CN101260625A - Nanometer formaldehyde-free dye-fixing agent and method for making same - Google Patents
Nanometer formaldehyde-free dye-fixing agent and method for making same Download PDFInfo
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- CN101260625A CN101260625A CNA2008100606586A CN200810060658A CN101260625A CN 101260625 A CN101260625 A CN 101260625A CN A2008100606586 A CNA2008100606586 A CN A2008100606586A CN 200810060658 A CN200810060658 A CN 200810060658A CN 101260625 A CN101260625 A CN 101260625A
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Abstract
The invention discloses a nano nonformaldehyde fixing agent and a preparation method thereof. The fixing agent takes a diene-CDESA as a monomer, takes a diallyl amine and a nano zinc oxide as carriers and takes a sodium peroxydisulfate and a sodium meta-bisulphite as a multipolymer synthesized by an evocating agent. Compared with the prior art, the nano nonformaldehyde fixing agent synthesized by the invention does not contain formaldehyde or APEO, has good color fixing performance and effect and provides an ideal green fixing agent; the textile using the fixing agent to fix color does not change the color, has the dry and wet frictional fastness, the light fastness, the fastness to chlorine and the anti-staining fastness which are up to the Euramerican standard and the international ecological textiles standard, and has the functions of insect resistance, rot resistance and UV protection.
Description
Technical field
The present invention relates to a kind of nanometer formaldehyde-free dye-fixing agent and preparation method thereof, belong to the printing and dyeing assistant technical field.
Background technology
Current textile dyeing is mainly based on reactive dyeing, owing to contain hydrophily groups such as sulfonic group, carboxylic acid group in the reactive dyestuff molecule structure, it is limited to tend to the amount of dye that takes place because of its set of excessive concentration when dying dark color, make and had a large amount of not set dyestuffs on the dyeing and weaving thing, cause dyefastness defective, wet colour fastness is poor; The dye particle size also can influence the soaping fastness of dyeing, causes wet colour fastness defective; Therefore must improve by the dyefastness of dyeing and weaving thing with color-fixing agent.The color-fixing agent that past adopts contains formaldehyde or APEO (alkylphenol polyoxyethylene) mostly, but outstanding because of its fixing property, and the many producers of economical and practical dark audient welcome.But people's environmental consciousness constantly strengthens in recent years, along with the restriction of some country PARA FORMALDEHYDE PRILLS(91,95) content with to the control of limiting the quantity of of APEO, make the color-fixing agent that contains formaldehyde or APEO be eliminated gradually, the environment-friend substitution work of formaldehyde, APEO is very urgent in the textile auxiliary, and printing and dyeing producer also grows with each passing day to the demand of environment protection type color fixing agent.
Recent years, formaldehyde-free color fixing agent has report in disclosed patent documentation the time, as the patent application that application number is 01119412, name is called environment protection type color fixing agent, this environment protection type color fixing agent is made up of chitin, high-efficient penetrant OP-6, fatty alcohol-polyoxyethylene ether, water, though do not contain formaldehyde, but its fixing property and effect are not ideal, and OP series belongs to octyl phenol, and being under an embargo is used for textiles and leather and fur products; The patent No. is that 03114001.7 patent also discloses the formaldehyde-free color fixing agent that a kind of diethylenetriamine and epoxychloropropane are made, but its prescription is single, and colour fixation is undesirable; Application number is that 200610096042.5 patent application discloses the formaldehyde-free color fixing agent that a kind of ethyl acrylate, acrylic acid, sodium pyrosulfite and diethylenetriamine, epoxychloropropane are made again, increased by three kinds of raw materials on 03114001.7 basis, its colour fixation is also not ideal enough.
Summary of the invention
The objective of the invention is to, a kind of nanometer formaldehyde-free dye-fixing agent and preparation method thereof is provided.The present invention is directed to the deficiency of existing not environmental protection of color-fixing agent (containing formaldehyde or APEO) and formaldehyde-free color fixing agent performance, is monomer with the diallyl ammonium chloride, has synthesized the good environmental type color-fixing agent of a kind of colour fixation through causing copolymerization.
