CN105568722B - The preparation method of cationic fixing agent lotion - Google Patents
The preparation method of cationic fixing agent lotion Download PDFInfo
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- CN105568722B CN105568722B CN201511012962.XA CN201511012962A CN105568722B CN 105568722 B CN105568722 B CN 105568722B CN 201511012962 A CN201511012962 A CN 201511012962A CN 105568722 B CN105568722 B CN 105568722B
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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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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
Invention is related to chemical production technical field, is related to a kind of production method, refers in particular to a kind of preparation method of cationic fixing agent lotion.It is the following steps are included: reaction kettle is added in the diallylamine of 18%-25% by (a)；(b) pH is adjusted, 8%-12% acrylamide and 48%-55% water (c) is added；(d) initiator and molecular weight regulator 0.2% ~ 0.3% is added；(e) 1% diethyl diallyl ammonium chloride solution is added；(f) 8%-15% dimethylamine-epichlorohydrin polymer is added.The advantages of invention is: by the manufacturing process, it is simple to can be realized processing technology, easily manufactured, low in cost, the cationic fixing agent lotion of high yield rate；Fixation is carried out by the way that cationic fixing agent lotion is added, product colour fixation is excellent, rub resistance (grade) 3-4, washable (grade) 3-4, and water-fast (grade) can reach 3-4.
Description
Technical field
Invention is related to chemical production technical field, is related to a kind of production method, refers in particular to a kind of cationic fixing agent cream
The preparation method of liquid.
Background technique
Since dyeing mechanism of the dyestuff on different fibers and dyefastness are different, so the fixation principle of color fixing agent
It is different.The fixation principle of all kinds of dye fixing agent is as follows: generating insoluble color lake direct dyes, acidity using color fixing agent and dyestuff
Dyestuff and reactive dye reduce dyestuff and interfibrous affinity when meeting water because containing hydrophilic radical.Utilize fixation agent molecule
In cationic charge and dyestuff anionic group formed electrostatical binding, generate dyestuff and color fixing agent on fiber insoluble
Color lake, reduces the water solubility of dyestuff, to improve wet colour fastness, improves soaping and calico staining fastness, color fixing agent for dyestuff
Cationic it is stronger, soap, calico staining fastness it is better.If direct dyes, reactive dye are handled with cationic fixing agent,
Generate color lake handled to improve wet fastness direct copper dye with mantoquita, handled after acid dyeing with chromic salts, make dyestuff with
Chelating object is formed between fiber, so that its water solubility is reduced, to improve dyeing.But regardless of being which kind of color fixing agent, current color fixing agent
Production and not perfect, the effect of color fixing agent and effect are simultaneously bad.Usually using PDMDAAC and diethylenetriamine-epoxy chloropropionate
Alkane polymer can only achieve 2-3 as color fixing agent, rub resistance (grade) and washable (grade).
Summary of the invention
The purpose of invention is in view of the above-mentioned problems, providing a kind of can make rub resistance and the high cationic fixation of washable grade
The preparation method of agent emulsion.
In order to achieve the above objectives, invention uses following technical proposal: the preparation method of cationic fixing agent lotion, special
Sign is, comprising the following steps: reaction kettle is added in the diallylamine of 18%-25% by (a)；(b) it adjusts PH: passing through acid-base accommodation
Agent is transferred to 2~3 to adjust PH, and acid regulator includes hydrochloric acid, sulfuric acid, and alkali regulator is liquid alkaline；(c) 8%-12% propylene is added
Amide and 48%-55% water: while stirring is started, warming while stirring is to 30-50 DEG C；(d) initiator and molecular-weight adjusting is added
Agent 0.2%~0.3%；(e) 1% diethyl diallyl ammonium chloride solution is added: keeping temperature in the kettle at 30~50 DEG C, dropwise addition
Between 0.5-2 hours, after dripping off, then heat up 80-90 DEG C, insulation reaction 4-6 hours；After measuring residual list≤2%；(f) 8%- is added
15% dimethylamine-epichlorohydrin polymer: it is kept the temperature again at 50-60 DEG C, is reacted 3-5 hours.
In a kind of preparation method of above-mentioned cationic fixing agent lotion, the initiator is APS, and additive amount is
0.5—3%。
In a kind of preparation method of above-mentioned cationic fixing agent lotion, the molecular weight regulator is isopropanol.
In a kind of preparation method of above-mentioned cationic fixing agent lotion, the reaction kettle is stainless using 2-10 liters
Steel reaction kettle, 100-500 revs/min of speed of agitator.
In a kind of preparation method of above-mentioned cationic fixing agent lotion, the content (%) of the diallylamine: big
In or be 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 (%): greater than or be equal to 50%, be less than or equal to 100%.
In a kind of preparation method of above-mentioned cationic fixing agent lotion, the dimethylamine-epoxychloropropane polymerization
The solid content: greater than of object is equal to 50%, less than or equal to 100%, PH(1%): 6-9, viscosity: 500-6500cps.
