CN112812246B - Environment-friendly textile size and preparation method thereof - Google Patents
Environment-friendly textile size and preparation method thereof Download PDFInfo
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- CN112812246B CN112812246B CN202110087114.4A CN202110087114A CN112812246B CN 112812246 B CN112812246 B CN 112812246B CN 202110087114 A CN202110087114 A CN 202110087114A CN 112812246 B CN112812246 B CN 112812246B
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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
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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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
- D06M15/15—Proteins 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
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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
- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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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
- D06M2200/35—Abrasion, pilling or fibrillation resistance
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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
- D06M2200/40—Reduced friction resistance, lubricant properties; Sizing compositions
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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
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Abstract
The invention belongs to the technical field of textile materials, and relates to environment-friendly textile size and a preparation method thereof. The environment-friendly textile size is prepared from 6-9 parts of monomers, 14-21 parts of gelatin, 70-80 parts of water and the like. The preparation method comprises the following steps: adding gelatin into water at the temperature of 80-86 ℃, stirring until the gelatin is completely dissolved, filtering insoluble impurities, adding an initiator, and then sequentially dropwise adding different monomers; and heating to 90-95 ℃, keeping the temperature for 60-100 min, then cooling to 55-65 ℃, adding a neutralizing agent for neutralization, adjusting the pH value to 6-7, adding a preservative, and finally filtering and discharging to obtain the environment-friendly textile size. The sizing agent has good stability, low viscosity, good film forming property and excellent sizing property, and can replace the traditional PVA sizing agent in the sizing process of the high-proportion polyester-cotton blended yarn.
Description
Technical Field
The invention belongs to the technical field of textile materials, and relates to environment-friendly textile size and a preparation method thereof.
Background
The textile production mainly comprises a plurality of working procedures of spinning, weaving, dyeing and finishing and the like, the warp sizing working procedure before weaving is a very critical step, and the quality of slashing directly influences the weaving efficiency and the product quality. There are correspondingly suitable sizing agents for different types of yarn. Sizing is essential in the textile industry.
At present, the whole direction of the textile industry is green, environment-friendly, energy-saving and consumption-reducing, and the sizing technology also conforms to the development of the direction. Certain achievements are applied to actual production at home and abroad, and mainly comprise research and development and application of green environment-friendly sizing agent, exploration and application of a novel green environment-friendly energy-saving sizing process and the like. The varieties of the sizing agent are mainly as follows: starch, polyvinyl alcohol (PVA) and polypropylene. Among them, polyvinyl alcohol (PVA) is widely used in warp sizing because of its excellent water solubility, film forming property, binding power and emulsifying property as an excellent chemical size. But PVA-containing sizing causes that desizing wastewater contains polyvinyl alcohol which is not easy to biodegrade, thereby causing great harm to the environment. The use of PVA sizing is definitely forbidden in some developed countries, so the research and development of green environment-friendly biodegradable textile size for replacing PVA becomes the leading edge and the hot spot in the field of textile size.
The research and development of green textile size and the application of the energy-saving and consumption-reducing slashing process have been a necessary trend, and under the joint efforts of numerous textile workers and size developers, the slashing of yarns below C9.84tex by using modified starch instead of PVA is realized, while in conventional polyester-cotton yarns, particularly in high-proportion polyester-cotton blended yarns, due to the strong hydrophobicity and smooth surface of polyester, the sizing is still performed by using PVA.
At present, most of high-proportion polyester-cotton fabrics are mainly sized by adopting a sizing agent formula which takes PVA as a main material and takes modified starch and propylene sizing agent as auxiliary materials. The sizing agent formula mainly based on PVA has the problems of poor slashing permeability, poor flexibility, more secondary hairiness and the like, and finally causes more defects on the cloth surface and low weaving efficiency. But the high proportion of polyester cotton still cannot leave the PVA sizing for conventional blends.
Disclosure of Invention
In view of the above, the invention aims to provide an environment-friendly textile size and a preparation method thereof, the size has good stability, low viscosity, good film forming property and excellent sizing property, can replace the traditional PVA size in the sizing process of high-proportion polyester-cotton blended yarns, and finally realizes green and environment-friendly warp sizing.
In order to realize the purpose, the invention provides environment-friendly textile size which is prepared from the following raw materials in parts by weight: 6-9 parts of a monomer, 14-21 parts of gelatin and 70-80 parts of water, wherein the monomer comprises acrylic acid, butyl acrylate and methyl methacrylate.
Further, the monomer also comprises styrene.
Furthermore, in the monomers, the mass ratio of acrylic acid, butyl acrylate, methyl methacrylate and styrene is 1:3:2: 2.
