CN112961282B - Starch-grafted environment-friendly stiffening agent and preparation method thereof - Google Patents
Starch-grafted environment-friendly stiffening agent and preparation method thereof Download PDFInfo
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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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/12—Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/11—Starch or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
- D06M15/333—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/20—Treatment influencing the crease behaviour, the wrinkle resistance, the crease recovery or the ironing ease
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Abstract
The invention discloses a starch grafted novel environment-friendly stiffening agent and a preparation method thereof, wherein the stiffening agent is prepared from the following raw materials in percentage by weight: 30-40% of vinyl acetate; 3-4% of methyl methacrylate; 10-15% of cationic starch pasting liquid; 20-30% of polyvinyl alcohol solution; 0.1-0.3% of an initiator; 0.3-0.6% of a pH regulator; 20-30% of water; the environment-friendly stiffening agent disclosed by the invention can enhance the stiffness of the fabric, endows the fabric with thick hand feeling and has no obvious influence on the strength of the fabric; the raw materials used have wide sources and low price, do not add an emulsifier, do not contain APEO, have no formaldehyde release, and are environment-friendly and harmless.
Description
Technical Field
The invention particularly relates to a starch-grafted novel environment-friendly stiffening agent and a preparation method thereof, belonging to the technical field of textiles.
Background
The information in this background section is disclosed only to enhance an understanding of the general background of the disclosure and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The stiffening agent belongs to one of textile fabric after-finishing agents, is a functional auxiliary agent mainly used for enhancing the stiffness of the fabric and endowing the fabric with a thick sense, and is mainly applied to the processing process of fabrics such as curtains, cases, tents, tools, lining cloth, shoe materials and the like.
Currently, common stiffening agents on the market mainly comprise melamine formaldehyde resin, urea formaldehyde resin, polyacrylate, polyvinyl acetate-acrylate copolymer, polyvinyl alcohol, starch and the like.
The fabric treated by the thermosetting stiffening agents such as melamine formaldehyde resin and urea formaldehyde resin has high stiffness, but can release formaldehyde in the using process, cannot meet the requirement of environmental protection, has poor storage stability and is limited to use.
Polyvinyl alcohol and starch stiffening agents have a good stiffening effect on cellulosic fabrics, but have poor water-washability.
At present, polyvinyl acetate, polyacrylate and polyvinyl acetate-acrylate copolymer stiffening agents are widely used, and the stiffening agents are characterized by good yellowing resistance effect, high storage stability, good water washing resistance and no generation of free formaldehyde.
The polyvinyl acetate-acrylate co-clustering stiffening agent has the characteristics of low cost and high stiffness, and the product is nonionic, can be used in one bath with other cationic finishing agents, and has a wider application range. However, the stiffening agents have a different stiffening effect on the fabric compared with thermosetting stiffening agents such as melamine formaldehyde resin and urea formaldehyde resin.
Disclosure of Invention
In view of the above prior art and the above background art, the present disclosure aims to provide an environmentally friendly fabric stiffening agent with excellent stiffening performance, which has the characteristics of environmental protection, low cost, high stiffness, thick hand feeling, etc.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the present disclosure, a starch-grafted environment-friendly stiffening agent is provided, which is prepared from the following raw materials by mass:
30-40% of vinyl acetate;
3-4% of methyl methacrylate;
10-15% of cationic starch pasting liquid;
20-30% of polyvinyl alcohol solution;
0.1-0.3% of an initiator;
0.3-0.6% of a pH regulator;
20-30% of water;
the cationic starch pasting liquid is prepared from the following raw materials in percentage by mass:
15-20% of cationic starch;
75.5-83% of water;
2-4% of hydrogen peroxide;
0.2-0.5% of ascorbic acid.
