CN113388113A - Fluorine-free water repellent softening agent, preparation method and application thereof - Google Patents
Fluorine-free water repellent softening agent, preparation method and application thereof Download PDFInfo
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- CN113388113A CN113388113A CN202110747039.XA CN202110747039A CN113388113A CN 113388113 A CN113388113 A CN 113388113A CN 202110747039 A CN202110747039 A CN 202110747039A CN 113388113 A CN113388113 A CN 113388113A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
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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
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
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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
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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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
- D06M2200/50—Modified hand or grip properties; Softening compositions
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Abstract
The application discloses a fluorine-free water-repellent softening agent, a preparation method and application thereof, wherein the preparation method of the fluorine-free water-repellent softening agent comprises the following steps: s1, mixing an organic silicon monomer, an emulsifier and water to prepare a first emulsion; s2, adding a catalyst into the first emulsion to react to obtain a first product; s3, removing low-boiling-point substances in the first product to obtain a second product; and S4, adding an aminosilane coupling agent into the second product for reaction to obtain a third product. The fluorine-free water repellent softening agent has the advantages that active group hydroxyl groups are arranged at two ends of a molecular chain, amino groups are further arranged in chain segments, the fabric can be endowed with an excellent water repellent effect, the softening agent does not contain fluorine substances, the environmental friendliness is good, the content of low ring bodies D4, D5 and D6 is lower than 1000ppm, and the fluorine-free water repellent softening agent has a smooth hand feeling when being applied to the fabric.
Description
Technical Field
The application relates to the field of fabric finishing agents, in particular to a fluorine-free water repellent softening agent, a preparation method and application thereof.
Background
The fabric waterproof agent on the market is mainly made of fluorine-containing compounds, but the production and use processes of the fabric waterproof agent have harmful effects on human bodies and the environment. Since 7/4 of 2020, the european union formally started the management of PFOA, its salts and related substances. REACH has a limit value of 25ppb for PFOA-related substances. In addition, the touch feeling of the fabric finished by the fluorine-containing waterproof agent in the market is not soft and smooth, so more and more people put efforts into the research field of the fluorine-free fabric waterproof agent, and the fabric has a certain water repellent effect and soft hand feeling by utilizing the water repellent silane chain segment. In the synthesis process of the silicone oil assistant, D4 (octamethylcyclotetrasiloxane) or a linear body is generally used as a raw material to synthesize the silicone oil, and a large amount of low-ring D4, D5 (decamethylcyclopentasiloxane) and D6 (dodecamethylcyclohexasiloxane) often remain in the reaction process. REACH regulation batch 19, 10 SVHC listings, promulgate the restriction of low ring D4, D5, D6, requiring chemicals with D4, D5, D6 levels below 1000 ppm. How to prepare the low-ring water-repellent softening agent is the focus of research and development at present.
Disclosure of Invention
An object of the present application is to provide a fluorine-free water repellent softener having a low content of D4, D5, and D6 ring bodies, and a method for preparing the same.
In order to achieve the above object, the present application provides a method for preparing a fluorine-free water repellent softening agent, comprising the steps of:
s1, mixing an organic silicon monomer, an emulsifier and water to prepare a first emulsion;
s2, adding a catalyst into the first emulsion to react to obtain a first product;
s3, removing low-boiling-point substances in the first product to obtain a second product;
and S4, adding an aminosilane coupling agent into the second product for reaction to obtain a third product.
Further, the first product comprises polysiloxane with a hydroxyl end group, the content of octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane and dodecamethylcyclohexasiloxane in the second product is less than 1000ppm, and the third product comprises polysiloxane with a hydroxyl end group and an amino group in a chain segment.
Further, the silicone monomer comprises a mixture of one or more of: hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane.
Further, the aminosilane coupling agent is selected from a mixture of one or more of: n-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-diethylenetriaminepropylmethyldimethoxysilane, N-2-aminoethyl-3-aminopropyltrimethoxysilane, N-2-aminoethyl-3-aminopropylmethyldimethoxysilane, gamma-aminopropylmethyldiethoxysilane, 3-piperazinylpropylmethyldimethoxysilane, aminoethylaminopropyltrimethoxysilane.
Further, the emulsifier is selected from a mixture of one or more of: fatty alcohol polyoxyethylene ether, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride; the catalyst is selected from one of potassium hydroxide, sodium hydroxide and tetramethyl ammonium hydroxide.
