阅读说明：本技术 一种三层涂层柔性热防护材料产品及其制备方法 (Three-layer coating flexible thermal protection material product and preparation method thereof ) 是由 赵晓明 刘国熠 谌玉红 刘元军 于 2020-06-05 设计创作，主要内容包括：本发明公开了一种三层涂层柔性热防护材料产品及其制备方法,该类柔性热防护材料包括气凝胶绝热层、耐火隔热层和耐热辐射层,涂层基布为连续玄武岩纤维织物。采用所公开的三层涂层柔性热防护材料的制备方法所制备出的材料兼具耐明火、反射热辐射和高效隔热等功能。该产品的制备工艺分为气凝胶绝热涂层、耐火隔热层和耐热辐射层等三步,所制得三层涂层柔性热防护材料具备轻薄、耐高温和热防护性能优异等功能特点。(The invention discloses a three-layer coating flexible thermal protection material product and a preparation method thereof. The material prepared by the preparation method of the disclosed three-layer coating flexible thermal protection material has the functions of open fire resistance, heat radiation reflection, high-efficiency heat insulation and the like. The preparation process of the product comprises three steps of the aerogel heat insulation coating, the fire-resistant heat insulation layer, the heat radiation resistant layer and the like, and the prepared three-layer coating flexible heat protection material has the functional characteristics of lightness, thinness, high temperature resistance, excellent heat protection performance and the like.)

1. A three-layer coated flexible thermal protective material product comprising: the continuous basalt fiber fabric used as a base material and the organic silicon resin used as a coating matrix are subjected to a three-layer coating process by adding different types of functional fillers into the organic silicon resin, and are cured and molded at a high temperature to obtain the flexible protective material product.

2. A three-layer coated flexible thermal protective material product according to claim 1, wherein the mass ratio of said silicone resin to said coupling agent is 50-250: 1.

3. A three-layer coated flexible thermal protective material product according to claim 2, wherein the coupling agent is at least one of a borate coupling agent, a bimetallic coupling agent, a silane coupling agent, and a titanate coupling agent.

4. A three-layer coated flexible thermal protection material product according to claim 1, having a thickness of only about 1 mm.

Cutting the continuous basalt fiber fabric into a sample of 15cm multiplied by 40cm, wherein the dosage of the corresponding organic silicon resin is 55-80 g.

5. The three-layer coating flexible thermal protection material product according to claim 1, wherein the silicone resin is diluted by adding 5-10 mL of absolute ethyl alcohol.

6. A three-layer coated flexible thermal protection material product according to claim 1, having a thickness of around 1 mm.

7. A three-layer coated flexible thermal protective material product according to claim 1, comprising the steps of:

step 1 aerogel heat insulation coating preparation process

Preferably, the continuous basalt fiber fabric is cut into a sample of 15cm × 40cm, and the corresponding amount of the silicone resin is 55-80 g.

Preferably, the mass ratio of the organic silicon resin to the coupling agent is 50-250: 1.

Preferably, the coupling agent is at least one of a borate coupling agent, a bimetallic coupling agent, a silane coupling agent and a titanate coupling agent.

Preferably, absolute ethyl alcohol with the mass of 5-10 mL is added into the organic silicon resin to dilute the organic silicon resin.

The aerogel heat insulation layer coating agent comprises the following components in percentage by mass:

aerogel: 5-20%;

mica powder: 3-15%;

kaolin: 0.5-28%;

talc powder: 1 to 10 percent

Preferably, the thickness of the coating is 0.1-2 mm.

Preferably, after the back of the fabric is coated by using a sample coating machine, the fabric is placed into an oven to be dried for 30-60 min at the temperature of 50-150 ℃.

Step 2 preparation process of refractory heat-insulating coating

Preferably, the dosage of the organic silicon resin is 25-50 g.

Preferably, the mass ratio of the organic silicon resin to the coupling agent is 80-200: 1.

Preferably, the coupling agent is at least one of a borate coupling agent, a bimetallic coupling agent, a silane coupling agent and a titanate coupling agent.

Preferably, absolute ethyl alcohol with the mass of 9-15mL is added into the organic silicon resin to dilute the organic silicon resin.

