阅读说明：本技术 用于特殊防护服的防火复合材料制备方法 (Preparation method of fireproof composite material for special protective clothing ) 是由 马超强 马俊 赵梦洋 于 2020-04-09 设计创作，主要内容包括：本发明公开了一种用于特殊防护服的防火复合材料制备方法,涉及服装材料技术领域,本发明通过阻燃面料的制备、改性环氧树脂的制备、胶液的配制和复合材料的制备制得了具有良好阻燃性能的复合材料,其中利用1-羟基苯并三唑在环氧树脂上的接枝来优化环氧树脂的阻燃性能,而1-羟基苯并三唑并不属于本领域已知的能够作为环氧树脂阻燃改性剂的物质,所制复合材料适用于加工制成具有防火功能的防护服。(The invention discloses a preparation method of a fireproof composite material for special protective clothing, which relates to the technical field of clothing materials, and the composite material with good flame retardant property is prepared through the preparation of flame retardant fabric, the preparation of modified epoxy resin, the preparation of glue solution and the preparation of the composite material, wherein the flame retardant property of the epoxy resin is optimized by utilizing the grafting of 1-hydroxybenzotriazole on the epoxy resin, and the 1-hydroxybenzotriazole does not belong to the substances which are known in the field and can be used as the flame retardant modifier of the epoxy resin, so that the prepared composite material is suitable for being processed into the protective clothing with the fireproof function.)

1. The preparation method of the fireproof composite material for the special protective clothing is characterized by comprising the following preparation steps:

(1) preparing a flame-retardant fabric: the meta-aramid fiber, the sepiolite fiber and the alumina fiber are blended, twisted and woven to prepare the flame-retardant fabric;

(2) preparation of modified epoxy resin: heating the epoxy resin to a molten state at a heating rate of 5-10 ℃/min, then preserving heat and mixing, adding 1-hydroxybenzotriazole and an alkaline catalyst, continuing preserving heat and mixing in the molten state, naturally cooling, washing with water, and drying to obtain a modified epoxy resin;

(3) preparing glue solution: adding the modified epoxy resin and the dicyandiamide curing agent into a solvent, and uniformly mixing to obtain a glue solution;

(4) preparing a composite material: and (3) soaking the prepared composite fiber fabric in the prepared glue solution, taking out, drying and curing to obtain the composite material.

2. A method of making a fire resistant composite material for use in special protective apparel in accordance with claim 1, wherein: the mass ratio of the intermediate aramid fiber, the sepiolite fiber and the alumina fiber in the step (1) is (5-20): (0.5-5): 0.5-5).

3. A method of making a fire resistant composite material for use in special protective apparel in accordance with claim 1, wherein: in the step (2), the mass ratio of the epoxy resin to the 1-hydroxybenzotriazole is (50-150) to (1-20), and the dosage of the alkaline catalyst is 3-10% of that of the 1-hydroxybenzotriazole.

4. A method of making a fire resistant composite material for use in special protective apparel in accordance with claim 1, wherein: and (3) in the step (2), the alkaline catalyst is one of quaternary ammonium salt, sodium hydroxide and potassium hydroxide.

5. A method of making a fire resistant composite material for use in special protective apparel in accordance with claim 1, wherein: the mass ratio of the modified epoxy resin to the dicyandiamide curing agent in the step (3) is (80-90) to (10-20).

6. A method of making a fire resistant composite material for use in special protective apparel in accordance with claim 1, wherein: the solid content of the glue solution in the step (3) is 40-60%.

7. A method of making a fire resistant composite material for use in special protective apparel in accordance with claim 1, wherein: and (3) the solvent in the step (3) is ethanol or ethanol water solution.

8. A method of making a fire resistant composite material for use in special protective apparel in accordance with claim 1, wherein: in the step (4), the dipping temperature is 30-50 ℃, and the dipping time is 10-30 min.

9. A method of making a fire resistant composite material for use in special protective apparel in accordance with claim 1, wherein: the curing temperature in the step (4) is 180-200 ℃, and the curing time is 1-5 h.

The technical field is as follows:

the invention relates to the technical field of clothing materials, in particular to a preparation method of a fireproof composite material for special protective clothing.

Background art:

the protective clothing types include fire-fighting protective clothing, industrial protective clothing, medical protective clothing, military protective clothing and protective clothing used by special people. The protective clothing is mainly applied to the industries and departments of fire fighting, military industry, ships, petroleum, chemical industry, paint spraying, cleaning and disinfection, laboratories and the like.

At present, a plurality of protective clothes require processed fabrics to have good fireproof performance to deal with the occurrence of fire, so the processed fabrics of the protective clothes can be made of flame-retardant fabrics. The existing flame-retardant fabric is endowed with certain flame-retardant performance by adopting an after-finishing agent, a large amount of flame retardant needs to be added in a large amount to show good flame-retardant effect, and excessive addition of the flame retardant influences the flexibility and comfortableness of the fabric.