Further, the step S1 includes the following steps:
s11, uniformly mixing the organic silicon monomer with the emulsifier to obtain a first mixture;
s12, adding the first mixture and the water into a high-pressure homogenizer for homogenization until the liquid turns blue to obtain a first emulsion, wherein the particle size of the first emulsion is less than 100 nm;
in the step S2, heating the first emulsion to 60-80 ℃, adding the catalyst, heating to 80-90 ℃, and reacting for 7-8 hours in a heat preservation manner to obtain the first product;
in the step S3, removing low-boiling-point substances in the first product under the conditions that the temperature is 130-150 ℃, the vacuum degree is-0.08-0.1 MPa, and the time is 10-12 hours to obtain the second product;
in the step S4, after the vacuum is stopped, the aminosilane coupling agent is added into the second product, and the heat preservation reaction is carried out for 3-8 hours to obtain the third product.
Further, the step S4 is followed by the step S5: and cooling the third product, adding a pH regulator, and uniformly mixing to obtain a fourth product.
Further, the organic silicon monomer is 25-30 parts by mass, the emulsifier is 8-10 parts by mass, the water is 50-65 parts by mass, the catalyst is 0.01-0.03 part by mass, and the aminosilane coupling agent is 2-4 parts by mass.
Further, the content of octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane and dodecamethylcyclohexasiloxane in the second product is less than 800 ppm.
The application also provides a fluorine-free water repellent softening agent prepared by the preparation method.
Compared with the prior art, the beneficial effect of this application lies in: active group hydroxyl groups are arranged at two ends of a molecular chain of the fluorine-free water repellent softening agent, amino groups are further arranged in chain segments, and both the hydroxyl groups and the amino groups can form chemical bonds with polar groups in fibers, so that the molecular chain is firmly combined on the surface of a fabric, a compact siloxane film can be formed after high-temperature qualitative drying, and the fluorine-free water repellent softening agent has an excellent water repellent effect. The softener does not contain fluorine substances, has good environmental protection, and the content of the low ring bodies D4, D5 and D6 in the softener is less than 1000ppm, thereby meeting the restriction requirement of REACH on the low ring bodies. The fluorine-free water repellent softening agent prepared by the application has smooth hand feeling when being applied to the fabric, namely, the touch feeling of the fabric can be improved.
Detailed Description
The present application is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
It is noted that the terms first, second and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order.
The terms "comprises," "comprising," and "having," and any variations thereof, in the description and claims of this application, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The application provides a preparation method of a fluorine-free water repellent softening agent, which comprises the following steps:
s1, mixing an organic silicon monomer, an emulsifier and water to prepare a first emulsion;
s2, adding a catalyst into the first emulsion to react to obtain a first product, wherein the first product comprises polysiloxane with a hydroxyl end group;
s3, removing low-boiling-point substances in the first product to obtain a second product, wherein the content of octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5) and dodecamethylcyclohexasiloxane (D6) in the second product is lower than 1000 ppm;
and S4, adding an aminosilane coupling agent into the second product to react to obtain a third product, wherein the third product comprises polysiloxane of which the end group is hydroxyl and the chain segment contains amino.
As will be understood by those skilled in the art, the low boiling components in the first product are mainly low molecular weight ring members such as D4, D5, D6, etc.
Active group hydroxyl groups are arranged at two ends of a molecular chain of the fluorine-free water repellent softening agent, amino groups are further arranged in chain segments, and both the hydroxyl groups and the amino groups can form chemical bonds with polar groups in fibers, so that the molecular chain is firmly combined on the surface of a fabric, a compact siloxane film can be formed after high-temperature qualitative drying, and the fluorine-free water repellent softening agent has an excellent water repellent effect. The softener does not contain fluorine substances, has good environmental protection, and the content of the low ring bodies D4, D5 and D6 in the softener is less than 1000ppm, thereby meeting the restriction requirement of REACH on the low ring bodies. The fluorine-free water repellent softening agent prepared by the application has smooth hand feeling when being applied to the fabric, namely, the touch feeling of the fabric can be improved.
In some embodiments, the silicone monomer comprises a mixture of one or more of the following: hexamethylcyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), and dodecamethylcyclohexasiloxane (D6).
In some embodiments, the silicone monomer is a Dimethylcyclosiloxane Mixture (DMC).
