CN108341924A - A kind of preparation method of dye fixing agent - Google Patents
A kind of preparation method of dye fixing agent Download PDFInfo
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- CN108341924A CN108341924A CN201810137266.9A CN201810137266A CN108341924A CN 108341924 A CN108341924 A CN 108341924A CN 201810137266 A CN201810137266 A CN 201810137266A CN 108341924 A CN108341924 A CN 108341924A
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/6685—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 C08G18/3225 or polyamines of C08G18/38
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- C08G18/83—Chemically modified polymers
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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
- D06P1/5264—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
- D06P1/5285—Polyurethanes; Polyurea; Polyguanides
Abstract
The present invention relates to dye fixing agent technical fields, and in particular to a kind of preparation method of dye fixing agent.The present invention is by polypropylene glycol, polyethylene glycol is dehydrated, isophorone diisocyanate is added dropwise, it stirs evenly, the dibutyl tin laurate added is mixed, obtain mixture, by water soluble chitosan, distillation, water is mixed, stirring, again with mixture, deionized water is mixed, catalyst is added, acetone, 1, 4 butanediols, ethylenediamine base ethanesulfonic acid sodium solution, it stirs evenly, add deionized water, ethylenediamine, stirring, vacuum rotates, object must be rotated, by tetraethylenepentamine, epoxychloropropane, triethylamine, heating, heat preservation, finally and distilled water, rotate object mixing, stirring, up to dye fixing agent.The present invention solves current dye fixing agent and has a single function, and contains carboxymethyl, can release free formaldehyde, harmful problem when being more than certain value.
Description
Technical field
The present invention relates to dye fixing agent technical fields, and in particular to a kind of preparation method of dye fixing agent.
Background technology
Color fixing agent is one of the important auxiliary agent in dyeing.In recent years, with the development of science and technology, dyeing and finishing technique
Significant raising is obtained, the raising of expansion and people's living standard, environmental consciousness due to World Textile trade, it is desirable that weaving
Product are comfortable, clean, safety.From 20 century 70s, after Germany releases blue angels plan first, some are flourishing in the world
Country（Japan, U.S. etc.)）Relevant laws, regulation are passed in succession through and implemented, it is specified that the various indexs of textile.Green Textile Base
Product require to be forbidden to use in dyeing and printing process in the poor and certain aromatic amine of the carcinogenic of defined in regulation, teratogenesis and biological degradability
The dye material of mesosome production, while also requiring used auxiliary agent without heavy metal ion and not generating free formaldehyde, that is,
It uses " Green Additives ", it is by organic amine and epoxy chloropropionate that the exploitation and application of aldehyde-free colour stabilizer, which just meet this to require color fixing agent,
Polymerisation occurs for alkane, then is acidified with hydrochloric acid to obtain color fixing agent, its fixation for activity, directly, after sulfur dye dye cotton, energy
" bridge formation " forms compound between dyestuff and fiber, i.e., is reacted simultaneously with dye molecule, is crosslinked with cellulose fibre, forms height
Diversification cross-linking system makes dyestuff more firmly be combined with fiber, prevents dyestuff from falling off from fiber, improves dyefastness
Active material in color fixing agent can be mutually condensed, and form solid netted film in fiber surface, dyestuff is closed, cloth is increased
The smoothness in face reduces friction coefficient and is not easy to gall, the dyestuff occurred during wet friction is further prevented to be swollen, is molten
It solves, fall off, improve wet rubbing fastness.
After fabric is dyed, although bright fabric can be dyed, due to carrying water-soluble base on some dyestuffs
Group, keeps wet colour fastness poor, and fugitive color and staining keep fabric stale, can also be to other fabric staining, if leading to after textile dyeing
After crossing washing, soap boiling, washing, the color fastness of fabric cannot still reach requirement, then need to be handled with color fixing agent, be knitted to improve dyeing
The color fastness of object.Traditional color fixing agent contains carboxymethyl, can release free formaldehyde, harmful when being more than certain value, Gu
The effect of toner is so that dyestuff is formed dye salt not soluble in water, or dye molecule is made to increase and be insoluble in water, is contaminated so as to improving
The fastness of material.
In summary, nowadays color fixing agent is primarily present a few point defects below in the market：Traditional color fixing agent work(
Can be single, and contain carboxymethyl, free formaldehyde can be released, it is harmful when being more than certain value.