In a second aspect of the present disclosure, there is provided a method for preparing a starch-grafted environmentally friendly stiffening agent according to the first aspect, the method comprising the following steps:
(1) preparing a cationic starch pasting solution: mixing cationic starch with water, heating to 45-55 ℃, adding hydrogen peroxide, heating to 65-75 ℃, adding ascorbic acid, boiling for 20-40 min, and cooling to room temperature to obtain a colorless and transparent cationic starch pasting solution;
(2) mixing the prepared cationic starch pasting liquid, a polyvinyl alcohol solution, part of vinyl acetate and part of an initiator, heating to 60-65 ℃, stopping heating, and carrying out heat preservation reaction for 0.5-1.5 h after the temperature is raised to 70-75 ℃;
(3) adding the rest of vinyl acetate, methyl methacrylate and the rest of initiator into the reaction system after heat preservation in the step (2), wherein the reaction temperature is 75-85 ℃, and the adding time is controlled to be 4-5 h; after the addition is finished, heating to 82-86 ℃, preserving heat for 0.5-1.5 h, heating to 88-92 ℃, preserving heat for 0.5-1.5 h; and (3) adding a pH regulator after the reaction is finished, cooling, discharging, and preparing to obtain the starch grafted environment-friendly stiffening agent.
The invention has the beneficial effects that: the starch-grafted environment-friendly stiffening agent and the preparation method thereof adopt a soap-free emulsion polymerization method, and the soap-free emulsion polymerization overcomes the defects of polymer in stiffening performance, fabric thickness and the like caused by the existence of an emulsifier in the traditional emulsion polymerization.
(1) The soap-free emulsion polymerization is adopted, and the cationic starch pasting liquid is used for replacing the traditional emulsifier, so that the cost is reduced, and the pollution of the emulsifier to the environment is avoided. Meanwhile, the cationic starch can be independently used as a stiffening agent, and the stiffening effect of the vinyl acetate on the cellulose fabric can be obviously improved by graft copolymerization of the starch chain segment and the vinyl acetate monomer.
(2) The method is characterized in that hydrogen peroxide and ascorbic acid are added during preparation of the cationic starch pasting liquid to play a role in hydrolyzing starch, and the degradation degree of starch molecules is adjusted by adjusting the using amounts of the hydrogen peroxide and the ascorbic acid in the production process, so that the viscosity and the molecular weight of a starch pasting liquid system are adjusted.
(3) The stiffening agent can endow the fabric with stiff, smooth and thick hand feeling; the finished fabric is not easy to absorb moisture and soften and has certain washing resistance; does not contain APEO, does not release formaldehyde, and is environment-friendly and harmless.
(4) The stiffening agent can be matched with an organic silicon product for use, so that the fabric has an excellent stiffening style.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
The starch-grafted environment-friendly stiffening agent is prepared from the following raw materials in percentage by mass:
30-40% of vinyl acetate;
3-4% of methyl methacrylate;
10-15% of cationic starch pasting liquid;
20-30% of polyvinyl alcohol solution;
0.1-0.3% of an initiator;
0.3-0.6% of a pH regulator;
the cationic starch pasting solution is prepared from the following raw materials in percentage by mass:
15-20% of cationic starch;
75.5-83% of water;
2-4% of hydrogen peroxide;
0.2-0.5% of ascorbic acid.
In one or more embodiments of the present disclosure, the cationic starch gelatinization liquid is one of a tapioca cationic starch gelatinization liquid and a potato cationic starch gelatinization liquid. The cationic starch pasting liquid is used as an emulsifier for soap-free emulsion polymerization, and emulsion polymerization is carried out under the conditions of certain temperature, time and initiator, so that the polymer has high stability.
In one or more embodiments of the present disclosure, the cationic starch gelatinization liquid is prepared by the following method: mixing cationic starch with water, adding hydrogen peroxide when the temperature is raised to 45-55 ℃, adding ascorbic acid when the temperature is raised to 65-75 ℃, then boiling for 20-40 min, and cooling to room temperature to obtain colorless and transparent cationic starch pasting liquid. The gelatinization speed of the starch can be obviously improved by adopting a hydrogen peroxide and ascorbic acid system, and uniform semitransparent gelatinization liquid with different viscosities can be obtained by adjusting the dosage of the hydrogen peroxide and the ascorbic acid.
Specifically, the cationic starch pasting liquid prepared by hydrogen peroxide and ascorbic acid can reduce the viscosity of a pasting liquid system, and is beneficial to actual production operation.
Tests prove that the cationic starch pasting liquid has good emulsifying capacity to a system.
In one or more embodiments of the present disclosure, the polyvinyl alcohol solution is at least one of a polyvinyl alcohol 1788 solution, a polyvinyl alcohol 2088 solution, and a polyvinyl alcohol 2488 solution.