Technical scheme of the present invention: a kind of nanometer formaldehyde-free dye-fixing agent, it is to be monomer with the diallyl ammonium chloride, and diallyl ammonium and nanometer titanium dioxide zinc are carrier, and sodium peroxydisulfate and sodium pyrosulfite are the synthetic copolymer of initator, and its structural formula is:
Specifically, according to listed as parts by weight, it is that raw material reaction is synthetic for 3～5 parts with 800～880 parts of diallyl ammonium chlorides, 70～90 parts of diallyl ammoniums, 8～12 parts on nanometer titanium dioxide zinc, 3～5 parts of sodium peroxydisulfates and sodium pyrosulfite.
More precisely, according to listed as parts by weight, it is that raw material reaction is synthetic for 4 parts with 840 parts of diallyl ammonium chlorides, 80 parts of diallyl ammoniums, 10 parts on nanometer titanium dioxide zinc, 4 parts of sodium peroxydisulfates and sodium pyrosulfite.
The particle diameter of described nanometer titanium dioxide zinc is 30～100nm.
Described nanometer titanium dioxide zinc is used the strong acid acidifying of equivalent weight in advance; Described sodium peroxydisulfate and sodium pyrosulfite each deionized water dissolving with 10 times of weight in advance are mixed with the aqueous solution.
The preparation method of nanometer formaldehyde-free dye-fixing agent is: nanometer titanium dioxide zinc is mixed with two rare propyl ammoniums with after the strong acid acidifying of equivalent weight, place containers for future use; With each deionized water dissolving with 10 times of weight of sodium peroxydisulfate and sodium pyrosulfite, it is standby to be mixed with the aqueous solution; Diallyl ammonium chloride is added in the reactor, open and stir, when being warming up to 50 ℃ the mixture adding of two rare propyl ammoniums and nanometer titanium dioxide zinc is stirred; When rising to 60 ℃, reactor temperature stops to heat, open cooling water, begin intersection and drip sodium peroxydisulfate, metabisulfite solution, reactor temperature stops when rising to 80 ℃ dripping, treat to be cooled to 80 ℃ after the product implode in the still, again remaining sodium peroxydisulfate and metabisulfite solution are dropwised, survey the pH value and the viscosity of product in the still behind 80 ℃～85 ℃ insulation reaction 1h, when pH value is 4～6, be reaction end during viscosity 500～1500mPas, cooling discharge promptly gets nanometer formaldehyde-free dye-fixing agent.
Described strong acid is hydrochloric acid or sulfuric acid.
This color-fixing agent utilization has the alkene of quaternary ammonium salt, and the high polymer that is polymerized as two rare propyl ammonium chlorides and two rare propyl ammoniums (homopolymers or with the copolymer of basic ammonium monomer copolymerization) is by cation group and film forming and reach best fixation purpose.And in polymerization process grafting have the nanometer titanium dioxide zinc of antiultraviolet, mothproof, antimildew function.4～5 grades of the fabric unlubricated friction fastness of handling with this color-fixing agent, wet 2.5～3 grades of the fastness of rubbing, 4 grades of light fastnesss, 3～4 grades of chlorine fastness, 4～5 grades of anti-staining fastnesses meet American-European standard and international ecological textile standards fully, and every index is considerably beyond traditional color-fixing agent.
Compared with prior art, the present invention is monomer with the diallyl ammonium chloride, does not contain formaldehyde and APEO through causing the synthetic nanometer formaldehyde-free dye-fixing agent of copolymerization, and fixing property and colour fixation are good, and a kind of even more ideal environmental type color-fixing agent is provided; With the colourless change of the fabric of this color-fixing agent fixation, do, the wet fastness of rubbing, light fastness, chlorine fastness, anti-staining fastness has all reached American-European standard and international ecological textile standards, and has the function of mothproof, mildew-resistant, antiultraviolet.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment.
Embodiments of the invention 1: get diallyl ammonium chloride 840Kg, diallyl ammonium 80Kg, nanometer titanium dioxide zinc (50～80nm) 10Kg, sodium peroxydisulfate 4Kg, sodium pyrosulfite 4Kg.
Preparation technology:, place containers for future use with mixing with two rare propyl ammoniums behind the nanometer titanium dioxide zinc usefulness 10Kg hcl acidifying; Each uses the 40Kg deionized water dissolving with sodium peroxydisulfate and sodium pyrosulfite, and it is standby to be mixed with the aqueous solution; Diallyl ammonium chloride is added in the reactor, open and stir, when being warming up to 50 ℃ the mixture adding of two rare propyl ammoniums and nanometer titanium dioxide zinc is stirred; When rising to 60 ℃, reactor temperature stops to heat, open cooling water, begin intersection and drip sodium peroxydisulfate, metabisulfite solution, reactor temperature stops when rising to 80 ℃ dripping, treat to be cooled to 80 ℃ after the product implode in the still, again remaining sodium peroxydisulfate and metabisulfite solution are dropwised, survey the pH value and the viscosity of product in the still behind 80 ℃～85 ℃ insulation reaction 1h, when pH value is 4～6, be reaction end during viscosity 500～1500mPas, cooling discharge promptly gets nanometer formaldehyde-free dye-fixing agent.