Therefore, we it is necessary to again prepare a kind of novel color fixing agent, nowadays consolidating in the market is solved with this
Technical bug present in toner is preferably adapted to people’s lives production requirement with this.
Invention content
The technical problems to be solved by the invention：It is had a single function for current dye fixing agent, and contains carboxymethyl, can released
Free formaldehyde is released, harmful problem, provides a kind of preparation method of dye fixing agent when being more than certain value.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of dye fixing agent, the preparation method include the following steps：
（1）In mass ratio 1：2, polypropylene glycol, polyethylene glycol are dehydrated at 100 ~ 120 DEG C of temperature, dehydrate is obtained, by dehydrate
It is put into container, is warming up to 40 ~ 50 DEG C, the isophorone diisocyanate of dehydration amount of substance 20 ~ 30% is added dropwise, stirs evenly, then
The dibutyl tin laurate that dehydration amount of substance 8 ~ 10% is added is mixed, and is stood at 50 ~ 60 DEG C of temperature, is obtained mixture；
（2）In mass ratio 1：0.5~0.6：5 ~ 6, water soluble chitosan, distillation, water are mixed, at 28 ~ 32 DEG C of temperature
Stirring, stirs evenly, obtains stirring liquid, in mass ratio 1：8 ~ 10, mixture, deionized water are mixed, stirred evenly, is added
The stirring liquid of mixture quality 1 ~ 2% stirs evenly at 28 ~ 32 DEG C of temperature, obtains mixing liquid；
（3）It counts in parts by weight, takes 50 ~ 60 parts liquid, 20 ~ 30 parts of deionized waters, 10 ~ 15 parts of acetone, 5 ~ 6 parts of second two are mixed
Amido ethanesulfonic acid sodium solution, 3 ~ 4 parts of 1,4-butanediol, 1 ~ 2 part of ethylenediamine, 0.1 ~ 0.2 part of catalyst will be mixed liquid, urge
Agent, acetone are mixed, and are kept at 70 ~ 80 DEG C of temperature, and 1,4-butanediol is added, and are stood 1 ~ 2h, are cooled to 30 ~ 35 DEG C,
Ethylenediamine base ethanesulfonic acid sodium solution is added, deionized water, ethylenediamine, stirring is added in stirring, and vacuum revolving obtains revolving object；
（4）Tetraethylenepentamine is put into container, is placed in 10 ~ 20 DEG C of water-baths of temperature, is stirred, dropwise addition tetraethylenepentamine quality 5 ~
6 times of epoxychloropropane, is warming up to 28 ~ 30 DEG C, and stirring is added dropwise the triethylamine of 1 ~ 1.2 times of tetraethylenepentamine quality, is warming up to 65
~ 70 DEG C, heat preservation obtains heat preservation object, in mass ratio 1：7 ~ 8, heat preservation object, distilled water are put into container and are mixed, temperature is placed in
In 10 ~ 20 DEG C of water-baths, the revolving object of heat preservation amount of substance 30 ~ 40% is added under stiring, adjusts pH value to 6 ~ 7, stirs to get dye
Expect color fixing agent.
The step（2）Middle distillation is in mass ratio 1：1.2：0.01, epoxidized soybean oil, isooctanol fluoboric acid are carried out
Mixing, 1 ~ 2h of oil bath at 98 ~ 100 DEG C of temperature, obtains mixture, in mass ratio 1：10 ~ 15, mixture, ethyl acetate are carried out
Mixing, is diluted to neutrality with deionized water, stands 3 ~ 4h, separate organic layer, and organic layer is carried out vacuum revolving, is evaporated under reduced pressure,
Up to distillation.
The step（3）Middle catalyst is stannous octoate.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention prepares aqueous polyurethane using polypropylene glycol, polyethylene glycol as raw material, and a large amount of ehter bonds deposits in polyurethane soft segment
Fixation agent molecule certain flexibility and elasticity are being imparted, is being knitted after being conducive to fixation treatment caused by improving color fixing agent segment
The shortcomings that object feel is deteriorated, while being blended using water soluble chitosan solution, by introducing hydrophilic segment in polyurethane
The penetrability of polyurethane is improved, to be further increased with the crosslinking degree of fiber molecule, what is generated between fiber is partial cross-linked
Cause wrinkle recovery angle of woven fabrics using viscoelasticity theory to have downward trend, there is certain crease-resistant function to make color fixing agent also, due also to the suction of chitosan
The distillation of absorption is modified polyurethane by attached effect, due to containing multiple hydroxyls on distillation molecule, to again
The crosslink density in polyurethane is improved, while adding the film forming containing cation group and chitosan, in drying course
In, color fixing agent can form one layer of protective film with some strength in fabric and fiber surface to be made coating dye on fiber
Be not easy split away off from fabric, and a part of hole of fabric can have been blocked, the transmission of ultraviolet light can be prevented, from
And color fixing agent has anti-ultraviolet function.
