阅读说明：本技术 一种耐真空紫外辐照有机硅氧烷及其设计与制备方法 (Vacuum ultraviolet radiation resistant organosiloxane and design and preparation method thereof ) 是由 李朝龙 朴明星 王啸 史浩飞 于 2021-07-02 设计创作，主要内容包括：本发明提供一种耐真空紫外辐照有机硅氧烷及其设计与制备方法。通过化学方法,在石墨烯量子点或者富勒烯表面接枝聚合有机硅氧烷分子链,获得一种杂化结构的耐真空紫外辐照树脂。克服了现有有机硅氧烷树脂材料耐紫外性能低的缺陷。(The invention provides vacuum ultraviolet radiation resistant organosiloxane and a design and preparation method thereof. By a chemical method, organic siloxane molecular chains are grafted and polymerized on the surface of graphene quantum dots or fullerene to obtain the vacuum ultraviolet radiation resistant resin with a hybrid structure. Overcomes the defect of low ultraviolet resistance of the existing organic siloxane resin material.)

1. A preparation method of vacuum ultraviolet radiation resistant organosiloxane is characterized by comprising the following steps:

adding aminated graphene quantum dots or aminated fullerene into toluene, and performing ultrasonic treatment to obtain a dispersion liquid A;

adding the silicone oil into the dispersion liquid A to obtain a dispersion liquid B;

heating the dispersion liquid B, and reacting under the protection of inert gas;

after the reaction is finished, cooling the reaction product;

and 5, distilling the toluene in the reaction product to obtain the ultraviolet-resistant organosiloxane resin.

2. The method for designing and preparing vacuum ultraviolet radiation resistant organosiloxane as claimed in claim 1, wherein the method comprises the following steps: in the step 1, the ratio of the mass (g) of the aminated graphene quantum dots or aminated fullerene to the volume (mL) of toluene is (1-5): 100-300.

3. The method for designing and preparing vacuum ultraviolet radiation resistant organosiloxane as claimed in claim 1, wherein the method comprises the following steps: in the step 1, the ultrasonic power is 200-2000W, and the treatment time is 30-60 minutes.

4. The method for designing and preparing vacuum ultraviolet radiation resistant organosiloxane as claimed in claim 1, wherein the method comprises the following steps: in step 1, the selected type of the aminated fullerene is C60.

5. The method for designing and preparing the vacuum ultraviolet radiation resistant organosiloxane as claimed in claim 1 or 2, wherein the method comprises the following steps: in the step 1, the particle size of the selected aminated graphene quantum dot is 20-100 nm.

6. The method for designing and preparing vacuum ultraviolet radiation resistant organosiloxane as claimed in claim 1, wherein the method comprises the following steps: the mass ratio of the aminated graphene quantum dots or aminated fullerene in the step 1 to the silicone oil in the step 2 is (1-5) to (95-99).

7. The method for designing and preparing vacuum ultraviolet radiation resistant organosiloxane as claimed in claim 1 or 5, wherein the method comprises the following steps: in the step 2), the silicone oil is epoxy group modified silicone oil.

8. The method for designing and preparing vacuum ultraviolet radiation resistant organosiloxane as claimed in claim 1, wherein the method comprises the following steps: in the step 3, the heating reaction temperature is 80 ℃, and the reaction time is 120-240 min.

9. The method for designing and preparing vacuum ultraviolet radiation resistant organosiloxane as claimed in claim 1, wherein the method comprises the following steps: in the step 4, cooling to 60 ℃; in step 5, the solvent toluene was distilled off under reduced pressure.

10. Vacuum UV radiation resistant organosiloxane obtainable by a process according to any one of claims 1 to 9.

Technical Field

The invention relates to the technical field of high polymer materials, in particular to a preparation method of vacuum ultraviolet radiation resistant organic siloxane resin.

Background

The organic siloxane resin is a polymer capable of realizing a highly cross-linked structure, has the dual characteristics of organic resin and inorganic materials, has unique physical and chemical properties, and has good electrical insulation property, temperature resistance and waterproof effects. The coating is an ideal material for protecting the surface layer by heat resistance, heat resistance and moisture resistance treatment.

The vacuum ultraviolet is only applied to vacuum because ultraviolet rays in the wave band are strongly absorbed by oxygen in air, and the long wave limit of the vacuum ultraviolet is roughly 150-200 nm. The vacuum ultraviolet radiation energy is high, and the silicon-oxygen bond in the molecular structure of the organic siloxane is easy to break, so that the organic siloxane material is quickly ineffective.

Disclosure of Invention

The invention aims to provide a preparation method of vacuum ultraviolet radiation resistant organosiloxane, which is characterized by comprising the following steps:

adding aminated graphene quantum dots or aminated fullerene into toluene, and performing ultrasonic treatment to obtain a dispersion liquid A;

adding silicone oil into the dispersion liquid A to obtain a dispersion liquid B;

heating the dispersion liquid B, and reacting under the protection of inert gas;

after the reaction is finished, cooling the reaction product;

and 5, distilling the toluene in the reaction product to obtain the ultraviolet-resistant organosiloxane resin.