The invention also provides a preparation method of the environment-friendly textile size, which comprises the following steps:
s1, adding gelatin into water at 80-86 ℃, stirring until the gelatin is completely dissolved, and filtering insoluble impurities to obtain a gelatin water solution;
s2, keeping the temperature and the stirring speed in the step S1 unchanged, adding an initiator into the gelatin aqueous solution, and then sequentially dropwise adding different monomers;
s3, heating the whole reaction system to 90-95 ℃, preserving heat for 60-100 min, then cooling to 55-65 ℃, adding a neutralizing agent for neutralization, adjusting the pH value to 6-7, filtering and discharging to obtain the environment-friendly textile size.
Further, the stirring speed is 200-300 r/min.
Further, the initiator is ammonium persulfate.
Further, the mass ratio of the ammonium persulfate to the total amount of the monomers is 1 (20-50).
Further, in step S2, the dropping of different monomers in sequence specifically includes: and (3) sequentially dripping acrylic acid, butyl acrylate and methyl methacrylate at the time interval of 50-90 min, wherein the dripping time of the acrylic acid, the butyl acrylate and the methyl methacrylate is 60 min.
Further, in step S2, the dropping of different monomers in sequence specifically includes: and (3) sequentially dripping acrylic acid, butyl acrylate, methyl methacrylate and styrene at the time interval of 50-90 min, wherein the dripping time of the acrylic acid, the butyl acrylate, the methyl methacrylate and the styrene is 60 min.
Further, in step S3, the neutralizing agent is ammonia water.
Compared with the prior art, the invention takes the gelatin as a special protein, and acrylic acid, butyl acrylate, methyl methacrylate and styrene are dripped into the gelatin aqueous solution for graft reaction, on one hand, the gelatin has a large amount of hydroxyl carboxyl and amino, and the prepared slurry has excellent film forming property, good hydrophilicity, good adhesiveness with natural fiber, good wear resistance and low cost; on the other hand, the water solubility, stability, hardness, wear resistance and adhesion of high-proportion polyester-cotton blended yarns of the environment-friendly textile size obtained by grafting modification treatment of acrylic acid, butyl acrylate, methyl methacrylate and styrene are improved, and the environment-friendly textile size has the characteristics of good stability, low viscosity, good film forming property and the like, does not generate PVA which is difficult to biodegrade in a desizing process, has no pollution to the environment, and finally realizes green and environment-friendly sizing.
Drawings
FIG. 1 is a SEM image of polyester cotton blended yarn fibers;
FIG. 2 is an SEM (scanning Electron microscope) spectrum of yarn fibers of the polyester-cotton blended yarn shown in FIG. 1 after being sized by the environment-friendly textile size obtained in example 1 of the invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes or modifications can be made by those skilled in the art after reading the teaching of the present invention, and equivalents also fall within the scope of the claims of the present application.
Example 1
In the environment-friendly textile size of the embodiment, the usage amount of each raw material is as follows: the total amount of the monomers (acrylic acid, butyl acrylate, methyl methacrylate and styrene in a mass ratio of 1:3:2:2) is 30g, the gelatin (industrial gelatin) is 70g, and the distilled water is 360 ml.
Step 1, dissolving gelatin: putting 70g of gelatin and 360ml of distilled water into a reaction kettle, mechanically stirring at 85 ℃ at the speed of 200r/min for 60min, and filtering insoluble impurities to obtain a gelatin aqueous solution after complete dissolution;
step 2, grafting reaction: 0.6g of ammonium persulfate was dissolved in 40ml of distilled water for standby, then the gelatin aqueous solution was placed in a three-necked flask, and under the conditions of the original temperature and stirring speed, the initiator ammonium persulfate was added first, and then acrylic acid (3.75g), butyl acrylate (11.25g), methyl methacrylate (7.5g) and styrene (7.5g) were added dropwise in this order. The dropping time of the monomer is 60min each time, and the temperature is kept for 60min, which is 480min in total.
Step 3, material blending and discharging: and heating the whole reaction system to 90 ℃, preserving heat for 90min, adding 15ml of neutralizing agent ammonia water for neutralization when the temperature is reduced to 65 ℃, adjusting the pH value to 6-7, and finally filtering and discharging to obtain the environment-friendly textile size.
The yarn was tested using SU8040 scanning electron microscope (hitachi high and new technology limited), and the sample was a high-ratio 90/10 polyester-cotton blended yarn that was not sized and that was sized with the environment-friendly textile size of example 1, and the arrangement morphology of the yarn fibers before and after sizing was observed and compared, and the SEM spectra of the polyester-cotton blended yarn fibers that were not sized are shown in fig. 1, and the SEM spectra of the high-ratio 90/10 polyester-cotton blended yarn fibers that were sized with the environment-friendly textile size of example 1 are shown in fig. 2.
