CN113089345B - Amphoteric polyamine high-molecular polymerization viscose cotton blending leveling agent and preparation method thereof - Google Patents
Amphoteric polyamine high-molecular polymerization viscose cotton blending leveling agent and preparation method thereof Download PDFInfo
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- CN113089345B CN113089345B CN202110520183.XA CN202110520183A CN113089345B CN 113089345 B CN113089345 B CN 113089345B CN 202110520183 A CN202110520183 A CN 202110520183A CN 113089345 B CN113089345 B CN 113089345B
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- acryloylethylenediamine
- ethylenediamine
- succinic acid
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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
- 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
- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5207—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- D06P1/525—Polymers of unsaturated carboxylic acids or functional derivatives thereof
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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
- 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
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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
- 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
- D06P3/82—Textiles which contain different kinds of fibres
- D06P3/8204—Textiles which contain different kinds of fibres fibres of different chemical nature
- D06P3/828—Textiles which contain different kinds of fibres fibres of different chemical nature mixtures of fibres containing hydroxyl groups
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention discloses an amphoteric polyamine high molecular polymerization viscose cotton blending leveling agent and a preparation method thereof, wherein the viscose cotton leveling agent comprises the following components: the polymer of the acryloylethylenediamine and the acryloylethylenediamine succinic acid, the polycondensate of the polyacrylaylethylenediamine succinic acid and ethylenediamine, a solvent and deionized water. The invention adopts the amphoteric polyamine high molecular polymerization viscose cotton blending leveling agent and the preparation method to synthesize a series of amphoteric ion polymers and polyamide compounds, no waste gas is generated in the synthesis process, the purpose of leveling is achieved by solubilizing and slowly dyeing the dye, and the leveling agent has almost no stimulation to organisms and is easy to biodegrade.
Description
Technical Field
The invention relates to the technical field of fabric treatment, in particular to an amphoteric polyamine high-molecular polymerization viscose cotton blending leveling agent and a preparation method thereof.
Background
The viscose belongs to regenerated cellulose fibers, is prepared from natural fibers through chemical modification, has multiple advantages of the chemical fibers and the cellulose fibers, has good soft and smooth fabric hand feeling, and is superior in fabric taking, but the viscose fibers are poor in heat resistance, alkali resistance and friction resistance, so that the viscose blend fibers are fast in growth in recent years, and particularly, the viscose and cotton blends are outstanding.
Viscose cotton blend fibers are usually dyed by a reactive dye one-bath method, however, the dyeing properties of the two fibers are greatly different. The reactive dye is usually dyed in amorphous areas of cellulose fibers through three steps of diffusion, adsorption and fixation. The ratio of the surface layer structure to the amorphous region of the cellulose fiber greatly influences the diffusion and adsorption processes of the reactive dye. Unlike cotton fibers, the amorphous area ratio of melt spun viscose fibers is high. The unique sheath-core structure of the viscose fiber results in an increased initial difficulty in diffusing the dye into the interior. The structural difference of the two fibers is combined, so that the final color of the viscose is deeper than that of the cotton fibers and the probability of the surface color flowers is larger. This can lead to particularly difficult control of the dyeing uniformity of viscose cotton.
According to the composition and the preparation method of the reactive printing leveling agent for the rayon, the penetration and dispersion of dye to viscose fibers are improved through the compounding of alkyl polyether modified pyrrolidone carboxylic acid alkali metal salt and aliphatic amine polyether, and the uniform color of the viscose fibers is ensured. However, this merely promotes the penetration of viscose fiber in the core structure, and the color light difference caused by the difference of the amorphous front region of cotton cellulose is not solved. And dyeing is different from printing, and the dyeing characteristics of the dye are also greatly different under the condition of taking a large amount of water as a solvent and high salt and high alkali. Viscose cotton blend fiber dyeing is always a problem to be solved in the printing and dyeing industry, and the most central problem for solving the problem is the research and development of a high-performance leveling agent for fabric processing.
