阅读说明：本技术 一种耐高温低介电弹性体材料制备方法 (Preparation method of high-temperature-resistant low-dielectric elastomer material ) 是由 张文政 于永健 李一多 何悦萌 张庭豪 于 2020-12-14 设计创作，主要内容包括：一种耐高温低介电弹性体材料的制备方法,涉及一种弹性体介电材料制备方法,该制备方法包括步骤1：采用苯并环丁烯树脂对气相法纳米白炭黑进行包覆处理,得到分散液；步骤2：在分散液中溶入液体氢化丁腈/丁腈橡胶等混合物,得到混炼胶溶液；步骤3：将聚酰亚胺纤维浸渍混炼胶溶液中并取出,经脱除溶剂得到预浸料；步骤4：将步骤3得到的预浸料裁剪后制成层压板,层压板经高温硫化即可得到耐高温的低介电弹性体材料。得到的复合材料具有优良的弹性。增强材料纤维聚酰亚胺纤维不但介电常数低,而且耐高温,液体氢化丁腈/丁腈橡胶的硫化胶亦具有150℃以上的耐温性,上述材料的协同作用使之可以在150℃下长期使用。(A preparation method of a high-temperature-resistant low-dielectric elastomer material relates to a preparation method of an elastomer dielectric material, and comprises the following steps of 1: coating the fumed nano white carbon black by adopting benzocyclobutene resin to obtain dispersion liquid; step 2: dissolving a mixture of liquid hydrogenated butyronitrile/nitrile rubber and the like in the dispersion liquid to obtain a rubber compound solution; and step 3: soaking polyimide fibers in the mixed rubber solution, taking out the polyimide fibers, and removing the solvent to obtain a prepreg; and 4, step 4: and (4) cutting the prepreg obtained in the step (3) to prepare a laminated board, and vulcanizing the laminated board at high temperature to obtain the high-temperature-resistant low-dielectric elastomer material. The resulting composite material has excellent elasticity. The reinforced material fiber polyimide fiber has low dielectric constant and high temperature resistance, and the vulcanized rubber of liquid hydrogenated butyronitrile/nitrile rubber has temperature resistance over 150 deg.c, and the synergistic effect of the said materials makes it possible to use at 150 deg.c for long period.)

1. The preparation method of the high-temperature-resistant low-dielectric elastomer material is characterized by comprising the following preparation processes of:

step 1: dispersing the gas-phase nano white carbon black into a solvent at a stirring speed of 1000rpm to form a dispersion liquid;

step 2: adding benzocyclobutene resin into the dispersion liquid obtained in the step 1, and polymerizing the benzocyclobutene resin after the dispersion liquid is subjected to nitrogen passing and oxygen discharging to obtain a gas-phase nano white carbon black mixed liquid coated with the benzocyclobutene resin;

and step 3: adding a mixture of liquid hydrogenated butyronitrile/nitrile rubber and the like into the mixed solution obtained in the step 2, and uniformly mixing to obtain a mixed rubber solution;

and 4, step 4: dipping polyimide fibers with low dielectric constant into the mixed rubber solution obtained in the step (3) to obtain a prepreg;

and 5: and (4) cutting the prepreg obtained in the step (4) to prepare a laminated board, and vulcanizing the laminated board to obtain the high-temperature-resistant low-dielectric elastomer material.

2. The method for preparing a high temperature resistant low dielectric constant elastomer material as claimed in claim 1, wherein in the step 1, the gas phase method nano white carbon black in the dispersion liquid is 0.1-10% by mass of the mixed liquid.

3. The method for preparing high temperature resistant low dielectric constant elastomer material according to claim 1, wherein in the step 1, the fumed silica is dispersed in benzene, toluene and xylene or their mixture.

4. The method for preparing the high temperature resistant low dielectric elastomer material according to claim 1, wherein in the step 2, after the benzocyclobutene resin is added into the dispersion liquid in the step 1, nitrogen is introduced for oxygen discharge for at least 20min, and then polymerization is carried out for 1-4h at 140 ℃ and 2atm, wherein the benzocyclobutene resin is 5-50% of the mass fraction of the fumed silica.

5. The preparation method of the high-temperature-resistant low-dielectric elastomer material as claimed in claim 1, wherein in the step 3, the liquid hydrogenated nitrile-butadiene/nitrile-butadiene rubber mixture comprises the following components in parts by weight: 80 parts of hydrogenated butyronitrile, 20 parts of butyronitrile, N55070 parts of carbon black, active MgO 2 parts, Rhizoctonia solani 0072 parts, RD 1 parts, 1 part of stearic acid, MB 2 parts, 5 parts of zinc oxide, 4.5 parts of DCP, 3 parts of TAlC and 0.3 part of sulfur.

6. The preparation method of the high-temperature-resistant low-dielectric elastomer material as claimed in claim 1, wherein the mass fraction of the liquid hydrogenated nitrile butadiene/nitrile butadiene rubber mixture in the dispersion liquid is 10-60% in the mixed liquid.