Further, the mass fraction of the polyvinyl alcohol solution is 8-12%;
furthermore, the mass fraction of the polyvinyl alcohol solution is 10%, and in actual production, the polyvinyl alcohol solution with the mass fraction is found to be easier to prepare, and the formed solution is uniform and transparent and has moderate viscosity.
In one or more embodiments of the present disclosure, the initiator is at least one of ammonium persulfate, sodium persulfate, and potassium persulfate.
In one or more embodiments of the present disclosure, the pH adjusting agent is at least one of sodium carbonate, sodium bicarbonate, and sodium hydroxide.
In a second exemplary embodiment of the present disclosure, there is provided a method for preparing a starch-grafted environmentally friendly stiffening agent as described in the first exemplary embodiment, the method comprising the steps of:
(1) preparing a cationic starch pasting solution: mixing cationic starch with water, heating to 45-55 ℃, adding hydrogen peroxide, heating to 65-75 ℃, adding ascorbic acid, boiling for 20-40 min, and cooling to room temperature to obtain a colorless and transparent cationic starch pasting solution;
(2) mixing the prepared cationic starch pasting solution, a polyvinyl alcohol solution, part of vinyl acetate and part of an initiator, heating to 60-65 ℃, stopping heating, and reacting for 0.5-1.5 hours in a heat preservation manner after the temperature is raised to 70-75 ℃;
(3) adding the rest of vinyl acetate, methyl methacrylate and the rest of initiator into the reaction system after heat preservation in the step (2), wherein the reaction temperature is 75-85 ℃, and the adding time is controlled to be 4-5 h; after the addition is finished, heating to 82-86 ℃, preserving heat for 0.5-1.5 h, heating to 88-92 ℃, preserving heat for 0.5-1.5 h; and (3) adding a pH regulator after the reaction is finished, cooling, discharging, and preparing to obtain the starch grafted environment-friendly stiffening agent.
In one or more embodiments of the present disclosure, in the step (2), part of the vinyl acetate accounts for 18 to 20% of the total mass of the vinyl acetate; part of the initiator accounts for 18-20% of the total mass of the initiator;
further, part of the vinyl acetate accounts for 20 percent of the total mass of the vinyl acetate; part of the initiator accounts for 20 percent of the total mass of the initiator, and is more beneficial to the effective polymerization of polar monomers in a soap-free environment.
In order to make the technical solutions of the present disclosure more clearly understood by those skilled in the art, the technical solutions of the present disclosure will be described in detail below with reference to specific embodiments.
Example 1
Step S101) adding 15 parts of cassava cationic starch into 82.8 parts of deionized water, adding 2 parts of hydrogen peroxide when the temperature is raised to 50 ℃, adding 0.2 part of ascorbic acid when the temperature is raised to 70 ℃, then boiling for 30 minutes, and cooling to room temperature to obtain colorless and transparent cationic starch pasting liquid.
Step S102) adding 10 parts of polyvinyl alcohol into 90 parts of water, heating to 85-90 ℃, stirring for dissolving, and filtering to obtain a colorless transparent solution, namely a polyvinyl alcohol solution with the mass fraction of 10%.
Step S103) putting 12 parts of prepared cationic starch pasting liquid, 25 parts of polyvinyl alcohol solution, 7 parts of vinyl acetate, 0.04 part of initiator potassium persulfate and 10 parts of deionized water into a reaction kettle, heating to 60-65 ℃, stopping heating, generating a large amount of foams in the system, starting to generate reflux, heating to 75 ℃, and then preserving heat for reacting for 1 hour.
And step S104) starting to dropwise add 28 parts of vinyl acetate and 3 parts of methyl methacrylate by using a dropwise adding tank, controlling the reaction temperature to be about 80 ℃, dropwise adding after 4.5 hours, dropwise adding 0.8 part of 20% initiator solution while dropwise adding the monomer, and requiring that the dropwise adding is completed simultaneously with the monomer. Then heating to 85 ℃ and preserving heat for 1 hour, heating to 90 ℃ and preserving heat for 1 hour, adding 14.5 parts of deionized water to adjust the viscosity, adding 0.3 part of pH regulator-sodium hydroxide solution to adjust the pH to 6-7, finally cooling to below 35 ℃ and discharging to obtain a stiffening agent FYT-05;
example 2
Step S201) adding 17 parts of cassava cationic starch into 79.65 parts of deionized water, adding 3 parts of hydrogen peroxide when the temperature is raised to 50 ℃, adding 0.35 part of ascorbic acid when the temperature is raised to 70 ℃, then boiling for 35 minutes, and cooling to room temperature to obtain colorless and transparent cationic starch pasting liquid.