In summary, it can be seen that, for processing viscose cotton fabric, the conventional active leveling agent with chelating and dispersing functions as the main components cannot meet the process requirements. In order to ensure uniform color light of viscose cotton, the need for new efficient reactive leveling agents would be urgent and necessary.
Disclosure of Invention
The invention aims to provide a amphoteric polyamine high molecular polymerization viscose cotton blending leveling agent and a preparation method thereof, and a series of amphoteric ion polymers and polyamide compounds are synthesized, and no waste gas is generated in the synthesis process; the dye is solubilized and slowly dyed to achieve the aim of leveling, and the leveling agent has almost no stimulation to organisms and is easy to biodegrade.
In order to achieve the above purpose, the invention provides a zwitterionic polymeric viscose cotton blending leveling agent, which comprises the following components: the polymer of the acryloylethylenediamine and the acryloylethylenediamine succinic acid, the polycondensate of the polyacrylaylethylenediamine succinic acid and ethylenediamine, a solvent and deionized water;
the structural formula of the copolymer of ethylene propylene diamine and sodium ethylene propylene diamine succinate is as follows:
the structural formula of the polycondensate of the poly (ethylene diamine succinate) and the ethylene diamine is as follows:
wherein the weight ratio of each component is as follows: 10-30% of ethylene diamine propylene, 10-30% of ethylene diamine propylene succinate and ethylene diamine polycondensate, and 20-50% of deionized water.
Preferably, the components and weight ratio thereof are 20-30% of copolymer of acrylic ethylenediamine and propylene ethylenediamine succinic acid, 20-30% of polycondensate of acrylic ethylenediamine succinic acid and ethylenediamine, and 30-50% of deionized water.
The preparation method of the zwitterionic polymeric viscose cotton blending leveling agent is characterized by comprising the following steps of:
(1) Synthesis of copolymer of Acryloylethylenediamine and propylene Ethylenediamine succinic acid
a. Adding acrylamide ethylenediamine and deionized water into a four-neck flask with a thermometer, a water separator and a condensation reflux device, and filling nitrogen to remove air;
b. starting a stirring device, slowly heating to 70-110 ℃, starting to slowly dropwise add the initiator aqueous solution, finishing dropwise adding within 1-2h, and performing constant-temperature reaction for 2-3h after dropwise adding;
c. cooling to 50-70deg.C, adding maleic anhydride, stirring thoroughly, keeping the temperature for 2-3 hr, adding alkaline agent, adjusting pH to 8-9, and charging nitrogen to drive away air;
d. adding 4-dimethylaminopyridine, sealing the reaction kettle, opening a condensing reflux device, heating to 110-160 ℃, keeping the temperature for 2-3 hours, and cooling and discharging;
(2) Synthesis of polycondensates of polyacrylamidesuccinic acid and ethylenediamine
e. Adding acrylamide ethylenediamine and deionized water into a four-neck flask with a thermometer, a water separator and a condensation reflux device, and filling nitrogen to remove air;
f. starting a stirring device, slowly heating to 70-110 ℃, starting to slowly dropwise add an initiator aqueous solution, finishing dropwise adding within 1-2h, and performing constant-temperature reaction for 2-3h after dropwise adding;
g. cooling to 50-70deg.C, adding maleic anhydride, stirring thoroughly, keeping the temperature for 2-3 hr, adding alkaline agent, adjusting pH to 9-10, and charging nitrogen to drive away air;
h. adding 4-dimethylaminopyridine, sealing the reaction kettle, opening a condensing reflux device, heating to 110-160 ℃, keeping the temperature for 2-3 hours, cooling, adding an acid agent for acidification, precipitating, filtering, drying and crystallizing;
i. adding the crystallized product into the four-mouth flasks, adding ethylenediamine, heating to 60-80 ℃, fully stirring, and filling nitrogen to drive air;
j. adding an amidation reaction catalyst, stopping pumping nitrogen, starting pumping vacuum, slowly heating to 140-160 ℃, keeping the temperature for 3-5 hours, and cooling to obtain the material;
(2) Compounding of viscose cotton leveling agent
According to the formula amount, the ethylene diamine and propylene copolymer, the poly (ethylene diamine) succinate and the ethylene diamine polycondensate and deionized water are compounded, fully and uniformly stirred at 60-80 ℃, and then cooled, filtered and discharged.
