CN106565910A - Formaldehyde-free hydrophilic color fixing agent for cotton, preparation method for color fixing agent and use method for color fixing agent - Google Patents
Formaldehyde-free hydrophilic color fixing agent for cotton, preparation method for color fixing agent and use method for color fixing agent Download PDFInfo
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- CN106565910A CN106565910A CN201611002739.1A CN201611002739A CN106565910A CN 106565910 A CN106565910 A CN 106565910A CN 201611002739 A CN201611002739 A CN 201611002739A CN 106565910 A CN106565910 A CN 106565910A
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- fixing agent
- color fixing
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- 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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
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- 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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
-
- 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 provides a formaldehyde-free hydrophilic color fixing agent for cotton, a preparation method for the color fixing agent and a use method for the color fixing agent. The formaldehyde-free hydrophilic color fixing agent for the cotton contains the following raw material ingredients in parts by weight: 5-20 parts of intermediate polyamine, 60-120 parts of functional quaternary ammonium salt cationic monomer, 11-22 parts of hydrophilic functional monomer, 5-10 parts of unsaturated olefin amine monomer, 2-12 parts of pH value regulator, 0.005-0.02 part of metal ion chelating agent, 0.8-1.5 parts of initiator and 10-30 parts of deionized water. The formaldehyde-free hydrophilic color fixing agent for the cotton, provided by the invention, is applied to dyed color fixation finishing of reactive dye dyed cotton fabrics and employs an oxidation-reduction free-radical initiation system, the initiator is low in decomposition activation energy and can initiate polymerization at quite low temperatures, and thus, the aims of saving energy and reducing emissions are achieved.
Description
Technical field
The invention belongs to the printing and dyeing assistant of textile product, a kind of cotton being especially directed to without the hydrophilic color fixing agent of aldehyde and
Its preparation method.
Background technology
, it is known that according to the traditional sorting technique of industry, fabric fibre can be divided into natural fiber and synthetic fibers, with people
The enhancing of the awareness of environment protection and health, natural fiber are comfortable and easy to wear because of which, increasingly by people's the advantages of sucting wet air permeability is good
Favor, plays very important role on the stage of fabric fibre.Adding for rear road will be carried out as cotton fabric dyeing process is latter
Carefully and neatly done reason can be only achieved preferable color fastness.
With the progress of social science and technology, people's environmental consciousness and quality of life improve a lot than ever, to textile
Also more and more higher is required, therefore is developed for dyeing assistant is also required that to environmental protection, energy-efficient direction, also gone out in recent years
Existing some new color fixing agent.
Wherein Polycationic color fixing agent is to compare a concerned class color fixing agent in recent years, real through the application of printing and dyeing mill
Discovery is trampled, this kind of color fixing agent has excellent colour fixation.However, find through constantly test, although this kind of color fixing agent is solid
Color effect is good, but there is following deficiency, and when high temperature bakes sizing, high molecular polymer can form hydrophobic in fabric face
Thin film, so that the moisture absorption hydrophilic of bafta itself has declined.As towel cloth and some to it is hydrophilic require it is higher
Cotton fabric, even if in rear road hand feel finishing, being also unable to reach good moisture absorption hydrophilic effect using hydrophilic consistent lubricant essence.
In this regard, industry also just have developed hydrophilic color fixing agent product accordingly, country for hygroscopic regulation be 5 seconds with
It is interior.Find through market feedback, the hydrophilic color fixing agent of this class, although moisture pick-up propertiess reach national requirements, but colour fixation
Bad, these hydrophilic color fixing agent all can not be taken into account colour fixation simultaneously and not affect the hygroscopicity of bafta itself.
Therefore, it is necessory to good and do not affect bafta moisture absorption itself to research and develop a kind of preparation process is simple, colour fixation
Hydrophilic hydrophilic color fixing agent, overcomes defect of the prior art.
The content of the invention
It is an object of the invention to provide a kind of cotton is with without the hydrophilic color fixing agent of aldehyde, the existing color fixing agent of effectively solving can not be simultaneously
Take into account bafta colour fixation and ensure the technical problem of two aspect advantage of bafta hygroscopicity itself.
To achieve these goals, the technical solution used in the present invention is as follows：
A kind of cotton is with without the hydrophilic color fixing agent of aldehyde, including the preparing raw material component of following weight portion：
Intermediate polyamine 5-20 parts；
Feature quaternary ammonium salt cationic monomer 60-120 parts；
Hydrophilic function monomer 11-22 parts；
Unsaturated olefin amine monomers 5-10 parts；
PH value regulator 2-12 part；
Metal ion chelation agent 0.005-0.02 parts；
Initiator 0.8-1.5 parts；And
Deionized water 10-30 parts.