The fireproof heat-insulating coating agent comprises the following components in percentage by mass:

hollow ceramic microbeads: 5-30%;

mica powder: 3-15%;

kaolin: 2-12%;

talc powder: 1 to 5 percent

Preferably, the thickness of the coating is 0.1-2 mm.

Preferably, after coating by using a sample coating machine, the sample is placed into an oven to be dried for 30-60 min at the temperature of 50-150 ℃.

Step 3 heat-resistant radiation coating preparation process

Preferably, the dosage of the organic silicon resin is 25-40 g.

Preferably, the mass ratio of the organic silicon resin to the coupling agent is 80-200: 1.

Preferably, the coupling agent is at least one of a borate coupling agent, a bimetallic coupling agent, a silane coupling agent and a titanate coupling agent.

Preferably, absolute ethyl alcohol with the mass of 9-15mL is added into the organic silicon resin to dilute the organic silicon resin.

The heat-resistant radiation coating agent comprises the following components in percentage by mass:

nano-scale potassium hexatitanate whiskers: 5-20%;

mica powder: 3-13%;

kaolin: 2-10%;

talc powder: 2 to 5 percent

Preferably, the thickness of the coating is 0.1-2 mm.

Preferably, after coating by using a sample coating machine, the sample is placed into an oven to be dried for 30-60 min at 50-150 ℃, and then the temperature is raised to 180-250 ℃ to be dried for 60-120 min.

Technical Field

The invention relates to a thermal protection composite material product, in particular to a three-layer coating flexible thermal protection material product with good thermal protection performance and a preparation method thereof, wherein the three-layer coating flexible thermal protection material product takes a continuous basalt fiber fabric as a base material and organic silicon resin as a matrix.

Background

A continuous basalt fiber fabric. The basalt fiber is prepared by melting and drawing at the temperature of over 1400 ℃, so that the basalt fiber has the performance of low temperature resistance and high temperature resistance, and the long-term use temperature range is-260-700 ℃. Besides excellent heat resistance, the basalt fiber has outstanding mechanical properties, the elastic modulus is in the range of 80-93 GPa, the tensile strength is more than 3000MPa, and the elongation at break is about 3%. Its excellent thermal stability and mechanical properties are due to its developed Q4 silicon molecular network, which requires more energy to break its Si-O bonds. However, the basalt fiber has a dark color, so that the radiation heat reflection performance is poor, and the treatment such as coating modification is required to enhance the protection performance.

Composite materials are multiphase materials prepared from two or more materials with different properties, such as metals, ceramics, high molecular materials and the like, by physical or chemical preparation processes. The various materials composing the composite material are complementary in performance and characteristics, make up for deficiencies and generate synergistic effect, so that the comprehensive performance of the composite material is superior to that of the original composite material, and various different requirements in daily life and industrial production are met. The composite material has the characteristics of light weight, high strength, convenient processing and forming, excellent elasticity, chemical corrosion resistance, good weather resistance and the like, gradually replaces wood and metal alloy, is widely applied to the fields of aerospace, automobiles, electronics and electrical, buildings, body building equipment and the like, and is developed rapidly in recent years.

Coated fabrics (Coated fabrics) belong to the class of composite materials, which are textiles with a coating binder material forming a single or multiple layer coating in situ on one or both the front and back sides of the fabric. Consisting of two or more layers of material, at least one of which is a textile and the other layer or layers being a fully continuous polymer coating. The product has the advantages of both. In addition, from a microscopic perspective, the coating on the fabric can be viewed as a space in which substances having specific functions but not reacting with the fibers to be fixed can be accommodated, so that the application range of the textile can be expanded, the traditional field is not limited, and the combination of one or more functions can be realized through the method.

In a high-temperature fire field, heat flow generated by an open fire source is mostly transmitted to the periphery in the form of electromagnetic waves, and the peak value of heat flow generated by flame is concentrated at 167-226 kW.m^-2Within the range, the wave crest is about 2 μm, and the wavelength range is 1-6 μm. This indicates that the radiant heat generated in the open flame environment is mostly electromagnetic waves in the near infrared region. In a common fire, the radiation wavelength range of a fire source is 2-20 mu m, and in a high-temperature open fire scene, visible light (0.4-0.8 mu m) also generates a heat effect, so that in the high-temperature fire sceneIn the method, the wavelength range of the radiant rays which can be absorbed and generate the thermal effect is 0.4-20 mu m, namely the radiant rays, and the thermal radiation effect generated by the radiant rays accounts for 80% of the total heat flow of the high-temperature fire field, so that the enhancement of the radiant heat reflection performance of the coating fabric composite material is a main way for improving the thermal protection effect of the coating fabric in the fire field.