（2）The present invention prepares Polyamine Type color fixing agent with tetraethylenepentamine, epoxychloropropane, triethylamine, and is gathered using modified
Urethane is grafted, and so that color fixing agent is had both the double grading of Polyamine Type color fixing agent and polyurethane, the cationic quaternary ammonium group in segment
Color lake can be formed by electrostatical binding with the anionic group in reactive dyestuff molecule, enclose the water solubility in reactive dye
Group prevents molten in water-washing process of reactive dye to fall, and improves color fastness, and the polyurethane segment being grafted increases polyamines
The molecular mass of color fixing agent reduces the water solubility of polyamines fixation agent molecule, is conducive to promote colour fixation.Therefore, of the invention
There is crease-resistant, anti-ultraviolet function, no carboxymethyl will not be damaged to human body for dye fixing agent.
Specific implementation mode
Water soluble chitosan is by 1：10 ~ 15, the acetic acid solution of chitosan, volume fraction 2% is mixed, stirring is equal
It is even, the methanol of 10 ~ 15 times of chitosan mass is added, the acetic anhydride of chitosan 1 ~ 2% is added dropwise, is stored at room temperature 10 ~ 12h, adjusts pH value
It to 6 ~ 7, centrifuges, filtering, collection filtrate, in mass ratio 1：10 ~ 15, filtrate, absolute ethyl alcohol are subjected to mixed precipitation, centrifuges, receives
Collect sediment, sediment is washed 3 ~ 4 times with absolute ethyl alcohol, is dried in vacuo to get water soluble chitosan.
Distillation is in mass ratio 1：1.2：0.01, epoxidized soybean oil, isooctanol fluoboric acid are mixed, in temperature 98
1 ~ 2h of oil bath at ~ 100 DEG C, obtains mixture, in mass ratio 1：10 ~ 15, mixture, ethyl acetate are mixed, deionization is used
Water is diluted to neutrality, stands 3 ~ 4h, separates organic layer, and organic layer is carried out vacuum revolving, is evaporated under reduced pressure to get distillation.
Catalyst is stannous octoate.
A kind of preparation method of dye fixing agent, the preparation method include the following steps：
（1）In mass ratio 1：2, by polypropylene glycol, polyethylene glycol at 0.09 ~ 0.1 MPa of vacuum pressure, 100 ~ 120 DEG C of temperature
It is dehydrated 1 ~ 2h, dehydrate is obtained, dehydrate is put into container, is warming up to 40 ~ 50 DEG C, the different Buddhist of dehydration amount of substance 20 ~ 30% is added dropwise
That ketone diisocyanate, stirs evenly, and the dibutyl tin laurate for adding dehydration amount of substance 8 ~ 10% is mixed, in temperature
1 ~ 2h is stood at 50 ~ 60 DEG C of degree, obtains mixture；
（2）In mass ratio 1：0.5~0.6：5 ~ 6, water soluble chitosan, distillation, water are mixed, at 28 ~ 32 DEG C of temperature
Stirring 20 ~ for 24 hours, it stirs evenly, obtains stirring liquid, in mass ratio 1：8 ~ 10, mixture, deionized water are mixed, stirring is equal
It is even, the stirring liquid of mixture quality 1 ~ 2% is added, is stirred evenly at 28 ~ 32 DEG C of temperature, obtains mixing liquid；
（3）Count in parts by weight, take 50 ~ 60 parts be mixed liquid, 20 ~ 30 parts of deionized waters, 10 ~ 15 parts of acetone, 5 ~ 6 parts
0.1mol/L ethylenediamine base ethanesulfonic acids sodium solution, 3 ~ 4 parts of 1,4-butanediol, 1 ~ 2 part of ethylenediamine, 0.1 ~ 0.2 part of catalyst, will mix
Close stirring liquid, catalyst, acetone are mixed, keep 1 ~ 2h at 70 ~ 80 DEG C of temperature, 1,4-butanediol be added, stands 1 ~ 2h,
30 ~ 35 DEG C are cooled to, ethylenediamine base ethanesulfonic acid sodium solution is added, stirs 50 ~ 60min, deionized water, ethylenediamine is added, with 800
~ 900r/min stirs 8 ~ 10min, and vacuum revolving obtains revolving object；
（4）Tetraethylenepentamine is put into container, is placed in 10 ~ 20 DEG C of water-baths of temperature, 10 ~ 20min is stirred, four ethylene five are added dropwise
The epoxychloropropane that 5 ~ 6 times of amine quality is warming up to 28 ~ 30 DEG C, stirs 1 ~ 2h, and the three of 1 ~ 1.2 times of tetraethylenepentamine quality are added dropwise
Ethamine is warming up to 65 ~ 70 DEG C, keeps the temperature 4 ~ 5h, obtains heat preservation object, in mass ratio 1：7 ~ 8, heat preservation object, distilled water are put into container
It is mixed, is placed in 10 ~ 20 DEG C of water-baths of temperature, the revolving of heat preservation amount of substance 30 ~ 40% is added with stirring in 200 ~ 300r/min
Object adjusts pH value to 6 ~ 7,1 ~ 2h is stirred to get dye fixing agent with 800 ~ 900r/min.
