阅读说明：本技术 一种纺织品阻燃剂的制备方法 (Preparation method of textile flame retardant ) 是由 王若梅 于 2020-12-26 设计创作，主要内容包括：本发明属于纺织品领域,具体涉及一种纺织品阻燃剂的制备方法。本发明以丙烯酰胺、马来酸酐作为基础原料,与添加剂等进行混合,形成原料A,再以甲基丙烯酸缩水甘油酯等作为基础原料,形成原料B,随后两者通过引发剂等的作用进行反应,形成了具有孔隙结构,马来酸酐改性丙烯酰胺包裹丙烯酸酯类的聚合物,增加了阻燃效果,随后通过利用硫酸铜,在次磷酸钠的作用下形成纳米铜,沉积在聚合物同时,同时添加氨基硅烷提高耐水性,以及增加与织物的结合性能,并且利用聚谷氨酸与聚合物进行复配,通过氨基硅烷降低其降解性能,同时利用聚谷氨酸可以很好的对香叶醇进行包裹结合,形成纺织品阻燃剂,有效解决了目前阻燃剂阻燃效果差的问题。(The invention belongs to the field of textiles, and particularly relates to a preparation method of a textile flame retardant. The invention takes acrylamide and maleic anhydride as basic raw materials to be mixed with additives and the like to form a raw material A, then takes glycidyl methacrylate and the like as basic raw materials to form a raw material B, and the raw materials and the raw material B react under the action of initiators and the like to form a polymer which has a pore structure and is prepared by coating acrylic ester with maleic anhydride modified acrylamide, so that the flame retardant effect is improved, and then by utilizing copper sulfate, nano copper is formed under the action of sodium hypophosphite and is deposited on a polymer, and meanwhile, amino silane is added to improve the water resistance and the binding property with fabrics, and polyglutamic acid is compounded with the polymer, the degradation performance of the polyglutamic acid is reduced by aminosilane, meanwhile, the polyglutamic acid can be used for wrapping and combining the geraniol to form a textile flame retardant, so that the problem of poor flame retardant effect of the conventional flame retardant is effectively solved.)

1. The preparation method of the textile flame retardant is characterized by comprising the following steps:

(1) taking 100-120 parts of water, 40-50 parts of mixed monomer, 12-16 parts of additive, 3-7 parts of cross-linking agent and 2-5 parts of emulsifier by weight, stirring the water, the mixed monomer, the cross-linking agent and the emulsifier, adding the additive, and mixing to obtain a raw material A;

(2) taking 90-110 parts by weight of acetone, 35-45 parts by weight of glycidyl methacrylate, 2-7 parts by weight of N-hydroxymethyl acrylamide and 2-5 parts by weight of citric acid fatty glyceride, and stirring and mixing to obtain a raw material B;

(3) putting the raw material A into a reactor, stirring at 1100r/min, then dropwise adding a raw material B accounting for 90-95% of the volume of the raw material A, continuously stirring, adding an initiator accounting for 5-8% of the mass of the raw material A, heating, stirring, discharging, filtering, washing, drying, and collecting a dried substance;

(4) taking 120-130 parts of water, 50-60 parts of a dry matter, 20-23 parts of sodium hypophosphite, 12-15 parts of copper sulfate, 11-14 parts of polyglutamic acid, 10-20 parts of geraniol and 6-8 parts of r-aminopropyltriethoxysilane by weight, firstly putting the water, the dry matter, the sodium hypophosphite and the copper sulfate into a reactor, adjusting the pH to 2.0, heating, stirring, cooling, standing, adding the polyglutamic acid, the geraniol and the r-aminopropyltriethoxysilane, stirring, discharging, freeze-drying, crushing, sieving, collecting sieved particles, and obtaining the textile flame retardant.

2. The preparation method of the textile flame retardant according to claim 1, wherein the mixed monomer in the step (1) is prepared by mixing acrylamide and maleic anhydride according to a mass ratio of 9: 1-2.

3. The method for preparing the flame retardant for the textile according to claim 1, wherein the additive in the step (1) is any one of sodium bicarbonate and sodium carbonate.

