CN108729269A - A kind of active dye fixing agent and preparation method thereof - Google Patents
A kind of active dye fixing agent and preparation method thereof Download PDFInfo
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- CN108729269A CN108729269A CN201810736099.XA CN201810736099A CN108729269A CN 108729269 A CN108729269 A CN 108729269A CN 201810736099 A CN201810736099 A CN 201810736099A CN 108729269 A CN108729269 A CN 108729269A
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- Prior art keywords
- fixing agent
- active dye
- dye fixing
- ammonium
- reaction kettle
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Classifications
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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
- 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
-
- 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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
Abstract
The present invention relates to a kind of active dye fixing agents and preparation method thereof, and its step are as follows：(1) quaternary organic ammonium compounds, carboxylated chitosan, unsaturated isocyanate compound, deionized water with epoxy group, turn on agitator are sequentially added in equipped with heating device and churned mechanically ultrasound reactor, and are heated up；(2) when the temperature in reaction kettle rises to 85~120 DEG C, start ultrasonoscope, ultrasonic power is 100~1000W, and frequency is 40~200kHz, is reacted 1~10 minute；(3) initiator solution that mass concentration is 1~10% is added dropwise in reaction kettle again, this initiator solution is formulated by the initiator and the part deionized water, and time for adding was controlled at 3~6 hours, and cooling discharge is to get the color fixing agent.
Description
Technical field
The invention belongs to technical field of textile printing, more particularly to a kind of active dye fixing agent and preparation method thereof.
Background technology
With the improvement of people's life quality, people are higher and higher to the performance requirement of textile, textile towards environmental protection,
Healthy, harmless direction is developed.This also requires printing and dyeing assistant to be upgraded accordingly.In entire field of printing and dyeing, color fixing agent is most
For important one of textile auxiliary, the use of color fixing agent can improve dyestuff soap on the fabric, the auxiliary agent of perspiration fastness, spinning
It knits dyeing to be widely used, but also brings some problems, as formaldehyde content of textiles is exceeded.So exploitation one
Kind meets fixation and processing requirement, and meets environmental protection, and the novel color fixing agent that green requires is to meet current industry development trend.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of active dye fixing agent and its preparation sides
Method, which can more preferably improve fabric fastness to wet rubbing and color fastness to washing, and not discharge formaldehydeless gas in use
Body.
To achieve the goals above, the present invention uses following technical scheme：
A kind of active dye fixing agent, the raw material components mainly matched by following mass fractions are made：
The quaternary organic ammonium compounds with epoxy group are glycidyltrimetiiylammonium ammonium chloride, glycidyl three
Ethyl ammonium chloride, glycidyl tripropyl ammonium chloride, glycidyltrimetiiylammonium ammonium bromide, glycidyl triethyl group bromination
One or more of ammonium, glycidyl tripropyl ammonium bromide are with the mixed mixture of arbitrary ratio.
The carboxylated chitosan is one kind or two in carboxymethyl chitosan, carboxyetbyl chitosan, carboxylic propyl chitosan
Kind or more with the mixed mixture of arbitrary ratio.
The unsaturated isocyanate compound is acryloyloxyethyl isocyanate, propenoyl isocyanate, first
One or more of base acryloyloxyethyl isocyanate, methacryloyl isocyanate are with arbitrary ratio mixing
Mixture.
The initiator is that one or more of ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate are mixed with arbitrary ratio
Mixture.
A kind of preparation method of active dye fixing agent, it is characterised in that：It is achieved by the steps of：
(1) it is sequentially added with the organic of epoxy group in equipped with heating device and churned mechanically ultrasound reactor
Quaternary ammonium compound, carboxylated chitosan, unsaturated isocyanate compound, deionized water, turn on agitator, and heat up；
(2) when the temperature in reaction kettle rises to 85~120 DEG C, starting ultrasonoscope, ultrasonic power is 100~1000W,
Frequency is 40~200kHz, is reacted 1~10 minute；
(3) initiator solution that mass concentration is 1~10% is added dropwise in reaction kettle again, this initiator solution is drawn by described
Hair agent and the part deionized water are formulated, and time for adding was controlled at 3~6 hours, and cooling discharge is to get the fixation
Agent.