Embodiment 1
Water soluble chitosan is by 1：10, the acetic acid solution of chitosan, volume fraction 2% is mixed, is stirred evenly, is added
The acetic anhydride of chitosan 1% is added dropwise in the methanol that 10 times of chitosan mass, is stored at room temperature 10h, adjusts pH value to 6, centrifuges, filtering,
Collection filtrate, in mass ratio 1：10, filtrate, absolute ethyl alcohol are subjected to mixed precipitation, centrifugation collects sediment, sediment is used
Absolute ethyl alcohol washs 3 times, is dried in vacuo to get water soluble chitosan.
Distillation is in mass ratio 1：1.2：0.01, epoxidized soybean oil, isooctanol fluoboric acid are mixed, in temperature 98
Oil bath 1h at DEG C obtains mixture, in mass ratio 1：10, mixture, ethyl acetate are mixed, in being diluted to deionized water
Property, 3h is stood, organic layer is separated, organic layer is subjected to vacuum revolving, is evaporated under reduced pressure to get distillation.
Catalyst is stannous octoate.
A kind of preparation method of dye fixing agent, the preparation method include the following steps：
（1）In mass ratio 1：2, polypropylene glycol, polyethylene glycol are dehydrated 1h at 0.09 MPa of vacuum pressure, 100 DEG C of temperature, obtained
Dehydrate is put into container by dehydrate, is warming up to 40 DEG C, and the isophorone diisocyanate of dehydration amount of substance 20% is added dropwise, stirs
Mix uniformly, add dehydration amount of substance 8% dibutyl tin laurate mixed, stand 1h under temperature 50 C, must mix
Object；
（2）In mass ratio 1：0.5：5, water soluble chitosan, distillation, water are mixed, 20h is stirred at 28 DEG C of temperature,
It stirs evenly, obtains stirring liquid, in mass ratio 1：8, mixture, deionized water are mixed, stirred evenly, compounding substances are added
The stirring liquid of amount 1% stirs evenly at 28 DEG C of temperature, obtains mixing liquid；
（3）It counts in parts by weight, takes 50 parts liquid, 20 parts of deionized waters, 10 parts of acetone, 5 parts of 0.1mol/L ethylenediamines are mixed
Base ethanesulfonic acid sodium solution, 3 parts of 1,4-butanediol, 1 part of ethylenediamine, 0.1 part of catalyst, will be mixed liquid, catalyst, acetone into
Row mixing, keeps 1h under temperature 70 C, and 1,4-butanediol is added, and stands 1h, is cooled to 30 DEG C, and ethylenediamine base ethanesulfonic acid is added
Sodium solution stirs 50min, and deionized water, ethylenediamine is added, and stirs 8min with 800r/min, vacuum revolving obtains revolving object；
（4）Tetraethylenepentamine is put into container, is placed in 10 DEG C of water-baths of temperature, 10min is stirred, tetraethylenepentamine quality is added dropwise
5 times of epoxychloropropane is warming up to 28 DEG C, stirs h, and the triethylamine of 1 times of tetraethylenepentamine quality is added dropwise, and is warming up to 65 DEG C, protects
Warm 4h obtains heat preservation object, in mass ratio 1：7, heat preservation object, distilled water are put into container and are mixed, 10 DEG C of water-baths of temperature are placed in
In, it is added with stirring the revolving object of heat preservation amount of substance 30% in 200r/min, pH value is adjusted to 6,1h is stirred with 800r/min, i.e.,
Obtain dye fixing agent.