4. The preparation method of the textile flame retardant according to claim 1, wherein the crosslinking agent in the step (1) is any one of ethylene glycol dimethacrylate and N, N-methylene bisacrylamide.

5. The preparation method of the textile flame retardant according to claim 1, wherein the emulsifier in the step (1) is any one of Tween 80 and Span 80.

6. The method for preparing the flame retardant for the textile according to claim 1, wherein the initiator in the step (3) is any one of benzoyl peroxide and benzoyl peroxide tert-butyl ester.

Technical Field

The invention belongs to the field of textiles, and particularly relates to a preparation method of a textile flame retardant.

Background

The cotton fiber has excellent moisture absorption and air permeability, good dyeing property and ecological relevance, wide sources and economy, thus being widely welcomed by people. However, cotton fibers are flammable fibers and have a burning risk, and the fire caused by the cotton fabrics seriously affects the life and property safety of people. The cellulose fiber brings various products to people and also brings fire hazard to people. A large number of textiles such as those used on airplanes, trains, ships, and upholstery including ground a kind of woolen fabric made in Xizang Autonomous Region, curtains, wallpaper, etc., are very flammable substances. Against this situation, many fire-retardant regulations are being set up in each country. In order to prevent fire and protect the safety of human life and property. As an important component of flame retardant products, the development and application of cellulose fiber flame retardant products are more urgent.

The traditional cotton fabric flame retardant is mainly phosphorus flame retardant and -containing flame retardant. The flame retardant has good flame retardant performance, good washability and flame retardant durability, but has the problems of easy discoloration of fabrics, formaldehyde generation, odor, toxicity and the like; the halogen-containing flame retardant has good flame retardant effect, but is easy to generate secondary pollution in the using process. With the enhancement of environmental protection requirements, boron flame retardants are attracting attention due to their excellent characteristics of flame retardance, low toxicity, smoke suppression and the like, and meet the development trends of non-halogenation, non-toxicity and smoke suppression of the flame retardants.

However, the existing novel flame retardant has poor flame retardant effect, and other flame retardants are required to be compounded or compounded for use, so that the flame retardant requirement can be met.

Disclosure of Invention

The technical problems to be solved by the invention are as follows: aiming at the problem of poor flame retardant effect of the flame retardant, the preparation method of the textile flame retardant is provided.

In order to solve the technical problems, the invention adopts the following technical scheme:

a preparation method of a textile flame retardant comprises the following steps:

(1) taking 100-120 parts of water, 40-50 parts of mixed monomer, 12-16 parts of additive, 3-7 parts of cross-linking agent and 2-5 parts of emulsifier by weight, stirring the water, the mixed monomer, the cross-linking agent and the emulsifier, adding the additive, and mixing to obtain a raw material A;

(2) taking 90-110 parts by weight of acetone, 35-45 parts by weight of glycidyl methacrylate, 2-7 parts by weight of N-hydroxymethyl acrylamide and 2-5 parts by weight of citric acid fatty glyceride, and stirring and mixing to obtain a raw material B;

(3) putting the raw material A into a reactor, stirring at 1100r/min, then dropwise adding a raw material B accounting for 90-95% of the volume of the raw material A, continuously stirring, adding an initiator accounting for 5-8% of the mass of the raw material A, heating, stirring, discharging, filtering, washing, drying, and collecting a dried substance;

(4) taking 120-130 parts of water, 50-60 parts of a dry matter, 20-23 parts of sodium hypophosphite, 12-15 parts of copper sulfate, 11-14 parts of polyglutamic acid, 10-20 parts of geraniol and 6-8 parts of r-aminopropyltriethoxysilane by weight, firstly putting the water, the dry matter, the sodium hypophosphite and the copper sulfate into a reactor, adjusting the pH to 2.0, heating, stirring, cooling, standing, adding the polyglutamic acid, the geraniol and the r-aminopropyltriethoxysilane, stirring, discharging, freeze-drying, crushing, sieving, collecting sieved particles, and obtaining the textile flame retardant.

