CN105568722A - Preparation method of cationic fixing agent emulsion - Google Patents
Preparation method of cationic fixing agent emulsion Download PDFInfo
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- CN105568722A CN105568722A CN201511012962.XA CN201511012962A CN105568722A CN 105568722 A CN105568722 A CN 105568722A CN 201511012962 A CN201511012962 A CN 201511012962A CN 105568722 A CN105568722 A CN 105568722A
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- cationic fixing
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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
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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
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a single or double bond to nitrogen
- C08F226/04—Diallylamine
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Abstract
The invention relates to the technical field of chemical production, relates to a production method, and especially relates to a preparation method of a cationic fixing agent emulsion. The preparation method comprises the following steps: 1, adding 18-25% of diallylamine to a reaction kettle; 2, adjusting the pH value; 3, adding 8-12% of acrylamide and 48-55% of water; 4, adding 0.2-0.3% of an initiator and a molecular weight adjusting agent; 5, adding 1% of a diethyldiallylammonium chloride solution; and 6, adding 8-15% of a dimethylamine-chloropropylene oxide polymer. The preparation method allows the cationic fixing agent emulsion with the advantages of simple processing process, convenient preparation, low cost and high yield to be prepared; and the cationic fixing agent emulsion is added to fix the color, so the color fixing effect is excellent, the friction resistance (grade) is 3-4, the washing resistance (grade) is 3-4, and the water resistance (grade) can reach 3-4.
Description
Technical field
Invention relates to chemical production technical field, relates to a kind of production method, refers in particular to a kind of preparation method of cationic fixing agent emulsion.
Background technology
Because the dyeing mechanism of dyestuff on different fiber is all different with dyefastness, so the fixation principle of color-fixing agent is also different.The fixation principle of all kinds of dye fixing agent is as follows: utilize color-fixing agent and dyestuff to generate insoluble color lake direct dyes, ACID DYES and REACTIVE DYES because of containing hydrophilic radical, reduce dyestuff and interfibrous affinity when meeting water.The anionic group of the cationic charge in color-fixing agent molecule and dyestuff is utilized to form electrostatical binding, make dyestuff and color-fixing agent on fiber, generate insoluble color lake, reduce the water-soluble of dyestuff, thus raising wet colour fastness, improve soaping and calico staining fastness of dyestuff, the cationic of color-fixing agent is stronger, and it is soaped, calico staining fastness is better.As direct dyes, REACTIVE DYES cationic fixing agent process, generate color lake and improve the process of wet fastness direct copper dye mantoquita, use chromic salts process after acid dyeing, make between dyestuff and fiber, to form huge legendary turtle compound, thus reduce that it is water-soluble, to improve dyeing.And no matter be which kind of color-fixing agent, the making of current color-fixing agent imperfection, the effect of color-fixing agent is also bad.Usual use PDMDAAC and diethylenetriamine-epichlorohydrin polymer are as color-fixing agent, and rub resistance (level) and washable (level) can only reach 2-3.
Summary of the invention
The object of invention is for the problems referred to above, provides a kind of preparation method that can make rub resistance and the high cationic fixing agent emulsion of washable grade.
For achieving the above object, invention have employed following technical proposal: the preparation method of cationic fixing agent emulsion, is characterized in that, comprises the following steps: the diallylamine of 18%-25% is added reactor by (a); B () regulates PH: regulate PH to be transferred to 2 ~ 3 by acid-base modifier, acid regulator comprises hydrochloric acid, sulfuric acid, and alkali conditioning agent is that liquid caustic soda just can; C () adds 8%-12% acrylamide and 48%-55% water: start stirring, warming while stirring is to 30-50 DEG C simultaneously; D () adds initator and molecular weight regulator 0.2% ~ 0.3%; E () adds 1% diethyl diallyl ammonium chloride solution: keep temperature in the kettle at 30 ~ 50 DEG C, about 0.5-2 hours of time for adding, after dripping off, then heats up 80-90 DEG C, insulation reaction 4-6 hour; After measuring residual list≤2%; F () adds 8%-15% dimethylamine-epichlorohydrin polymer: be incubated at 50-60 DEG C again, reacts 3-5 hours.
