CN110565370A - preparation method of natural flame-retardant finishing agent - Google Patents
preparation method of natural flame-retardant finishing agent Download PDFInfo
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- CN110565370A CN110565370A CN201910953612.5A CN201910953612A CN110565370A CN 110565370 A CN110565370 A CN 110565370A CN 201910953612 A CN201910953612 A CN 201910953612A CN 110565370 A CN110565370 A CN 110565370A
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- D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
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- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
- D06M13/256—Sulfonated compounds esters thereof, e.g. sultones
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- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
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- 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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- 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
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- 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
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- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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Abstract
the invention provides a preparation method of a natural flame-retardant finishing agent, which comprises the following steps: (1) mixing nano-composite material nano-attapulgite and nano-SiO2Treating with HCl solution to prepare acidified nanometer composite material; (2) compounding acidified nano powdermodifying the composite material by using a silane coupling agent to obtain a modified nano composite material; (3) reacting carboxymethyl chitosan with the modified nano composite material to prepare carboxymethyl chitosan modified nano composite material solution; (4) and (4) adding diammonium hydrogen phosphate, polyethylene glycol, sodium dodecyl diphenyl ether disulfonate, a closed water-based isocyanate crosslinking agent, polyvinyl alcohol and cocoyl monoethanolamine into the reaction solution obtained in the step (3) to obtain the natural flame-retardant finishing agent. After the finishing agent finishes the fabric, the fabric has good flame retardant property and mechanical strength, so that the finishing agent has important application value in the field of preparation of flame retardant fabrics.
Description
Technical Field
The invention belongs to the technical field of textiles, and particularly relates to a preparation method of a natural flame-retardant finishing agent.
Background
Natural fiber articles have excellent water permeability, air permeability, comfort, good biodegradability, etc., so that they are widely used in various aspects of daily life. However, these products have a low minimum oxygen demand when burning, are very prone to fire risks when exposed to sparks or at high temperatures, and spread quickly, thereby causing serious damage to people's lives and property. Therefore, the natural fiber raw material is subjected to flame retardant treatment to prevent oxygen and heat transmission, so that the flame retardant property is endowed, and the flame retardant treatment plays an important role in preventing fire.
Conventional flame retardants mainly include halogen-based, phosphorus-based, nitrogen-based, sulfur-based, silicon-based, hydroxide-based, and the like, and the most widely used flame retardant is a halogen-based flame retardant. Although the flame retardant property is excellent, the material treated by the flame retardant will emit substances harmful to the environment and human body, such as hydrogen halide, under high temperature condition, and cause secondary pollution to the environment. Nitrogen-containing flame retardants are generally used in practical applications with other types of built flame retardants. The preparation process of the phosphorus flame retardant is relatively complex and expensive.
therefore, the green and environment-friendly high-performance flame retardant is the main direction of research in the field, and the nano material is widely applied to the research in a plurality of fields, has the advantages of good stability, green and environment friendliness and the like, and has poor adhesion force, so that the flame retardant performance of the nano material is poor.
disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a preparation method of a natural flame retardant finishing agent.
in order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a natural flame-retardant finishing agent comprises the following steps:
(1) Adding the nano composite material into 1-10% HCl solution according to the mass ratio of 10-20% under the condition of stirring, stirring and reacting for 5-10h at the temperature of 30-40 ℃, obtaining a precipitate through suction filtration, and washing the precipitate with deionized water until the precipitate is neutral; vacuum drying the treated nano composite material at the temperature of 60 ℃, grinding and sieving the dried nano composite material to obtain an acidified nano composite material;
(2) Adding the acidified nano composite material prepared in the step (1) into absolute ethyl alcohol according to the mass ratio of 10-20% under the stirring condition, continuously stirring for 5-10min, adding a silane coupling agent with the final concentration of 5-10%, slowly raising the temperature to 50-70 ℃ under the stirring condition, keeping the temperature for reaction for 5-8h, cooling the reaction system to room temperature, performing suction filtration, washing for 2-3 times by using absolute ethyl alcohol, and performing vacuum drying, grinding and sieving on the collected nano composite material to obtain a modified nano composite material;
(3) dissolving carboxymethyl chitosan in an aqueous solution to prepare 20-40% by mass, adding the modified nano composite material prepared in the step (2) under the stirring condition, slowly raising the temperature to 70-90 ℃ under the stirring condition, keeping the temperature, and continuously reacting for 3-6 hours to obtain a carboxymethyl chitosan modified nano composite material solution;
(4) Adding 10-20 parts of diammonium hydrogen phosphate, 5-10 parts of polyethylene glycol, 4-8 parts of sodium dodecyl diphenyl ether disulfonate, 6-12 parts of a closed water-based isocyanate crosslinking agent, 3-6 parts of polyvinyl alcohol and 2-5 parts of cocoyl monoethanolamine into 50-80 parts of the reaction solution obtained in the step (3), and continuously stirring and reacting at the temperature of 40-60 ℃ for 3-5 hours to obtain a natural flame-retardant finishing agent;
The nano composite material comprises the following components in percentage by mass (1-5): (1-3) Nano Attapulgite and Nano SiO2。
furthermore, the screening meshes of the steps (1) and (2) are 50-100 meshes.