Step S202), adding 10 parts of polyvinyl alcohol into 90 parts of water, heating to 85-90 ℃, stirring for dissolving, and filtering to obtain a colorless transparent solution, namely a polyvinyl alcohol solution with the mass fraction of 10%.
Step S203) adding 12 parts of prepared cationic starch pasting liquid, 25 parts of polyvinyl alcohol solution, 7 parts of vinyl acetate, 0.04 part of initiator-ammonium persulfate and 10 parts of deionized water into a reaction kettle, heating to 60-65 ℃, stopping heating, generating a large amount of foams in the system, starting to generate reflux, heating to 75 ℃, and then carrying out heat preservation reaction for 1 hour.
And step S204), starting to dropwise add 28 parts of vinyl acetate and 3 parts of methyl methacrylate by using a dropwise adding tank, controlling the reaction temperature to be about 80 ℃, dropwise adding after 4.5 hours, dropwise adding 0.8 part of 20% initiator solution while dropwise adding the monomer, and requiring that the dropwise adding is completed simultaneously with the monomer. And then heating to 85 ℃ and preserving heat for 1 hour, heating to 90 ℃ and preserving heat for 1 hour, adding 14.5 parts of deionized water to adjust the viscosity, adding 0.3 part of pH regulator-sodium hydroxide solution to adjust the pH to 6-7, finally cooling to below 35 ℃ and discharging to obtain the stiffening agent FYT-06.
Example 3
Step S301) adding 20 parts of cassava cationic starch into 75.5 parts of deionized water, adding 4 parts of hydrogen peroxide when the temperature is raised to 50 ℃, adding 0.5 part of ascorbic acid when the temperature is raised to 70 ℃, then boiling for 30 minutes, and cooling to room temperature to obtain colorless and transparent cationic starch pasting liquid.
Step S302), adding 10 parts of polyvinyl alcohol into 90 parts of water, heating to 85-90 ℃, stirring for dissolving, and filtering to obtain a colorless transparent solution, namely a polyvinyl alcohol solution with the mass fraction of 10%.
Step S303) adding 12 parts of prepared cationic starch pasting liquid, 25 parts of polyvinyl alcohol solution, 8 parts of vinyl acetate, 0.06 part of initiator potassium persulfate and 10 parts of deionized water into a reaction kettle, heating to 60-65 ℃, stopping heating, generating a large amount of foams in the system, starting to generate reflux, heating to 75 ℃, and then preserving heat for reacting for 1 hour.
And step S304) beginning to dropwise add 32 parts of vinyl acetate and 4 parts of methyl methacrylate by using a dropwise adding tank, controlling the reaction temperature to be about 80 ℃, dropwise adding after 4 hours, dropwise adding 1.2 parts of 20% initiator solution while dropwise adding the monomer, and requiring that the dropwise adding is completed simultaneously with the monomer. And then heating to 85 ℃ and preserving heat for 1 hour, heating to 90 ℃ and preserving heat for 1 hour, adding 8.3 parts of deionized water to adjust the viscosity, adding 0.4 part of pH regulator-sodium carbonate solution to adjust the pH to 6-7, finally cooling to below 35 ℃ and discharging to obtain the stiffening agent FYT-07.
Comparative example 1
Step S301) of example 3 was replaced with tapioca cationic starch by corn cationic starch.
Tests prove that the polymer obtained by adopting the corn cationic starch has low viscosity, the storage stability is weaker than that of an emulsion polymer formed by cassava cations, and the treated cotton cloth has low stiffness compared with the treated cotton cloth.
Comparative example 2
Step 1) step S301 as in example 3);
step 2) step S302) as in example 3);
step 3) as in example 3 step S303);
step 4): 32 parts of vinyl acetate, 4 parts of methyl methacrylate and 2 parts of emulsifier peregal O-40 are dripped from a dripping tank, the reaction temperature is controlled to be about 80 ℃, after dripping is finished within 4 hours, 1.2 parts of 20 percent initiator solution is dripped while monomer is dripped, and the dripping is required to be finished simultaneously with the monomer. Then heating to 85 ℃ and preserving heat for 1 hour, heating to 90 ℃ and preserving heat for 1 hour, adding 7.3 parts of deionized water to adjust the viscosity, adding 0.4 part of pH regulator-sodium carbonate solution to adjust the pH to 6-7, finally cooling to below 35 ℃ and discharging to obtain the polymer emulsion.