Further, in different embodiments, the intermediate polyamine is the condensation polymer of amine and epichlorohydrin；Described
In the preparation of intermediate polyamine, the amine for using is 1～1.5 with the mol ratio of the epichlorohydrin：1；The amine includes
At least one in monomethyl amine, dimethylamine, ethylenediamine, diethylenetriamine, triethylene tetramine and TEPA.
Further, in different embodiments, the amine includes monomethyl amine, dimethylamine, ethylenediamine, divinyl three
At least one in amine, triethylene tetramine and TEPA.
Further, in different embodiments, the feature quaternary ammonium salt cationic monomer includes two allyl of dimethyl
Ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac, tetra allyl ammonium chloride, methylacryoyloxyethyl dimethyl benzyl chlorine
Change ammonium, methacryl hydroxypropyltrimonium chloride, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, diethyl diallyl chlorine
Change at least one in ammonium.
Further, in different embodiments, the hydrophilic function monomer includes component and the weight of each component
Number is：Acrylamide 5-10 parts, dicyandiamide 6-12 parts.
Further, in different embodiments, the unsaturated olefin amine monomers include N- amides,
One or more kinds of mixture in allyl amine, diallylamine or triallylamine.
Further, in different embodiments, the pH value regulator is included in hydrochloric acid, glacial acetic acid, citric acid extremely
Few one kind.
Further, in different embodiments, the metal ion chelation agent includes aminotriacetic acid sodium salt, ethylenediamine
One or more kinds of mixture in tetrem acid sodium-salt, 1,2-diaminocyclohexane tetraacetic acid sodium salt, ethylenediamine tetrapropionic acid sodium salt.
Further, in different embodiments, the initiator includes persulfate-bisulfites, persulfuric acid
At least one in salt-sulphite or azo-bis-isobutyrate hydrochloride.
The further embodiment of the present invention provides a kind of manufacture cotton according to the present invention with without the hydrophilic color fixing agent of aldehyde
Preparation method, comprises the following steps：
Prepare intermediate polyamine；
Prepare metal ion chelation agent solution and initiator solution；
The intermediate polyamine, the feature quaternary ammonium salt cationic monomer, the hydrophilic are sequentially added in reaction vessel
The whole of function monomer, the unsaturated olefin amine monomers total amount, obtains raw mixture；
PH value regulator and deionized water are added in the reaction vessel, starts stirring, by the pH value of the raw mixture
It is adjusted to 3～8；
The metal ion chelation agent solution is added to the reaction vessel；
Steam heats the reaction vessel, is warming up to 45～55 DEG C, stops heating；
To in the reaction vessel with three of initiator solution total amount described in the first Deca of the speed of 30～40 drop/minutes/
One；During first Deca, the initiator solution and the raw mixture exothermic heat of reaction, temperature in the reaction vessel
Rise；
When temperature rises to 60～70 DEG C in the reaction vessel, the reaction vessel is cooled down；After first completion of dropwise addition, hold
Continuous cooling；
When temperature drops to 50～60 DEG C in the reaction vessel, stop cooling, dripped with the speed of 30～40 drop/minutes again
Plus 2/3rds of the initiator solution total amount；
After completion of dropwise addition again, steam heats the reaction vessel, is warming up to 80～90 DEG C；
By temperature control in the reaction vessel at 80～90 DEG C, sustained response 1～3 hour；
Stop heating, cool down the reaction vessel, be cooled to 45～55 DEG C；
Stop stirring, discharging obtains the cotton with without the hydrophilic color fixing agent of aldehyde.
Further, in different embodiments, it is described to prepare intermediate polyamine, specifically include following steps：
Epichlorohydrin is added dropwise in amine with the speed of 30～50 drop/minutes, opens stirring, by the temperature control in the reactor
System is at 20-40 DEG C；The amine is 1～1.5 with the mol ratio of the epichlorohydrin:1；
After completion of dropwise addition, steam heats the reaction vessel, is warming up to 70～80 DEG C；
By the temperature control in the reactor at 70～80 DEG C, sustained response stopped heating after 3～5 hours；
The reaction vessel is cooled down, 40～50 DEG C are cooled to, stops stirring, discharging obtains intermediate polyamine.
Further, in different embodiments, in the metal ion chelation agent solution, each component and its parts by weight
Including 0.005～0.02 part of metal ion chelation agent, 0.1～0.4 part of deionized water；In the initiator solution, each component and
Its parts by weight includes 0.8～1.5 part of initiator, 16～30 parts of deionized water.
Another embodiment of the invention provides a kind of cotton according to the present invention with the user without the hydrophilic color fixing agent of aldehyde
Method, comprises the steps：
Cotton according to the present invention is configured to into 1%-2% (o.w.f) color fixing agent working solution with without the hydrophilic color fixing agent of aldehyde and water；
Pending wollen fabrics are impregnated in the color fixing agent working solution；
The wollen fabrics from the color fixing agent working solution are taken out and dried；Wherein, in dipping process, dipping temperature is
50～60 DEG C, dipping bath ratio is 1:15, dip time is 20～30 minutes.