Preferably, the monomer mixture in the step (1) is prepared by mixing acrylamide and maleic anhydride according to a mass ratio of 9: 1-2.

Preferably, the additive in the step (1) is any one of sodium bicarbonate and sodium carbonate.

Preferably, the crosslinking agent in the step (1) is any one of ethylene glycol dimethacrylate and N, N-methylene bisacrylamide.

Preferably, the emulsifier in the step (1) is any one of Tween 80 and Span 80.

Preferably, the initiator in the step (3) is any one of benzoyl peroxide and benzoyl tert-butyl peroxide.

Compared with other methods, the method has the beneficial technical effects that:

(1) the invention takes acrylamide and maleic anhydride as basic raw materials to be mixed with additives and the like to form a raw material A, then takes glycidyl methacrylate and the like as basic raw materials to form a raw material B, then the raw materials and the glycidyl methacrylate react under the action of initiators and the like to form a polymer with a pore structure, the maleic anhydride modified acrylamide wraps acrylic esters, the direct bonding performance with fabrics is improved through the modification of the maleic anhydride, the adsorption performance to carbon dioxide is improved, the additives are loaded, the flame retardant effect is increased, then nano copper is formed under the action of sodium hypophosphite by utilizing copper sulfate, amino silane is added to improve the water resistance and the bonding performance with the fabrics when the nano copper is deposited on the polymer, and the polyglutamic acid is compounded with the polymer to reduce the degradation performance of the polymer through the amino silane, meanwhile, the polyglutamic acid can be used for wrapping and combining the geraniol well;

(2) when the fabric is used, the polymer is used for rapidly absorbing carbon dioxide in the air, so that high-density carbon dioxide is formed on the surface of the fabric, the flammability of the fabric can be effectively reduced, the geraniol can be catalyzed to form aldehyde at high temperature by using the action of the nano-copper, the aldehyde can be promoted to be combined with the fiber, the flame retardant effect can be effectively improved, and gases such as carbon dioxide and the like are formed due to the decomposition of the aldehyde, so that the flame retardant effect is further improved.

Detailed Description

The mixed monomer is formed by mixing acrylamide and maleic anhydride according to a mass ratio of 9: 1-2.

The additive is any one of sodium bicarbonate and sodium carbonate.

The cross-linking agent is any one of ethylene glycol dimethacrylate and N, N-methylene bisacrylamide.

The emulsifier is Tween 80 or Span 80.

The initiator is any one of benzoyl peroxide and benzoyl peroxide tert-butyl ester.

A preparation method of a textile flame retardant comprises the following steps:

(1) taking 100-120 parts of water, 40-50 parts of mixed monomers, 12-16 parts of additives, 3-7 parts of cross-linking agents and 2-5 parts of emulsifiers by weight parts, stirring the water, the mixed monomers, the cross-linking agents and the emulsifiers at 900r/min for 30min, adding the additives, and mixing for 20min to obtain a raw material A;

(2) taking 90-110 parts by weight of acetone, 35-45 parts by weight of glycidyl methacrylate, 2-7 parts by weight of N-hydroxymethyl acrylamide and 2-5 parts by weight of citric acid fatty glyceride, and stirring and mixing to obtain a raw material B;

(3) putting the raw material A into a reactor, stirring for 10min at the speed of 1100r/min, then dropwise adding a raw material B with the volume of 90-95% of that of the raw material A, continuously stirring for 1h, adding an initiator with the mass of 5-8% of that of the raw material A, heating to 60-70 ℃, stirring for 9h, discharging, filtering, washing filter residues with ethanol, drying, and collecting dried substances;

(4) taking 120-130 parts of water, 50-60 parts of a dry matter, 20-23 parts of sodium hypophosphite, 12-15 parts of copper sulfate, 11-14 parts of polyglutamic acid, 10-20 parts of geraniol and 6-8 parts of r-aminopropyltriethoxysilane by weight, firstly putting the water, the dry matter, the sodium hypophosphite and the copper sulfate into a reactor, adjusting the pH to 2.0, heating to 60-70 ℃, stirring for 8 hours at 800r/min, cooling to room temperature, standing for 5 hours, then adding the polyglutamic acid, the geraniol and the r-aminopropyltriethoxysilane, stirring, discharging, freeze drying, crushing, sieving, collecting and sieving particles to obtain the textile flame retardant.