In the present application, the emulsifier is mainly a nonionic emulsifier, and a small amount of an anionic emulsifier may be added. In some embodiments, the emulsifier is selected from a mixture of one or more of: fatty alcohol polyoxyethylene ether, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride. The emulsifier with a higher HLB value is preferably selected, the particle size of the emulsion is smaller after high-pressure homogenization, and the application stability of the product in the later period is greatly improved, such as high temperature resistance, strong alkali resistance, strong acid resistance, salt resistance and the like.
In some embodiments, the catalyst is selected from one of potassium hydroxide, sodium hydroxide, tetramethylammonium hydroxide.
In some embodiments, the aminosilane coupling agent is selected from a mixture of one or more of: n-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-diethylenetriaminepropylmethyldimethoxysilane, N-2-aminoethyl-3-aminopropyltrimethoxysilane, N-2-aminoethyl-3-aminopropylmethyldimethoxysilane, gamma-aminopropylmethyldiethoxysilane, 3-piperazinylpropylmethyldimethoxysilane, aminoethylaminopropyltrimethoxysilane.
In some embodiments, step S1 includes the steps of:
s11, uniformly mixing the organic silicon monomer and the emulsifier to obtain a first mixture;
s12, adding the first mixture and water into a high-pressure homogenizer for homogenizing until the liquid turns blue to obtain a first emulsion, wherein the particle size of the first emulsion is less than 300nm, and preferably, the particle size of the first emulsion is less than 100 nm.
Further, in step S11, the organic silicon monomer is 25-30 parts by mass, the emulsifier is 8-10 parts by mass, and the water in step S12 is 50-65 parts by mass.
In some embodiments, in step S2, the temperature of the first emulsion is raised to 60 to 80 ℃, then a catalyst is added, the temperature is raised to 80 to 90 ℃, and the reaction is performed for 7 to 8 hours under a thermal insulation condition, so as to obtain a first product.
Further, in step S2, the catalyst is 0.01 to 0.03 parts by mass.
In some embodiments, in step S3, the low boiling point substance in the first product is removed under the conditions of temperature of 130 to 150 ℃, vacuum degree of-0.08 to-0.1 MPa, and time of 10 to 12 hours to obtain the second product.
In some embodiments, in step S4, after the vacuum is stopped, adding an aminosilane coupling agent to the second product, and reacting for 3-8 hours under a heat preservation condition to obtain a third product.
Further, in step S4, 2 to 4 parts by mass of an aminosilane coupling agent.
In some embodiments, step S4 is further followed by step S5: and cooling the third product, adding a pH regulator, and uniformly mixing to obtain a fourth product.
Further, in step S5, the pH adjuster is 0.5 to 2 parts by mass.
In some embodiments, the second product has less than 800ppm octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), and dodecamethylcyclohexasiloxane (D6).
It is worth mentioning that the contents of D4, D5, D6 in the second product were determined by gas chromatography.
Taking the organosilicon monomer as octamethylcyclotetrasiloxane and the aminosilane coupling agent as N- β - (aminoethyl) - γ -aminopropylmethyldimethoxysilane as an example, the reaction occurring in step S2 is as follows:
the reaction that occurs in step S4 is as follows:
[ example 1 ]
The method comprises the following steps: putting 9g of fatty alcohol-polyoxyethylene ether and 28g of organic silicon monomer (DMC) into a stirrer, and starting stirring to uniformly mix the fatty alcohol-polyoxyethylene ether and the organic silicon monomer;
step two: putting the uniformly mixed materials in the step one into a high-pressure homogenizer, adding 60g of water, homogenizing until the liquid turns blue, and stopping homogenizing after the particle size of the emulsion is tested to be less than 100 nm;
step three: putting the homogenized liquid into a clean reactor, heating to 70 ℃, adding 0.01g of sodium hydroxide, heating to 80 ℃, and preserving heat for 7 hours;
step four: heating to 130 ℃, keeping the vacuum degree of-0.1 MPa for 10 hours, and stopping vacuum until the content of low ring bodies is lower than 800ppm through gas chromatography detection;
step five: 2.5g of gamma-aminopropyl triethoxysilane is added, and the temperature is kept for 5 hours;
step six: cooling to 45 ℃, adding 0.5g of pH regulator, stirring uniformly, and discharging.