Another embodiment of the invention provides a kind of cotton according to the present invention with the user without the hydrophilic color fixing agent of aldehyde
Method, comprises the steps：
Cotton according to the present invention is configured to into color fixing agent working solution with without the hydrophilic color fixing agent of aldehyde and water；The color fixing agent working solution
In, mass concentration of the cotton without the hydrophilic color fixing agent of aldehyde is 15～30g/L；By pending wollen fabrics in the color fixing agent
Two leachings two in working solution are rolled；
By the wollen fabrics in 90～100 DEG C of prebakes 2～2.5 minutes；And
The wollen fabrics are bakeed 30～40 seconds at 150～160 DEG C.
Relative to prior art, the beneficial effects of the present invention is：Cotton according to the present invention is answered with without the hydrophilic color fixing agent of aldehyde
For the fixing finish after cotton fabrics dyed with reactive dyes dyeing, which adopts oxidoreduction free radical initiator system, this kind of initiation
The decomposition activation energy of agent is low, can cause polymerization at a lower temperature, so as to effectively reduce energy consumption, reaches the mesh of energy-saving and emission-reduction
's.Cotton according to the present invention with without the hydrophilic color fixing agent of aldehyde can solve dyed cotton fabric colour fixation while, will not also shadow
Ring the hygroscopicity of bafta itself.
Further, cotton according to the present invention is with without the hydrophilic color fixing agent of aldehyde, with intermediate polyamine, feature quaternary ammonium salt sun from
Sub- monomer, hydrophilic function monomer and unsaturated olefin amine monomers are primary raw material, by Raolical polymerizable, are carried out many
Unit's polymerization.In the polymeric chain of synthesis, existing quaternary ammonium salt cationic can form water-fast color with reactive dye
Form sediment, lift washing color fastness and fastness to rubbing of dyed cotton fabric etc., it is ensured that fixing property；Hydrophilic is introduced simultaneously
Function monomer participates in copolymerization, by a certain amount of hydrophilic group (- OH ,-NH2 ,-COOH) on polymeric chain, protects
The moisture absorption hydrophilic for having demonstrate,proved dyed cotton fabric is barely affected.
Moreover, it relates to cotton do not contain APEO and formaldehyde with without the hydrophilic color fixing agent of aldehyde, while meeting environmental requirement,
The performance of color fixing agent itself can also be lifted.
Specific embodiment
Below with reference to embodiment, to a kind of skill of the cotton according to the present invention without the hydrophilic color fixing agent of aldehyde and preparation method thereof
Art scheme is described in further detail.
An embodiment of the invention provides a kind of cotton with without the hydrophilic color fixing agent of aldehyde, including the preparation of following weight portion
Raw material components：Intermediate polyamine 5-20 parts, feature quaternary ammonium salt cationic monomer 60-120 parts, hydrophilic function monomer 11-22
Part (including acrylamide 5-10 parts, dicyandiamide 6-12 parts), unsaturated olefin amine monomers 5-10 parts, pH value regulator 2-12
Part, metal ion chelation agent 0.005-0.02 parts, initiator 0.8-1.5 parts and deionized water 10-30 parts.
Below with reference to the cotton according to the present invention specific embodiment of the preparation method without the hydrophilic color fixing agent of aldehyde, to this
It is bright to be described further.
Embodiment 1
The following raw material for calculating the weight is provided：10 parts of intermediate polyamine, 100 parts of methacryloxypropyl ethylene trimethyl ammonium chlorides, 5
Part acrylamide, 8 parts of dicyandiamides, 6 parts of allyl amines, 0.02 part of metal ion chelation agent and 15 parts of deionized waters.Initiator is adopted
With 1 part of Ammonium persulfate .-sodium sulfite.
The cotton according to the present invention is with comprising the steps without the concrete preparation process of the hydrophilic color fixing agent of aldehyde：
Under nitrogen atmosphere, sequentially add in a kettle. intermediate polyamine, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, third
Acrylamide, dicyandiamide and allyl amine；
By 0.02 part of metal ion chelation agent, aqueous solution is configured to the deionized water of 20 times of weight and is added to aforesaid reaction vessel
In；
By 1.0 parts of Ammonium persulfate .-sodium sulfite, initiator solution is made with the deionized water dissolving of 20 times of weight, it is standby；
Steam reacting by heating kettle, when the temperature in reaction system rises to 50 DEG C, drips above-mentioned initiator solution suction head tank
Plus in tank, with 1/3rd of initiator solution total amount described in the first Deca of the speed of 30～40 drop/minutes, reactor is warming up to
60～70 DEG C of back flow reaction；
When temperature is down to 60～50 DEG C, stop cooling, with the speed of 30～40 drop/minutes initiator solution described in Deca again
2/3rds of total amount, time for adding are 2 hours；
After dripping, at 80 DEG C, continue isothermal reaction 3 hours, cool to 50 DEG C, discharge, the cotton is obtained final product with without aldehyde parent
Water color fixing agent.