Preferably, the components are 80-110 parts of the acrylamide ethylenediamine, 0.5-1 part of the initiator, 10-22 parts of the maleic anhydride, 1-2 parts of the affinity addition catalyst, 3-8 parts of the alkaline agent, 5-15 parts of the ethylenediamine and 0.5-2 parts of the amidation reaction catalyst.
Preferably, the nucleophilic addition catalyst is 4-dimethylaminopyridine.
Preferably, the amidation reaction catalyst is ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride.
Preferably, the initiator is one or more of ammonium persulfate and potassium persulfate.
Preferably, the alkaline agent is one or more of sodium hydroxide and sodium carbonate.
Preferably, the acid agent is hydrochloric acid.
The invention has the beneficial effects that:
(1) The reactive dye can be effectively solubilized by compounding the copolymer of the acryloylethylenediamine and the propylene ethylenediamine succinic acid and the polycondensate of the polyacrylaylethylenediamine succinic acid and ethylenediamine, and the reactive dye is prevented from aggregation and sedimentation under the condition of high salt, which is different from the anion dispersion stabilization mechanism of the conventional leveling agent.
(2) The product provided by the invention contains a large amount of amine and amide groups, anionic dye can be dissolved by charge effect, and simultaneously, the double-ion can ensure that the ionic bonding of the viscose cotton leveling agent and the reactive dye is weak bonding, and the fiber is dyed gradually along with the rising of temperature, so that the effect of slow dyeing is achieved.
(3) The large amount of amine groups in the leveling agent system can neutralize the negative charge of the fiber, is favorable for reducing the consumption of anhydrous sodium sulfate dyed in the dye bath, and the catalytic activity of the amide can improve the fixation efficiency of the reactive dye in the dye bath, so that the aim of reducing the discharge of high salt and high alkali is fulfilled.
The technical scheme of the invention is further described in detail through examples.
Detailed Description
The technical scheme of the invention is further described below by examples.
Example 1
85 parts of acryloylethylenediamine, 0.5 part of initiator, 13 parts of maleic anhydride, 1 part of affinity addition catalyst, 4 parts of alkaline agent, 6 parts of ethylenediamine and 0.5 part of amidation reaction catalyst, wherein the nucleophilic addition catalyst is 4-dimethylaminopyridine, the amide condensation catalyst is ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, the initiator is ammonium persulfate, the alkaline agent is sodium hydroxide and the acid agent is hydrochloric acid.
(1) Synthesis of copolymer of Acryloylethylenediamine and propylene Ethylenediamine succinic acid
a. The four-mouth flask equipped with a thermometer, a water separator and a condensation reflux device is filled with acrylamide ethylenediamine and deionized water, and nitrogen is filled to remove air.
b. And (3) starting a stirring device, slowly heating to 70-110 ℃, starting to slowly dropwise add the ammonium persulfate aqueous solution, finishing dropwise adding within 1-2h, and performing constant-temperature reaction for 2-3h after dropwise adding.
c. Cooling to 50-70deg.C, adding maleic anhydride, stirring thoroughly, keeping the temperature for 2-3 hr, adding sodium hydroxide to adjust pH to 8-9, and charging nitrogen gas to drive away air.
d. Adding 4-dimethylaminopyridine, sealing the reaction kettle, and opening a condensing reflux device. Heating to 110-160 ℃, keeping the temperature for 2-3 hours, and then cooling and discharging.
