation |
| CN101914587A embodiments 1 | There is precipitation |
| CN101914587A embodiments 2 | There is precipitation |
| CN101914587A embodiments 3 | There is precipitation |
| CN101914587A embodiments 4 | There is precipitation |
Fastness is determined and determined by GB5711-5718-85.
Scale：GB250-1995 dyefastness fading sample cards.
By subordinate list 1 as can be seen that the bafta color fastness of the reactive dyeing with Product organization of the present invention
It is significantly increased.
By subordinate list 2 as can be seen that the color fastness of the pigment printing arranged with this product, dry and wet crock fastness
More than 3.5 grades can be reached.
By subordinate list 3 as can be seen that the emulsion mechanical stability of this product is generally better than patent
CN101914857。
Claims (10)
1. a kind of preparation method of fixation aqueous polyurethane dispersion, it is characterised in that it includes following
Step：
Step 1：Polymerisation is carried out by polyisocyanates and oligomer polyol and small molecule dihydroxylic alcohols,
Base polyurethane prepolymer for use as is obtained；
Step 2：In a solvent, the base polyurethane prepolymer for use as step 1 being obtained carries out being crosslinked instead with crosslinking agent
Should, obtain cross-linked polyurethane；
Step 3：The cross-linked polyurethane and deionized water that step 2 is obtained, carry out dispersion and emulsion, obtain
Cross-linked polyurethane dispersion；
Step 4：The cross-linked polyurethane dispersion that step 3 is obtained carries out chain extending reaction with diamines, obtains
Cross-linked polyurethane after chain extension；
Step 5：Cross-linked polyurethane after the chain extension that step 4 is obtained is carried out with Amino End Group silane coupler
End capping reaction, obtains fixation aqueous polyurethane dispersion.
2. the preparation method of fixation aqueous polyurethane dispersion as claimed in claim 1, its feature
It is：In step 1, described polyisocyanates is toluene di-isocyanate(TDI), the isocyanic acid of hexa-methylene two
Ester, IPDI and 4, one or more in 4 '-dicyclohexyl methyl hydride diisocyanate；
And/or,
In step 1, described oligomer polyol is polyoxypropylene dihydroxylic alcohols, polyoxyethylene dihydroxylic alcohols,
One or more in polytetramethylene glycol and polydiethylene glycol adipate ether；
And/or,
In step 1, the mass ratio of the cross-linked polyurethane after described oligomer polyol and described chain extension
Be worth is 0.1~0.8；
And/or,
In step 1, the mass values of the cross-linked polyurethane after described polyisocyanates and described chain extension
It is 0.1~0.8；
And/or,
In step 1, described small molecule dihydroxylic alcohols is ethylene glycol, 1,3-PD, BDO
With one or more in 1,6- hexylene glycols；
And/or,
In step 1, cross-linked polyurethane after the quality of described small molecule dihydroxylic alcohols and described chain extension
Mass values are 0.01~0.06；
And/or,
In step 1, in described polyisocyanates and described oligomer polyol and small molecule dihydroxylic alcohols
The molar ratio of hydroxyl is 1.1~5；
And/or,
In step 1, the temperature of described polymerisation is 50 DEG C~100 DEG C；
And/or,
In step 1, the time of described polymerisation is 1 hour~5 hours；
And/or,
Step 1 is carried out under conditions of initiator presence.