The synthesis of wherein described intermediate polyamine, which can specifically include following steps：
In a kettle., by dimethylamine and the mol ratio 1 of epichlorohydrin:1 allotment raw material, is initially charged dimethylamine in reactor, so
Afterwards by epichlorohydrin suction head tank dropping tank, stirring is opened, is slowly added dropwise；
Epichlorohydrin is added dropwise in amine with the speed of 30～50 drop/minutes, opens stirring, by the temperature control in the reactor
System is at 20-40 DEG C；
After completion of dropwise addition, steam heats the reaction vessel, is warming up to 70 DEG C；
In 70 DEG C of insulation reaction 4 hours, stop heating；
The reaction vessel is cooled down, 50～40 DEG C are cooled to, stops stirring, discharging obtains intermediate polyamine.
Embodiment 2
The following raw material for calculating the weight is provided：15 parts of intermediate polyamine, 90 parts of acryloyl-oxy ethylene trimethyl ammonium chlorides, 6 part third
Acrylamide, 9 parts of dicyandiamides, 8 parts of allyl amines, 0.015 part and 30 parts deionized waters of metal ion chelation agent.Initiator is adopted
1.2 parts of potassium peroxydisulfate-sodium sulfitees.
The cotton is with comprising the steps without the concrete preparation process of the hydrophilic color fixing agent of aldehyde：
Under nitrogen atmosphere, sequentially add in a kettle.：15 parts of intermediate polyamine, 90 parts of acryloyl-oxy ethylene trimethyl ammonia chlorides
Ammonium, 6 parts of acrylamides, 9 parts of dicyandiamides, 8 parts of allyl amines and 30 parts of deionized waters；
By 0.015 part of metal ion chelation agent, aqueous solution is configured to the deionized water of 20 times of weight and is added in reactor；
By 1.2 parts of Ammonium persulfate .-sodium sulfite, initiator solution is made with the deionized water dissolving of 20 times of weight, it is standby；
Steam reacting by heating kettle, when the temperature in reaction system rises to 50 DEG C, drips above-mentioned initiator solution suction head tank
Plus in tank, with 1/3rd of initiator solution total amount described in the first Deca of the speed of 30～40 drop/minutes, reactor is warming up to
60～70 DEG C of back flow reaction；
When temperature is down to 60～50 DEG C, stop cooling, with the speed of 30～40 drop/minutes initiator solution described in Deca again
2/3rds of total amount, time for adding are 1.5 hours；
After dripping, at 80 DEG C, continue isothermal reaction 2 hours, cool to 45 DEG C, discharge, the cotton is obtained final product with without aldehyde parent
Water color fixing agent.
The synthesis of wherein described intermediate polyamine comprises the steps：
In a kettle., by diethylenetriamine and the mol ratio 1.2 of epichlorohydrin:1 allotment raw material, is initially charged diethylenetriamine in anti-
In answering kettle, then by epichlorohydrin suction head tank dropping tank, stirring is opened, is slowly added dropwise；
Epichlorohydrin is added dropwise in amine with the speed of 30～50 drop/minutes, opens stirring, by the temperature control in the reactor
System is at 20-40 DEG C；
After completion of dropwise addition, steam heats the reaction vessel, is warming up to 70 DEG C；
In 70 DEG C of insulation reaction 4 hours, stop heating；
The reaction vessel is cooled down, 50～40 DEG C are cooled to, stops stirring, discharging obtains intermediate polyamine.
Embodiment 3
The following raw material for calculating the weight is provided：18 parts of intermediate polyamine, 110 parts of dimethyl diallyl ammonium chlorides, 8 parts of acryloyls
Amine, 10 parts of dicyandiamides, 10 parts of diallylamines, 0.018 part and 35 parts deionized waters of metal ion chelation agent.Initiator is adopted
1.5 parts of potassium peroxydisulfate-sodium sulfitees.
