阅读说明：本技术 一种高硅氧-酚醛树脂复合防热板的制备方法 (Preparation method of high-silica-phenolic resin composite heat-proof plate ) 是由 肖艳 肖志超 李振东 秦文杰 许保顺 于 2021-09-18 设计创作，主要内容包括：本发明公开了一种高硅氧-酚醛树脂复合防热板的制备方法,具体为：将高硅氧玻璃纤维和酚醛树脂混合均匀,烘干制成预混料,放入烘料筛中进行预热；采用工业丙酮清洗模具,使用脱模剂均匀的涂抹模具的凹凸模内型面,对模具进行预热；将预混料均匀平铺在模具的模腔内,进行合模,开启模压机,进行升温模压,出模后打磨飞边毛刺,得到高硅氧-酚醛树脂复合防热板。通过使用高硅氧玻璃纤维-酚醛树脂预混料,辅之以合适的成型方式,制备出隔热性能、高温性能和耐候性优良的防热板；同时,该成型工艺简单、快捷且生产成本低,更利于批量产。(The invention discloses a preparation method of a high silica-phenolic resin composite heat-proof plate, which comprises the following steps: uniformly mixing high silica glass fiber and phenolic resin, drying to prepare a premix, and putting the premix into a drying sieve for preheating; cleaning the mold by using industrial acetone, uniformly coating a mold release agent on the inner molded surface of the concave-convex mold of the mold, and preheating the mold; and uniformly paving the premix in a die cavity of a die, closing the die, starting a molding press, heating for molding, removing the die, and polishing burrs and fins to obtain the high-silica-phenolic resin composite heat-proof plate. The heat-proof plate with excellent heat-insulating property, high-temperature property and weather resistance is prepared by using the high-silica glass fiber-phenolic resin premix and assisting a proper forming mode; meanwhile, the forming process is simple and rapid, the production cost is low, and the batch production is facilitated.)

1. The preparation method of the high silica-phenolic resin composite heat-proof plate is characterized by comprising the following steps:

step 1, uniformly mixing high silica glass fiber and phenolic resin, and drying to prepare a premix; then putting the premix into a material drying sieve for preheating;

step 2, cleaning the mold by using industrial acetone, uniformly coating a mold release agent on the inner molded surface of the concave-convex mold of the mold, fixedly connecting the mold on a molding press, and preheating the mold;

and 3, after the step 2, uniformly spreading the premix in a die cavity of a die, closing the die, starting a molding press, heating for molding, removing the die, and polishing burrs and fins to obtain the high silica-phenolic resin composite heat-proof plate.

2. The preparation method of the high silica-phenolic resin composite heat-proof plate according to claim 1, wherein in the step 1, the mass fraction of the high silica glass fiber is 56% -64%; the mass fraction of the phenolic resin is 36-44%.

3. The preparation method of the high silica-phenolic resin composite heat-proof plate according to claim 1, wherein in the step 1, the drying temperature is 70-80 ℃, and the drying time is 80-100 min; preheating temperature is 80-90 deg.C, and preheating time is 10-15 min.

4. The method for preparing the high silica-phenolic resin composite heat-proof plate according to claim 1, wherein in the step 2, the preheating temperature is 70-80 ℃, and the preheating time is 15-30 min.

5. The method for preparing the high silica-phenolic resin composite heat-proof plate according to claim 1, wherein in the step 3, the specific process of temperature-rising die pressing comprises the following steps: heating to 90 deg.C at a rate of 1.5 deg.C/min under 2-5Mpa, maintaining for 30-50min, providing pressure of 9-20Mpa when the mold temperature is 80-110 deg.C, heating to 110 deg.C at a rate of 0.33 deg.C/min, maintaining for 1.5-5h without pressure compensation, heating to 175 deg.C at a rate of 0.24-0.27 deg.C/min, maintaining for 2-6h, and cooling to below 45 deg.C with a molding press.

6. The method for preparing a high silica-phenolic resin composite heat-proof plate according to claim 1, wherein in the step 3, the specific process of temperature-rising die pressing can be as follows: heating to 90 deg.C under 2-5Mpa for 10min, maintaining for 30-50min, applying pressure of 9-20Mpa when the mold temperature is 80-110 deg.C, heating to 110 deg.C for 1h, maintaining for 1.5-5h without pressure compensation, heating to 175 deg.C for 4-4.5h, maintaining for 2-6h, and cooling to below 45 deg.C with a molding press.