3. the preparation method of fixation aqueous polyurethane dispersion as claimed in claim 2, its feature
It is：In step 1, described polyoxypropylene dihydroxylic alcohols hydroxyl value is 40~200 milligrams KOH/ grams, acid
Value is not more than 0.2 milligram KOH/ grams；
And/or,
In step 1, described polyoxyethylene dihydroxylic alcohols hydroxyl value is 40~200 milligrams KOH/ grams, acid number
No more than 0.2 milligram KOH/ grams；
And/or,
In step 1, described polytetramethylene glycol hydroxyl value is 40~200 milligrams KOH/ grams, acid number
No more than 0.2 milligram KOH/ grams；
And/or,
In step 1, described polydiethylene glycol adipate ether hydroxyl value is 40~200 milligrams KOH/ grams,
Acid number is 0.1~1.2 milligram KOH/ grams；
And/or,
In step 1, the mass ratio of the cross-linked polyurethane after described oligomer polyol and described chain extension
Be worth is 0.34~0.60；
And/or,
In step 1, the mass values of the cross-linked polyurethane after described polyisocyanates and described chain extension
It is 0.25~0.56；
And/or,
In step 1, cross-linked polyurethane after the quality of described small molecule dihydroxylic alcohols and described chain extension
Mass values are 0.018~0.043；
And/or,
In step 1, in described polyisocyanates and described oligomer polyol and small molecule dihydroxylic alcohols
The molar ratio of hydroxyl is 1.5~4；
And/or,
In step 1, the temperature of described polymerisation is 70 DEG C~85 DEG C；
And/or,
In step 1, the time of described polymerisation is 2 hours~3 hours；
And/or,
When step 1 is carried out under conditions of initiator presence, described initiator is the fourth of tin dilaurate two
Ji Xi；
And/or,
When step 1 is carried out under conditions of initiator presence, after described initiator and described chain extension
Cross-linked polyurethane mass values be 0~0.0050.
4. the preparation method of fixation aqueous polyurethane dispersion as claimed in claim 3, its feature
It is：In step 1, the quality of the cross-linked polyurethane after described oligomer polyol and described chain extension
Ratio is 0.43,0.46 or 0.48；
And/or,
In step 1, the mass values of the cross-linked polyurethane after described polyisocyanates and described chain extension
It is 0.38,0.41 or 0.46；
And/or,
In step 1, cross-linked polyurethane after the quality of described small molecule dihydroxylic alcohols and described chain extension
Mass values are 0.025 or 0.02；
And/or,
In step 1, in described polyisocyanates and described oligomer polyol and small molecule dihydroxylic alcohols
The molar ratio of hydroxyl is 2.48 or 3；
And/or,
In step 1, the temperature of described polymerisation is 75 DEG C~85 DEG C or 70 DEG C~80 DEG C；
And/or,
When step 1 is carried out under conditions of initiator presence, after described initiator and described chain extension
Cross-linked polyurethane mass values be 0.00034~0.0026.
5. the preparation method of fixation aqueous polyurethane dispersion as claimed in claim 1, its feature
It is：In step 2, described crosslinking agent is trimethylolpropane, trimethylolpropane polyglycol ether,
One or more in triethanolamine and diethylenetriamine；
And/or,
In step 2, the mass ratio of the cross-linked polyurethane after the quality of described crosslinking agent and described chain extension
Be worth is 0.02~0.1；
And/or,
In step 2, the temperature of described cross-linking reaction is 50 DEG C~100 DEG C；
And/or,
In step 2, the time of described cross-linking reaction is 2 hours~6 hours；
And/or,
In step 3, described solvent is ketones solvent and/or ether solvent；
And/or,
In step 3, the mass values of the cross-linked polyurethane after described solvent and described chain extension are
0.30~1.2；
And/or,
In step 3, the solid content of described cross-linked polyurethane dispersion is 15%~45%；
And/or,
In step 3, the temperature of described dispersion and emulsion is 0 DEG C~50 DEG C；
And/or,
In step 3, the time of described dispersion and emulsion is 1 hour~2 hours；
And/or,
In step 3, described dispersion and emulsion is carried out under conditions of stirring.