Embodiment 2
Water soluble chitosan is by 1：12, the acetic acid solution of chitosan, volume fraction 2% is mixed, is stirred evenly, is added
The acetic anhydride of chitosan 1% is added dropwise in the methanol that 12 times of chitosan mass, is stored at room temperature 11h, adjusts pH value to 6.5, centrifuges, mistake
Filter, collection filtrate, in mass ratio 1：12, filtrate, absolute ethyl alcohol are subjected to mixed precipitation, centrifugation collects sediment, by sediment
It is washed 3 times, is dried in vacuo to get water soluble chitosan with absolute ethyl alcohol.
Distillation is in mass ratio 1：1.2：0.01, epoxidized soybean oil, isooctanol fluoboric acid are mixed, in temperature 99
Oil bath 1.5h at DEG C obtains mixture, in mass ratio 1：12, mixture, ethyl acetate are mixed, are diluted to deionized water
Neutrality stands 3.5h, separates organic layer, and organic layer is carried out vacuum revolving, is evaporated under reduced pressure to get distillation.
Catalyst is stannous octoate.
A kind of preparation method of dye fixing agent, the preparation method include the following steps：
（1）In mass ratio 1：2, polypropylene glycol, polyethylene glycol are dehydrated 1.5h at 0.09 MPa of vacuum pressure, 110 DEG C of temperature,
Dehydrate is obtained, dehydrate is put into container, is warming up to 45 DEG C, the isophorone diisocyanate of dehydration amount of substance 25% is added dropwise,
It stirs evenly, the dibutyl tin laurate for adding dehydration amount of substance 9% is mixed, and is stood 1.5h at 55 DEG C of temperature, is obtained
Mixture；
（2）In mass ratio 1：0.5：5, water soluble chitosan, distillation, water are mixed, 22h is stirred at 30 DEG C of temperature,
It stirs evenly, obtains stirring liquid, in mass ratio 1：9, mixture, deionized water are mixed, stirred evenly, compounding substances are added
The stirring liquid of amount 1.5% stirs evenly at 30 DEG C of temperature, obtains mixing liquid；
（3）It counts in parts by weight, takes 55 parts liquid, 25 parts of deionized waters, 12 parts of acetone, 5 parts of 0.1mol/L ethylenediamines are mixed
Liquid, catalyst, acetone will be mixed in base ethanesulfonic acid sodium solution, 3 parts of 1,4-butanediol, 1 part of ethylenediamine, 0.15 part of catalyst
It is mixed, 1h is kept at 75 DEG C of temperature, 1,4-butanediol is added, stand 1h, be cooled to 32 DEG C, ethylenediamine base second sulphur is added
Acid sodium solution stirs 55min, and deionized water, ethylenediamine is added, and stirs 9min with 850r/min, vacuum revolving obtains revolving object；
（4）Tetraethylenepentamine is put into container, is placed in 15 DEG C of water-baths of temperature, 15min is stirred, tetraethylenepentamine quality is added dropwise
5 times of epoxychloropropane is warming up to 29 DEG C, stirs 1h, and the triethylamine of 1.1 times of tetraethylenepentamine quality is added dropwise, is warming up to 68 DEG C,
4.5h is kept the temperature, heat preservation object, in mass ratio 1 are obtained：7.5, heat preservation object, distilled water are put into container and are mixed, temperature 15 is placed in
In DEG C water-bath, it is added with stirring the revolving object of heat preservation amount of substance 35% in 250r/min, pH value is adjusted to 6, is stirred with 850r/min
1.5h is to get dye fixing agent.
Embodiment 3
Water soluble chitosan is by 1：15, the acetic acid solution of chitosan, volume fraction 2% is mixed, is stirred evenly, is added
The acetic anhydride of chitosan 2% is added dropwise in the methanol that 15 times of chitosan mass, is stored at room temperature 12h, adjusts pH value to 7, centrifuges, filtering,
Collection filtrate, in mass ratio 1：15, filtrate, absolute ethyl alcohol are subjected to mixed precipitation, centrifugation collects sediment, sediment is used
Absolute ethyl alcohol washs 4 times, is dried in vacuo to get water soluble chitosan.