Further, the silane coupling agent in the step (2) is KH550, KH572 or DL 602.
Preferably, the weight parts of the raw materials in the step (4) are as follows: 65 parts of reaction solution obtained in the step (3), 15 parts of diammonium hydrogen phosphate, 8 parts of polyethylene glycol, 6 parts of sodium dodecyl diphenyl ether disulfonate, 9 parts of a closed water-based isocyanate crosslinking agent, 4.5 parts of polyvinyl alcohol and 3.5 parts of cocoyl monoethanolamine.
further, the nano-unevennessthe particle size of the attapulgite is 10-25nm, and the nano SiO is2The particle size of (A) is 40-80 nm.
The natural flame-retardant finishing agent prepared by the preparation method is provided by the invention.
The method for finishing the textile fabric by using the finishing agent comprises the following steps:
(1) Diluting the finishing agent by 5-10 times by using deionized water;
(2) Mixing the fabric in a proportion of 1: immersing the raw materials into a finishing agent at a bath ratio of 10-20 for three-dipping and three-rolling treatment at 40-60 ℃ for 60-90min, wherein the rolling residual rate is 70-90%, drying at 80 ℃, and baking at 120 ℃ for 1-2 min.
has the advantages that: the invention provides a preparation method of a natural flame-retardant finishing agent, which uses nano-attapulgite and nano-SiO2As a nano composite material, firstly, the material is subjected to acidification treatment to expose hydroxyl groups on the surface, then a silane coupling agent is modified on the surface of the material to enable the hydroxyl groups on the surface of the material to react with silanol groups of the silane coupling agent, and then an active group at the other end of the silane coupling agent is utilized to react with chitosan, so that the chitosan-modified nano composite material is prepared. The limiting oxygen index LOI of the treated cotton and linen fabric by the finishing agent is as high as 52, the burning rate is as low as 2.8mm/s, the breaking strength of the fabric is improved after the treatment by the finishing agent, the breaking strength is as high as 453.8N, the breaking elongation of the fabric is reduced although the breaking elongation of the fabric tends to be reduced, the reduction range is low, and the integral mechanical property of the fabric cannot be greatly influenced. Therefore, the finishing agent prepared by the invention has important use value in the field of preparation of flame-retardant fabrics.
Detailed Description
The present invention is further described below with reference to specific examples, which are only exemplary and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Example 1
A preparation method of a natural flame-retardant finishing agent comprises the following steps:
(1) Adding the nano composite material into 5% HCl solution according to the mass ratio of 15% under the condition of stirring, stirring and reacting for 8 hours at the temperature of 35 ℃, obtaining precipitates through suction filtration, and washing the precipitates with deionized water until the precipitates are neutral; vacuum drying the treated nano composite material at the temperature of 60 ℃, grinding and sieving the dried nano composite material to obtain an acidified nano composite material;
(2) Adding the acidified nano composite material prepared in the step (1) into absolute ethyl alcohol according to the mass ratio of 15% under the stirring condition, continuously stirring for 5-10min, adding a silane coupling agent with the final concentration of 8%, slowly raising the temperature to 60 ℃ under the stirring condition, keeping the temperature for reacting for 6.5h, cooling the reaction system to room temperature, performing suction filtration, washing with absolute ethyl alcohol for 2-3 times, and performing vacuum drying, grinding and sieving on the collected nano composite material to obtain a modified nano composite material;
(3) Dissolving carboxymethyl chitosan in an aqueous solution to prepare 30 mass percent, adding the modified nano composite material prepared in the step (2) under the stirring condition, slowly raising the temperature to 80 ℃ under the stirring condition, keeping the temperature, and continuously reacting for 4.5 hours to prepare a carboxymethyl chitosan modified nano composite material solution;
(4) Adding 15 parts of diammonium hydrogen phosphate, 8 parts of polyethylene glycol, 6 parts of sodium dodecyl diphenyl ether disulfonate, 9 parts of a closed water-based isocyanate crosslinking agent, 4.5 parts of polyvinyl alcohol and 3.5 parts of cocoyl monoethanolamine into 65 parts of the reaction solution obtained in the step (3), and continuously stirring and reacting at the temperature of 50 ℃ for 4 hours to obtain a natural flame-retardant finishing agent;
The nano composite material is prepared from the following components in percentage by mass: 1 nano-attapulgiteAnd nano SiO2。
The screening meshes of the steps (1) and (2) are 80 meshes.