The cotton is with comprising the steps without the concrete preparation process of the hydrophilic color fixing agent of aldehyde：
Under nitrogen atmosphere, sequentially add in reactor：18 parts of intermediate polyamine, 110 parts of dimethyl diallyl ammonium chlorides, 8
Part acrylamide, 10 parts of dicyandiamides, 10 parts of diallylamines and 35 parts of deionized waters；
By 0.018 part of metal ion chelation agent, aqueous solution is configured to the deionized water of 20 times of weight and is added in reactor；
By 1.5 parts of Ammonium persulfate .-sodium sulfite, initiator solution is made with the deionized water dissolving of 20 times of weight, it is standby；
Steam reacting by heating kettle, when the temperature in reaction system rises to 50 DEG C, drips above-mentioned initiator solution suction head tank
Plus in tank, with 1/3rd of initiator solution total amount described in the first Deca of the speed of 30～40 drop/minutes, reactor is warming up to
60～70 DEG C of back flow reaction；
When temperature is down to 60～50 DEG C, stop cooling, with the speed of 30～40 drop/minutes initiator solution described in Deca again
2/3rds of total amount, time for adding are 2 hours；
After dripping, at 80 DEG C, continue isothermal reaction 3 hours, cool to 55 DEG C, discharge, the cotton is obtained final product with without aldehyde parent
Water color fixing agent.
The synthesis of wherein described intermediate polyamine may include steps of：
In a kettle., by monomethyl amine and the mol ratio 1.3 of epichlorohydrin:1 allotment raw material, is initially charged monomethyl amine in reactor,
Then by epichlorohydrin suction head tank dropping tank, stirring is opened, is slowly added dropwise；
Epichlorohydrin is added dropwise in amine with the speed of 30～50 drop/minutes, opens stirring, by the temperature control in the reactor
System is at 20-40 DEG C；
After completion of dropwise addition, steam heats the reaction vessel, is warming up to 70 DEG C；
In 70 DEG C of insulation reaction 4 hours, stop heating；
The reaction vessel is cooled down, 50～40 DEG C are cooled to, stops stirring, discharging obtains intermediate polyamine.
Embodiment 4
The following raw material for calculating the weight is provided：12 parts of intermediate polyamine, 120 parts of methylacryoyloxyethyl dimethyl benzyl chlorinations
Ammonium, 8 parts of acrylamides, 10 parts of dicyandiamides, 10 parts of amides, 0.02 part and 40 parts deionizations of metal ion chelation agent
Water.Initiator adopts 1.4 parts of potassium peroxydisulfate-sodium sulfitees
The cotton is with comprising the steps without the concrete preparation process of the hydrophilic color fixing agent of aldehyde：
Under nitrogen atmosphere, sequentially add in reactor：12 parts of intermediate polyamine, 120 parts of methylacryoyloxyethyl diformazans
Base benzyl ammonium chloride, 8 parts of acrylamides, 10 parts of dicyandiamides, 10 parts of amides and 40 parts of deionized waters；
By 0.02 part of metal ion chelation agent, aqueous solution is configured to the deionized water of 20 times of weight and is added in reactor；
By 1.4 parts of Ammonium persulfate .-sodium sulfite, initiator solution is made with the deionized water dissolving of 20 times of weight, it is standby；
Steam reacting by heating kettle, when the temperature in reaction system rises to 50 DEG C, drips above-mentioned initiator solution suction head tank
Plus in tank, with 1/3rd of initiator solution total amount described in the first Deca of the speed of 30～40 drop/minutes, reactor is warming up to
60～70 DEG C of back flow reaction；
When temperature is down to 60～50 DEG C, stop cooling, with the speed of 30～40 drop/minutes initiator solution described in Deca again
2/3rds of total amount, time for adding are 2 hours；
After dripping, at 80 DEG C, continue isothermal reaction 2 hours, cool to 50 DEG C, discharge, the cotton is obtained final product with without aldehyde parent
Water color fixing agent.
The synthesis of wherein described intermediate polyamine may include steps of：
In a kettle., by triethylene tetramine and the mol ratio 1 of epichlorohydrin:1 allotment raw material, is initially charged triethylene tetramine in reaction
In kettle, then by epichlorohydrin suction head tank dropping tank, stirring is opened, is slowly added dropwise；
Epichlorohydrin is added dropwise in amine with the speed of 30～50 drop/minutes, opens stirring, by the temperature control in the reactor
System is at 20-40 DEG C；
After completion of dropwise addition, steam heats the reaction vessel, is warming up to 70 DEG C；
In 70 DEG C of insulation reaction 4 hours, stop heating；
The reaction vessel is cooled down, 50～40 DEG C are cooled to, stops stirring, discharging obtains intermediate polyamine.
The cotton provided by above-described embodiment with without the hydrophilic color fixing agent of aldehyde, be used to process cotton fabrics dyed with reactive dyes,
Wherein, the dependence test result to the embodiment 1 and embodiment 2, is shown in Table 1, table 2.In table 1, table 2, washing color fastness
By GB/T3921-2008《Textile color stability is tested：Washing color fastness》Method is determined；GB/T250- is used in rating respectively
2008 discoloration gray scales and GB/T251-2008 staining gray scales.