Distillation is in mass ratio 1：1.2：0.01, epoxidized soybean oil, isooctanol fluoboric acid are mixed, in temperature
Oil bath 2h at 100 DEG C, obtains mixture, in mass ratio 1：15, mixture, ethyl acetate are mixed, diluted with deionized water
To neutrality, 4h is stood, organic layer is separated, organic layer is subjected to vacuum revolving, is evaporated under reduced pressure to get distillation.
Catalyst is stannous octoate.
A kind of preparation method of dye fixing agent, the preparation method include the following steps：
（1）In mass ratio 1：2, polypropylene glycol, polyethylene glycol are dehydrated 2h at 0.1 MPa of vacuum pressure, 120 DEG C of temperature, obtained
Dehydrate is put into container by dehydrate, is warming up to 50 DEG C, and the isophorone diisocyanate of dehydration amount of substance 30% is added dropwise, stirs
Mix uniformly, add dehydration amount of substance 10% dibutyl tin laurate mixed, stand 2h under temperature 60 C, obtain mixed
Close object；
（2）In mass ratio 1：0.6：6, water soluble chitosan, distillation, water are mixed, stirred for 24 hours at 32 DEG C of temperature,
It stirs evenly, obtains stirring liquid, in mass ratio 1：10, mixture, deionized water are mixed, stirred evenly, mixture is added
The stirring liquid of quality 2% stirs evenly at 32 DEG C of temperature, obtains mixing liquid；
（3）It counts in parts by weight, takes 60 parts liquid, 30 parts of deionized waters, 15 parts of acetone, 6 parts of 0.1mol/L ethylenediamines are mixed
Base ethanesulfonic acid sodium solution, 4 parts of 1,4-butanediol, 2 parts of ethylenediamines, 0.2 part of catalyst, will be mixed liquid, catalyst, acetone into
Row mixing, keeps 2h at 80 DEG C of temperature, and 1,4-butanediol is added, and stands 2h, is cooled to 35 DEG C, and ethylenediamine base ethanesulfonic acid is added
Sodium solution stirs 60min, and deionized water, ethylenediamine is added, and stirs 10min with 900r/min, vacuum revolving obtains revolving object；
（4）Tetraethylenepentamine is put into container, is placed in 20 DEG C of water-baths of temperature, 20min is stirred, tetraethylenepentamine quality is added dropwise
6 times of epoxychloropropane is warming up to 30 DEG C, stirs 2h, and the triethylamine of 1.2 times of tetraethylenepentamine quality is added dropwise, is warming up to 70 DEG C,
5h is kept the temperature, heat preservation object, in mass ratio 1 are obtained：8, heat preservation object, distilled water are put into container and are mixed, 20 DEG C of water of temperature are placed in
In bath, it is added with stirring the revolving object of heat preservation amount of substance 40% in 300r/min, pH value is adjusted to 7,2h is stirred with 900r/min,
Up to dye fixing agent.
Comparative example：The dye fixing agent of Wuxi City company production.
Color fastness is tested：
Soaping fastness:By GB/T3921-2008《Textile color stability is tested:Soaping fastness》Method measures；
Crock fastness:By GB/T3920-2008《Textile color stability is tested:Crock fastness》Method measures；
Perspiration fastness:It is tested by GB/T3922-2013；
Rating is respectively with GB/T250-2008 discoloration gray scales and staining gray scale；
Feel is tested：
Close mesh touch arrange after fabric grade using 10 people as a small group, according to different feels by PRINTED FABRIC into
Row hand feel evaluation, specific assessment method are：Feel grading is carried out in terms of flexibility, smooth feeling two, is divided into 5 grades, 1 grade is worst,
Fabric feeling is harder, and sliding glutinous sense is poor, and 5 grades preferably, and fabrics feel soft, cunning are glutinous；
Burst size of methanal：It is detected by 4.59 condensed steam waters in GB/T17657-2013；
Antiultraviolet is tested：By GB/T18830-2009《The evaluation of ultraviolet resistance of fabric》Method measures, test equipment
For UV-2600 ultraviolet specrophotometers, it is 2mm that UV, which transmits filter disc thickness,.
Specific grading such as table 1.
Security test：Dye fixing agent obtained by above-described embodiment is coated in hand skin surface, 30d, 30d is observed continuously
Afterwards without allergic phenomena, illustrate that the present invention is harmless.