(2) Synthesis of polycondensates of polyacrylamidesuccinic acid and ethylenediamine
e. The four-mouth flask equipped with a thermometer, a water separator and a condensation reflux device is filled with acrylamide ethylenediamine and deionized water, and nitrogen is filled to remove air.
f. And (3) starting a stirring device, slowly heating to 70-110 ℃, starting to slowly dropwise add the ammonium persulfate aqueous solution, finishing dropwise adding within 1-2h, and performing constant-temperature reaction for 2-3h after dropwise adding.
g. Cooling to 50-70deg.C, adding maleic anhydride, stirring thoroughly, keeping the temperature for 2-3 hr, adding sodium hydroxide to adjust pH to 9-10, and charging nitrogen gas to drive away air.
h. Adding 4-dimethylaminopyridine, sealing the reaction kettle, and opening a condensing reflux device. Heating to 110-160 ℃, keeping the temperature for 2-3 hours, cooling, adding hydrochloric acid for acidification, precipitating, filtering, drying and crystallizing.
i. And adding the crystallized product into the four-mouth reaction four-mouth flask, adding ethylenediamine, heating to 60-80 ℃, fully stirring, and flushing nitrogen to drive air.
j. Adding an amidation reaction catalyst ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, fully stirring, stopping pumping nitrogen, starting vacuumizing, slowly heating to 140-160 ℃, keeping the temperature for 3-5 hours, and cooling to obtain the product.
(3) Compounding of viscose cotton leveling agent
And (3) compounding the ethylene diamine and propylene copolymer, the poly (ethylene diamine) succinate and the poly (ethylene diamine) polycondensate with deionized water, compounding according to 30%, 25% and 45%, fully and uniformly stirring at 60-80 ℃, cooling, filtering and discharging.
Example 2
Unlike the above cases, the main components of this scheme were 95 parts of acrylamide ethylenediamine, 0.5 part of initiator, 20 parts of maleic anhydride, 2 parts of affinity addition catalyst, 5 parts of alkaline agent, 8 parts of ethylenediamine, and 0.5 part of amidation reaction catalyst. The nucleophilic addition catalyst is 4-dimethylaminopyridine, the amide condensation catalyst is ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, the initiator is potassium persulfate, the alkaline agent is sodium carbonate, and the acid agent is hydrochloric acid.
Compounding of viscose cotton leveling agent
The preparation method comprises the steps of compounding the ethylene diamine and propylene ethylene diamine succinic acid copolymer, the polyethylene diamine succinic acid and ethylene diamine polycondensate and deionized water, compounding according to 25%, 25% and 50%, fully and uniformly stirring at 60-80 ℃, cooling, filtering and discharging.
The leveling property of the viscose cotton leveling agent is tested, and the test results are shown in table 1.
Two fabrics were taken, one fabric was dyed using the viscose cotton leveling agent prepared in this example 1, and the other fabric was dyed using a conventional reactive dye, then 6 points were taken on each of the two fabrics, the apparent depth K/S was measured, and then the average value and standard deviation Sr were calculated, with the smaller standard deviation, the better leveling property.
Table 1 data for leveling property test of viscose leveling agent
The standard deviation is the square root of the variance, so that the leveling property of the viscose cotton leveling agent prepared by the invention is good.
Claims (8)
1. A zwitterionic polymeric viscose cotton blending leveling agent is characterized in that the viscose cotton leveling agent comprises the components of copolymer of acryloylethylenediamine and acryloylethylenediamine succinic acid, polycondensate of the acryloylethylenediamine succinic acid and ethylenediamine and deionized water;
the structural formula of the copolymer of the acryloylethylenediamine and the acryloylethylenediamine succinic acid is as follows:
the structural formula of the polycondensate of the poly (ethylene diamine succinate) and the ethylene diamine is as follows:
wherein the weight ratio of each component is as follows: 10-30% of copolymer of acryloylethylenediamine and acryloylethylenediamine succinic acid, 10-30% of polycondensate of polyacrylaylethylenediamine succinic acid and ethylenediamine, and the balance of deionized water.
2. The zwitterionic polymeric viscose cotton blending leveling agent according to claim 1, characterized in that: the components and weight ratio are 20-30% of copolymer of acryloylethylenediamine and acryloylethylenediamine succinic acid, 20-30% of polycondensate of polyacylethylenediamine succinic acid and ethylenediamine, and the balance of deionized water.