The silane coupling agent in the step (2) is KH 550.
the particle size of the nano attapulgite is 10-20nm, and the nano SiO is2has a particle diameter of 50-60 nm.
the method for finishing the textile fabric by using the finishing agent comprises the following steps:
(1) Diluting the finishing agent by 8 times by using deionized water;
(2) Mixing the fabric in a proportion of 1: 15 bath ratio, the treatment temperature is 50 ℃, the treatment time is 75min, the rolling residue rate is 80%, the mixture is dried at 80 ℃, and then the mixture is baked at 120 ℃ for 1-2 min.
Example 2
A preparation method of a natural flame-retardant finishing agent comprises the following steps:
(1) Adding the nano composite material into 1% HCl solution according to the mass ratio of 10% under the condition of stirring, stirring and reacting for 5 hours at the temperature of 30 ℃, obtaining precipitates through suction filtration, and washing the precipitates with deionized water until the precipitates are neutral; vacuum drying the treated nano composite material at the temperature of 60 ℃, grinding and sieving the dried nano composite material to obtain an acidified nano composite material;
(2) adding the acidified nano composite material prepared in the step (1) into absolute ethyl alcohol according to the mass ratio of 10% under the stirring condition, continuously stirring for 5-10min, adding a silane coupling agent with the final concentration of 5%, slowly raising the temperature to 50 ℃ under the stirring condition, keeping the temperature for reaction for 5h, cooling the reaction system to room temperature, performing suction filtration, washing with absolute ethyl alcohol for 2-3 times, and performing vacuum drying, grinding and sieving on the collected nano composite material to obtain a modified nano composite material;
(3) dissolving carboxymethyl chitosan in an aqueous solution to prepare 20% by mass, adding the modified nano composite material prepared in the step (2) under the stirring condition, slowly raising the temperature to 70 ℃ under the stirring condition, keeping the temperature, and continuously reacting for 3 hours to obtain a carboxymethyl chitosan modified nano composite material solution;
(4) Adding 10 parts of diammonium hydrogen phosphate, 5 parts of polyethylene glycol, 4 parts of sodium dodecyl diphenyl ether disulfonate, 6 parts of a closed water-based isocyanate crosslinking agent, 3 parts of polyvinyl alcohol and 2 parts of cocoyl monoethanolamine into 50 parts of the reaction solution obtained in the step (3), and continuously stirring and reacting for 3 hours at the temperature of 40 ℃ to obtain a natural flame-retardant finishing agent;
The nano composite material is prepared from the following components in percentage by mass: 2 nano-attapulgite and nano-SiO2。
The screening meshes of the steps (1) and (2) are 50 meshes.
The silane coupling agent in the step (2) is KH 572.
the particle size of the nano attapulgite is 15-25nm, and the nano SiO is2the particle size of (A) is 40-50 nm.
The method for finishing the textile fabric by using the finishing agent comprises the following steps:
(1) diluting the finishing agent by 5 times by using deionized water;
(2) mixing the fabric in a proportion of 1: immersing the raw materials into a finishing agent at a bath ratio of 10 for three-dipping and three-rolling treatment, wherein the treatment temperature is 40 ℃, the treatment time is 60min, the rolling residue rate is 70%, then drying the raw materials at 80 ℃, and then baking the raw materials for 1-2min at 120 ℃.