1 embodiment of table is to the colour fixation after dyed cotton fabric arrangement
| Without the hydrophilic color fixing agent of aldehyde | Big silk cotton is knitting/hydrophilic (second) | Black cotton is knitting/hydrophilic (second) |
| Embodiment 1 | 1 | 2 |
| Embodiment 2 | 2 | Drop is oozed |
| Embodiment 3 | Drop is oozed | 1 |
| Embodiment 4 | 2 | 1 |
| Former cloth (non-fixation) | Drop is oozed | Drop is oozed |
Hydrophilic of 2 embodiment of table to dyed cotton fabric
Cotton obtained by the present embodiment with without the hydrophilic color fixing agent of aldehyde, by GB/T3921-2008《Textile color stability is tested：It is water-fast
Wash color fastness》Method is determined, with excellent colour fixation, while the moisture absorption of the bafta after determining fixing finish is hydrophilic
Property be respectively less than 5 seconds, meet the moisture absorption hydrophilic requirement of the textile of national regulation.
Another embodiment of the invention provides a kind of cotton according to the present invention with the user without the hydrophilic color fixing agent of aldehyde
Method, comprises the steps：
By the cotton according to the present invention color fixing agent working solution that 1%-2% (o.w.f) is configured to without the hydrophilic color fixing agent of aldehyde and water；
Pending wollen fabrics are impregnated in the color fixing agent working solution；
The wollen fabrics from the color fixing agent working solution are taken out and dried；
Wherein, in dipping process, dipping temperature is 50～60 DEG C, and dipping bath ratio is 1:15, dip time is 20～30 minutes.
Cotton according to the present invention is configured to into color fixing agent working solution with without the hydrophilic color fixing agent of aldehyde and water；The color fixing agent work
In liquid, mass concentration of the cotton without the hydrophilic color fixing agent of aldehyde is 15～30g/L；By pending wollen fabrics in the fixation
Two leachings two in agent working solution are rolled；
By the wollen fabrics in 90～100 DEG C of prebakes 2～2.5 minutes；
The wollen fabrics are bakeed 30～40 seconds at 150～160 DEG C.
Cotton according to the present invention is with without the hydrophilic color fixing agent of aldehyde, the fixation being applied to after cotton fabrics dyed with reactive dyes dyeing
Arrange, which adopts oxidoreduction radical initiator, and the decomposition activation energy of this kind of initiator is low, can cause at a lower temperature
Polymerization, can reach the purpose of energy-saving and emission-reduction.
Cotton according to the present invention with without the hydrophilic color fixing agent of aldehyde, with intermediate polyamine, feature quaternary ammonium salt cationic monomer,
Acrylamide, dicyandiamide and unsaturated olefin amine monomers are primary raw material, by Raolical polymerizable, are carried out polynary poly-
Close.In the polymeric chain of synthesis, existing quaternary ammonium salt cationic can form water-fast color lake with reactive dye, come
Lift washing color fastness and fastness to rubbing of dyed cotton fabric etc., it is ensured that fixing property；Introduce hydrophilic sexual function simultaneously
Monomer participates in copolymerization, by a certain amount of hydrophilic group (- OH ,-NH2 ,-COOH) on polymeric chain, it is ensured that
The moisture absorption hydrophilic of dyed cotton fabric is barely affected.
Moreover, it relates to cotton do not contain APEO and formaldehyde with without the hydrophilic color fixing agent of aldehyde, while meeting environmental requirement,
The performance of color fixing agent itself can also be lifted.
The technical scope of the present invention is not limited solely to the content in described above, and those skilled in the art can not take off
On the premise of the technology of the present invention thought, many variations and modifications are carried out to above-described embodiment, and these deformations and modification all should
When being within the scope of the present invention.
Claims (10)
1. a kind of cotton is with without the hydrophilic color fixing agent of aldehyde, it is characterised in that the parts by weight bag of the component and each component of its preparing raw material
Include：
Intermediate polyamine 5-20 parts；
Feature quaternary ammonium salt cationic monomer 60-120 parts；
Hydrophilic function monomer 11-22 parts；
Unsaturated olefin amine monomers 5-10 parts；
PH value regulator 2-12 part；
Metal ion chelation agent 0.005-0.02 parts；
Initiator 0.8-1.5 parts；And
Deionized water 10-30 parts.
2. cotton according to claim 1 is with without the hydrophilic color fixing agent of aldehyde, it is characterised in that
The intermediate polyamine is the condensation polymer of amine and epichlorohydrin；
In the preparation of the intermediate polyamine, the amine for using is 1 ~ 1.5 with the mol ratio of the epichlorohydrin：1；
During the amine includes monomethyl amine, dimethylamine, ethylenediamine, diethylenetriamine, triethylene tetramine and TEPA
It is at least one.
3. cotton according to claim 1 is with without the hydrophilic color fixing agent of aldehyde, it is characterised in that wherein described feature quaternary ammonium salt sun
Ion monomer includes dimethyl diallyl ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac, tetra allyl ammonium chloride, methyl
Acryloxyethyldimethyl benzyl ammonium chloride, methacryl hydroxypropyltrimonium chloride, methylacryoyloxyethyl front three
At least one in ammonium chloride, diethyl diallyl ammonium chloride.