The invention content is as follows:

the technical problem to be solved by the invention is to provide a preparation method of a fireproof composite material for special protective clothing, the flame retardant property of the prepared composite material is optimized through the preparation of flame retardant fabric and the preparation of modified epoxy resin, and meanwhile, the adopted operation condition is clear and has good repeatability, and the preparation method is suitable for large-scale production.

The technical problem to be solved by the invention is realized by adopting the following technical scheme:

the preparation method of the fireproof composite material for the special protective clothing comprises the following preparation steps:

(1) preparing a flame-retardant fabric: the meta-aramid fiber, the sepiolite fiber and the alumina fiber are blended, twisted and woven to prepare the flame-retardant fabric;

(2) preparation of modified epoxy resin: heating the epoxy resin to a molten state at a heating rate of 5-10 ℃/min, then preserving heat and mixing, adding 1-hydroxybenzotriazole and an alkaline catalyst, continuing preserving heat and mixing in the molten state, naturally cooling, washing with water, and drying to obtain a modified epoxy resin;

(3) preparing glue solution: adding the modified epoxy resin and the dicyandiamide curing agent into a solvent, and uniformly mixing to obtain a glue solution;

(4) preparing a composite material: and (3) soaking the prepared composite fiber fabric in the prepared glue solution, taking out, drying and curing to obtain the composite material.

The mass ratio of the intermediate aramid fiber, the sepiolite fiber and the alumina fiber in the step (1) is (5-20): (0.5-5): 0.5-5).

In the step (2), the mass ratio of the epoxy resin to the 1-hydroxybenzotriazole is (50-150) to (1-20), and the dosage of the alkaline catalyst is 3-10% of that of the 1-hydroxybenzotriazole.

And (3) in the step (2), the alkaline catalyst is one of quaternary ammonium salt, sodium hydroxide and potassium hydroxide.

The mass ratio of the modified epoxy resin to the dicyandiamide curing agent in the step (3) is (80-90) to (10-20).

The solid content of the glue solution in the step (3) is 40-60%.

And (3) the solvent in the step (3) is ethanol or ethanol water solution.

In the step (4), the dipping temperature is 30-50 ℃, and the dipping time is 10-30 min.

The curing temperature in the step (4) is 180-200 ℃, and the curing time is 1-5 h.

Under the high temperature condition and the action of an alkaline catalyst, hydroxyl contained in the 1-hydroxybenzotriazole structure and part of epoxy groups contained in the epoxy resin structure generate ether groups through ring-opening reaction.

The technical problem to be solved by the invention can also be realized by adopting the following technical scheme:

the preparation method of the fireproof composite material for the special protective clothing comprises the following preparation steps:

(1) preparing a flame-retardant fabric: the meta-aramid fiber, the sepiolite fiber and the alumina fiber are blended, twisted and woven to prepare the flame-retardant fabric;

(2) preparation of modified epoxy resin: heating the epoxy resin to a molten state at a heating rate of 5-10 ℃/min, then preserving heat and mixing, adding 1-hydroxybenzotriazole and an alkaline catalyst, continuing preserving heat and mixing in the molten state, naturally cooling, washing with water, and drying to obtain a modified epoxy resin;

(3) preparing glue solution: adding the modified epoxy resin and the dicyandiamide curing agent into a solvent, and uniformly mixing to obtain a glue solution;

(4) preparing a composite material: and (3) soaking the prepared composite fiber fabric in the prepared glue solution, taking out the glue solution, drying the glue solution, and performing ultrasonic curing to obtain the composite material.

The ultrasonic frequency of the ultrasonic curing is 40kHz and 500W.

The operating conditions and control parameters for the remaining preparation steps are as described above.

The invention adopts ultrasonic waves during resin curing, and shortens the curing time by the assistance of the ultrasonic waves, thereby shortening the production period of the composite fabric.

The invention has the beneficial effects that: the composite material with good flame retardant property is prepared by preparing the flame retardant fabric, preparing the modified epoxy resin, preparing the glue solution and preparing the composite material, wherein the flame retardant property of the epoxy resin is optimized by grafting the 1-hydroxybenzotriazole on the epoxy resin, the 1-hydroxybenzotriazole does not belong to substances which are known in the field and can be used as flame retardant modifiers of the epoxy resin, and the prepared composite material is suitable for being processed into protective clothing with a fireproof function.

The specific implementation mode is as follows:

in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.

The epoxy resins of the following examples and comparative examples were purchased from E-44, Jinan resins Ltd, epoxy equivalent 210-250g/eq, softening point 12-20 ℃; meta-aramid fiber was purchased from dupont aramid kevlar K29400D (440 Dtex); sepiolite fibers were purchased from sepiolite limited of Xingxi county; alumina fibers were purchased from javanic crystal fibers ltd.