In the preparation method of above-mentioned a kind of cationic fixing agent emulsion, described initator is APS, and addition is 0.5-3%.
In the preparation method of above-mentioned a kind of cationic fixing agent emulsion, described molecular weight regulator is isopropyl alcohol.
In the preparation method of above-mentioned a kind of cationic fixing agent emulsion, described reactor adopts 2-10 to rise stainless steel cauldron, speed of agitator 100-500 revs/min.
In the preparation method of above-mentioned a kind of cationic fixing agent emulsion, the content (%) of described diallylamine: be more than or equal to 99%, be less than or equal to 100%, boiling point (DEG C): 111-112 DEG C, fusing point (DEG C) :-88.4 DEG C, index of refraction (20%): 1.440, moisture content (%): be more than or equal to 50%, be less than or equal to 100%.
In the preparation method of above-mentioned a kind of cationic fixing agent emulsion, the solid content of described dimethylamine-epichlorohydrin polymer: be more than or equal to 50%, be less than or equal to 100%, PH(1%): 6-9, viscosity: 500-6500cps.
In the preparation method of above-mentioned a kind of cationic fixing agent emulsion, the content of described acrylamide: be more than or equal to 99%, is less than or equal to 100%, relative density (20 DEG C): 1.122.
In the preparation method of above-mentioned a kind of cationic fixing agent emulsion, the content of described diethyl diallyl ammonium chloride: be more than or equal to 60%, is less than or equal to 100%, PH (%1): 5-7, sodium chloride (%) :≤2%.
Compared with prior art, the advantage of invention is: by this manufacturing technique, can realize processing technology simple, easily manufactured, with low cost, the cationic fixing agent emulsion that yield rate is high; Carry out fixation by adding cationic fixing agent emulsion, product colour fixation is excellent, rub resistance (level) 3-4, washable (level) 3-4, and water-fast (level) can reach 3-4.
Detailed description of the invention
Below in conjunction with in use embodiment, carry out clear, complete description to the technical scheme in inventive embodiments, obviously, described embodiment is only a part of embodiment of invention, instead of whole embodiments.Based on the embodiment in invention, those of ordinary skill in the art are not making the every other embodiment obtained under creative work prerequisite, all belong to the scope of invention protection.
Embodiment 1:
The preparation method of cationic fixing agent emulsion, comprises the following steps: the diallylamine of 18% is added reactor by (a); Reactor adopts 2 liter stainless steel cauldrons, speed of agitator 100 revs/min, the content (%) of described diallylamine: 99%, boiling point (DEG C): 111 DEG C, fusing point (DEG C) :-88.4 DEG C, index of refraction (20%): 1.440; B () regulates PH: regulated by acid-base modifier, acid regulator comprises hydrochloric acid, sulfuric acid, and alkali conditioning agent is that liquid caustic soda just can; C () adds 8% acrylamide and 48% water: start stirring simultaneously, and warming while stirring is to 30 DEG C; The content of described acrylamide: 99.0%, relative density (20 DEG C): 1.122.D () adds initator and the molecular weight regulator of 0.25%, wherein initator is 0.1%, and molecular weight regulator is 0.15%, and initator is APS, and addition is 0.5; Described molecular weight regulator is isopropyl alcohol.E () adds 1% diethyl diallyl ammonium chloride solution: keep temperature in the kettle at 30 DEG C, about 0.5 hour of time for adding, after dripping off, then heats up 80 DEG C, insulation reaction 4 hours; F () adds 8% dimethylamine-epichlorohydrin polymer: be incubated at 50 DEG C again, reacts 3 hours, the solid content of described dimethylamine-epichlorohydrin polymer: 50%, PH(1%): 6, viscosity: 500cps.Finally draw product (silver spins No. 58), outward appearance: pale yellow viscous liquid, solid content: 50 ± 1%, PH(1%): 5-7, viscosity: 1000-6000CPS, residual list (%) :≤2%, inorganic salts (%) :≤2%.
Product colour fixation
Interpretation of result
Show that CATION solid emulsion of the present invention has superior serviceability from above-mentioned fixation result.
