CN106638042B - Dyed fabric increases deep finishing agent and preparation method - Google Patents
Dyed fabric increases deep finishing agent and preparation method Download PDFInfo
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- CN106638042B CN106638042B CN201610870107.0A CN201610870107A CN106638042B CN 106638042 B CN106638042 B CN 106638042B CN 201610870107 A CN201610870107 A CN 201610870107A CN 106638042 B CN106638042 B CN 106638042B
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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
- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5207—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- D06P1/525—Polymers of unsaturated carboxylic acids or functional derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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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
- C08G18/4829—Polyethers containing at least three hydroxy groups
-
- 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
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6688—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3271
-
- 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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/73—Polyisocyanates or polyisothiocyanates acyclic
-
- 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
- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5264—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
- D06P1/5285—Polyurethanes; Polyurea; Polyguanides
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Coloring (AREA)
Abstract
Dyed fabric of the present invention increases deep finishing agent and preparation method, by polypropylene oxide triol, N methyldiethanol amine, hexamethylene diisocyanate, acetone, acetoxime, dimethyl suflfate, glacial acetic acid, sodium hydrogensulfite, deionized water, watersoluble closed property polyurethane resin made from dibutyl tin laurate with by methyl acrylate, acrylonitrile, dimethylaminoethyl methacrylate, trifluoroethyl methacrylate, hydroxy-ethyl acrylate, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, azo-bis-isobutyrate hydrochloride, water-based acrylic resin mixture made from deionized water is made.And anti-slippage, resistant slide, colour fixation are good.
Description
Technical field
The present invention relates to the increasing depth finishing agents for dyed cotton fabric or dyeing chemical & blended fabric, are a kind of watersoluble closed
Property the dyed fabric that mixes of polyurethane resin and water-based acrylic resin increase deep finishing agent.
Background technology
The increasing depth finishing agent of dyed fabric is that organic silicon increases deep finishing agent mostly at present.
CN101956324B " dyed cotton fabric increases the gorgeous finishing agent of deep increasing and preparation method ", discloses a kind of poly-organosilicon
Oxygen alkane lotion and Methyl Hydrogen Polysiloxane Fluid lotion 100:The dyed cotton fabric that 5-10 is mixed increases the deep gorgeous finishing agent of increasing.
《Printing and dyeing assistant》Magazine 01 phase in 2004, Xie Hongde have been delivered " preparation and its application study of deep-dyeing agent ", are proposed
Methyltrimethoxysilane sun/nonionic surfactant in the presence of, passes through emulsion polymerization and average grain is made with KH-560
0.31 μm of diameter or less, the translucent organic sesqui siloxane dispersion liquid dispersion liquids with blue light again with it is epoxychloropropane modified
Amino silicon oil emulsion compounds, and dyed fabric is made and increases deep finishing agent.
《Printing and dyeing assistant》Magazine 08 phase in 2009, Yang Zhuo, Ge Fengyan etc. have delivered that " organosilicon grinds cotton fabric effect
Study carefully ", it is proposed that dyed cotton fabric is carried out using amido organosilicon lotion and increases deep arrange.
Since organosilicon is typically the product by octamethylcy-clotetrasiloxane ring-opening polymerisation.And octamethylcy-clotetrasiloxane
Refractive index relatively low 1.396.The lower deep effect of substance increasing of refractive index is more apparent, and organosilicon has preferable darkening effect, but
It is that the polarity of organosilicon is weak, surface tension is small, surface energy is low, smooth, although increasing deep effect with preferable, be easy to cause
Fiber slippage, slippage, are especially used for the arrangement of dacron, and sliding, slippage become apparent.
Invention content
The object of the present invention is to provide it is a kind of have increase with the good dyed fabric of anti-slippage, resistant slide, tint retention it is deep whole
Manage agent and preparation method.
Dyed fabric of the present invention increases deep finishing agent, is a kind of watersoluble closed property polyurethane resin and water-based acrylic resin group
Increase deep finishing agent made of conjunction, that is, consists of two parts：
First, watersoluble closed property polyurethane resin；
Second is that water-based acrylic resin.