[ example 2 ]
The method comprises the following steps: putting 8g of fatty alcohol-polyoxyethylene ether and 29g of organic silicon monomer (DMC) into a stirrer, and starting stirring to uniformly mix the fatty alcohol-polyoxyethylene ether and the organic silicon monomer;
step two: putting the uniformly mixed materials in the step one into a high-pressure homogenizer, adding 59g of water, homogenizing until the liquid turns blue, and stopping homogenizing after the particle size of the emulsion is tested to be less than 100 nm;
step three: putting the homogenized liquid into a clean reactor, heating to 70 ℃, adding 0.01g of sodium hydroxide, heating to 90 ℃, and keeping the temperature for 8 hours;
step four: heating to 150 ℃, keeping the vacuum degree of-0.08 MPa for 12 hours, and stopping vacuum until the content of low ring bodies is lower than 800ppm through gas chromatography detection;
step five: adding 3g of gamma-aminopropyltrimethoxysilane, and keeping the temperature for 5-6 hours;
step six: cooling to 45 ℃, adding 0.5g of pH regulator, stirring uniformly, and discharging.
[ example 3 ]
The method comprises the following steps: putting 8g of fatty alcohol-polyoxyethylene ether and 27g of organic silicon monomer (DMC) into a stirrer, and starting stirring to uniformly mix the fatty alcohol-polyoxyethylene ether and the organic silicon monomer;
step two: putting the uniformly mixed materials in the step one into a high-pressure homogenizer, adding 59.5g of water, homogenizing until the liquid turns blue, and stopping homogenizing after the particle size of the emulsion is tested to be less than 100 nm;
step three: putting the homogenized liquid into a clean reactor, heating to 70 ℃, adding 0.01g of sodium hydroxide, heating to 80 ℃, and preserving heat for 7 hours;
step four: heating to 140 ℃, keeping the vacuum degree of-0.09 MPa for 10 hours, and stopping vacuum until the content of low ring bodies is lower than 800ppm through gas chromatography detection;
step five: adding 1g of gamma-aminopropyltriethoxysilane and 3g of aminoethylaminopropyltrimethoxysilane, and keeping the temperature for 6 hours;
step six: cooling to 45 ℃, adding 0.5g of pH regulator, stirring uniformly, and discharging.
[ example 4 ]
Example 4 differs from example 1 in that in step two, homogenization is stopped after the particle size of the emulsion is less than 250 nm.
[ example 5 ]
Example 5 differs from example 3 in that in step five, 1g of gamma-aminopropyltriethoxysilane was added and the incubation continued for 5-6 hours.
The silicone softeners prepared in examples 1-5 were compared with two commercially available silicone softeners. Wherein, the mile (Momentive)168 is an organosilicon finishing agent produced by the American mile corporation; RH-NB-9903 is an organosilicon finishing agent sold by the applicant and has the following structural formula:
the contents of D4, D5 and D6 in each softener were measured by gas chromatography. Each softener was then applied to a fabric finish and the fabric was then tested in relation to the results shown in table 1. The test method for evaluating the hand feeling comprises the following steps: evaluating by a hand touch method, adopting a 1-5-point grading method, wherein 1 point is the worst, 5 points are the best, 5 persons evaluate simultaneously, and taking an average value; the water repellency was tested according to the standard AATCC 22 fabric water repellency spray test.
TABLE 1
From the experimental data of example 1 and example 4, it can be seen that the smaller the particle size of the emulsion when homogenized, the better the hand feel of the fabric, and the lower the amount of residual low ring bodies in the product. From the experimental data of the embodiment 2, the embodiment 3 and the embodiment 5, it can be seen that the addition of the aminosilane coupling agent has obvious influence on the content of low ring bodies in the softener and the hand feeling of the fabric, and when the addition amount of the aminosilane coupling agent is insufficient, the content of low ring bodies in the softener is higher, and the hand feeling of the fabric is poorer. In summary, the process provided herein results in softeners having lower levels of cyclic bodies than commercially available silicone finishes and better water repellency.
The foregoing has described the general principles, essential features, and advantages of the application. It will be understood by those skilled in the art that the present application is not limited to the embodiments described above, which are merely illustrative of the principles of the application, but that various changes and modifications may be made without departing from the spirit and scope of the application, and these changes and modifications are intended to be within the scope of the application as claimed. The scope of protection claimed by this application is defined by the following claims and their equivalents.