In summary, dye fixing agent of the present invention has the advantages that good hand touch, formaldehydeless release, uvioresistant, is a kind of
Safety and the preparation method of efficient dye fixing agent, are worthy to be popularized and use.
Claims (3)
1. a kind of preparation method of dye fixing agent, which is characterized in that the preparation method includes the following steps：
（1）In mass ratio 1：2, polypropylene glycol, polyethylene glycol are dehydrated at 100 ~ 120 DEG C of temperature, dehydrate is obtained, by dehydrate
It is put into container, is warming up to 40 ~ 50 DEG C, the isophorone diisocyanate of dehydration amount of substance 20 ~ 30% is added dropwise, stirs evenly, then
The dibutyl tin laurate that dehydration amount of substance 8 ~ 10% is added is mixed, and is stood at 50 ~ 60 DEG C of temperature, is obtained mixture；
（2）In mass ratio 1：0.5~0.6：5 ~ 6, water soluble chitosan, distillation, water are mixed, at 28 ~ 32 DEG C of temperature
Stirring, stirs evenly, obtains stirring liquid, in mass ratio 1：8 ~ 10, mixture, deionized water are mixed, stirred evenly, is added
The stirring liquid of mixture quality 1 ~ 2% stirs evenly at 28 ~ 32 DEG C of temperature, obtains mixing liquid；
（3）It counts in parts by weight, takes 50 ~ 60 parts liquid, 20 ~ 30 parts of deionized waters, 10 ~ 15 parts of acetone, 5 ~ 6 parts of second two are mixed
Amido ethanesulfonic acid sodium solution, 3 ~ 4 parts of 1,4-butanediol, 1 ~ 2 part of ethylenediamine, 0.1 ~ 0.2 part of catalyst will be mixed liquid, urge
Agent, acetone are mixed, and are kept at 70 ~ 80 DEG C of temperature, and 1,4-butanediol is added, and are stood 1 ~ 2h, are cooled to 30 ~ 35 DEG C,
Ethylenediamine base ethanesulfonic acid sodium solution is added, deionized water, ethylenediamine, stirring is added in stirring, and vacuum revolving obtains revolving object；
（4）Tetraethylenepentamine is put into container, is placed in 10 ~ 20 DEG C of water-baths of temperature, is stirred, dropwise addition tetraethylenepentamine quality 5 ~
6 times of epoxychloropropane, is warming up to 28 ~ 30 DEG C, and stirring is added dropwise the triethylamine of 1 ~ 1.2 times of tetraethylenepentamine quality, is warming up to 65
~ 70 DEG C, heat preservation obtains heat preservation object, in mass ratio 1：7 ~ 8, heat preservation object, distilled water are put into container and are mixed, temperature is placed in
In 10 ~ 20 DEG C of water-baths, the revolving object of heat preservation amount of substance 30 ~ 40% is added under stiring, adjusts pH value to 6 ~ 7, stirs to get dye
Expect color fixing agent.
2. the preparation method of dye fixing agent according to claim 1, which is characterized in that the step（2）Middle distillation is
In mass ratio 1：1.2：0.01, epoxidized soybean oil, isooctanol fluoboric acid are mixed, at 98 ~ 100 DEG C of temperature oil bath 1 ~
2h obtains mixture, in mass ratio 1：10 ~ 15, mixture, ethyl acetate are mixed, neutrality is diluted to deionized water, it is quiet
3 ~ 4h is set, organic layer is separated, organic layer is subjected to vacuum revolving, is evaporated under reduced pressure to get distillation.
3. the preparation method of dye fixing agent according to claim 1, which is characterized in that the step（3）Middle catalyst is
Stannous octoate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110656520A (en) * | 2019-10-24 | 2020-01-07 | 艾绳瑞 | Alkaline color fixing agent for reactive dye and preparation method thereof |
| CN111072907A (en) * | 2019-12-31 | 2020-04-28 | 江苏领瑞新材料科技有限公司 | Preparation method of waterborne polyurethane for bulletproof armor plate |
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2018
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110656520A (en) * | 2019-10-24 | 2020-01-07 | 艾绳瑞 | Alkaline color fixing agent for reactive dye and preparation method thereof |
| CN111072907A (en) * | 2019-12-31 | 2020-04-28 | 江苏领瑞新材料科技有限公司 | Preparation method of waterborne polyurethane for bulletproof armor plate |
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