Dyed fabric of the present invention increase deep finishing agent, i.e., watersoluble closed property polyurethane resin and water-based acrylic resin combination and
At the deep finishing agent of increasing preparation method：
Component A：The preparation of watersoluble closed property polyurethane resin
Raw material mass mixture ratio：
60-120 parts of polypropylene oxide triol number average molecular weight 3000
10-30 parts of N methyldiethanol amine
30-80 parts of hexamethylene diisocyanate
30-60 parts of acetone
6-20 parts of acetoxime
10-30 parts of dimethyl suflfate
8-16 parts of glacial acetic acid
1.5-6.0 parts of sodium hydrogensulfite
200-600 parts of deionized water
0.05-0.5 parts of dibutyl tin laurate
Preparation method：
(1) polypropylene oxide triol, N methyldiethanol amine, hexamethylene diisocyanate, acetone, tin dilaurate two
Butyl tin is added in reaction kettle, is warming up to 60-80 DEG C, is reacted 4.5-5.5 hours；
(2) acetoxime is added, reacts 2.5-3.5 hours at 60-80 DEG C, then；
(3) dimethyl suflfate is added, is reacted 20-40 minutes at 60-80 DEG C；
(4) in blowing to emulsifying kettle, 20-40 DEG C is cooled to, is stirred evenly in acetic acid to emulsifying kettle on the rocks；
(5) sodium hydrogensulfite is dissolved in deionized water, is added in emulsifying kettle together, stirring and emulsifying is completed after emulsifying again
Stirring 30-40 minutes filters blowing, obtains watersoluble closed property polyurethane resin.
Component：The preparation of water-based acrylic resin
Raw material mass mixture ratio：
50-100 parts of methyl acrylate
0-10 parts of acrylonitrile
6-20 parts of dimethylaminoethyl methacrylate
10-30 parts of trifluoroethyl methacrylate
2-10 parts of hydroxy-ethyl acrylate
10-30 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
0.6-1.5 parts of azo-bis-isobutyrate hydrochloride
300-800 parts of deionized water
Preparation method：
(1) by methyl acrylate, acrylonitrile, dimethylaminoethyl methacrylate, trifluoroethyl methacrylate, propylene
Sour hydroxyl ethyl ester, which is added in dropping funel, is stirred into monomer mixed solution, for use；
(2) above-mentioned deionized water, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride are added in reaction kettle, stirring and dissolving first
Base acrylyl oxy-ethyl-trimethyl salmiac；
(3) it is warming up to 60-70 DEG C of addition azo-bis-isobutyrate hydrochloride, then in 60-70 DEG C of a dropping step (1) dropping liquid
Monomer mixed solution in funnel is added dropwise for 60-80 minutes, is warming up to 75-85 DEG C, reacts 60-120 minutes；
(4) 20-40 DEG C is cooled to, blowing is filtered, obtains water-based acrylic resin.
The dyed fabric that watersoluble closed property polyurethane resin and water-based acrylic resin are composed increases matching for deep finishing agent
System（By quality proportioning）；
The watersoluble closed property polyurethane resin component B water-based acrylic resins of component A=30-100 30-100 mixing is equal
Even, the dyed fabric that as watersoluble closed property polyurethane resin and water-based acrylic resin are composed increases deep finishing agent.
Dyed fabric of the present invention increases deep finishing agent, is a kind of watersoluble closed property polyurethane resin and water-based acrylic resin group
Dyed fabric made of conjunction increases deep finishing agent, and being that a kind of heat reactivity resin type dyed fabric increasing without organosilicon is deep arranges
Agent.