Example 1

The mixed monomer is prepared by mixing acrylamide and maleic anhydride according to the mass ratio of 9: 2.

The additive is any one of sodium bicarbonate and sodium carbonate.

The cross-linking agent is any one of ethylene glycol dimethacrylate and N, N-methylene bisacrylamide.

The emulsifier is Tween 80 or Span 80.

The initiator is any one of benzoyl peroxide and benzoyl peroxide tert-butyl ester.

A preparation method of a textile flame retardant comprises the following steps:

(1) taking 120 parts of water, 50 parts of mixed monomer, 16 parts of additive, 7 parts of cross-linking agent and 5 parts of emulsifier according to parts by weight, stirring the water, the mixed monomer, the cross-linking agent and the emulsifier at 900r/min for 30min, adding the additive, and mixing for 20min to obtain a raw material A;

(2) taking 110 parts of acetone, 45 parts of glycidyl methacrylate, 7 parts of N-hydroxymethyl acrylamide and 5 parts of citric acid fatty glyceride in parts by weight, and stirring and mixing to obtain a raw material B;

(3) putting the raw material A into a reactor, stirring for 10min at the speed of 1100r/min, then dropwise adding a raw material B with the volume of 95% of that of the raw material A, continuously stirring for 1h, adding an initiator with the mass of 8% of that of the raw material A, heating to 70 ℃, stirring for 9h, discharging, filtering, washing filter residues with ethanol, drying, and collecting a dried substance;

(4) according to the weight parts, 130 parts of water, 60 parts of a dry matter, 23 parts of sodium hypophosphite, 15 parts of copper sulfate, 14 parts of polyglutamic acid, 20 parts of geraniol and 8 parts of r-aminopropyltriethoxysilane are taken, firstly, the water, the dry matter, the sodium hypophosphite and the copper sulfate are put into a reactor, the pH value is adjusted to 2.0, the temperature is increased to 70 ℃, the mixture is stirred for 8 hours at the speed of 800r/min, the mixture is cooled to the room temperature and stands for 5 hours, then, the polyglutamic acid, the geraniol and the r-aminopropyltriethoxysilane are added, the mixture is stirred, the discharged material is frozen and dried, crushed, sieved, and sieved particles are collected, so that the textile flame retardant is.

Example 2

The mixed monomer is prepared by mixing acrylamide and maleic anhydride according to the mass ratio of 9: 1.5.

The additive is any one of sodium bicarbonate and sodium carbonate.

The cross-linking agent is any one of ethylene glycol dimethacrylate and N, N-methylene bisacrylamide.

The emulsifier is Tween 80 or Span 80.

The initiator is any one of benzoyl peroxide and benzoyl peroxide tert-butyl ester.

A preparation method of a textile flame retardant comprises the following steps:

(1) taking 110 parts of water, 45 parts of mixed monomer, 15 parts of additive, 5 parts of cross-linking agent and 4 parts of emulsifier according to parts by weight, stirring the water, the mixed monomer, the cross-linking agent and the emulsifier at 900r/min for 30min, adding the additive, and mixing for 20min to obtain a raw material A;

(2) taking 100 parts of acetone, 40 parts of glycidyl methacrylate, 6 parts of N-hydroxymethyl acrylamide and 4 parts of citric acid fatty glyceride in parts by weight, and stirring and mixing to obtain a raw material B;

(3) putting the raw material A into a reactor, stirring for 10min at the speed of 1100r/min, then dropwise adding a raw material B with the volume of 93% of that of the raw material A, continuously stirring for 1h, adding an initiator with the mass of 7% of that of the raw material A, heating to 65 ℃, stirring for 9h, discharging, filtering, washing filter residues with ethanol, drying, and collecting a dried substance;