4. cotton according to claim 1 is with without the hydrophilic color fixing agent of aldehyde, it is characterised in that the hydrophilic function monomer includes
Component and the parts by weight of each component be：5 ~ 10 parts of acrylamide, 6 ~ 12 parts of dicyandiamide.
5. cotton according to claim 1 is with without the hydrophilic color fixing agent of aldehyde, it is characterised in that the unsaturated olefin amine monomers
It is one or more kinds of mixed in including N- amides, allyl amine, diallylamine or triallylamine
Compound；The pH value regulator includes at least one in hydrochloric acid, glacial acetic acid, citric acid；The metal ion chelation agent includes
One kind in aminotriacetic acid sodium salt, disodium edta, 1,2-diaminocyclohexane tetraacetic acid sodium salt, ethylenediamine tetrapropionic acid sodium salt or
The two or more mixture of person；The initiator includes persulfate-bisulfites, persulfate-sulphite or idol
At least one in two 2,2-Dimethylaziridine hydrochlorate of nitrogen.
6. one kind preparation method of cotton without the hydrophilic color fixing agent of aldehyde according to any one of claim 1 ~ 5, it is characterised in that
Comprise the following steps：
Prepare intermediate polyamine；
Preparing metal ion chelating agent solution and initiator solution；
The intermediate polyamine, the feature quaternary ammonium salt cationic monomer, the hydrophilic are sequentially added in reaction vessel
The whole of function monomer, the unsaturated olefin amine monomers total amount, obtains raw mixture；
PH value regulator and deionized water are added in the reaction vessel, starts stirring, by the pH value of the raw mixture
It is adjusted to 3 ~ 8；
The metal ion chelation agent solution is added to the reaction vessel；
Steam heats the reaction vessel, is warming up to 45 ~ 55 DEG C, stops heating；
To in the reaction vessel with 1/3rd of initiator solution total amount described in the first Deca of the speed of 30 ~ 40 drop/minutes；
During first Deca, the initiator solution and the raw mixture exothermic heat of reaction, in the reaction vessel in temperature
Rise；
When temperature rises to 60 ~ 70 DEG C in the reaction vessel, the reaction vessel is cooled down；After first completion of dropwise addition, hold
Continuous cooling；
When temperature drops to 50 ~ 60 DEG C in the reaction vessel, stop cooling, with the speed of 30 ~ 40 drop/minutes Deca again
2/3rds of the initiator solution total amount；
After completion of dropwise addition again, steam heats the reaction vessel, is warming up to 80 ~ 90 DEG C；
By temperature control in the reaction vessel at 80 ~ 90 DEG C, sustained response 1 ~ 3 hour；
Stop heating, cool down the reaction vessel, be cooled to 45 ~ 55 DEG C；
Stop stirring, discharging obtains the cotton with without the hydrophilic color fixing agent of aldehyde.
7. preparation method of the cotton according to claim 6 without the hydrophilic color fixing agent of aldehyde, it is characterised in that in the middle of the preparation
Body polyamine, specifically includes following steps：
Epichlorohydrin is added dropwise in amine with the speed of 30 ~ 50 drop/minutes, opens stirring, by the temperature control in the reactor
System is at 20-40 DEG C；The amine is 1 ~ 1.5 with the mol ratio of the epichlorohydrin:1；
After completion of dropwise addition, steam heats the reaction vessel, is warming up to 70 ~ 80 DEG C；
By the temperature control in the reactor at 70 ~ 80 DEG C, sustained response stopped heating after 3 ~ 5 hours；
The reaction vessel is cooled down, 40 ~ 50 DEG C are cooled to, stops stirring, discharging obtains intermediate polyamine.
8. preparation method of the cotton according to claim 6 without the hydrophilic color fixing agent of aldehyde, it is characterised in that the metal ion
In chelating agent solution, each component and its parts by weight include 0.005 ~ 0.02 part of metal ion chelation agent, deionized water 0.1 ~ 0.4
Part；In the initiator solution, each component and its parts by weight include 0.8 ~ 1.5 part of initiator, 16 ~ 30 parts of deionized water.
9. using method of a kind of cotton without the hydrophilic color fixing agent of aldehyde, it is characterised in that comprise the steps：
Cotton any one of claim 1 ~ 5 is configured to into 1%-2% with without the hydrophilic color fixing agent of aldehyde and water（o.w.f）Fixation
Agent working solution；
Non- fixation reactive dyeing cloth is impregnated in the color fixing agent working solution；
The reactive dyeing cloth from the color fixing agent working solution is taken out and dried；
Wherein, in dipping process, dipping temperature is 50 ~ 60 DEG C, and dipping bath ratio is 1:15, dip time is 20 ~ 30 minutes.