Dyed fabric of the present invention increases deep finishing agent and contains heat reactivity polyurethane resin（I.e. containing closure isocyanates
Polyurethane resin）To fixation, improves dry and wet fastness of rubbing and have apparent contribution.It more importantly solves organosilicon deep-dyeing agent easily to make
At fabric fibre sliding, slippage problem.Because the polyurethane resin containing closure isocyanates, is crosslinked during heating
Film forming, solid yarn, fixation in being crosslinked film forming procedure avoid slippage, the sliding of fabric fibre.
The present invention selects the lower raw material of refractive index, and adds two kinds of isocyanate blocking agents, acetoxime and sulfurous acid
Hydrogen sodium, manufactured dyed fabric increase deep finishing agent, sulfur dioxide gas and acetoxime steam, meeting are discharged in heating film forming procedure
Micro- hole is formed on the surface of film, reduces the refractive index of light, achievees the purpose that increase depth, refractive index is lower, and darkening effect is more apparent.
Dyed fabric of the present invention increases deep finishing agent, is a kind of watersoluble closed property polyurethane resin and water-based acrylic resin group
Dyed fabric deep-dyeing agent made of conjunction, increasing is deep with obvious effects, and will not cause fiber slippage, sliding, also tint retention.
Specific implementation mode
Embodiment 1, the preparation of the watersoluble closed property polyurethane resin of component A：
(1) polypropylene oxide triol（Number average molecular weight 3000）120 parts, 26 parts of N methyldiethanol amine, six methylenes
70.2 parts of group diisocyanate, 55 parts of acetone, 0.4 part of dibutyl tin laurate, are added in reaction kettle, are warming up to 65 DEG C,
65 DEG C are reacted 5.5 hours；
(2) 16 parts of acetoxime is added, reacts 3.5 hours at 65 DEG C, then；
(3) 25 parts of dimethyl suflfate is added, is reacted 40 minutes at 65 DEG C；
(4) 20 DEG C are cooled in blowing to emulsifying kettle, is stirred evenly in 13 parts of acetic acid on the rocks to emulsifying kettle；
(5) 5.8 parts of sodium hydrogensulfite is added in 560 parts of deionized water and is uniformly dissolved, is added in emulsifying kettle together, stirred
Emulsification is stirred for 40 minutes after completing emulsification, is filtered blowing, is obtained watersoluble closed property polyurethane resin A1.
It is prepared by embodiment 2, the watersoluble closed property polyurethane resin of component A：
(1) polypropylene oxide triol（Number average molecular weight 3000）62 parts, it is 11.9 parts of N methyldiethanol amine, six sub-
33 parts of methyl diisocyanate, 30 parts of acetone, 0.06 part of dibutyl tin laurate, are added in reaction kettle, are warming up to 75 DEG C,
It is reacted 5 hours at 75 DEG C；
(2) 7.6 parts of acetoxime is added, reacts 3 hours at 75 DEG C, then；
(3) 11 parts of dimethyl suflfate is added, is reacted 30 minutes at 75 DEG C；
(4) 25 DEG C are cooled in blowing to emulsifying kettle, is stirred evenly in 8 parts of acetic acid on the rocks to emulsifying kettle；
(5) 3 parts of sodium hydrogensulfite is added in 280 parts of deionized water and is uniformly dissolved, is added in emulsifying kettle together, stirring breast
Change, be stirred for 35 minutes after completing emulsification, filters blowing, obtain watersoluble closed property polyurethane resin A2.
It is prepared by embodiment 3, the watersoluble closed property polyurethane resin of component A：
(1) polypropylene oxide triol（Number average molecular weight 3000）100 parts, 20 parts of N methyldiethanol amine, six methylenes
55 parts of group diisocyanate, 40 parts of acetone, 0.3 part of dibutyl tin laurate, are added in reaction kettle, 70 DEG C are warming up to, 70
DEG C reaction 5.5 hours；
(2) 12.7 parts of acetoxime is added, reacts 3 hours at 70 DEG C, then；
(3) 20 parts of dimethyl suflfate is added, is reacted 40 minutes at 70 DEG C；
(4) 35 DEG C are cooled in blowing to emulsifying kettle, is stirred evenly in 11 parts of acetic acid on the rocks to emulsifying kettle；
(5) 4.6 parts of sodium hydrogensulfite is added in 450 parts of deionized water and is uniformly dissolved, is added in emulsifying kettle together, stirred
Emulsification is stirred for after forty minutes, filtering blowing, obtaining watersoluble closed property polyurethane resin A3 after completing emulsification.