3. A method for preparing the zwitterionic polymeric viscose cotton blending levelling agent as claimed in claim 1 or 2, which is characterized by comprising the following steps:
(1) Synthesis of copolymers of acrylamides and acrylamides succinic acid
a. Adding acrylamide ethylenediamine and deionized water into a four-neck flask with a thermometer, a water separator and a condensation reflux device, and filling nitrogen to remove air;
b. starting a stirring device, slowly heating to 70-110 ℃, starting to slowly dropwise add the initiator aqueous solution, finishing dropwise adding within 1-2h, and performing constant-temperature reaction for 2-3h after dropwise adding;
c. cooling to 50-70deg.C, adding maleic anhydride, stirring thoroughly, keeping the temperature for 2-3 hr, adding alkaline agent, adjusting pH to 8-9, and charging nitrogen to drive away air;
d. adding nucleophilic addition catalyst 4-dimethylaminopyridine, sealing the reaction kettle, opening a condensing reflux device, heating to 110-160 ℃, keeping the temperature for 2-3 hours, and cooling and discharging;
(2) Synthesis of polycondensates of polyacrylamidesuccinic acid and ethylenediamine
e. Adding acrylamide ethylenediamine and deionized water into a four-neck flask with a thermometer, a water separator and a condensation reflux device, and filling nitrogen to remove air;
f. starting a stirring device, slowly heating to 70-110 ℃, starting to slowly dropwise add an initiator aqueous solution, finishing dropwise adding within 1-2h, and performing constant-temperature reaction for 2-3h after dropwise adding;
g. cooling to 50-70deg.C, adding maleic anhydride, stirring thoroughly, keeping the temperature for 2-3 hr, adding alkaline agent, adjusting pH to 9-10, and charging nitrogen to drive away air;
h. adding nucleophilic addition catalyst 4-dimethylaminopyridine, sealing the reaction kettle, opening a condensing reflux device, heating to 110-160 ℃, keeping the temperature for 2-3 hours, cooling, adding an acid agent for acidification, precipitating, filtering, drying and crystallizing;
i. adding the crystallized product into the four-mouth flasks, adding ethylenediamine, heating to 60-80 ℃, fully stirring, and filling nitrogen to drive air;
j. adding an amidation reaction catalyst, stopping pumping nitrogen, starting pumping vacuum, slowly heating to 140-160 ℃, keeping the temperature for 3-5 hours, and cooling to obtain the material;
(3) Compounding of viscose cotton leveling agent
According to the formula amount, the acryloylethylenediamine and acryloylethylenediamine succinic acid copolymer, the polyacrylaylethylenediamine succinic acid and ethylenediamine polycondensate and deionized water are compounded, fully and uniformly stirred at 60-80 ℃, and then cooled, filtered and discharged.
4. The method for preparing the zwitterionic polymeric viscose cotton blending levelling agent according to claim 3, which is characterized in that: the components are 80-110 parts of the acryloylethylenediamine, 0.5-1 part of the initiator, 10-22 parts of the maleic anhydride, 1-2 parts of the nucleophilic addition catalyst, 3-8 parts of the alkaline agent, 5-15 parts of the ethylenediamine and 0.5-2 parts of the amidation reaction catalyst.
5. The method for preparing the zwitterionic polymeric viscose cotton blending levelling agent according to claim 3, which is characterized in that: the amidation reaction catalyst is 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride.
6. The method for preparing the zwitterionic polymeric viscose cotton blending levelling agent according to claim 3, which is characterized in that: the initiator is one or more of ammonium persulfate and potassium persulfate.
7. The method for preparing the zwitterionic polymeric viscose cotton blending levelling agent according to claim 3, which is characterized in that: the alkaline agent is one or more of sodium hydroxide and sodium carbonate.
8. The method for preparing the zwitterionic polymeric viscose cotton blending levelling agent according to claim 3, which is characterized in that: the acid agent is hydrochloric acid.
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