example 3
a preparation method of a natural flame-retardant finishing agent comprises the following steps:
(1) Adding the nano composite material into 3% HCl solution according to the mass ratio of 12% under the condition of stirring, stirring and reacting for 6 hours at the temperature of 33 ℃, obtaining precipitates through suction filtration, and washing the precipitates with deionized water until the precipitates are neutral; vacuum drying the treated nano composite material at the temperature of 60 ℃, grinding and sieving the dried nano composite material to obtain an acidified nano composite material;
(2) adding the acidified nano composite material prepared in the step (1) into absolute ethyl alcohol according to the mass ratio of 12% under the stirring condition, continuously stirring for 5-10min, adding a silane coupling agent with the final concentration of 6%, slowly raising the temperature to 55 ℃ under the stirring condition, keeping the temperature for reacting for 6h, cooling the reaction system to room temperature, performing suction filtration, washing with absolute ethyl alcohol for 2-3 times, and performing vacuum drying, grinding and sieving on the collected nano composite material to obtain a modified nano composite material;
(3) Dissolving carboxymethyl chitosan in an aqueous solution to prepare 25 mass percent, adding the modified nano composite material prepared in the step (2) under the stirring condition, slowly raising the temperature to 75 ℃ under the stirring condition, keeping the temperature, and continuously reacting for 4 hours to obtain a carboxymethyl chitosan modified nano composite material solution;
(4) Adding 12 parts of diammonium hydrogen phosphate, 6 parts of polyethylene glycol, 5 parts of sodium dodecyl diphenyl ether disulfonate, 7 parts of a closed water-based isocyanate crosslinking agent, 4 parts of polyvinyl alcohol and 3 parts of cocoyl monoethanolamine into 50-80 parts of the reaction solution obtained in the step (3), and continuously stirring and reacting at the temperature of 45 ℃ for 3.5 hours to obtain a natural flame-retardant finishing agent;
The nano composite material is prepared from the following components in percentage by mass: 1 nano-attapulgite and nano-SiO2。
The screening meshes of the steps (1) and (2) are 60 meshes.
The silane coupling agent in the step (2) is DL 602.
The particle size of the nano attapulgite is 10-15nm, and the nano SiO is2Has a particle diameter of 50-60 nm.
the method for finishing the textile fabric by using the finishing agent comprises the following steps:
(1) Diluting the finishing agent by 6 times by using deionized water;
(2) Mixing the fabric in a proportion of 1: and (3) immersing the steel plate into a finishing agent according to the bath ratio of 12 for three-immersion and three-rolling treatment, wherein the treatment temperature is 45 ℃, the treatment time is 70min, the rolling residue rate is 75%, then drying the steel plate at 80 ℃, and then baking the steel plate at 120 ℃ for 1-2 min.
Example 4
a preparation method of a natural flame-retardant finishing agent comprises the following steps:
(1) adding the nano composite material into 10% HCl solution according to the mass ratio of 20% under the condition of stirring, stirring and reacting for 10 hours at the temperature of 40 ℃, obtaining precipitates through suction filtration, and washing the precipitates with deionized water until the precipitates are neutral; vacuum drying the treated nano composite material at the temperature of 60 ℃, grinding and sieving the dried nano composite material to obtain an acidified nano composite material;
(2) Adding the acidified nano composite material prepared in the step (1) into absolute ethyl alcohol by a mass ratio of 20% under the condition of stirring, continuously stirring for 5-10min, adding a silane coupling agent with a final concentration of 10%, slowly raising the temperature to 70 ℃ under the condition of stirring, keeping the temperature for reacting for 8h, cooling a reaction system to room temperature, performing suction filtration, washing with absolute ethyl alcohol for 2-3 times, and performing vacuum drying, grinding and sieving on the collected nano composite material to obtain a modified nano composite material;
(3) Dissolving carboxymethyl chitosan in an aqueous solution to prepare 40% by mass, adding the modified nano composite material prepared in the step (2) under the stirring condition, slowly raising the temperature to 90 ℃ under the stirring condition, keeping the temperature, and continuously reacting for 6 hours to obtain a carboxymethyl chitosan modified nano composite material solution;
(4) Adding 20 parts of diammonium hydrogen phosphate, 10 parts of polyethylene glycol, 8 parts of sodium dodecyl diphenyl ether disulfonate, 12 parts of a closed water-based isocyanate crosslinking agent, 6 parts of polyvinyl alcohol and 5 parts of cocoyl monoethanolamine into 80 parts of the reaction solution obtained in the step (3), and continuously stirring and reacting for 5 hours at the temperature of 40-60 ℃ to obtain a natural flame-retardant finishing agent;
the nano composite material is prepared from the following components in percentage by mass: 1 nano-attapulgite and nano-SiO2。
The screening meshes of the steps (1) and (2) are 100 meshes.
the silane coupling agent in the step (2) is KH 550.
the particle size of the nano attapulgite is 2025nm, and the nano SiO is2the particle size of (A) is 70-80 nm.