It is prepared by embodiment 4, the watersoluble closed property polyurethane resin of component A：
(1) polypropylene oxide triol（Number average molecular weight 3000）90 parts, 10 parts of N methyldiethanol amine, six methylenes
32.6 parts of group diisocyanate, 45 parts of acetone, 0.08 part of dibutyl tin laurate, are added in reaction kettle, are warming up to 75 DEG C,
It is reacted 4.5 hours at 75 DEG C；
(2) 7.6 parts of acetoxime is added, reacts 3.5 hours at 75 DEG C, then；
(3) 10 parts of dimethyl suflfate is added, is reacted 30 minutes at 75 DEG C；
(4) 30 DEG C are cooled in blowing to emulsifying kettle, is stirred evenly in 8 parts of acetic acid on the rocks to emulsifying kettle；
(5) 2.8 parts of sodium hydrogensulfite is added in 350 parts of deionized water and is uniformly dissolved, is added in emulsifying kettle together, stirred
Emulsification is completed after being stirred for 35 minutes after emulsifying, filters blowing, obtain watersoluble closed property polyurethane resin A4.
It is prepared by embodiment 5, the watersoluble closed property polyurethane resin of component A：
(1) polypropylene oxide triol（Number average molecular weight 3000）70 parts, 22 parts of N methyldiethanol amine, six methylenes
55.4 parts of group diisocyanate, 40 parts of acetone, 0.2 part of dibutyl tin laurate, are added in reaction kettle, are warming up to 68 DEG C,
It is reacted 5 hours at 68 DEG C；
(2) 12.8 parts of acetoxime is added, reacts 3.5 hours at 68 DEG C, then；
(3) 21 parts of dimethyl suflfate is added, is reacted 40 minutes at 68 DEG C；
(4) 35 DEG C are cooled in blowing to emulsifying kettle, is stirred evenly in 11.1 parts of acetic acid on the rocks to emulsifying kettle；
(5) 4.7 parts of sodium hydrogensulfite is added to after being uniformly dissolved in 370 parts of deionized water, is added in emulsifying kettle, stirs together
Emulsification is mixed, is stirred for after forty minutes, filtering blowing, obtaining watersoluble closed property polyurethane resin A5 after completing emulsification.
It is prepared by embodiment 6, B component water-based acrylic resin：
(1) by 80 parts of methyl acrylate, 6 parts of acrylonitrile, 12 parts of dimethylaminoethyl methacrylate, methacrylic acid three
12 parts of fluorine ethyl ester, 6 parts of hydroxy-ethyl acrylate, is added in dropping funel and is stirred into monomer mixed solution, for use；
(2) it by 23 parts of 560 parts of deionized water and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, is added in reaction kettle, stirs
Mix dissolving MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride；
(3) 63 ± 3 DEG C are warming up to, 1.1 parts of azo-bis-isobutyrate hydrochloride is added, then in 63 ± 3 DEG C of a dropping steps (1)
Monomer mixed solution in dropping funel is added dropwise for 60-80 minutes, is warming up to 78 ± 3 DEG C and reacts 60 minutes；
(4) after cooling to 40 DEG C, blowing is filtered, water-based acrylic resin B1 is obtained.