Embodiment two
The preparation method of cationic fixing agent emulsion, comprises the following steps: the diallylamine of 21% is added reactor by (a); Reactor adopts 6 liter stainless steel cauldrons, speed of agitator 300 revs/min, the content (%) of described diallylamine: 99.5%, boiling point (DEG C): 111.5 DEG C, fusing point (DEG C) :-88.4 DEG C, index of refraction (20%): 1.440; B () regulates PH: regulated by acid-base modifier, acid regulator comprises hydrochloric acid, sulfuric acid, and alkali conditioning agent is that liquid caustic soda just can; C () adds 10% acrylamide and 51% water: start stirring simultaneously, and warming while stirring is to 40 DEG C; The content of described acrylamide: 99.5%, relative density (20 DEG C): 1.122.D () adds initator and the molecular weight regulator of 0.29%, wherein initator is 0.12%, and molecular weight regulator is 0.17%, and initator is APS, and addition is 2%; Described molecular weight regulator is isopropyl alcohol.E () adds 1% diethyl diallyl ammonium chloride solution: keep temperature in the kettle at 40 DEG C, about 1.2 hours of time for adding, after dripping off, then heats up 85 DEG C, insulation reaction 5 hours; After measuring residual list 1%; F () adds 11% dimethylamine-epichlorohydrin polymer: be incubated at 55 DEG C again, reacts 4 hours, the solid content of described dimethylamine-epichlorohydrin polymer: 75%, PH(1%): 7.5, viscosity: 3000ps.Finally draw product (silver spins No. 58), outward appearance: light yellow viscous liquid, solid content: 50 ± 1%, PH(1%): 5-7, viscosity: 1000-6000CPS, residual list (%) :≤2%, inorganic salts (%) :≤2%.
Product colour fixation
Interpretation of result
Show that CATION solid emulsion of the present invention has superior serviceability from above-mentioned fixation result.
Embodiment three
The preparation method of cationic fixing agent emulsion, comprises the following steps: the diallylamine of 25% is added reactor by (a); Reactor adopts 10 liter stainless steel cauldrons, speed of agitator 500 revs/min, the content (%) of described diallylamine: 100%, boiling point (DEG C): 112 DEG C, fusing point (DEG C) :-88.4 DEG C, index of refraction (20%): 1.440; B () regulates PH: regulated by acid-base modifier, acid regulator comprises hydrochloric acid, sulfuric acid, and alkali conditioning agent is that liquid caustic soda just can; C () adds 12% acrylamide and 55% water: start stirring simultaneously, and warming while stirring is to 50 DEG C; The content of described acrylamide: 100%, relative density (20 DEG C): 1.122.D () adds initator and the molecular weight regulator of 0.3%, wherein initator is 0.15%, and molecular weight regulator is 0.2%, and initator is APS, and addition is 3%; Described molecular weight regulator is isopropyl alcohol.E () adds 1% diethyl diallyl ammonium chloride solution: keep temperature in the kettle at 50 DEG C, time for adding is approximately 2 hours, after dripping off, then heats up 90 DEG C, insulation reaction 6 hours; After measuring residual list 2%; F () adds 15% dimethylamine-epichlorohydrin polymer: be incubated at 60 DEG C again, reacts 5 hours, the solid content of described dimethylamine-epichlorohydrin polymer: 100%, PH(1%): 9, viscosity: 6500cps.Finally draw product (silver spins No. 58), outward appearance: yellow viscous liquid, solid content: 50 ± 1%, PH(1%): 5-7, viscosity: 1000-6000CPS, residual list (%) :≤2%, inorganic salts (%) :≤2%.
Product colour fixation
Interpretation of result
Show that CATION solid emulsion of the present invention has superior serviceability from above-mentioned fixation result.
The foregoing is only invention preferred embodiment, not in order to restriction invention, within all spirit in invention and principle, any amendment made, equivalent replacement, improvement etc., within the protection domain that all should be included in invention.