Disclosure of Invention

The invention solves the technical problem of providing a three-layer coating flexible thermal protection material product which takes continuous basalt fiber fabric as a base material and organic silicon resin as a matrix and has good thermal protection performance in a high-temperature fire scene and can be used as an outer layer material of fire-fighting fire-protection clothes. Meanwhile, the technology adopts a three-layer coating mode to enable the fabric material to have ablation resistance, radiant heat reflection and heat insulation functions at the same time, and adopts the continuous basalt fiber fabric with lower price to replace the high silica glass fiber fabric with higher price, so that the problem of low utilization rate caused by high price of the traditional thermal protection fabric for the high-temperature fire field is solved. The invention provides a technical scheme for solving the problems, and the technical scheme is to provide a three-layer coating flexible thermal protection material product, which comprises the following components: the continuous basalt fiber fabric used as a base material and the organic silicon resin used as a coating matrix are subjected to a three-layer coating process by adding different types of functional fillers into the organic silicon resin, and are cured and molded at a high temperature to obtain the flexible protective material product.

1. The technological parameters of the three-layer coating flexible thermal protection material product are characterized by comprising the following steps:

step 1 aerogel heat insulation coating preparation process

Preferably, the continuous basalt fiber fabric is cut into a sample of 15cm × 40cm, and the amount of the corresponding silicone resin is 20-45 g.

Preferably, the mass ratio of the organic silicon resin to the coupling agent is 50-250: 1.

Preferably, the coupling agent is at least one of a borate coupling agent, a bimetallic coupling agent, a silane coupling agent and a titanate coupling agent.

Preferably, absolute ethyl alcohol with the mass of 5-10 mL is added into the organic silicon resin to dilute the organic silicon resin.

The aerogel heat insulation layer coating agent comprises the following components in percentage by mass:

aerogel: 5-20%;

mica powder: 3-15%;

kaolin: 0.5-28%;

talc powder: 1 to 10 percent

Preferably, the thickness of the coating is 0.1-2 mm.

Preferably, after the back of the fabric is coated by using a sample coating machine, the fabric is placed into an oven to be dried for 30-60 min at the temperature of 50-150 ℃.

Step 2 preparation process of refractory heat-insulating layer

Preferably, the dosage of the organic silicon resin is 25-50 g.

Preferably, the mass ratio of the organic silicon resin to the coupling agent is 80-200: 1.

Preferably, the coupling agent is at least one of a borate coupling agent, a bimetallic coupling agent, a silane coupling agent and a titanate coupling agent.

Preferably, absolute ethyl alcohol with the mass of 9-15mL is added into the organic silicon resin to dilute the organic silicon resin.

The refractory heat-insulating layer coating agent comprises the following components in percentage by mass:

hollow ceramic microbeads: 5-30%;

mica powder: 3-15%;

kaolin: 2-12%;

talc powder: 1 to 5 percent

Preferably, the thickness of the coating is 0.1-2 mm.

Preferably, after the front surface of the fabric is coated by using a sample coating machine, the fabric is placed into an oven to be dried for 30-60 min at the temperature of 50-150 ℃.

Step 3 preparation process of heat-resistant radiation layer

Preferably, the dosage of the organic silicon resin is 25-40 g.

Preferably, the mass ratio of the organic silicon resin to the coupling agent is 80-200: 1.

Preferably, the coupling agent is at least one of a borate coupling agent, a bimetallic coupling agent, a silane coupling agent and a titanate coupling agent.

Preferably, absolute ethyl alcohol with the mass of 9-15mL is added into the organic silicon resin to dilute the organic silicon resin.

The coating agent of the heat-resistant radiation layer comprises the following components in percentage by mass:

nano-scale potassium hexatitanate whiskers: 5-20%;

mica powder: 3-13%;

kaolin: 2-10%;

talc powder: 2 to 5 percent

Preferably, the thickness of the coating is 0.1-2 mm.