It is prepared by embodiment 7, B component water-based acrylic resin：
(1) by 100 parts of methyl acrylate, 16 parts of dimethylaminoethyl methacrylate, trifluoroethyl methacrylate 18
Part, 9 parts of hydroxy-ethyl acrylate is added in dropping funel and is stirred into monomer mixed solution, for use；
(2) it by 29 parts of 700 parts of deionized water and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, is added in reaction kettle, stirs
Mix dissolving MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride；
(3) 65 ± 3 DEG C are warming up to, 1.4 parts of azo-bis-isobutyrate hydrochloride is added, then in 65 ± 3 DEG C of a dropping steps (1)
Monomer mixed solution in dropping funel is added dropwise for 60-80 minutes, is warming up to 80 ± 3 DEG C and reacts 70 minutes；
（4）After cooling to 35 DEG C, blowing is filtered, water-based acrylic resin B2 is obtained.
It is prepared by embodiment 8, B component water-based acrylic resin：
(1) by 60 parts of methyl acrylate, 8 parts of acrylonitrile, 11 parts of dimethylaminoethyl methacrylate, methacrylic acid three
11 parts of fluorine ethyl ester, 3 parts of hydroxy-ethyl acrylate, is added in dropping funel and stirs evenly into monomer mixed solution, for use；
(2) it by 16 parts of 440 parts of deionized water and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, is added in reaction kettle, stirs
Mix dissolving MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride；
(3) 66 ± 3 DEG C are warming up to, 0.8 part of azo-bis-isobutyrate hydrochloride is added, then in 66 ± 3 DEG C of a dropping steps
(1) monomer mixed solution in dropping funel is added dropwise for 60-80 minutes, is warming up to 79 ± 3 DEG C and reacts 80 minutes；
(4) after cooling to 30 DEG C, blowing is filtered, water-based acrylic resin B3 is obtained.
It is prepared by embodiment 9, B component water-based acrylic resin：
(1) by 98 parts of methyl acrylate, 9 parts of acrylonitrile, 19 parts of dimethylaminoethyl methacrylate, methacrylic acid three
25 parts of fluorine ethyl ester, 8 parts of hydroxy-ethyl acrylate, is added in dropping funel and stirs evenly into monomer mixed solution, for use；
(2) it by 28 parts of 760 parts of deionized water and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, is added in reaction kettle, stirs
Mix dissolving MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride；
(3) 64 ± 3 DEG C are warming up to, 1.5 parts of azo-bis-isobutyrate hydrochloride is added, then in 64 ± 3 DEG C of a dropping steps
(1) monomer mixed solution in dropping funel is added dropwise for 60-80 minutes, is warming up to 81 ± 3 DEG C and reacts 100 minutes；
（4）After cooling to 25 DEG C, blowing is filtered, water-based acrylic resin B4 is obtained.
It is prepared by embodiment 10, B component water-based acrylic resin：
(1) by 50 parts of methyl acrylate, 9 parts of acrylonitrile, 16 parts of dimethylaminoethyl methacrylate, methacrylic acid three
21 parts of fluorine ethyl ester, 3 parts of hydroxy-ethyl acrylate, is added in dropping funel and stirs evenly into monomer mixed solution, for use；
(2) it by 16 parts of 450 parts of deionized water and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, is added in reaction kettle, stirs
Mix dissolving MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride；
(3) 67 ± 3 DEG C are warming up to, 0.6 part of azo-bis-isobutyrate hydrochloride is added, then in 67 ± 3 DEG C of a dropping steps
(1) monomer mixed solution in dropping funel is added dropwise for 60-80 minutes, is warming up to 80 ± 3 DEG C and reacts 120 minutes；
(4) after 20 DEG C of cooling, blowing is filtered, water-based acrylic resin B5 is obtained.
Test experience：
Dyed fabric increases deep finishing agent（The dyeing that watersoluble closed property polyurethane resin and water-based acrylic resin are composed
Fabric increases deep finishing agent）It prepares, is prepared by mass fraction, is uniformly mixed：
Test example 1
Watersoluble closed property polyurethane resin A1：100 parts
Water-based acrylic resin B1：50 parts.
Test example 2
Watersoluble closed property polyurethane resin A2：60 parts
Water-based acrylic resin B2：80 parts.