The quaternary organic ammonium compounds with epoxy group are glycidyltrimetiiylammonium ammonium chloride, glycidyl three
Ethyl ammonium chloride, glycidyl tripropyl ammonium chloride, glycidyltrimetiiylammonium ammonium bromide, glycidyl triethyl group bromination
One or more of ammonium, glycidyl tripropyl ammonium bromide are with the mixed mixture of arbitrary ratio.
The carboxylated chitosan is one kind or two in carboxymethyl chitosan, carboxyetbyl chitosan, carboxylic propyl chitosan
Kind or more with the mixed mixture of arbitrary ratio.
The unsaturated isocyanate compound is acryloyloxyethyl isocyanate, propenoyl isocyanate, first
One or more of base acryloyloxyethyl isocyanate, methacryloyl isocyanate are with arbitrary ratio mixing
Mixture.
The initiator is that one or more of ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate are mixed with arbitrary ratio
Mixture.
Compared with prior art, the present invention has following remarkable result：
1, by the polymerization of several monomers, the color fixing agent prepared is made to contain hydroxyl, carboxyl, isocyanate group, amide
The groups such as base, epoxy group, quaternary ammonium salt play " bridge formation " between fiber and dyestuff, can be with the reactive base of dye molecule
Hydroxyl crosslinking in group, cellulosic molecule, forms height diversification interconnected system, so that dyestuff is combined with fiber more secured,
So as to significantly improve the dry fastness, fastness to wet rubbing and color fastness to washing of reactive dye, and the color of product is not influenced
Light and feel.
2, prepared color fixing agent has dyefastness high, dry and wet fastness, deionization Washing can be improved, to sensitivity
Color coloured light influences small, the advantages that dosage is few, and when fixation does not generate form and aspect variation, and formaldehydeless pollution substantially, effectively reduces and knits
Object content of formaldehyde promotes the quality of fabric, has a vast market foreground.
Specific implementation mode
The present invention is further elaborated on reference to embodiments.
A kind of active dye fixing agent of the present invention, the raw material components matched by following mass fractions are made：
The quaternary organic ammonium compounds with epoxy group are glycidyltrimetiiylammonium ammonium chloride, glycidyl three
Ethyl ammonium chloride, glycidyl tripropyl ammonium chloride, glycidyltrimetiiylammonium ammonium bromide, glycidyl triethyl group bromination
One or more of ammonium, glycidyl tripropyl ammonium bromide are with the mixed mixture of arbitrary ratio.
The carboxylated chitosan is one kind or two in carboxymethyl chitosan, carboxyetbyl chitosan, carboxylic propyl chitosan
Kind or more with the mixed mixture of arbitrary ratio.
The unsaturated isocyanate compound is acryloyloxyethyl isocyanate, propenoyl isocyanate, first
One or more of base acryloyloxyethyl isocyanate, methacryloyl isocyanate are with arbitrary ratio mixing
Mixture.
The initiator is that one or more of ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate are mixed with arbitrary ratio
Mixture.
A kind of preparation method of active dye fixing agent of the present invention, is achieved by the steps of：
(1) it is sequentially added with the organic of epoxy group in equipped with heating device and churned mechanically ultrasound reactor
Quaternary ammonium compound, carboxylated chitosan, unsaturated isocyanate compound, deionized water, turn on agitator, and heat up；
(2) when the temperature in reaction kettle rises to 85~120 DEG C, starting ultrasonoscope, ultrasonic power is 100~1000W,
Frequency is 40~200kHz, is reacted 1~10 minute；
(3) initiator solution that mass concentration is 1~10% is added dropwise in reaction kettle again, this initiator solution is drawn by described
Hair agent and the part deionized water are formulated, and time for adding was controlled at 3~6 hours, and cooling discharge is to get the fixation
Agent.