Technical Field

The invention belongs to the technical field of composite material preparation, and particularly relates to a preparation method of a high-silica-phenolic resin composite heat-proof plate.

Background

The increasingly prominent advantages of heat insulating materials enable the heat insulating materials to be widely developed in various industries, such as air conditioner heat preservation, boiler heat preservation, dust collectors, petrochemical engineering, ships, automobiles, military aerospace devices and the like. Thermal insulation materials, which can block the transfer of heat flow, are generally classified into three types, porous materials, heat reflective materials and vacuum materials. A fibrous material having pores which are thermally insulating and in which the thermal conductivity of air or an inert gas contained in the pores is low; metals such as gold, silver, nickel and the like reflect heat out due to high reflection coefficients; the vacuum insulation material insulates heat by blocking convection of heat flow. In the industries of aviation, aerospace, war industry and the like, the heat insulation material has strict requirements on the weight and the volume of the heat insulation material, and also has other special requirements on the aspects of sound insulation, shock absorption, corrosion resistance, weather resistance and the like.

High silica glass fiber, SiO₂The content is more than or equal to 95 percent, the excellent performance and the low cost make the alloy widely favored, the softening point of 1700 ℃ is higher, the alloy can work for a long time at 900 ℃ and can resist instantaneous high temperature. The adhesive has good insulating property even in high-temperature and high-humidity environment, and has good adhesive property with high-temperature adhesive. These all make it have extensive application in the aspects of aerospace apparatus heat-proof and ablation-resistant, high-temperature heat insulation, metal melting filtration and purification, etc.

The phenolic resin has the advantages of high temperature resistance, impact resistance, low smoke generation, low cost, simple forming process, high strength and modulus, and excellent performance, so that the phenolic resin is comparable to plastics, and is mainly applied to transportation industry, building industry, mining industry, military industry and the like. The composite material produced by combining the high-silica glass fiber and the high-silica glass fiber has the advantages of the high-silica glass fiber and the high-silica glass fiber, has other new advantages, and has low density, low heat conduction, good heat absorption capacity and high temperature performance. Based on the excellent performance of the high-silica-phenolic resin composite material, in order to widen the application of the high-silica-phenolic resin composite material, the high-silica-phenolic resin composite material is used as a base material of a heat-proof plate, and the preparation and forming processes of the heat-proof plate composite materials with different shapes and different thicknesses are explored.

Disclosure of Invention

The invention aims to provide a preparation method of a high-silica-phenolic resin composite heat-proof plate, which solves the problems of poor heat-insulating property and poor high-temperature property of the heat-proof plate in the prior art.

The technical scheme adopted by the invention is that the preparation method of the high silica-phenolic resin composite heat-proof plate is implemented according to the following steps:

step 1, uniformly mixing high silica glass fiber and phenolic resin, and drying to prepare a premix; then putting the premix into a material drying sieve for preheating;

step 2, cleaning the mold by using industrial acetone, uniformly coating a mold release agent on the inner molded surface of the concave-convex mold of the mold, fixedly connecting the mold on a molding press, and preheating the mold;

and 3, after the step 2, uniformly spreading the premix in a die cavity of a die, closing the die, starting a molding press, heating for molding, removing the die, and polishing burrs and fins to obtain the high silica-phenolic resin composite heat-proof plate.

The present invention is also characterized in that,

in the step 1, the mass fraction of the high silica glass fiber is 56-64%; the mass fraction of the phenolic resin is 36-44%.

In the step 1, the drying temperature is 70-80 ℃, and the drying time is 80-100 min; preheating temperature is 80-90 deg.C, and preheating time is 10-15 min.

In the step 2, the preheating temperature is 70-80 ℃, and the preheating time is 15-30 min.

In the step 3, the specific process of temperature rise die pressing is as follows: heating to 90 deg.C at a rate of 1.5 deg.C/min under 2-5Mpa, maintaining for 30-50min, providing pressure of 9-20Mpa when the mold temperature is 80-110 deg.C, heating to 110 deg.C at a rate of 0.33 deg.C/min, maintaining for 1.5-5h without pressure compensation, heating to 175 deg.C at a rate of 0.24-0.27 deg.C/min, maintaining for 2-6h, and cooling to below 45 deg.C with a molding press.