Test example 3
Watersoluble closed property polyurethane resin A3：40 parts
Water-based acrylic resin B3：100 parts.
Test example 4
Watersoluble closed property polyurethane resin A4：100 parts
Water-based acrylic resin B4：100 parts.
Test example 5
Watersoluble closed property polyurethane resin A5：100 parts
Water-based acrylic resin B5：70 parts.
Examination example tests 6
Watersoluble closed property polyurethane resin A1：100 parts
Water-based acrylic resin B2：60 parts.
Test example 7
Watersoluble closed property polyurethane resin A2：60 parts
Water-based acrylic resin B3：80 parts.
Test example 8
Watersoluble closed property polyurethane resin A3：30 parts
Water-based acrylic resin B5：100 parts.
Test example 9
Watersoluble closed property polyurethane resin A1：100 parts
Water-based acrylic resin B4：100 parts.
Test example 10
Watersoluble closed property polyurethane resin A5：100 parts
Water-based acrylic resin B1：30 parts.
Processing 1 is padded in experiment：
Base fabric:Black terylene fabric（190T black polyester pongees）
Technique：Increase deep finishing agent with the dyed fabric that test example 1-10 is obtained, is made into padding finishing working solution respectively
40g/L, respectively to base fabric carry out an immersing and rolling, pick-up rate 80%, 100~120 DEG C dry 1 minute → bake (160~170
DEG C 1~2 minute), take cloth specimen to detect.
Testing result tabulated below 1
。
Processing 2 is padded in experiment：
Base fabric:Black pure cotton fabric（40 × 40/133 × 72 black jeans）
Technique：Increase deep finishing agent with the dyed fabric that test example 1-10 is obtained, is made into padding finishing working solution respectively
40g/L, respectively to base fabric carry out an immersing and rolling, pick-up rate 80%, 100~120 DEG C dry 1 minute → bake（160~170
DEG C × 1~2 minute）, cloth specimen is taken to detect.
Testing result is included in table 2
1, blackness：Visual method detects；
2, fabric is done, fastness to wet rubbing detects：By GB/T 3920-2008 standard detections；
3, the measurement of textile woven fabric seam crossing yarn resistant slide：By GB/T 13772.2-2008 standard detections.
As can be seen from Table 1 and Table 2, dyed fabric of the present invention, which increases deep finishing agent, has fine darkening effect, passes through range estimation
Just there are positive effect, resistant slide apparent.Especially test example 1 and 10, because watersoluble closed property polyurethane resin content is higher,
1 watersoluble closed property polyurethane resin of test example accounts for 66.67%, and 10 watersoluble closed property polyurethane resin of test example accounts for 76.92%, aqueous
Closure polyurethane resin is thermal response polyurethane resin, is crosslinked during heating, by the solid yarn of crosslinking, so anti-slipping property
Better than other test example anti-slipping properties.The sliding of fabric after usual organosilicon deep-dyeing agent arrangement is more than blank cloth（I.e.
Unfinished cloth specimen）This is that those skilled in the art are known.