With specific embodiment, the present invention is described in detail below, but the present invention is not limited only to this.
Embodiment 1
A kind of active dye fixing agent of the present invention, the raw material components matched by following mass fractions are made：
A kind of preparation method of active dye fixing agent of the present invention, is achieved by the steps of：
(1) 21 parts of glycidyl front threes are sequentially added in equipped with heating device and churned mechanically ultrasound reactor
Ammonium chloride, 1.3 parts of carboxymethyl chitosans, 2 parts of acryloyloxyethyl isocyanates, 65.7 parts of deionized waters open stirring
Device, and heat up；
(2) when the temperature in reaction kettle rises to 88 DEG C, start ultrasonoscope, ultrasonic power 200W, frequency is
50kHz reacts 1.5 minutes；
(3) the initiator ammonium salt solution that mass concentration is 8.5% is added dropwise in reaction kettle again, this initiator solution is by 0.85 part
Ammonium persulfate and 9.15 deionized waters are formulated, and time for adding was controlled at 3.3 hours, and cooling discharge is to get the color fixing agent.
Embodiment 2
A kind of active dye fixing agent of the present invention, the raw material components matched by following mass fractions are made：
A kind of preparation method of active dye fixing agent of the present invention, is achieved by the steps of：
(1) 23 parts of three second of glycidyl are sequentially added in equipped with heating device and churned mechanically ultrasound reactor
Ammonium chloride, 2.2 parts of carboxymethyl chitosans, 4 parts of propenoyl isocyanates, 60.8 parts of deionized waters, turn on agitator, and rise
Temperature；
(2) when the temperature in reaction kettle rises to 92 DEG C, start ultrasonoscope, ultrasonic power 300W, frequency is
75kHz reacts 3 minutes；
(3) initiator solution that mass concentration is 7% is added dropwise in reaction kettle again, this initiator solution is by 0.7 part of over cure
Sour ammonium and 9.3 parts of deionized waters are formulated, and time for adding was controlled at 3.8 hours, and cooling discharge is to get the color fixing agent.
Embodiment 3
A kind of active dye fixing agent of the present invention, the raw material components matched by following mass fractions are made：
A kind of preparation method of active dye fixing agent of the present invention, is achieved by the steps of：
(1) 25 parts of glycidyls 3 third are sequentially added in equipped with heating device and churned mechanically ultrasound reactor
Ammonium chloride, 3.4 parts of carboxyetbyl chitosans, 6 parts of propenoyl isocyanates, 55.6 parts of deionized waters, turn on agitator, and rise
Temperature；
(2) when the temperature in reaction kettle rises to 99 DEG C, start ultrasonoscope, ultrasonic power 400W, frequency is
120kHz reacts 5 minutes；
(3) initiator solution that mass concentration is 5.5% is added dropwise in reaction kettle again, this initiator solution is by 0.55 part of mistake
Sodium sulphate and 9.45 parts of deionized waters are formulated, and time for adding 4 hours, cooling discharge is to get the color fixing agent.
Embodiment 4
A kind of active dye fixing agent of the present invention, the raw material components matched by following mass fractions are made：
A kind of preparation method of active dye fixing agent of the present invention, is achieved by the steps of：
(1) 26 parts of glycidyl front threes are sequentially added in equipped with heating device and churned mechanically ultrasound reactor
Base ammonium bromide, 4.6 parts of carboxyetbyl chitosans, 8 parts of methacryloxyethyl isocyanates, 51.4 parts of deionized waters are opened
Blender, and heat up；
(2) when the temperature in reaction kettle rises to 96 DEG C, start ultrasonoscope, ultrasonic power 650W, frequency is
150kHz reacts 6 minutes；
(3) initiator solution that mass concentration is 4% is added dropwise in reaction kettle again, this initiator solution is by 0.4 part of over cure
Sour sodium and 9.6 parts of deionized waters are formulated, and time for adding was controlled at 5 hours, and cooling discharge is to get the color fixing agent.