Example 2
In the environment-friendly textile size of the embodiment, the usage amount of each raw material is as follows: the total amount of the monomers (the mass ratio of acrylic acid, butyl acrylate and methyl methacrylate is 1.5:1.5:1) is 30g, the gelatin (industrial gelatin) is 70g, and the distilled water is 360 ml.
Step 1, dissolving gelatin: putting 70g of gelatin and 370ml of distilled water into a reaction kettle, mechanically stirring at 85 ℃ at the speed of 200r/min for 60min, and filtering insoluble impurities to obtain a gelatin aqueous solution after complete dissolution;
step 2, grafting reaction: 0.6g of ammonium persulfate is dissolved by 30ml of distilled water for standby, then the gelatin aqueous solution is placed in a three-neck flask, the initiator ammonium persulfate is added under the conditions of the original temperature and stirring speed, and then acrylic acid (11.25g), butyl acrylate (11.25g) and methyl methacrylate (7.5g) are sequentially added dropwise. In order to fully react, the monomer is dripped for 60min each time, and the temperature is kept for 60min for 360min in total.
Step 3, material blending and discharging: heating the whole reaction system to 90 ℃, preserving heat for 90min, adding 15ml of neutralizing agent ammonia water for neutralization when the temperature is reduced to 65 ℃, adjusting the pH value to 6-7, and finally filtering and discharging to obtain the environment-friendly textile size.
Example 3
In the environment-friendly textile size of the embodiment, the usage amount of each raw material is as follows: the total amount of the monomers (the mass ratio of acrylic acid, butyl acrylate and methyl methacrylate is 1.5:1.5:1:1) is 33g, the gelatin (industrial gelatin) is 70g, and the distilled water is 360 ml.
Step 1, dissolving gelatin: putting 70g of gelatin and 360ml of distilled water into a reaction kettle, mechanically stirring at 85 ℃ at the speed of 200r/min for 60min, and filtering insoluble impurities to obtain a gelatin aqueous solution after complete dissolution;
step 2, grafting reaction: firstly dissolving 1.5g of ammonium persulfate by using 40 g of distilled water for standby, then placing a gelatin aqueous solution into a three-neck flask, firstly adding an initiator under the conditions of original temperature and stirring speed, and then dropwise adding 9g of acrylic acid, 9g of butyl acrylate, 6g of methyl methacrylate and 6g of styrene in sequence. In order to fully react, the monomer is dripped for 60min each time, and the temperature is kept for 60 min. For a total of 480 min.
Step 3, material blending and discharging: and heating the whole reaction system to 90 ℃, preserving heat for 90min, adding 15ml of neutralizing agent for neutralization when the temperature is reduced to 65 ℃, adjusting the pH value to 6-7, and finally filtering and discharging to obtain the environment-friendly textile size.
Test example
The environment-friendly textile size prepared in the embodiments 1-3 of the invention and the PVA size purchased in the market are detected.
Slurry viscosity test
Will carry outThe environment-friendly textile size prepared in examples 1 to 3 and the commercially available PVA size were prepared into a solution having a solid content of 6%, and the viscosity was measured using an NDJ-5S digital rotational viscometer under the conditions of 25 ℃. + -. 0.5 ℃ and 1 ℃ using a # The rotor was set at 60rmp and the test results are shown in table 1:
TABLE 1 results of viscosity measurements
As can be seen from Table 1, the viscosity of the environment-friendly textile size prepared by the embodiment of the invention is much higher than that of the common PVA size.
Slurry adhesion test
Testing by roving
Experimental materials and instruments: modified gelatin slurry, polyester-cotton roving, a DF-101S heat collection type constant temperature heating magnetic stirrer, a JA103P electronic balance, a Y802 type eight-basket constant temperature drying box, an XJ803 electronic fabric strength instrument and a beaker.
Sample preparation: the environment-friendly textile size prepared in the example 1-3 and the PVA size purchased from the market are prepared into solutions with the solid content of 1 percent, each 1000ml of the solutions are poured into a constant-temperature stirrer with the temperature of 95 ℃ to be stirred for 30min until the solutions are stirred evenly, and then the solutions are poured into a self-made rectangular flat-bottom size tank with the constant-temperature water bath with the temperature of 95 ℃ for standby. Winding polyester-cotton roving on a self-made aluminum alloy frame, respectively soaking the polyester-cotton roving frame in a slurry tank for 5 minutes respectively on the front side and the back side to ensure that the front side and the back side of the roving are uniformly soaked, taking out the roving after the soaking, hanging and naturally drying the roving to obtain a roving sizing sample for later use.