6. the preparation method of fixation aqueous polyurethane dispersion as claimed in claim 5, its feature
It is：In step 2, described trimethylolpropane polyglycol ether hydroxyl value is 423 milligrams KOH/ grams,
Acid number is 0.1~1.2 milligram KOH/ grams；
And/or,
In step 2, the mass ratio of the cross-linked polyurethane after the quality of described crosslinking agent and described chain extension
Be worth is 0.035~0.091；
And/or,
In step 2, the temperature of described cross-linking reaction is 60 DEG C~70 DEG C；
And/or,
In step 2, the time of described cross-linking reaction is 4 hours；
And/or,
In step 3, described ketones solvent is acetone；
And/or,
In step 3, described ether solvent is tetrahydrofuran；
And/or,
In step 3, the mass values of the cross-linked polyurethane after described solvent and described chain extension are
0.40~1.08；
And/or,
In step 3, the solid content of described cross-linked polyurethane dispersion is 18%~40%；
And/or,
In step 3, the temperature of described dispersion and emulsion is 0 DEG C~20 DEG C；
And/or,
When the dispersion and emulsion described in step 3 under conditions of stirring when carrying out, the speed of described stirring
It is 1000 revs/min~1500 revs/min.
7. the preparation method of fixation aqueous polyurethane dispersion as claimed in claim 1, its feature
It is：In step 4, described diamines is ethylenediamine, piperazine, diethanol amine and N- methyl diethanols
One or more in amine；
And/or,
In step 4, described diamines is with the mass values of described fixation aqueous polyurethane dispersion
0.01~0.10；
And/or,
In step 4, described diamines uses two amine aqueous solutions；
And/or,
In step 4, described chain extending reaction is carried out under agitation；
And/or,
In step 4, the temperature of described chain extending reaction is 0 DEG C~50 DEG C；
And/or,
In step 4, the time of described chain extending reaction is 0.5 hour~1.5 hours；
And/or,
In step 5, described Amino End Group silane coupler is Amino End Group Silane coupling agent KH550；
And/or,
In step 5, the matter of the cross-linked polyurethane after described Amino End Group silane coupler and described chain extension
Amount ratio is 0.03~0.10；
And/or,
In step 5, the temperature of described end capping reaction is 10 DEG C~50 DEG C；
And/or,
In step 5, the time of described end capping reaction is 0.5 hour~2.5 hours.
8. the preparation method of fixation aqueous polyurethane dispersion as claimed in claim 7, its feature
It is：In step 4, the mass values of described diamines and described fixation aqueous polyurethane dispersion
It is 0.03~0.07；
And/or, when the diamines described in the step 4 uses two amine aqueous solutions, described two amine aqueous solutions
Mass concentration is 35%~45%, and described mass concentration refers to that the quality of diamines accounts for the total matter of two amine aqueous solutions
The percentage of amount；
And/or,
When chain extending reaction described in the step 4 is carried out under agitation, the speed of described stirring is
500 revs/min~1000 revs/min；
And/or,
In step 4, the temperature of described chain extending reaction is 0 DEG C~20 DEG C；
And/or,
In step 4, the time of described chain extending reaction is 1 hour；
And/or,
In step 5, the matter of the cross-linked polyurethane after described Amino End Group silane coupler and described chain extension
Amount ratio is 0.039~0.081；
And/or,
In step 5, the temperature of described end capping reaction is 35 DEG C~50 DEG C；
And/or,
In step 5, the time of described end capping reaction is 1 hour.
9. the preparation method of the fixation aqueous polyurethane dispersion as described in any one of claim 1~8
Obtained fixation aqueous polyurethane dispersion.