Embodiment 5
A kind of active dye fixing agent of the present invention, the raw material components matched by following mass fractions are made：
A kind of preparation method of active dye fixing agent of the present invention, is achieved by the steps of：
(1) 28 parts of three second of glycidyl are sequentially added in equipped with heating device and churned mechanically ultrasound reactor
Base ammonium bromide, 5.5 parts of carboxylic propyl chitosans, 10 parts of methacryloyl isocyanates, 46.5 parts of deionized waters open stirring
Device, and heat up；
(2) when the temperature in reaction kettle rises to 115 DEG C, start ultrasonoscope, ultrasonic power 800W, frequency is
160kHz reacts 7 minutes；
(3) initiator solution that mass concentration is 2.5% is added dropwise in reaction kettle again, this initiator solution is by 0.25 part of mistake
Potassium sulfate and 9.75 parts of deionized waters are formulated, and time for adding was controlled at 5.5 hours, and cooling discharge is to get the color fixing agent.
Embodiment 6
A kind of active dye fixing agent of the present invention, the raw material components matched by following mass fractions are made：
Wherein, carboxylated chitosan uses the mixture of carboxyetbyl chitosan and carboxylic propyl chitosan, and carboxyethyl shell is poly-
The mass ratio of sugar and carboxylic propyl chitosan is 1:1, that is, the dosage of carboxyetbyl chitosan and carboxylic propyl chitosan is 3.4 parts.
Unsaturated isocyanate compound uses methacryloxyethyl isocyanates and methylacryloyl isocyanide
The mixture of acid esters, and the mass ratio of methacryloxyethyl isocyanates and methacryloyl isocyanate is 1:3,
That is, the dosage of methacryloxyethyl isocyanates and methacryloyl isocyanate is respectively 3 parts and 9 parts.
Initiator uses the mixture of sodium peroxydisulfate and potassium peroxydisulfate, and the mass ratio of sodium peroxydisulfate and potassium peroxydisulfate is 1:
4, that is, the dosage of sodium peroxydisulfate and potassium peroxydisulfate is respectively 0.02 part and 0.08 part.
A kind of preparation method of active dye fixing agent of the present invention, is achieved by the steps of：
(1) 29 parts of glycidyls 3 third are sequentially added in equipped with heating device and churned mechanically ultrasound reactor
Base ammonium bromide, 3.4 parts of carboxyetbyl chitosans, 3.4 parts of carboxylic propyl chitosans, 3 parts of methacryloxyethyl isocyanates, 9
Part methacryloyl isocyanate, 42.2 parts of deionized waters, turn on agitator, and heat up；
(2) when the temperature in reaction kettle rises to 113 DEG C, start ultrasonoscope, ultrasonic power 950W, frequency is
190kHz reacts 9 minutes；
(3) initiator solution that mass concentration is 2% is added dropwise in reaction kettle again, this initiator solution is by 0.02 part of over cure
Sour sodium, 0.08 part of potassium peroxydisulfate and 9.9 parts of deionized waters are formulated, and time for adding control was at 5.8 hours, cooling discharge, i.e.,
Obtain the color fixing agent.
The color fixing agent that above-described embodiment 1~6 synthesizes is handled into the cotton fabric after reactive blue KGL dyeing respectively, using padding
Method color fixing process：Color fixing agent 15g/L (two leachings two are rolled, 90%) → drying (80 DEG C, 5min) → bakes (120 DEG C, 5min) → water
It washes → dries.Main performance index after cotton fabric fixation is as shown in table 1.
Main performance index of 1 cotton fabric of table after 1~6 fixation treatment of above-described embodiment
Remarks：
1. crock fastness test method presses GB/T3920-2008《Textile color stability tests colour fastness to rubbing》Method is surveyed
It is fixed；
2. soaping fastness test method presses GB/T3921-2008《Textile color stability tests color fastness to washing》Method is surveyed
It is fixed；
3. sweat, which soaks fastness test method, presses GB/T5713-2013《Textile color stability tests the color fastness of resistance to deionized water》Side
Method measures.