Embodiments of the invention 2: get diallyl ammonium chloride 800 weight portions, diallyl ammonium 90 weight portions, nanometer titanium dioxide zinc (30～100nm) 8 weight portions, sodium peroxydisulfate 5 weight portions, sodium pyrosulfite 3 weight portions.
Nanometer titanium dioxide zinc is mixed with two rare propyl ammoniums after with 8 weight portion sulfuric acid acidations, place containers for future use; Sodium peroxydisulfate is dissolved with 50 parts by weight of deionized water, and sodium pyrosulfite dissolves with 30 parts by weight of deionized water, and it is standby to be mixed with the aqueous solution separately; Be prepared into nanometer formaldehyde-free dye-fixing agent with embodiment 1 described method then.
Embodiments of the invention 3: get diallyl ammonium chloride 880 weight portions, diallyl ammonium 70 weight portions, nanometer titanium dioxide zinc 12 weight portions, sodium peroxydisulfate 3 weight portions, sodium pyrosulfite 5 weight portions.
Nanometer titanium dioxide zinc is mixed with two rare propyl ammoniums after with 12 weight portion hcl acidifyings, place containers for future use; Sodium peroxydisulfate is dissolved with 30 parts by weight of deionized water, and sodium pyrosulfite dissolves with 50 parts by weight of deionized water, and it is standby to be mixed with the aqueous solution separately; Be prepared into nanometer formaldehyde-free dye-fixing agent with embodiment 1 described method then.
Claims (7)
1. nanometer formaldehyde-free dye-fixing agent, it is characterized in that: it is to be monomer with the diallyl ammonium chloride, and diallyl ammonium and nanometer titanium dioxide zinc are carrier, and sodium peroxydisulfate and sodium pyrosulfite are the synthetic copolymer of initator, and its structural formula is:
2. nanometer formaldehyde-free dye-fixing agent according to claim 1, it is characterized in that: according to listed as parts by weight, it is to be that raw material reaction is synthetic for 3～5 parts with 800～880 parts of diallyl ammonium chlorides, 70～90 parts of diallyl ammoniums, 8～12 parts on nanometer titanium dioxide zinc, 3～5 parts of sodium peroxydisulfates and sodium pyrosulfite.
3. nanometer formaldehyde-free dye-fixing agent according to claim 2, it is characterized in that: according to listed as parts by weight, it is to be that raw material reaction is synthetic for 4 parts with 840 parts of diallyl ammonium chlorides, 80 parts of diallyl ammoniums, 10 parts on nanometer titanium dioxide zinc, 4 parts of sodium peroxydisulfates and sodium pyrosulfite.
4. according to claim 1,2 or 3 described nanometer formaldehyde-free dye-fixing agents, it is characterized in that: the particle diameter of described nanometer titanium dioxide zinc is 30～100nm.
5. according to claim 1,2 or 3 described nanometer formaldehyde-free dye-fixing agents, it is characterized in that: described nanometer titanium dioxide zinc is used the strong acid acidifying of equivalent weight in advance; Described sodium peroxydisulfate and sodium pyrosulfite each deionized water dissolving with 10 times of weight in advance are mixed with the aqueous solution.
6. as the preparation method of each described nanometer formaldehyde-free dye-fixing agent among the claim 1-5, it is characterized in that: nanometer titanium dioxide zinc is mixed with two rare propyl ammoniums with after the strong acid acidifying of equivalent weight, place containers for future use; With each deionized water dissolving with 10 times of weight of sodium peroxydisulfate and sodium pyrosulfite, it is standby to be mixed with the aqueous solution; Diallyl ammonium chloride is added in the reactor, open and stir, when being warming up to 50 ℃ the mixture adding of two rare propyl ammoniums and nanometer titanium dioxide zinc is stirred; When rising to 60 ℃, reactor temperature stops to heat, open cooling water, begin intersection and drip sodium peroxydisulfate, metabisulfite solution, reactor temperature stops when rising to 80 ℃ dripping, treat to be cooled to 80 ℃ after the product implode in the still, again remaining sodium peroxydisulfate and metabisulfite solution are dropwised, survey the pH value and the viscosity of product in the still behind 80 ℃～85 ℃ insulation reaction 1h, when pH value is 4～6, be reaction end during viscosity 500～1500mPas, cooling discharge promptly gets nanometer formaldehyde-free dye-fixing agent.