In a kind of preparation method of above-mentioned cationic fixing agent lotion, the content: greater than of the acrylamide or
Equal to 99%, it is less than or equal to 100%, relative density (20 DEG C): 1.122.
In a kind of preparation method of above-mentioned cationic fixing agent lotion, the diethyl diallyl ammonium chloride
Content: greater than is equal to 60%, less than or equal to 100%, PH (1%): 5-7, sodium chloride (%) :≤2%.
Compared with prior art, be the advantages of invention: by the manufacturing process, it is simple to can be realized processing technology,
It is easily manufactured, low in cost, the cationic fixing agent lotion of high yield rate；Consolidated by the way that cationic fixing agent lotion is added
Color, product colour fixation is excellent, rub resistance (grade) 3-4, washable (grade) 3-4, and water-fast (grade) can reach 3-4.
Specific embodiment
Below in conjunction with using in embodiment, clear, complete description is carried out to the technical solution in inventive embodiments, is shown
So, described embodiment is only invention a part of the embodiment, instead of all the embodiments.Based on the implementation in invention
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
Invent the range of protection.
Embodiment 1:
The preparation method of cationic fixing agent lotion, comprising the following steps: reaction is added in 18% diallylamine by (a)
Kettle；Reaction kettle use 2 liter stainless steel cauldrons, 100 revs/min of speed of agitator, the content (%) of the diallylamine:
99%, boiling point (DEG C): 111 DEG C, fusing point (DEG C): -88.4 DEG C, index of refraction (20%): 1.440；(b) it adjusts PH: passing through acid-base accommodation
Agent is adjusted, and acid regulator includes hydrochloric acid, sulfuric acid, and alkali regulator is liquid alkaline；(c) 8% acrylamide and 48% water is added: same
Shi Kaidong stirring, warming while stirring is to 30 DEG C；The content of the acrylamide: 99.0%, relative density (20 DEG C):
1.122.(d) 0.25% initiator and molecular weight regulator is added, wherein initiator is 0.1%, and molecular weight regulator is
0.15%, initiator APS, additive amount 0.5；The molecular weight regulator is isopropanol.(e) 1% diethyl diene is added
Propyl ammonium chloride solution: keeping temperature in the kettle at 30 DEG C, time for adding 0.5 hour, after dripping off, then heat up 80 DEG C, insulation reaction 4
Hour；(f) 8% dimethylamine-epichlorohydrin polymer is added: is kept the temperature again at 50 DEG C, is reacted 3 hours, the dimethylamine-
The solid content of epichlorohydrin polymer: 50%, PH(1%): 6, viscosity: 500cps.Finally obtain product (silver spins No. 58), outside
See: 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
From above-mentioned fixation the result shows that cationic solid emulsion of the invention has superior service performance.
Embodiment two
The preparation method of cationic fixing agent lotion, comprising the following steps: reaction is added in 21% diallylamine by (a)
Kettle；Reaction kettle use 6 liter stainless steel cauldrons, 300 revs/min of speed of agitator, the content (%) of the 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) it adjusts PH: passing through soda acid
Regulator is adjusted, and acid regulator includes hydrochloric acid, sulfuric acid, and alkali regulator is liquid alkaline；(c) 10% acrylamide and 51% is added
Water: while stirring is started, warming while stirring is to 40 DEG C；The content of the acrylamide: 99.5%, relative density (20 DEG C):
1.122.(d) 0.29% initiator and molecular weight regulator is added, wherein initiator is 0.12%, and molecular weight regulator is
0.17%, initiator APS, additive amount 2%；The molecular weight regulator is isopropanol.(e) 1% diethyl, two allyl is added
Ammonium chloride solution: it keeps temperature in the kettle at 40 DEG C, time for adding 1.2 hours, after dripping off, then heats up 85 DEG C, insulation reaction 5 is small
When；After measuring residual list 1%；(f) 11% dimethylamine-epichlorohydrin polymer is added: is kept the temperature again at 55 DEG C, is reacted 4 hours, institute
Dimethylamine-epichlorohydrin polymer the solid content stated: 75%, PH(1%): 7.5, viscosity: 3000ps.Finally obtain product
(silver spins No. 58), 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
From above-mentioned fixation the result shows that cationic solid emulsion of the invention has superior service performance.