Preferably, after the front surface of the fabric is coated by using a sample coating machine, the fabric is placed into an oven to be dried for 30-60 min at the temperature of 50-150 ℃, and then the temperature is raised to 180-250 ℃ to be dried for 60-120 min.

The invention also provides a preparation method of the coating agent of the three-layer coating flexible thermal protection material product, which comprises the following steps:

(1) preparation of the coating agent:

and adding the nano-filler into the alcohol according to the proportion, uniformly stirring, and then carrying out ultrasonic treatment for 10-20 min to remove the agglomeration phenomenon among the nano-fillers. Setting the rotating speed of a dispersion machine to be 100-500 r/min, slowly adding the nano filler into the resin, then adding other fillers, after the addition is finished, adjusting the rotating speed of the dispersion machine to be 1500-3000 r/min, stirring at a constant speed for 20-30 min, then adding the coupling agent, and stirring for 2-5 min.

(2) Implementation of the coating process:

and fixing the cut fabric on a needle board frame, adjusting the distance between a scraper and the fabric to a specified value, and reducing the scraping speed of the sample coating machine to be below 1-10 mm/s to implement uniform scraping.

(3) And (3) implementation of a drying film forming process:

after the coating processes of the heat insulation coating and the ablation-resistant heat insulation coating are implemented, pre-baking is required to be implemented. After the application process of the ablation-resistant reflective coating is finished, the pre-baking is required to be carried out firstly, and then the high-temperature curing process is carried out.

The technical scheme of the invention is summarized as follows:

taking organic silicon resin as a matrix of the flexible protective material product; because the organic silicon resin has certain viscosity, the absolute ethyl alcohol is added into the resin for dilution, thereby facilitating the implementation of the subsequent filler dispersion and coating process; the continuous basalt fiber woven fabric is used as a reinforcement, and the heat resistance of the continuous basalt fiber woven fabric has obvious influence on the high-temperature thermal stability of the flexible protective material product; the preparation method comprises the steps of sequentially carrying out aerogel heat insulation coating, fire-resistant heat insulation coating and heat radiation resistant coating on basalt fiber fabric, adding inorganic functional filler into functional layers with different structures according to a certain proportion, drying for a specified time at a curing temperature, and then forming, so that the compounding of multiple heat protection effects of ablation resistance, heat reflection, heat insulation and the like of the material is realized, and the three-layer coating flexible heat protection material product is prepared.

Has the advantages that:

the continuous basalt fiber fabric is used as a matrix of a three-layer flexible thermal protection material product, and has excellent high-temperature thermal stability and good mechanical properties. By utilizing the characteristics of the continuous basalt fiber fabric and adopting a simple and feasible three-layer coating method, the filler with corresponding functions is mixed into the organic silicon resin, the three-layer functional coating is carried out on the continuous basalt fiber fabric, and the continuous basalt fiber fabric is formed after the resin is cured at the film forming temperature. The product of the invention has the thickness of only about 1mm, is very light and thin, but has excellent thermal protection performance, simple preparation method, easy operation and lower cost.

Drawings

FIG. 1 is a flow chart of the preparation of the composite material of the present invention;

FIG. 2 is a schematic view of a model structure of the composite material of the present invention;

FIG. 3 is a graph showing the effect of hollow ceramic bead content on the radiation heat protection performance of a composite material;

FIG. 4 shows the effect of the content of the nano potassium hexatitanate whiskers on the flame ablation resistance of the composite material at 600 ℃.

Detailed Description

The invention is further described by the following specific embodiments in conjunction with the accompanying drawings. Unless otherwise specified, technical means not described in the embodiments may be implemented in a manner well known to those skilled in the art. In addition, the embodiments should be considered illustrative, and not restrictive, of the scope of the invention, which is defined solely by the claims. It will be apparent to those skilled in the art that various modifications, substitutions, and improvements in the materials, amounts, dimensions, and shapes of the embodiments disclosed herein may be made without departing from the spirit and scope of the invention, and the invention is to be limited only by the specific parameters set forth herein as the scope of the invention is to be determined with the permissible error.