(4) according to the weight parts, 125 parts of water, 55 parts of dry matter, 22 parts of sodium hypophosphite, 14 parts of copper sulfate, 13 parts of polyglutamic acid, 10 parts of geraniol and 7 parts of r-aminopropyltriethoxysilane are taken, firstly, the water, the dry matter, the sodium hypophosphite and the copper sulfate are put into a reactor, the pH value is adjusted to 2.0, the temperature is increased to 65 ℃, the mixture is stirred for 8 hours at the speed of 800r/min, the mixture is cooled to the room temperature and is kept stand for 5 hours, then, the polyglutamic acid, the geraniol and the r-aminopropyltriethoxysilane are added, the mixture is stirred, the discharged material is frozen and dried, crushed, sieved, and sieved particles are collected, so that the textile flame retardant.

Example 3

The mixed monomer is prepared by mixing acrylamide and maleic anhydride according to the mass ratio of 9:1.

The additive is any one of sodium bicarbonate and sodium carbonate.

The cross-linking agent is any one of ethylene glycol dimethacrylate and N, N-methylene bisacrylamide.

The emulsifier is Tween 80 or Span 80.

The initiator is any one of benzoyl peroxide and benzoyl peroxide tert-butyl ester.

A preparation method of a textile flame retardant comprises the following steps:

(1) taking 100 parts of water, 40 parts of mixed monomer, 12 parts of additive, 3 parts of cross-linking agent and 2 parts of emulsifier according to parts by weight, stirring the water, the mixed monomer, the cross-linking agent and the emulsifier at 900r/min for 30min, adding the additive, and mixing for 20min to obtain a raw material A;

(2) taking 90 parts by weight of acetone, 35 parts by weight of glycidyl methacrylate, 2 parts by weight of N-hydroxymethyl acrylamide and 2 parts by weight of citric acid fatty glyceride, and stirring and mixing to obtain a raw material B;

(3) putting the raw material A into a reactor, stirring for 10min at the speed of 1100r/min, then dropwise adding a raw material B accounting for 90% of the volume of the raw material A, continuously stirring for 1h, adding an initiator accounting for 5-8% of the mass of the raw material A, heating to 60 ℃, stirring for 9h, discharging, filtering, washing filter residues with ethanol, drying, and collecting a dried substance;

(4) according to the weight parts, 120 parts of water, 50 parts of dry matter, 20 parts of sodium hypophosphite, 12 parts of copper sulfate, 11 parts of polyglutamic acid, 10 parts of geraniol and 6 parts of r-aminopropyltriethoxysilane are taken, firstly, the water, the dry matter, the sodium hypophosphite and the copper sulfate are put into a reactor, the pH value is adjusted to 2.0, the temperature is increased to 60 ℃, the mixture is stirred for 8 hours at the speed of 800r/min, the mixture is cooled to the room temperature and is kept stand for 5 hours, then, the polyglutamic acid, the geraniol and the r-aminopropyltriethoxysilane are added, the mixture is stirred, the discharged material is frozen and dried, crushed, sieved, and sieved particles are collected, so that the textile flame retardant.

Comparative example 1

Essentially the same as example 2, except that copper sulfate was absent.

Comparative example 2

Essentially the same as example 2, except for the absence of geraniol.

The flame retardants for textiles prepared in examples 1-3 and comparative examples 1-2 were prepared into a flame retardant finishing liquid with a mass fraction of 35%, cotton cloth was finished by dipping twice into twice the finishing liquid (the gift rate was about 75%), and the finished pure cotton fabric was tested for vertical flammability by a vertical fabric flammability tester (Darong textile Standard Instrument factory in Wenzhou City) according to the requirements of the vertical textile flammability test. The results are shown in Table 1:

table 1:

test items	Example 1	Example 2	Example 3	Comparative example 1	Comparative example 2
						Duration of continuous combustion/s	0	0	0	8.9	12.3
Smoldering time/s	0	0	0	1.3	3.2
						Length of damage/mm	83	72	76	186	232

In sum, the textile flame retardant disclosed by the invention is better in flame retardant effect and worthy of being widely popularized and used.