Claims (10)
1. A preparation method of a fluorine-free water repellent softening agent is characterized by comprising the following steps:
s1, mixing an organic silicon monomer, an emulsifier and water to prepare a first emulsion;
s2, adding a catalyst into the first emulsion to react to obtain a first product;
s3, removing low-boiling-point substances in the first product to obtain a second product;
and S4, adding an aminosilane coupling agent into the second product for reaction to obtain a third product.
2. The method of claim 1, wherein the first product comprises a polysiloxane with hydroxyl end groups, the second product comprises octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane and dodecamethylcyclohexasiloxane in an amount less than 1000ppm, and the third product comprises a polysiloxane with hydroxyl end groups and amino groups in chain segments.
3. The method of preparing a fluorine-free water repellent softening agent of claim 1, wherein the silicone monomer comprises a mixture of one or more of: hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane.
4. The method of preparing a fluorine-free water repellent softening agent of claim 1, wherein the aminosilane coupling agent is selected from a mixture of one or more of: n-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-diethylenetriaminepropylmethyldimethoxysilane, N-2-aminoethyl-3-aminopropyltrimethoxysilane, N-2-aminoethyl-3-aminopropylmethyldimethoxysilane, gamma-aminopropylmethyldiethoxysilane, 3-piperazinylpropylmethyldimethoxysilane, aminoethylaminopropyltrimethoxysilane.
5. The method of preparing a fluorine-free water repellent softening agent according to claim 1, wherein the emulsifier is selected from a mixture of one or more of: fatty alcohol polyoxyethylene ether, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride; the catalyst is selected from one of potassium hydroxide, sodium hydroxide and tetramethyl ammonium hydroxide.
6. The method for preparing a fluorine-free water repellent softening agent according to any one of claims 1 to 5, wherein the step S1 comprises the steps of:
s11, uniformly mixing the organic silicon monomer with the emulsifier to obtain a first mixture;
s12, adding the first mixture and the water into a high-pressure homogenizer for homogenization until the liquid turns blue to obtain a first emulsion, wherein the particle size of the first emulsion is less than 100 nm;
in the step S2, heating the first emulsion to 60-80 ℃, adding the catalyst, heating to 80-90 ℃, and reacting for 7-8 hours in a heat preservation manner to obtain the first product;
in the step S3, removing low-boiling-point substances in the first product under the conditions that the temperature is 130-150 ℃, the vacuum degree is-0.08-0.1 MPa, and the time is 10-12 hours to obtain the second product;
in the step S4, after the vacuum is stopped, the aminosilane coupling agent is added into the second product, and the heat preservation reaction is carried out for 3-8 hours to obtain the third product.
7. The method for preparing a fluorine-free water repellent softening agent according to claim 6, further comprising step S5 after step S4: and cooling the third product, adding a pH regulator, and uniformly mixing to obtain a fourth product.
8. The method for preparing the fluorine-free water repellent softening agent according to claim 6, wherein the silicone monomer is 25 to 30 parts by mass, the emulsifier is 8 to 10 parts by mass, the water is 50 to 65 parts by mass, the catalyst is 0.01 to 0.03 part by mass, and the aminosilane coupling agent is 2 to 4 parts by mass.
9. A fluorine-free water repellent softening agent, which is obtained by the production method according to any one of claims 1 to 8.
10. A fabric prepared by finishing the fabric with the fluorine-free water repellent softening agent of claim 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114197214A (en) * | 2021-12-28 | 2022-03-18 | 清远市宏图助剂有限公司 | Soft smoothing agent for acrylic yarn and preparation method thereof |
| CN116284791A (en) * | 2022-12-31 | 2023-06-23 | 浙江汉邦新材料股份有限公司 | Nanometer self-cleaning antifouling finishing agent |
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| CN114197214A (en) * | 2021-12-28 | 2022-03-18 | 清远市宏图助剂有限公司 | Soft smoothing agent for acrylic yarn and preparation method thereof |
| CN114197214B (en) * | 2021-12-28 | 2024-03-29 | 清远市宏图助剂有限公司 | Soft smoothing agent for acrylic yarns and preparation method thereof |
| CN116284791A (en) * | 2022-12-31 | 2023-06-23 | 浙江汉邦新材料股份有限公司 | Nanometer self-cleaning antifouling finishing agent |
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