In step 3, the specific process of temperature-raising and mould-pressing can also be as follows: heating to 90 deg.C under 2-5Mpa for 10min, maintaining for 30-50min, applying pressure of 9-20Mpa when the mold temperature is 80-110 deg.C, heating to 110 deg.C for 1h, maintaining for 1.5-5h without pressure compensation, heating to 175 deg.C for 4-4.5h, maintaining for 2-6h, and cooling to below 45 deg.C with a molding press.

The invention has the beneficial effects that the heat-proof plate with excellent heat-insulating property, high-temperature property and weather resistance is prepared by using the high-silica glass fiber-phenolic resin premix and assisting with a proper forming mode; meanwhile, the forming process is simple and rapid, the production cost is low, and the batch production is facilitated.

Drawings

FIG. 1 is a topographical view of a high silicone-phenolic resin composite heat shield panel prepared in example 5 of the present invention;

figure 2 is a topographical view of a high silicone-phenolic resin composite heat shield panel made prior to the present invention.

Detailed Description

The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.

The invention relates to a preparation method of a high-silica-phenolic resin composite heat-proof plate, which is implemented according to the following steps:

step 1, uniformly mixing high silica glass fiber and phenolic resin, and drying to prepare a premix; then putting the premix into a material drying sieve for preheating;

the mass fraction of the high silica glass fiber is 56-64%; the mass fraction of the phenolic resin is 36-44%;

the drying temperature is 70-80 ℃, and the drying time is 80-100 min;

preheating at 80-90 deg.C for 10-15 min;

step 2, cleaning the mold by using industrial acetone, uniformly coating a mold surface of the mold in a concave-convex mold by using a release agent, fixedly connecting the mold on a molding press, starting the molding press, and preheating the mold;

preheating at 70-80 deg.C for 15-30 min.

The release agent is X-19W, and the mass of the release agent used each time is 10 g; the model of the molding press is 315T;

step 3, after the step 2, uniformly spreading the premix in a mold cavity of a mold, closing the mold, inserting a thermometer to record the temperature, starting a mold press, heating and molding, and polishing burrs and fins after demolding to obtain the high silica-phenolic resin composite heat-proof plate;

the specific process of temperature-rising die pressing comprises the following steps: heating to 90 deg.C at a rate of 1.5 deg.C/min under 2-5Mpa, maintaining for 30-50min, providing pressure of 9-20Mpa when the mold temperature is 80-110 deg.C, heating to 110 deg.C at a rate of 0.33 deg.C/min, maintaining for 1.5-5h without pressure compensation, heating to 175 deg.C at a rate of 0.24-0.27 deg.C/min, maintaining for 2-6h, and cooling to below 45 deg.C with a molding press;

the specific process of the temperature-rising die pressing can also be as follows: heating to 90 deg.C under 2-5Mpa for 10min, maintaining for 30-50min, applying pressure of 9-20Mpa when the mold temperature is 80-110 deg.C, heating to 110 deg.C for 1h, maintaining for 1.5-5h without pressure compensation, heating to 175 deg.C for 4-4.5h, maintaining for 2-6h, and cooling to below 45 deg.C with a molding press.

Example 1

The invention relates to a preparation method of a high-silica-phenolic resin composite heat-proof plate, which is implemented according to the following steps:

step 1, uniformly mixing high silica glass fiber and phenolic resin, and drying to prepare a premix; then putting the premix into a material drying sieve for preheating;

the mass fractions of the high silica glass fiber and the phenolic resin are respectively 64 percent and 36 percent;

the drying temperature is 80 ℃, and the drying time is 90 min;

preheating at 85 deg.C for 15 min;

step 2, cleaning the mold by using industrial acetone, uniformly coating a mold surface of the mold in a concave-convex mold by using a release agent, fixedly connecting the mold on a molding press, starting the molding press, and preheating the mold;

preheating temperature is 75 ℃, and preheating time is 15 min.