7. the preparation method of nanometer formaldehyde-free dye-fixing agent according to claim 6, it is characterized in that: described strong acid is hydrochloric acid or sulfuric acid.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100606586A CN101260625A (en) | 2008-04-24 | 2008-04-24 | Nanometer formaldehyde-free dye-fixing agent and method for making same |
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| CNA2008100606586A CN101260625A (en) | 2008-04-24 | 2008-04-24 | Nanometer formaldehyde-free dye-fixing agent and method for making same |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102409568A (en) * | 2011-11-17 | 2012-04-11 | 烟台大学 | Preparation method of hydrophilic cationic formaldehyde-free fixing agent |
| CN103114471A (en) * | 2013-02-04 | 2013-05-22 | 苏州经贸职业技术学院 | Method for synthesizing multi-functional color fixing agent of silk fabrics |
| CN103726369A (en) * | 2013-11-08 | 2014-04-16 | 绍兴鼎翔纺织品贸易有限公司 | Cationic fixing agent emulsion and preparation method thereof |
| CN103898777A (en) * | 2014-04-10 | 2014-07-02 | 广东溢达纺织有限公司 | Method for improving dyeing fixing rate of reactive dye |
| CN104328698A (en) * | 2014-09-25 | 2015-02-04 | 浙江弘盛印染有限公司 | Binary co-polymerized positive ion formaldehyde-free color-fixing agent and synthetic method thereof |
| CN104452366A (en) * | 2014-11-17 | 2015-03-25 | 太仓运通生物化工有限公司 | Formaldehyde-free color-fixing agent and preparation method of color-fixing agent |
| CN105755870A (en) * | 2016-02-26 | 2016-07-13 | 苏州三和开泰花线织造有限公司 | Alkali-resistant chlorine-resistant type aldehyde-free active dye color fixing agent and preparation method thereof |
| CN111287002A (en) * | 2020-03-26 | 2020-06-16 | 刘俊文 | Formaldehyde-free chlorine-resistant color fixing agent and preparation method thereof |
-
2008
- 2008-04-24 CN CNA2008100606586A patent/CN101260625A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102409568A (en) * | 2011-11-17 | 2012-04-11 | 烟台大学 | Preparation method of hydrophilic cationic formaldehyde-free fixing agent |
| CN102409568B (en) * | 2011-11-17 | 2013-06-19 | 烟台大学 | Preparation method of hydrophilic cationic formaldehyde-free fixing agent |
| CN103114471A (en) * | 2013-02-04 | 2013-05-22 | 苏州经贸职业技术学院 | Method for synthesizing multi-functional color fixing agent of silk fabrics |
| CN103726369A (en) * | 2013-11-08 | 2014-04-16 | 绍兴鼎翔纺织品贸易有限公司 | Cationic fixing agent emulsion and preparation method thereof |
| CN103898777A (en) * | 2014-04-10 | 2014-07-02 | 广东溢达纺织有限公司 | Method for improving dyeing fixing rate of reactive dye |
| CN103898777B (en) * | 2014-04-10 | 2016-02-24 | 广东溢达纺织有限公司 | A kind of method improving reactive dyeing degree of fixation |
| CN104328698A (en) * | 2014-09-25 | 2015-02-04 | 浙江弘盛印染有限公司 | Binary co-polymerized positive ion formaldehyde-free color-fixing agent and synthetic method thereof |
| CN104452366A (en) * | 2014-11-17 | 2015-03-25 | 太仓运通生物化工有限公司 | Formaldehyde-free color-fixing agent and preparation method of color-fixing agent |
| CN105755870A (en) * | 2016-02-26 | 2016-07-13 | 苏州三和开泰花线织造有限公司 | Alkali-resistant chlorine-resistant type aldehyde-free active dye color fixing agent and preparation method thereof |
| CN111287002A (en) * | 2020-03-26 | 2020-06-16 | 刘俊文 | Formaldehyde-free chlorine-resistant color fixing agent and preparation method thereof |
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Open date: 20080910 |