10. fixation aqueous polyurethane dispersion as claimed in claim 9 as color fixing agent application.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101818458A (en) * | 2009-12-15 | 2010-09-01 | 深圳天鼎精细化工制造有限公司 | Organosilicon modified polyurethane hyperchromic improver and preparation method thereof |
| CN101875253A (en) * | 2009-04-28 | 2010-11-03 | 大连路明发光科技股份有限公司 | Water-proof self-luminous printing film |
| CN101914857A (en) * | 2010-08-04 | 2010-12-15 | 辽宁恒星精细化工有限公司 | Method for preparing reactive polyurethane film-forming color fixing agent |
| CN102766246A (en) * | 2012-08-07 | 2012-11-07 | 丁军 | Waterborne polyurethane resin for shoe material ink |
| CN103709364A (en) * | 2013-12-27 | 2014-04-09 | 福建清源科技有限公司 | Preparation method of quaternary ammonium salt chitosan and organic silicon composite modified cationic water-based polyurethane fixing agent |
| CN105113255A (en) * | 2015-09-07 | 2015-12-02 | 杭州美高华颐化工有限公司 | Organosilicone modification polyurethane color fixing agent and preparation method thereof |
-
2015
- 2015-12-21 CN CN201510967560.9A patent/CN106893065A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101875253A (en) * | 2009-04-28 | 2010-11-03 | 大连路明发光科技股份有限公司 | Water-proof self-luminous printing film |
| CN101818458A (en) * | 2009-12-15 | 2010-09-01 | 深圳天鼎精细化工制造有限公司 | Organosilicon modified polyurethane hyperchromic improver and preparation method thereof |
| CN101914857A (en) * | 2010-08-04 | 2010-12-15 | 辽宁恒星精细化工有限公司 | Method for preparing reactive polyurethane film-forming color fixing agent |
| CN102766246A (en) * | 2012-08-07 | 2012-11-07 | 丁军 | Waterborne polyurethane resin for shoe material ink |
| CN103709364A (en) * | 2013-12-27 | 2014-04-09 | 福建清源科技有限公司 | Preparation method of quaternary ammonium salt chitosan and organic silicon composite modified cationic water-based polyurethane fixing agent |
| CN105113255A (en) * | 2015-09-07 | 2015-12-02 | 杭州美高华颐化工有限公司 | Organosilicone modification polyurethane color fixing agent and preparation method thereof |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107513872A (en) * | 2017-08-14 | 2017-12-26 | 盐城福汇纺织有限公司 | It is a kind of be exclusively used in washing, the mixed base dyeing technique of silk blend looped fabric |
| CN109629269A (en) * | 2018-11-20 | 2019-04-16 | 烟台大学 | A kind of suede color fixing agent and its preparation method and application |
| CN109629269B (en) * | 2018-11-20 | 2021-09-17 | 烟台大学 | Suede leather color fixing agent and preparation method and application thereof |
| CN109503801A (en) * | 2018-11-30 | 2019-03-22 | 西安工程大学 | Dacron Non-water washing continuous exhaust dyeing waterborne polyurethane resin synthetic method |
| CN110540630A (en) * | 2019-10-08 | 2019-12-06 | 刘军 | Novel waterborne polyurethane composition and preparation method thereof |
| CN110540630B (en) * | 2019-10-08 | 2021-12-24 | 刘军 | Waterborne polyurethane composition and preparation method thereof |
| CN110951040A (en) * | 2019-12-06 | 2020-04-03 | 嘉兴学院 | Cationic waterborne polyurethane leather color fixing agent and preparation method thereof |
| CN110951040B (en) * | 2019-12-06 | 2022-04-12 | 嘉兴学院 | Cationic waterborne polyurethane leather color fixing agent and preparation method thereof |
| CN112175165A (en) * | 2020-09-27 | 2021-01-05 | 西安工程大学 | Preparation method of novel wet rubbing fastness improver |
| CN112250833A (en) * | 2020-10-23 | 2021-01-22 | 万桦（常州）新材料科技有限公司 | Synthetase and fabric color fixing method |
| CN112341594A (en) * | 2020-10-30 | 2021-02-09 | 西安工程大学 | Preparation method of waterborne polyurethane color fixing agent |
| CN115612055A (en) * | 2022-10-11 | 2023-01-17 | 江苏富淼科技股份有限公司 | Solvent-free self-emulsified water-washing-resistant softening agent, and preparation method and application thereof |
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Application publication date: 20170627 |