7. The method for preparing high temperature resistant low dielectric constant elastomer material according to claim 1, wherein the prepreg obtained in step 4 is subjected to vacuum removal of benzene, toluene and xylene or their mixture.

8. The method for preparing the high-temperature-resistant low-dielectric elastomer material as claimed in claim 1, wherein in the step 5, the curing temperature of the laminated board is 151 ℃, the curing time is 25min, and the curing pressure is 0.1MPa to 0.3 MPa.

Technical Field

The invention relates to a preparation method of a dielectric material, in particular to a preparation method of a high-temperature-resistant low-dielectric elastomer material.

Background

Benzocyclobutene (Benzocyclobutene) is a novel active resin, can form a thermoplastic polymer and a thermosetting polymer, and has excellent electrical properties, low moisture absorption rate and high thermal stability, the thermal stability of the Benzocyclobutene resin is higher than that of common polymer resin, the glass transition temperature is more than 350 ℃, and the thermal decomposition temperature is more than 400 ℃. The benzocyclobutene has the advantages of chemical stability, acid and alkali resistance and other corrosive atmospheres, good solvent resistance and low swelling rate in an organic solvent, and is very suitable for being used as a dielectric material substrate.

At present, the dielectric constant and the glass transition temperature of a resin matrix with long-term use conditions at 350 ℃ are respectively as follows: polyimide resin (3.0, not less than 316 ℃), alkynyl silicon resin (2.8-3.0, not less than 400 ℃), cyano resin (3.0-3.2, not less than 350 ℃), and benzocyclobutene resin (not less than 2.65, not less than 350 ℃). The polyimide resin matrix composite material is earlier researched, but the coating effect of the material on the nano white carbon black is poor; the compatibility of alkynyl silicon resin and cyano resin with high surface energy nano white carbon black is also poor, and the operation steps are complicated. The invention provides a method for pre-polymerizing benzocyclobutene, which is characterized in that nano white carbon black is coated and then added into liquid hydrogenated butyronitrile/nitrile rubber compound rubber, the composite material obtained after vulcanization has excellent elasticity, the added polyimide fiber not only has the function of enhancing the elastomer, but also has low dielectric constant. Through the synergistic effect of the materials, the obtained product has low dielectric constant and can be used at 150 ℃ for a long time.

Disclosure of Invention

The invention aims to provide a preparation method of a high-temperature-resistant low-dielectric elastomer material, which has the following advantages: the composite material prepared by the invention has excellent elasticity. The reinforced material fiber polyimide fiber has low dielectric constant and high temperature resistance, and the vulcanized rubber of liquid hydrogenated butyronitrile/nitrile rubber has temperature resistance over 150 deg.c, and the synergistic effect of the said materials makes it possible to use at 150 deg.c for long period.

The purpose of the invention is realized by the following technical scheme:

a preparation method of a high-temperature-resistant low-dielectric elastomer material comprises the following preparation processes:

step 1: dispersing the gas-phase nano white carbon black into a solvent at a stirring speed of 1000rpm to form a dispersion liquid;

step 2: adding benzocyclobutene resin into the dispersion liquid obtained in the step 1, and polymerizing the benzocyclobutene resin after the dispersion liquid is subjected to nitrogen passing and oxygen discharging to obtain a gas-phase nano white carbon black mixed liquid coated with the benzocyclobutene resin;

and step 3: adding a mixture of liquid hydrogenated butyronitrile/nitrile rubber and the like into the mixed solution obtained in the step 2, and uniformly mixing to obtain a mixed rubber solution;

and 4, step 4: dipping polyimide fibers with low dielectric constant into the mixed rubber solution obtained in the step (3) to obtain a prepreg;

and 5: and (4) cutting the prepreg obtained in the step (4) to prepare a laminated board, and vulcanizing the laminated board to obtain the high-temperature-resistant low-dielectric elastomer material.

In the preparation method of the high-temperature-resistant low-dielectric elastomer material, in the step 1, the mass fraction of the gas-phase-method nano white carbon black in the mixed solution is 0.1-10%.

In the preparation method of the high-temperature-resistant low-dielectric elastomer material, in the step 1, the gas-phase-method nano white carbon black is dispersed in benzene, toluene and xylene or a mixed solution of the benzene, the toluene and the xylene.

In the step 2, after the benzocyclobutene resin is added into the dispersion liquid in the step 1, introducing nitrogen and discharging oxygen for at least 20min, and then carrying out polymerization reaction for 1-4h at 140 ℃ and 2atm, wherein the benzocyclobutene resin is 5-50% of the mass fraction of the fumed nano white carbon black.

In the step 3, the liquid hydrogenated butyronitrile/nitrile rubber mixture is prepared by the following steps in parts by weight: 80 parts of hydrogenated butyronitrile, 20 parts of butyronitrile, N55070 parts of carbon black, active MgO 2 parts, Rhizoctonia solani 0072 parts, RD 1 parts, 1 part of stearic acid, MB 2 parts, 5 parts of zinc oxide, 4.5 parts of DCP, 3 parts of TAlC and 0.3 part of sulfur.