As can be seen from tables 1 and 2 below, the stiffness and body of the fabric after the cotton cloth treatment was far less than that of example 3 by adding a conventional emulsifier to the system. It is demonstrated that the soap-free polymer emulsions of the disclosed invention significantly improve the defects of polymer-treated fabrics in the presence of emulsifiers.
Comparative example 3
In order to realize soap-free emulsion polymerization, the polar monomer and the component content thereof are researched by the disclosure, and the matching of vinyl acetate and methyl methacrylate with specific proportion amount is found, so that not only can soap-free emulsion polymerization reaction be smoothly carried out, but also the stiffness of the fabric can be remarkably improved.
The following is illustrated using comparative example 3:
step 1) step S301 as in example 3);
step 2) step S302) as in example 3);
step 3) as in example 3 step S303);
step 4): 24 parts of vinyl acetate, 4 parts of butyl acrylate, 4 parts of methyl acrylate and 4 parts of methyl methacrylate are dripped from a dripping tank, the reaction temperature is controlled to be about 80 ℃, after dripping is finished within 4 hours, 1.2 parts of 20 percent initiator solution is dripped while monomers are dripped, and the dripping is required to be finished simultaneously with the monomers. Then heating to 85 ℃ and preserving heat for 1 hour, heating to 90 ℃ and preserving heat for 1 hour, adding 9.3 parts of deionized water to adjust the viscosity, adding 0.4 part of pH regulator-sodium carbonate solution to adjust the pH to 6-7, finally cooling to below 35 ℃ and discharging to obtain the polymer emulsion.
It can be seen from comparative example 3, table 1 below and table 2 below that the components and component contents of the polar monomer have a great influence on the stability of the polymer emulsion, and if the polar monomer and component contents thereof are not appropriate, the soap-free emulsion polymerization cannot be performed well.
And (3) testing items: stiffness Performance determination and Thick feel evaluation
The stiffness was tested according to GB/T18318.1-2009 "determination of bending Properties of textiles part 1: bevel method test. The treated fabric was cut into 2.5cm by 20cm rectangles, the stiffness was measured on a fabric stiffness tester, each sample was tested 3 times, and the average was taken.
Results of stiffness test Table 1
| Sample (I) | Stiffness (cm) |
| Example 1 | 6.9 |
| Example 2 | 7.3 |
| Example 3 | 7.5 |
| Comparative example 1 | 6.4 |
| Comparative example 2 | 6.2 |
| Comparative example 3 | 6.7 |
2. Evaluation of Thick feeling: the score of 10 is the highest, indicating the highest feeling of fullness, and the score of 1 is the lowest, indicating the worst feeling of fullness. Ten individuals were randomly drawn to participate in the assessment of the feeling of fullness and the sum of the scores for each swatch was taken as the final result, as shown in table 2 below.
Results of the thickness test Table 2
| Sample (I) | Sum of scores |
| Example 1 | 75 |
| Example 2 | 81 |
| Example 3 | 89 |
| Comparative example 1 | 61 |
| Comparative example 2 | 53 |
| Comparative example 3 | 68 |
The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments, and it should be understood by those skilled in the art that various modifications or changes can be made by those skilled in the art without inventive efforts based on the technical solutions of the present invention.
Claims (10)
1. The starch-grafted environment-friendly stiffening agent is characterized by being prepared from the following raw materials in percentage by mass:
30-40% of vinyl acetate;
3-4% of methyl methacrylate;
10-15% of cationic starch pasting liquid;
20-30% of polyvinyl alcohol solution;
0.1-0.3% of an initiator;
0.3-0.6% of a pH regulator;
20-30% of water;
the cationic starch pasting liquid is prepared from the following raw materials in percentage by mass:
15-20% of cationic starch;
75.5-83% of water;
2-4% of hydrogen peroxide;
0.2-0.5% of ascorbic acid;
the cationic starch pasting liquid is cassava cationic starch pasting liquid.