10. using method of a kind of cotton without the hydrophilic color fixing agent of aldehyde, it is characterised in that comprise the steps：
Cotton any one of claim 1 ~ 5 is configured to into color fixing agent working solution with without the hydrophilic color fixing agent of aldehyde and water；It is described
In color fixing agent working solution, mass concentration of the cotton without the hydrophilic color fixing agent of aldehyde is 15 ~ 30g/L；
By non-fixation reactive dyeing cloth, in the color fixing agent working solution, two leachings two are rolled；
By the reactive dyeing cloth in 90 ~ 100 DEG C of prebakes 2 ~ 2.5 minutes；And
The reactive dyeing cloth is bakeed 30 ~ 40 seconds at 150 ~ 160 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611002739.1A CN106565910A (en) | 2016-11-14 | 2016-11-14 | Formaldehyde-free hydrophilic color fixing agent for cotton, preparation method for color fixing agent and use method for color fixing agent |
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| CN201611002739.1A CN106565910A (en) | 2016-11-14 | 2016-11-14 | Formaldehyde-free hydrophilic color fixing agent for cotton, preparation method for color fixing agent and use method for color fixing agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107675524A (en) * | 2017-09-08 | 2018-02-09 | 安徽龙盛纺织科技有限公司 | A kind of environmentally friendly colouring method of the low bath raio of textile material |
| CN107747238A (en) * | 2017-11-22 | 2018-03-02 | 邢台学院 | For synchronously being dyed to fabric and the composition and its application method of fixation |
| CN108660811A (en) * | 2018-07-06 | 2018-10-16 | 李美琴 | A kind of quaternary ammonium salt cationic color fixing agent and preparation method thereof |
| CN108660812A (en) * | 2018-06-06 | 2018-10-16 | 苏州联胜化学有限公司 | A kind of blended color fixing agent of cross-linking type and its preparation and application |
| CN109778572A (en) * | 2019-01-18 | 2019-05-21 | 江西德盛精细化学品有限公司 | A kind of activity aldehyde-free colour stabilizer and preparation method thereof |
| CN111548448A (en) * | 2020-06-13 | 2020-08-18 | 广东传化富联精细化工有限公司 | Active hydrophilic color fixing agent for fabric and preparation method thereof |
| CN111676718A (en) * | 2020-07-16 | 2020-09-18 | 烟台源明纺织科技有限公司 | Weather-resistant color fastness improver for reactive dye and preparation method and application thereof |
| CN113637127A (en) * | 2021-08-16 | 2021-11-12 | 广东传化富联精细化工有限公司 | Color fixing agent for cotton for after-finishing and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107675524A (en) * | 2017-09-08 | 2018-02-09 | 安徽龙盛纺织科技有限公司 | A kind of environmentally friendly colouring method of the low bath raio of textile material |
| CN107747238A (en) * | 2017-11-22 | 2018-03-02 | 邢台学院 | For synchronously being dyed to fabric and the composition and its application method of fixation |
| CN107747238B (en) * | 2017-11-22 | 2020-03-17 | 邢台学院 | Composition for simultaneous dyeing and fixing of textiles and method of use thereof |
| CN108660812A (en) * | 2018-06-06 | 2018-10-16 | 苏州联胜化学有限公司 | A kind of blended color fixing agent of cross-linking type and its preparation and application |
| CN108660811A (en) * | 2018-07-06 | 2018-10-16 | 李美琴 | A kind of quaternary ammonium salt cationic color fixing agent and preparation method thereof |
| CN109778572A (en) * | 2019-01-18 | 2019-05-21 | 江西德盛精细化学品有限公司 | A kind of activity aldehyde-free colour stabilizer and preparation method thereof |
| CN111548448A (en) * | 2020-06-13 | 2020-08-18 | 广东传化富联精细化工有限公司 | Active hydrophilic color fixing agent for fabric and preparation method thereof |
| CN111676718A (en) * | 2020-07-16 | 2020-09-18 | 烟台源明纺织科技有限公司 | Weather-resistant color fastness improver for reactive dye and preparation method and application thereof |
| CN113637127A (en) * | 2021-08-16 | 2021-11-12 | 广东传化富联精细化工有限公司 | Color fixing agent for cotton for after-finishing and preparation method thereof |
| CN114753171A (en) * | 2022-05-18 | 2022-07-15 | 清远市宏图助剂有限公司 | Cationic formaldehyde-free hydrophilic polyester color fixing agent and preparation method thereof |
| CN114753171B (en) * | 2022-05-18 | 2023-01-17 | 清远市宏图助剂有限公司 | Cationic formaldehyde-free hydrophilic polyester color fixing agent and preparation method thereof |
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Application publication date: 20170419 |