The release agent is X-19W, and the mass of the release agent used each time is 10 g; the model of the molding press is 315T;

step 3, after the step 2, uniformly spreading 2.22Kg of premix in a die cavity of a die, closing the die, inserting a thermometer to record the temperature, starting a die press, heating and die pressing, and polishing burrs after die stripping to obtain a high silica-phenolic resin composite heat-proof plate with the thickness of 656mm multiplied by 340mm multiplied by 6 mm;

the specific process of temperature-rising die pressing comprises the following steps: heating to 90 deg.C under 2Mpa for 10min, maintaining for 30min, applying 10Mpa when the mold temperature is 80-110 deg.C, heating to 110 deg.C for 1h, maintaining for 1.5h, heating to 175 deg.C for 4h, maintaining for 2h, and cooling to below 45 deg.C with a molding press.

Example 2

The invention relates to a preparation method of a high-silica-phenolic resin composite heat-proof plate, which is implemented according to the following steps:

step 1, uniformly mixing high silica glass fiber and phenolic resin, and drying to prepare a premix; then putting the premix into a material drying sieve for preheating;

the mass fractions of the high silica glass fiber and the phenolic resin are respectively 56 percent and 44 percent;

the drying temperature is 70 ℃, and the drying time is 80 min;

preheating at 80 deg.C for 10 min;

step 2, cleaning the mold by using industrial acetone, uniformly coating a mold surface of the mold in a concave-convex mold by using a release agent, fixedly connecting the mold on a molding press, starting the molding press, and preheating the mold;

preheating temperature is 70 deg.C, and preheating for 20 min.

Step 3, after the step 2, uniformly paving 3.35Kg of premix in a die cavity of a die, closing the die, inserting a thermometer to record the temperature, starting a die press, heating and die pressing, and polishing burrs and fins after die stripping to obtain a high silica-phenolic resin composite heat-proof plate with the thickness of 656mm multiplied by 340mm multiplied by 9 mm;

the specific process of temperature-rising die pressing comprises the following steps: heating to 90 deg.C at a rate of 1.5 deg.C/min under 2Mpa, maintaining for 50min, applying pressure of 9Mpa when the mold temperature is 80-110 deg.C, heating to 110 deg.C at a rate of 0.33 deg.C/min, maintaining for 2h without pressure compensation, heating to 175 deg.C at a rate of 0.27 deg.C/min, maintaining for 3h, and cooling to below 45 deg.C with a molding press.

Example 3

The invention relates to a preparation method of a high-silica-phenolic resin composite heat-proof plate, which is implemented according to the following steps:

step 1, uniformly mixing high silica glass fiber and phenolic resin, and drying to prepare a premix; then putting the premix into a material drying sieve for preheating;

the mass fractions of the high silica glass fiber and the phenolic resin are respectively 62 percent and 38 percent;

the drying temperature is 80 ℃, and the drying time is 100 min;

preheating at 85 deg.C for 15 min;

step 2, cleaning the mold by using industrial acetone, uniformly coating a mold surface of the mold in a concave-convex mold by using a release agent, fixedly connecting the mold on a molding press, starting the molding press, and preheating the mold;

preheating temperature is 75 ℃, and preheating time is 15 min.

Step 3, after the step 2, uniformly spreading 21Kg of premix in a die cavity of a die, closing the die, inserting a thermometer to record the temperature, starting a molding press, heating and molding, and polishing burrs and fins after demolding to obtain the high silica-phenolic resin composite heat-proof plate with the thickness of 258mm multiplied by 177 mm;

the specific process of temperature-rising die pressing comprises the following steps: heating to 90 deg.C under 2Mpa for 10min, maintaining for 50min, applying 12Mpa when the mold temperature is 80-110 deg.C, heating to 110 deg.C for 1h, maintaining for 3.5h, heating to 175 deg.C for 4.5h, maintaining for 4h, and cooling to 45 deg.C;

example 4

The invention relates to a preparation method of a high-silica-phenolic resin composite heat-proof plate, which is implemented according to the following steps:

step 1, uniformly mixing high silica glass fiber and phenolic resin, and drying to prepare a premix; then putting the premix into a material drying sieve for preheating;

the mass fractions of the high silica glass fiber and the phenolic resin are respectively 60 percent and 40 percent;

the drying temperature is 80 ℃, and the drying time is 80 min;

preheating temperature is 90 deg.C, and preheating time is 10 min;

step 2, cleaning the mold by using industrial acetone, uniformly coating a mold surface of the mold in a concave-convex mold by using a release agent, fixedly connecting the mold on a molding press, starting the molding press, and preheating the mold;

preheating temperature is 80 deg.C, and preheating for 15 min.

