阅读说明：本技术 一种天然阻燃整理剂的制备方法 (preparation method of natural flame-retardant finishing agent ) 是由 许磊 于 2019-10-09 设计创作，主要内容包括：本发明提供了一种天然阻燃整理剂的制备方法,包括以下步骤：(1)将纳米复合材料纳米凹凸棒土和纳米SiO<Sub>2</Sub>用浓度为HCl溶液进行处理制备酸化纳米复合材料；(2)将酸化纳米复合材料用硅烷偶联剂进行修饰得到改性纳米复合材料；(3)将羧甲基壳聚糖与改性纳米复合材料进行反应,制得羧甲基壳聚糖改性的纳米复合材料溶液；(4)向步骤(3)的反应溶液中加入磷酸氢二铵、聚乙二醇、十二烷基二苯醚二磺酸钠、封闭型水性异氰酸酯交联剂、聚乙烯醇、椰油酰单乙醇胺,制得天然阻燃整理剂。该整理剂对面料进行整理后使得面料具有良好的阻燃性能和机械强度,因此,该整理剂在阻燃面料的制备领域具有重要的应用价值。(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-SiO 2 Treating 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.)

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.

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.