Embodiment three
The preparation method of cationic fixing agent lotion, comprising the following steps: reaction is added in 25% diallylamine by (a)
Kettle；Reaction kettle use 10 liter stainless steel cauldrons, 500 revs/min of speed of agitator, the content (%) of the diallylamine:
100%, boiling point (DEG C): 112 DEG C, fusing point (DEG C): -88.4 DEG C, index of refraction (20%): 1.440；(b) it adjusts PH: passing through acid-base accommodation
Agent is adjusted, and acid regulator includes hydrochloric acid, sulfuric acid, and alkali regulator is liquid alkaline；(c) 12% acrylamide and 55% water is added:
Stirring is started simultaneously, warming while stirring is to 50 DEG C；The content of the acrylamide: 100%, relative density (20 DEG C):
1.122.(d) 0.3% initiator and molecular weight regulator is added, wherein initiator is 0.15%, molecular weight regulator 0.2%,
Initiator is APS, additive amount 3%；The molecular weight regulator is isopropanol.(e) 1% diethyl diallyl chlorination is added
Ammonium salt solution: keeping temperature in the kettle at 50 DEG C, and time for adding is 2 hours, after dripping off, then heats up 90 DEG C, and insulation reaction 6 hours；It surveys
After fixed residual list 2%；(f) 15% dimethylamine-epichlorohydrin polymer is added: is kept the temperature again at 60 DEG C, reaction 5 hours, described two
Methylamine-epichlorohydrin polymer solid content: 100%, PH(1%): 9, viscosity: 6500cps.Finally show that (silver spins 58 to product
Number), 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
From above-mentioned fixation the result shows that cationic solid emulsion of the invention has superior service performance.
The foregoing is merely invention preferred embodiments, not to limit invention, all spirit and principle in invention
Within, any modification, equivalent substitution, improvement and etc. done should be included within the protection scope of invention.
Claims (9)
1. the preparation method of cationic fixing agent lotion, which comprises the following steps: (a) is by two allyls of 18%-25%
Reaction kettle is added in base amine；(b) it adjusts pH: adjusting pH by acid-base modifier and be transferred to 2~3, acid regulator includes hydrochloric acid, sulphur
Acid, alkali regulator are liquid alkaline；(c) 8%-12% acrylamide and 48%-55% water is added: while stirring is started, while stirring
It is warming up to 30-50 DEG C；(d) initiator and molecular weight regulator 0.2%~0.3% is added；(e) 1% diethyl diallyl is added
Ammonium chloride solution: keeping temperature in the kettle at 30~50 DEG C, time for adding 0.5-2 hours, after dripping off, then heat up 80-90 DEG C, protects
Temperature reaction 4-6 hours；After measuring residual list≤2%；(f) 8%-15% dimethylamine-epichlorohydrin polymer is added: keeping the temperature again
It 50-60 DEG C, reacts 3-5 hours.
2. the preparation method of cationic fixing agent lotion according to claim 1, which is characterized in that the initiator is
APS, additive amount are 0.5-3%.
3. the preparation method of cationic fixing agent lotion according to claim 1, which is characterized in that the molecular weight tune
Section agent is isopropanol.
4. the preparation method of cationic fixing agent lotion according to claim 1, which is characterized in that the reaction kettle is adopted
With 2-10 liters of stainless steel cauldrons, 100-500 revs/min of speed of agitator.
5. the preparation method of cationic fixing agent lotion according to claim 1, which is characterized in that the diallyl
The content (%): greater than of amine is equal to 99%, is less than or equal to 100%, boiling point (DEG C): 111-112 DEG C, moisture content (%): greater than or waiting
In 50%, it is less than or equal to 100%.
6. the preparation method of cationic fixing agent lotion according to claim 1, which is characterized in that the dimethylamine-
The solid content: greater than of epichlorohydrin polymer is equal to 50%, less than or equal to 100%, pH(1%): 6-9, viscosity: 500-
6500cps。
7. the preparation method of cationic fixing agent lotion according to claim 1, which is characterized in that the acrylamide
Content: greater than or be equal to 99%, be less than or equal to 100%.
8. the preparation method of cationic fixing agent lotion according to claim 1, which is characterized in that the acrylamide
Content: >=99.0%.
9. the preparation method of cationic fixing agent lotion according to claim 1, which is characterized in that the diethyl two
The content: greater than of allyl ammonium chloride is equal to 60%, less than or equal to 100%, pH(1%): 5-7, sodium chloride (%) :≤2%.
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| CN106220785B (en) * | 2016-08-11 | 2019-03-29 | 四川省纺织科学研究院 | A kind of preparation method and application of the reactivity polyquarternium-type without aldehyde fixation crosslinking agent |
| CN108118557A (en) * | 2016-12-12 | 2018-06-05 | 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 |
| CN106758516B (en) * | 2016-12-12 | 2018-03-23 | 江西德盛精细化学品有限公司 | A kind of preparation method of paper color fixing agent and obtained 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 |
| CN111676718B (en) * | 2020-07-16 | 2023-01-10 | 青岛福凯橡塑新材料有限公司 | Weather-resistant color fastness improver for reactive dye and preparation method and application thereof |
| CN115094654B (en) * | 2022-08-23 | 2022-12-20 | 江苏富淼科技股份有限公司 | Polymer color fixing agent and preparation method thereof |
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