The method for finishing the textile fabric by using the finishing agent comprises the following steps:
(1) diluting the finishing agent by 10 times by using deionized water;
(2) mixing the fabric in a proportion of 1: immersing the mixture into a finishing agent at a bath ratio of 20 for three-dipping and three-rolling treatment, wherein the treatment temperature is 60 ℃, the treatment time is 90min, and the rolling residue rate is 90%, then drying the mixture at 80 ℃, and then baking the mixture at 120 ℃ for 1-2 min.
comparative example 1
comparative example 1 is different from example 1 in that the carboxymethyl chitosan-modified nanocomposite solution prepared in steps (1) to (3) was not added to the finishing agent of comparative example 1.
comparative example 2
Comparative example 2 differs from example 1 in that the finish of comparative example 2 eliminates the process of step (3).
The characteristics of the cotton and linen fabrics finished by the finishing agents prepared in examples 1-4 and comparative examples 1-2 are shown in table 1, and the finishing agent prepared by the invention has good flame retardant property for the fabrics, the limiting oxygen index LOI of the finishing agent is as high as 52, the burning rate is as low as 2.8mm/s, the breaking strength of the fabrics is improved after the finishing agent is treated, the breaking strength of the fabrics is as high as 453.8N, the breaking elongation of the fabrics tends to be reduced, but the reduction range is lower, and the integral mechanical property of the fabrics cannot be greatly influenced. Therefore, the finishing agent prepared by the invention has important use value in the field of preparation of flame-retardant fabrics.
TABLE 1
。
Claims (7)
1. the preparation method of the natural flame-retardant finishing agent is characterized by comprising the following steps:
(1) Adding the nano composite material into 1-10% HCl solution according to the mass ratio of 10-20% under the condition of stirring, stirring and reacting for 5-10h at the temperature of 30-40 ℃, obtaining a precipitate through suction filtration, and washing the precipitate with deionized water until the precipitate is neutral; vacuum drying the treated nano composite material at the temperature of 60 ℃, grinding and sieving the dried nano composite material to obtain an acidified nano composite material;
(2) Adding the acidified nano composite material prepared in the step (1) into absolute ethyl alcohol according to the mass ratio of 10-20% under the stirring condition, continuously stirring for 5-10min, adding a silane coupling agent with the final concentration of 5-10%, slowly raising the temperature to 50-70 ℃ under the stirring condition, keeping the temperature for reaction for 5-8h, cooling the reaction system to room temperature, performing suction filtration, washing for 2-3 times by using absolute ethyl alcohol, and performing vacuum drying, grinding and sieving on the collected nano composite material to obtain a modified nano composite material;
(3) dissolving carboxymethyl chitosan in an aqueous solution to prepare 20-40% by mass, adding the modified nano composite material prepared in the step (2) under the stirring condition, slowly raising the temperature to 70-90 ℃ under the stirring condition, keeping the temperature, and continuously reacting for 3-6 hours to obtain a carboxymethyl chitosan modified nano composite material solution;
(4) Adding 10-20 parts of diammonium hydrogen phosphate, 5-10 parts of polyethylene glycol, 4-8 parts of sodium dodecyl diphenyl ether disulfonate, 6-12 parts of a closed water-based isocyanate crosslinking agent, 3-6 parts of polyvinyl alcohol and 2-5 parts of cocoyl monoethanolamine into 50-80 parts of the reaction solution obtained in the step (3), and continuously stirring and reacting at the temperature of 40-60 ℃ for 3-5 hours to obtain a natural flame-retardant finishing agent;
the nano composite material comprises the following components in percentage by mass (1-5): (1-3) Nano Attapulgite and Nano SiO2。
2. The preparation method of the natural flame retardant finishing agent according to the claim 1, characterized in that the screening mesh number of the steps (1) and (2) is 50-100 meshes.
3. the method for preparing a natural flame retardant finishing agent according to claim 1, wherein the silane coupling agent in the step (2) is KH550, KH572 or DL 602.