Step 3, after the step 2, uniformly paving 30.5Kg of premix in a die cavity of a die, closing the die, inserting a thermometer to record the temperature, starting a die press, heating and die pressing, and polishing burrs and fins after die stripping to obtain the high silica-phenolic resin composite heat-proof plate of 294mm multiplied by 206 mm;

the specific process of temperature-rising die pressing comprises the following steps: heating to 90 deg.C at a rate of 1.5 deg.C/min under 4Mpa, maintaining for 50min, applying 20Mpa when the mold temperature is 80-110 deg.C, heating to 110 deg.C at a rate of 0.33 deg.C/min, maintaining for 5h without pressure compensation, heating to 175 deg.C at a rate of 0.24 deg.C/min, maintaining for 6h, and cooling to below 45 deg.C;

example 5

The invention relates to a preparation method of a high-silica-phenolic resin composite heat-proof plate, which is implemented according to the following steps:

step 1, uniformly mixing high silica glass fiber and phenolic resin, and drying to prepare a premix; then putting the premix into a material drying sieve for preheating;

the mass fractions of the high silica glass fiber and the phenolic resin are 58 percent and 42 percent respectively;

the drying temperature is 80 ℃, and the drying time is 90 min;

preheating at 85 deg.C for 15 min;

step 2, cleaning the mold by using industrial acetone, uniformly coating a mold surface of the mold in a concave-convex mold by using a release agent, fixedly connecting the mold on a molding press, starting the molding press, and preheating the mold;

preheating temperature is 75 ℃, and preheating time is 15 min.

And 3, after the step 2, uniformly spreading 11.5Kg of premix in a die cavity of the die, closing the die, and pressing the variable-section heat-proof plate, wherein the thickness is increased from 59.5mm to 93mm, and the thickness is increased by 56.3%. Inserting a thermometer to record temperature, starting a mould press, heating and mould pressing, and polishing burrs and fins after demoulding to obtain the high silica-phenolic resin composite heat-proof plate;

the specific process of temperature-rising die pressing comprises the following steps: heating to 90 deg.C under 5Mpa for 10min, maintaining for 50min, applying 20Mpa when the mold temperature is 80-110 deg.C, heating to 110 deg.C for 1h, maintaining for 4.5h, heating to 175 deg.C for 4.5h, maintaining for 5h, and cooling to 45 deg.C or below with a molding press.

TABLE 1 Properties of the heat shield panels prepared according to the invention

From table 1, it can be known that each performance index of the heat-proof plate prepared by the invention is superior to the performance required in the application process, wherein the heat-proof plate is significantly superior to the theoretical value in three performances of ablation rate, tensile strength and thermal conductivity, which further indicates that the heat-proof plate has better ablation resistance and lower thermal conductivity, and therefore, the excellent comprehensive performance of the heat-proof plate is beneficial to the further application of the heat-proof plate in the new heat-proof field.

The macro-morphology of the heat-proof plate prepared in the embodiment 5 of the invention is shown in fig. 1, and in fig. 1, the surface of the heat-proof plate is flat and bright and has uniform color. Because the premix is made of the chopped high-silica glass fiber-phenolic resin, the distribution form of the premix can still be clearly seen after the heat-proof plate is formed, the premix is uniformly distributed and criss-cross, and the performance is uniform. The macro topography of the surface of the heat-proof plate prepared before the invention is shown in fig. 2, and in fig. 2, it can be clearly seen that the premix made of the high silica glass fiber-phenolic resin is not pressed and formed, the surface of the heat-proof plate is uneven, and a large amount of looseness exists. Figure 1 shows a significant improvement in both the forming process and performance compared to figure 2.

The invention prepares the heat-proof plates with different thicknesses, from a plane thin plate with the thickness of 6mm to a plane thick plate with the thickness of 206mm, wherein the thickness of the heat-proof plates is 34.3 times that of the thin plate; meanwhile, variable cross sections with different thicknesses can be realized in the same heat-proof plate. This opens up a wide space for the further development of the heat-proof plate and is also beneficial to obtaining good market application force.