2. The stiffening agent according to claim 1, wherein the cationic starch gelatinizing solution is prepared by the following method: mixing cationic starch with water, adding hydrogen peroxide when the temperature is raised to 45-55 ℃, adding ascorbic acid when the temperature is raised to 65-75 ℃, then boiling for 20-40 min, and cooling to room temperature to obtain colorless and transparent cationic starch pasting liquid.
3. The stiffening agent according to claim 1, wherein the polyvinyl alcohol solution is at least one of a polyvinyl alcohol 1788 solution, a polyvinyl alcohol 2088 solution, and a polyvinyl alcohol 2488 solution.
4. The stiffening agent according to claim 1, wherein the polyvinyl alcohol solution is 8 to 12% by mass.
5. The stiffening agent according to claim 4, wherein the polyvinyl alcohol solution is present in an amount of 10% by weight.
6. The stiffening agent according to claim 1, wherein the initiator is at least one of ammonium persulfate, sodium persulfate, and potassium persulfate.
7. The stiffening agent according to claim 1, wherein the pH adjusting agent is at least one of sodium carbonate, sodium bicarbonate, and sodium hydroxide.
8. The preparation method of the starch-grafted environment-friendly stiffening agent as claimed in any one of claims 1 to 7, characterized by comprising the following steps:
(1) preparing a cationic starch pasting solution: mixing cationic starch with water, heating to 45-55 ℃, adding hydrogen peroxide, heating to 65-75 ℃, adding ascorbic acid, boiling for 20-40 min, and cooling to room temperature to obtain a colorless and transparent cationic starch pasting solution;
(2) mixing the prepared cationic starch pasting liquid, a polyvinyl alcohol solution, part of vinyl acetate and part of an initiator, heating to 60-65 ℃, stopping heating, and carrying out heat preservation reaction for 0.5-1.5 h after the temperature is raised to 70-75 ℃;
(3) adding the rest of vinyl acetate, methyl methacrylate and the rest of initiator into the reaction system after heat preservation in the step (2), wherein the reaction temperature is 75-85 ℃, and the adding time is controlled to be 4-5 h; after the addition is finished, heating to 82-86 ℃, preserving heat for 0.5-1.5 h, heating to 88-92 ℃, preserving heat for 0.5-1.5 h; and (3) adding a pH regulator after the reaction is finished, cooling, discharging, and preparing to obtain the starch grafted environment-friendly stiffening agent.
9. The method according to claim 8, wherein in the step (2), part of the vinyl acetate accounts for 14-18% of the total mass of the vinyl acetate; part of the initiator accounts for 18-20% of the total mass of the initiator.
10. The process of claim 9, wherein a portion of the vinyl acetate is 15% by weight of the total vinyl acetate; part of the initiator accounts for 20% of the total mass of the initiator.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110375647.2A CN112961282B (en) | 2021-04-08 | 2021-04-08 | Starch-grafted environment-friendly stiffening agent and preparation method thereof |
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| CN202110375647.2A CN112961282B (en) | 2021-04-08 | 2021-04-08 | Starch-grafted environment-friendly stiffening agent and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1589483A (en) * | 1977-01-24 | 1981-05-13 | Kao Corp | Fabric stiffening composition |
| JP2000143742A (en) * | 1998-11-05 | 2000-05-26 | Clariant Polymer Kk | Cationic starch substrate, its production and liquid starch composition containing the same paste substrate |
| CN102617799A (en) * | 2012-04-13 | 2012-08-01 | 广东省造纸研究所 | Process for preparing starch grafting acrylamide paper reinforcing agent |
| CN104945554A (en) * | 2014-03-26 | 2015-09-30 | 东华大学 | Polyacrylate stiffening agent, and preparation method and application thereof |
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- 2021-04-08 CN CN202110375647.2A patent/CN112961282B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1589483A (en) * | 1977-01-24 | 1981-05-13 | Kao Corp | Fabric stiffening composition |
| JP2000143742A (en) * | 1998-11-05 | 2000-05-26 | Clariant Polymer Kk | Cationic starch substrate, its production and liquid starch composition containing the same paste substrate |
| CN102617799A (en) * | 2012-04-13 | 2012-08-01 | 广东省造纸研究所 | Process for preparing starch grafting acrylamide paper reinforcing agent |
| CN104945554A (en) * | 2014-03-26 | 2015-09-30 | 东华大学 | Polyacrylate stiffening agent, and preparation method and application thereof |
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