Claims (2)
1. dyed fabric increases deep finishing agent preparation method, it is characterized in that：
It is composed of watersoluble closed property polyurethane resin and water-based acrylic resin；
Component A：The preparation of watersoluble closed property polyurethane resin
Raw material mass mixture ratio：
60-120 parts of polypropylene oxide triol number average molecular weight 3000
10-30 parts of N methyldiethanol amine
30-80 parts of hexamethylene diisocyanate
30-60 parts of acetone
6-20 parts of acetoxime
10-30 parts of dimethyl suflfate
8-16 parts of glacial acetic acid
1.5-6.0 parts of sodium hydrogensulfite
200-600 parts of deionized water
0.05-0.5 parts of dibutyl tin laurate
Preparation method：
(1) polypropylene oxide triol, N methyldiethanol amine, hexamethylene diisocyanate, acetone, di lauric dibutyl
Tin is added in reaction kettle, is warming up to 60-80 DEG C, is reacted 4.5-5.5 hours；
(2) acetoxime is added, reacts 2.5-3.5 hours at 60-80 DEG C, then；
(3) dimethyl suflfate is added, is reacted 20-40 minutes at 60-80 DEG C；
(4) in blowing to emulsifying kettle, 20-40 DEG C is cooled to, is stirred evenly in acetic acid to emulsifying kettle on the rocks；
(5) sodium hydrogensulfite is dissolved in deionized water, is added in emulsifying kettle together, stirring and emulsifying is stirred for after completing emulsification
30-40 minutes, blowing is filtered, watersoluble closed property polyurethane resin is obtained；
B component：The preparation of water-based acrylic resin
Raw material mass mixture ratio：
50-100 parts of methyl acrylate
0-10 parts of acrylonitrile
6-20 parts of dimethylaminoethyl methacrylate
10-30 parts of trifluoroethyl methacrylate
2-10 parts of hydroxy-ethyl acrylate
10-30 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
0.6-1.5 parts of azo-bis-isobutyrate hydrochloride
300-800 parts of deionized water
Preparation method：
(1) by methyl acrylate, acrylonitrile, dimethylaminoethyl methacrylate, trifluoroethyl methacrylate, acrylic acid hydroxyl
Ethyl ester, which is added in dropping funel, is stirred into monomer mixed solution, for use；
(2) above-mentioned deionized water, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride are added in reaction kettle, stirring and dissolving methyl-prop
Alkene acyloxyethyl trimethyl ammonium chloride；
(3) it is warming up to 60-70 DEG C of addition azo-bis-isobutyrate hydrochloride, then in 60-70 DEG C of a dropping step (1) dropping funel
In monomer mixed solution, be added dropwise within 60-80 minutes, be warming up to 75-85 DEG C, react 60-120 minutes；
(4) 20-40 DEG C is cooled to, blowing is filtered, obtains water-based acrylic resin；
The watersoluble closed property polyurethane resin B component water-based acrylic resin=30-100 30-100 of component A, mixture.
2. the dyed fabric as claim 1 preparation method obtains increases deep finishing agent.
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| CN101638471A (en) * | 2009-09-01 | 2010-02-03 | 陕西科技大学 | Method for preparing water-base cation blocked polyisocyanates crosslinking and curing agent |
| CN102619106A (en) * | 2012-04-16 | 2012-08-01 | 辽宁恒星精细化工有限公司 | Real leather suede leather stereoscopic printing paste and preparation method |
| CN103233375A (en) * | 2013-05-04 | 2013-08-07 | 辽宁恒星精细化工有限公司 | Stereo printing paste for suede and preparation method thereof |
| CN103421158A (en) * | 2013-08-06 | 2013-12-04 | 陕西科技大学 | Preparation method and application method of fixation darkening agent used for dyeing superfine fiber synthetic leather |
| CN104074053A (en) * | 2014-06-27 | 2014-10-01 | 广东德美精细化工股份有限公司 | Efficient deep dyeing promoter, and preparation and after treatment application methods thereof |
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| CN101638471A (en) * | 2009-09-01 | 2010-02-03 | 陕西科技大学 | Method for preparing water-base cation blocked polyisocyanates crosslinking and curing agent |
| CN102619106A (en) * | 2012-04-16 | 2012-08-01 | 辽宁恒星精细化工有限公司 | Real leather suede leather stereoscopic printing paste and preparation method |
| CN103233375A (en) * | 2013-05-04 | 2013-08-07 | 辽宁恒星精细化工有限公司 | Stereo printing paste for suede and preparation method thereof |
| CN103421158A (en) * | 2013-08-06 | 2013-12-04 | 陕西科技大学 | Preparation method and application method of fixation darkening agent used for dyeing superfine fiber synthetic leather |
| CN104074053A (en) * | 2014-06-27 | 2014-10-01 | 广东德美精细化工股份有限公司 | Efficient deep dyeing promoter, and preparation and after treatment application methods thereof |
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