4. The preparation method of the natural flame retardant finishing agent according to claim 1, wherein the raw materials in the step (4) comprise, by weight: 65 parts of reaction solution obtained in the step (3), 15 parts of diammonium hydrogen phosphate, 8 parts of polyethylene glycol, 6 parts of sodium dodecyl diphenyl ether disulfonate, 9 parts of a closed water-based isocyanate crosslinking agent, 4.5 parts of polyvinyl alcohol and 3.5 parts of cocoyl monoethanolamine.
5. The preparation method of the natural flame retardant finishing agent according to claim 1, wherein the particle size of the nano-attapulgite is 10-25nm, and the nano-SiO is2the particle size of (A) is 40-80 nm.
6. a natural flame retardant finish made by the method of manufacture of any of claims 1-5.
7. A method of finishing a textile fabric with the finishing agent of claim 6, comprising the steps of:
(1) Diluting the finishing agent by 5-10 times by using deionized water;
(2) Mixing the fabric in a proportion of 1: immersing the raw materials into a finishing agent at a bath ratio of 10-20 for three-dipping and three-rolling treatment at 40-60 ℃ for 60-90min, wherein the rolling residual rate is 70-90%, drying at 80 ℃, and baking at 120 ℃ for 1-2 min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111893750A (en) * | 2020-08-11 | 2020-11-06 | 盐城工学院 | Preparation method of flame-retardant cotton fabric |
| CN114411422A (en) * | 2022-03-02 | 2022-04-29 | 杭州萧山正达纺织有限公司 | High-temperature-resistant flame-retardant composite fabric and preparation method thereof |
| CN115073118A (en) * | 2022-07-07 | 2022-09-20 | 河南中柏防火涂料科技有限公司 | Gypsum-based flame-retardant composite material and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107641958A (en) * | 2017-10-11 | 2018-01-30 | 陕西科技大学 | Bafta is fire-retardant attapulgite modified and preparation method thereof with hexachlorocyclotriph,sphazene |
| CN109280446A (en) * | 2018-10-29 | 2019-01-29 | 合肥晓拂新能源有限公司 | Water nano anti-flaming dope |
| CN109294344A (en) * | 2018-09-10 | 2019-02-01 | 华南理工大学 | Biology base highly effective flame-retardant coating with universality and the preparation method and application thereof |
| CN109503906A (en) * | 2018-11-22 | 2019-03-22 | 安徽明福电缆有限公司 | A kind of powerful permanent seal cooling flame-proof power cable sheath and preparation method thereof |
| CN110117899A (en) * | 2019-06-03 | 2019-08-13 | 陕西科技大学 | A kind of flame retardant type cotton fabric and preparation method thereof |
-
2019
- 2019-10-09 CN CN201910953612.5A patent/CN110565370A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107641958A (en) * | 2017-10-11 | 2018-01-30 | 陕西科技大学 | Bafta is fire-retardant attapulgite modified and preparation method thereof with hexachlorocyclotriph,sphazene |
| CN109294344A (en) * | 2018-09-10 | 2019-02-01 | 华南理工大学 | Biology base highly effective flame-retardant coating with universality and the preparation method and application thereof |
| CN109280446A (en) * | 2018-10-29 | 2019-01-29 | 合肥晓拂新能源有限公司 | Water nano anti-flaming dope |
| CN109503906A (en) * | 2018-11-22 | 2019-03-22 | 安徽明福电缆有限公司 | A kind of powerful permanent seal cooling flame-proof power cable sheath and preparation method thereof |
| CN110117899A (en) * | 2019-06-03 | 2019-08-13 | 陕西科技大学 | A kind of flame retardant type cotton fabric and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 高平强: "《无机纳米硼酸盐复合阻燃材料制备技术》", 31 March 2019, 吉林大学出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111893750A (en) * | 2020-08-11 | 2020-11-06 | 盐城工学院 | Preparation method of flame-retardant cotton fabric |
| CN111893750B (en) * | 2020-08-11 | 2022-11-11 | 盐城工学院 | Preparation method of flame-retardant cotton fabric |
| CN114411422A (en) * | 2022-03-02 | 2022-04-29 | 杭州萧山正达纺织有限公司 | High-temperature-resistant flame-retardant composite fabric and preparation method thereof |
| CN115073118A (en) * | 2022-07-07 | 2022-09-20 | 河南中柏防火涂料科技有限公司 | Gypsum-based flame-retardant composite material and preparation method thereof |
| CN115073118B (en) * | 2022-07-07 | 2024-02-13 | 河南中柏防火涂料科技有限公司 | Gypsum-based flame-retardant composite material and preparation method thereof |
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Application publication date: 20191213 |