According to the preparation method of the high-temperature-resistant low-dielectric elastomer material, the mass fraction of a liquid hydrogenated butyronitrile/nitrile rubber mixture in the dispersion liquid in the mixed liquid is 10-60%.

In the step 4, the prepreg obtained needs to be subjected to vacuum removal of benzene, toluene, xylene or a mixture thereof.

In the step 5, the curing temperature of the laminated board is 151 ℃, the curing time is 25min, and the curing pressure is 0.1MPa to 0.3 MPa.

The invention has the advantages and effects that:

the invention relates to a preparation method of a high-temperature-resistant low-dielectric elastomer material, and the obtained composite material has excellent elasticity. The reinforced material fiber polyimide fiber has low dielectric constant and high temperature resistance, and the vulcanized rubber of liquid hydrogenated butyronitrile/nitrile rubber has temperature resistance over 150 deg.c, and the synergistic effect of the said materials makes it possible to use at 150 deg.c for long period.

Detailed Description

The following detailed description is presented to enable one of ordinary skill in the art to more fully, accurately and completely understand the principles and techniques of the present invention.

Embodiment 1

Step 1: dispersing 30g of gas-phase nano white carbon black into 500g of dimethylbenzene at a stirring speed of 1000rpm to form a dispersion liquid;

step 2: adding 10g of benzocyclobutene resin into the dispersion liquid obtained in the step 1, and carrying out polymerization reaction for 1h at 140 ℃ and 2atm after nitrogen and oxygen are introduced and exhausted for 25min to obtain a gas-phase nano white carbon black mixed liquid coated with the benzocyclobutene resin;

and step 3: adding 250g of a mixture of liquid hydrogenated butyronitrile/nitrile rubber and the like into the mixed solution obtained in the step 2, and uniformly mixing to obtain a mixed rubber solution;

and 4, step 4: soaking polyimide fibers in the mixed rubber solution to obtain a prepreg, and then removing xylene from the prepreg under the vacuum condition of 133 pa;

and 5: and (4) cutting the prepreg obtained in the step (4) to prepare a laminated board, and curing for 25min at the temperature of 151 ℃ and the curing pressure of 0.1MPa to obtain the high-temperature-resistant low-dielectric elastomer material.

Embodiment 2

Step 1: dispersing 50g of gas-phase nano white carbon black into 500g of toluene at a stirring speed of 1000rpm to form a dispersion liquid;

step 2: adding 30g of benzocyclobutene resin into the dispersion liquid obtained in the step 1, and after nitrogen and oxygen are introduced and exhausted for 20min, carrying out polymerization reaction for 2h at 140 ℃ under the condition of 2atm to obtain a gas-phase nano white carbon black mixed liquid coated with the benzocyclobutene resin;

and step 3: adding 200g of a mixture of liquid hydrogenated butyronitrile/nitrile rubber and the like into the mixed solution obtained in the step 2, and uniformly mixing to obtain a mixed rubber solution;

and 4, step 4: soaking polyimide fibers in the mixed rubber solution to obtain a prepreg, and then removing toluene from the prepreg under the vacuum condition of 133 pa;

and 5: and (4) cutting the prepreg obtained in the step (4) to prepare a laminated board, and curing for 25min at the temperature of 151 ℃ and the curing pressure of 0.2MPa to obtain the high-temperature-resistant low-dielectric elastomer material.

Embodiment 3

Step 1: dispersing 40g of gas-phase nano white carbon black into 500g of benzene at a stirring speed of 1000rpm to form a dispersion liquid;

step 2: adding 10g of benzocyclobutene resin into the dispersion liquid obtained in the step 1, and after nitrogen and oxygen are introduced and exhausted for 30min, carrying out polymerization reaction for 3h at 140 ℃ under the condition of 2atm to obtain a gas-phase nano white carbon black mixed liquid coated with the benzocyclobutene resin;

and step 3: adding 220g of a mixture of liquid hydrogenated butyronitrile/nitrile rubber and the like into the mixed solution obtained in the step 2, and uniformly mixing to obtain a mixed rubber solution;

and 4, step 4: soaking polyimide fibers in the mixed rubber solution to obtain a prepreg, and then removing benzene from the prepreg under the vacuum condition of 133 pa;

and 5: and (4) cutting the prepreg obtained in the step (4) to prepare a laminated board, and curing for 25min at the temperature of 151 ℃ and the curing pressure of 0.3MPa to obtain the high-temperature-resistant low-dielectric elastomer material.

The above embodiments are only part of exemplary descriptions of the present invention, so that the specific implementation of the present invention is not limited by the above manner, and it is within the protection scope of the present invention as long as various insubstantial modifications are made by using the method concept and technical scheme of the present invention, or the concept and technical scheme of the present invention are directly applied to other occasions without modification.