4. color fixing agent 7 is commercially available cationic fixing agent.
Above-described embodiment is not intended to limit the invention, and any person skilled in the art all can be in the essence without prejudice to the present invention
God and under the scope of, carry out modifications and changes to above-described embodiment.Therefore, those of ordinary skill in the art exists such as
It, should be by the present invention's without departing from all equivalent modifications or change completed under disclosed spirit and technological thought
Claim is covered.
Claims (6)
1. a kind of preparation method of active dye fixing agent, it is characterised in that：It is achieved by the steps of：
(1) organic quaternary ammonium with epoxy group is sequentially added in equipped with heating device and churned mechanically ultrasound reactor
Compound, carboxylated chitosan, unsaturated isocyanate compound, deionized water, turn on agitator, and heat up；
(2) when the temperature in reaction kettle rises to 85~120 DEG C, start ultrasonoscope, ultrasonic power is 100~1000W, frequency
For 40~200kHz, react 1~10 minute；
(3) initiator solution that mass concentration is 1~10% is added dropwise in reaction kettle again, this initiator solution is by the initiator
It is formulated with the part deionized water, time for adding was controlled at 3~6 hours, and cooling discharge is to get the color fixing agent.
2. a kind of active dye fixing agent, it is characterised in that：The raw material components mainly matched by following mass fractions are made：
3. a kind of active dye fixing agent according to claim 2, it is characterised in that：It is described organic with epoxy group
Quaternary ammonium compound is glycidyltrimetiiylammonium ammonium chloride, glycidol triethylammonium chloride, glycidyl tripropyl chlorine
Change in ammonium, glycidyltrimetiiylammonium ammonium bromide, glycidyl triethylammonium bromide, glycidyl tripropyl ammonium bromide
One or more are with the mixed mixture of arbitrary ratio.
4. a kind of active dye fixing agent according to claim 2, it is characterised in that：The carboxylated chitosan is carboxylic first
One or more of base enclosure glycan, carboxyetbyl chitosan, carboxylic propyl chitosan are with the mixed mixture of arbitrary ratio.
5. a kind of active dye fixing agent according to claim 2, it is characterised in that：The unsaturated isocyanate chemical combination
Object is acryloyloxyethyl isocyanate, propenoyl isocyanate, methacryloxyethyl isocyanates, methyl-prop
One or more of enoyl- isocyanates is with the mixed mixture of arbitrary ratio.
6. a kind of active dye fixing agent according to claim 2, it is characterised in that：The initiator be ammonium persulfate,
One or more of sodium peroxydisulfate and potassium peroxydisulfate are with the mixed mixture of arbitrary ratio.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810736099.XA CN108729269A (en) | 2018-07-06 | 2018-07-06 | A kind of active dye fixing agent and preparation method thereof |
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| CN201810736099.XA CN108729269A (en) | 2018-07-06 | 2018-07-06 | A kind of active dye fixing agent and preparation method thereof |
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Family
ID=63925763
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| CN110016103A (en) * | 2018-12-28 | 2019-07-16 | 福建清源科技有限公司 | A kind of modified hydroxymethyl starch polymer and its preparation method and application |
| CN110041463A (en) * | 2018-12-28 | 2019-07-23 | 福建清源科技有限公司 | A kind of modified tamarind gum polymer and its preparation method and application |
| CN110656520A (en) * | 2019-10-24 | 2020-01-07 | 艾绳瑞 | Alkaline color fixing agent for reactive dye and preparation method thereof |
| CN113529445A (en) * | 2021-08-17 | 2021-10-22 | 新昌县高纤纺织有限公司 | Printing and dyeing auxiliary applied to blend fiber and preparation method thereof |
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| CN110656520A (en) * | 2019-10-24 | 2020-01-07 | 艾绳瑞 | Alkaline color fixing agent for reactive dye and preparation method thereof |
| CN113529445A (en) * | 2021-08-17 | 2021-10-22 | 新昌县高纤纺织有限公司 | Printing and dyeing auxiliary applied to blend fiber and preparation method thereof |
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