And (3) sample testing: and taking off the rough yarn on the frame, cutting the rough yarn into rough yarn strips with proper length, putting the rough yarn strips into an oven to be dried for 2 hours, setting the temperature to be 70 ℃, and taking out the rough yarn strips to test the breaking strength of the rough yarn strips. The test conditions are that the clamping length of the roving is 100mm and the stretching speed is 50 mm/min. The results are shown in table 2:
table 2 adhesion test results
As can be seen from Table 2, the adhesion of the environment-friendly textile size prepared by the embodiment of the invention is superior to that of the common PVA size.
Sizing Performance test
Breaking Strength, elongation at Break test
The experimental method comprises the following steps: the test method is in accordance with GB/T3916-2013. The base yarn is 90/10 polyester-cotton blended yarn. The breaking tenacity, breaking elongation and elongation of the raw yarn were 362cN, 17.2mm and 6.88%, respectively. The test results are shown in table 3.
TABLE 3 sizing Performance test results
As can be seen from the test results in Table 3, the mechanical properties of the environment-friendly textile size prepared by the embodiment of the invention are superior to those of the ordinary PVA size.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (10)
1. The environment-friendly textile size is characterized by being prepared from the following raw materials in parts by weight: 6-9 parts of a monomer, 14-21 parts of gelatin and 70-80 parts of water, wherein the monomer comprises acrylic acid, butyl acrylate and methyl methacrylate;
the preparation of the environment-friendly textile size comprises the following steps:
s1, adding gelatin into water at 80-86 ℃, stirring until the gelatin is completely dissolved, and filtering insoluble impurities to obtain a gelatin water solution;
s2, keeping the temperature and the stirring speed in the step S1 unchanged, adding an initiator into the gelatin aqueous solution, and then sequentially dropwise adding different monomers;
different monomers are sequentially dripped, and the method specifically comprises the following steps: sequentially dripping acrylic acid, butyl acrylate and methyl methacrylate at the time interval of 50-90 min, wherein the dripping time of the acrylic acid, the butyl acrylate and the methyl methacrylate is 60 min;
s3, heating the whole reaction system to 90-95 ℃, preserving heat for 60-100 min, then cooling to 55-65 ℃, adding a neutralizing agent for neutralization, adjusting the pH value to 6-7, filtering and discharging to obtain the environment-friendly textile size.
2. The environment-friendly textile size according to claim 1, wherein the monomer further comprises styrene.
3. The environment-friendly textile size according to claim 2, wherein the mass ratio of acrylic acid, butyl acrylate, methyl methacrylate and styrene in the monomers is 1:3:2: 2.
4. A method for preparing the environment-friendly textile size according to any one of claims 1 to 3, characterized by comprising the following steps:
s1, adding gelatin into water at 80-86 ℃, stirring until the gelatin is completely dissolved, and filtering insoluble impurities to obtain a gelatin water solution;
s2, keeping the temperature and the stirring speed in the step S1 unchanged, adding an initiator into the gelatin aqueous solution, and then sequentially dropwise adding different monomers;
s3, heating the whole reaction system to 90-95 ℃, preserving heat for 60-100 min, then cooling to 55-65 ℃, adding a neutralizing agent for neutralization, adjusting the pH value to 6-7, filtering and discharging to obtain the environment-friendly textile size.
5. The method according to claim 4, wherein the stirring speed is 200 to 300 r/min.
6. The method according to claim 4, wherein the initiator is ammonium persulfate.
7. The preparation method according to claim 6, wherein the mass ratio of the initiator to the total amount of the monomers is 1 (20-50).
8. The preparation method according to claim 4, wherein in step S2, the sequential dropwise addition of different monomers comprises: and (3) sequentially dripping acrylic acid, butyl acrylate and methyl methacrylate at the time interval of 50-90 min, wherein the dripping time of the acrylic acid, the butyl acrylate and the methyl methacrylate is 60 min.
9. The preparation method according to claim 4, wherein in step S2, the sequential dropwise addition of different monomers comprises: and (3) sequentially dripping acrylic acid, butyl acrylate, methyl methacrylate and styrene at the time interval of 50-90 min, wherein the dripping time of the acrylic acid, the butyl acrylate, the methyl methacrylate and the styrene is 60 min.
10. The method according to claim 4, wherein the neutralizing agent is ammonia water in step S3.
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