Claims (9)
1. the preparation method of cationic fixing agent emulsion, is characterized in that, comprises the following steps: the diallylamine of 18%-25% is added reactor by (a); B () regulates PH: regulate PH to be transferred to 2 ~ 3 by acid-base modifier, acid regulator comprises hydrochloric acid, sulfuric acid, and alkali conditioning agent is that liquid caustic soda just can; C () adds 8%-12% acrylamide and 48%-55% water: start stirring, warming while stirring is to 30-50 DEG C simultaneously; D () adds initator and molecular weight regulator 0.2% ~ 0.3%; E () adds 1% diethyl diallyl ammonium chloride solution: keep temperature in the kettle at 30 ~ 50 DEG C, about 0.5-2 hours of time for adding, after dripping off, then heats up 80-90 DEG C, insulation reaction 4-6 hour; After measuring residual list≤2%; F () adds 8%-15% dimethylamine-epichlorohydrin polymer: be incubated at 50-60 DEG C again, reacts 3-5 hours.
2. the preparation method of cationic fixing agent emulsion according to claim 1, is characterized in that, described initator is APS, and addition is 0.5-3%.
3. the preparation method of cationic fixing agent emulsion according to claim 1, is characterized in that, described molecular weight regulator is isopropyl alcohol.
4. the preparation method of cationic fixing agent emulsion according to claim 1, is characterized in that, described reactor adopts 2-10 to rise stainless steel cauldron, speed of agitator 100-500 revs/min.
5. the preparation method of cationic fixing agent emulsion according to claim 1, it is characterized in that, it is characterized in that, the content (%) of described diallylamine: be more than or equal to 99%, be less than or equal to 100%, boiling point (DEG C): 111-112 DEG C, moisture content (%): be more than or equal to 50%, be less than or equal to 100%.
6. the preparation method of cationic fixing agent emulsion according to claim 1, it is characterized in that, the solid content of described dimethylamine-epichlorohydrin polymer: be more than or equal to 50%, be less than or equal to 100%, PH(1%): 6-9, viscosity: 500-6500cps.
7. the preparation method of cationic fixing agent emulsion according to claim 1, is characterized in that, the content of described acrylamide: be more than or equal to 99%, is less than or equal to 100%.
8. the preparation method of cationic fixing agent emulsion according to claim 1, is characterized in that, the content of described acrylamide: >=99.0%.
9. the preparation method of cationic fixing agent emulsion according to claim 1, it is characterized in that, the content of described diethyl diallyl ammonium chloride: be more than or equal to 60%, be less than or equal to 100%, PH (%1): 5-7, sodium chloride (%) :≤2%.
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| CN201511012962.XA CN105568722B (en) | 2015-12-31 | 2015-12-31 | The preparation method of cationic fixing agent lotion |
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| CN201511012962.XA CN105568722B (en) | 2015-12-31 | 2015-12-31 | The preparation method of cationic fixing agent lotion |
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Cited By (6)
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| CN106220785A (en) * | 2016-08-11 | 2016-12-14 | 四川省纺织科学研究院 | A kind of reactive polyquarternium-type is without the preparation method and application of aldehyde fixation crosslinking agent |
| CN106480779A (en) * | 2016-12-12 | 2017-03-08 | 郑州艾莫弗信息技术有限公司 | A kind of paper surface color fixing agent and preparation method thereof |
| CN106758516A (en) * | 2016-12-12 | 2017-05-31 | 刘海平 | The preparation method and obtained color fixing agent of a kind of paper color fixing agent |
| CN110219187A (en) * | 2019-06-22 | 2019-09-10 | 浙江汉邦化工有限公司 | A kind of Roman cloth guarantor color finishing agent |
| 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 |
| CN115094654A (en) * | 2022-08-23 | 2022-09-23 | 江苏富淼科技股份有限公司 | Polymer color fixing agent and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106758516A (en) * | 2016-12-12 | 2017-05-31 | 刘海平 | The preparation method and obtained color fixing agent of a kind of paper color fixing agent |
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| CN110219187A (en) * | 2019-06-22 | 2019-09-10 | 浙江汉邦化工有限公司 | A kind of Roman cloth guarantor color finishing agent |
| 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 |
| CN115094654A (en) * | 2022-08-23 | 2022-09-23 | 江苏富淼科技股份有限公司 | Polymer color fixing agent and preparation method thereof |
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