It is worth noting that graphene quantum dots and fullerenes have strong absorption capacity for vacuum ultraviolet radiation, but both are poorly compatible with organosiloxane resins. The invention realizes the chemical bonding of the polymer and the inorganic material through the specific functional group on the surface of the inorganic nonmetal, and eliminates the interface negative effect between the inorganic material and the polymer, so as to obtain a new material with excellent performance.

Further, in the step 1, the ratio of the mass (g) of the aminated graphene quantum dots or aminated fullerene to the volume (mL) of toluene is (1-5): (100-300).

Further, in the step 1), the ultrasonic power is 200W, and the treatment time is 30-60 minutes.

Further, in step 1), the selected type of the aminated fullerene is C60.

Further, in the step 1), the particle size of the selected aminated graphene quantum dot is 20-100 nm.

Further, the mass ratio of the aminated graphene quantum dots or aminated fullerene in the step 1 to the silicone oil in the step 2 is (1-5) to (95-99).

Further, in the step 2), the silicone oil is epoxy group-modified silicone oil.

Further, in the step 3), the heating reaction temperature is 80 ℃, and the reaction time is 120-240 min.

Further, in the step 4, cooling to 60 ℃;

further, in step 5), the solvent toluene was distilled off under reduced pressure.

The invention also claims the vacuum ultraviolet radiation resistant organosiloxane obtained according to the method. The amination fullerene or graphene quantum dot and the epoxy organosiloxane are chemically bonded through the reaction of amino and epoxy groups, the grafting rate of the graphene quantum dot or C60 is 85-99%, and the vacuum ultraviolet irradiation resistant dose of the obtained resin can reach 8000 ESH.

Detailed Description

The present invention is further illustrated by the following examples, but it should not be construed that the scope of the above-described subject matter is limited to the following examples. Various substitutions and alterations can be made without departing from the technical idea of the invention and the scope of the invention is covered by the present invention according to the common technical knowledge and the conventional means in the field.

Example 1:

this example prepares a uv resistant organosiloxane resin comprising the steps of:

1, weighing 1g of aminated fullerene, adding the aminated fullerene into 100ml of toluene, and carrying out ultrasonic treatment for 30 minutes at 200W;

adding 99g of epoxy group modified silicone oil (epoxy group modified silicone oil with the epoxy equivalent of 300), uniformly stirring, heating the solution to 80 ℃, and reacting for 120min under the protection of nitrogen.

Cooling the reaction system to 60 ℃;

and (4) distilling the solvent toluene under reduced pressure to obtain the ultraviolet-resistant organosiloxane resin.

The obtained resin is tested, and the vacuum ultraviolet radiation resistant dose can reach 6000 ESH.

Example 2:

this example prepares a uv resistant organosiloxane resin comprising the steps of:

weighing 5g of aminated fullerene, adding the aminated fullerene into 300ml of toluene, and carrying out ultrasonic treatment for 60 minutes at 600W;

adding 95g of epoxy group modified silicone oil (epoxy group modified silicone oil with the epoxy equivalent of 180), uniformly stirring, heating the solution to 80 ℃, and reacting for 240min under the protection of nitrogen.

Cooling the reaction system to 60 ℃;

and (4) distilling the solvent toluene under reduced pressure to obtain the ultraviolet-resistant organosiloxane resin.

The obtained resin is tested, and the vacuum ultraviolet radiation resistant dose can reach 8000 ESH.

Example 3:

this example prepares a uv resistant organosiloxane resin comprising the steps of:

weighing 3g of aminated fullerene, adding the aminated fullerene into 200ml of toluene, and carrying out ultrasonic treatment at 2000W for 60 minutes;

adding 97g of epoxy group modified silicone oil (epoxy group modified silicone oil with epoxy equivalent of 260), uniformly stirring, heating the solution to 80 ℃, and reacting for 180min under the protection of nitrogen.

Cooling the reaction system to 60 ℃;

and (4) distilling the solvent toluene under reduced pressure to obtain the ultraviolet-resistant organosiloxane resin.

The obtained resin is tested, and the vacuum ultraviolet radiation resistant dose can reach 7000 ESH.

Example 4:

this example prepares a uv resistant organosiloxane resin comprising the steps of:

weighing 4g of aminated fullerene, adding the aminated fullerene into 280ml of toluene, and carrying out ultrasonic treatment for 60 minutes at 1000W;

adding 96g of epoxy group modified silicone oil (epoxy group modified silicone oil with epoxy equivalent of 260), uniformly stirring, heating the solution to 80 ℃, and reacting for 200min under the protection of nitrogen.

Cooling the reaction system to 60 ℃;

and (4) distilling the solvent toluene under reduced pressure to obtain the ultraviolet-resistant organosiloxane resin.

The obtained resin is tested, and the vacuum ultraviolet radiation resistant dose can reach 7600 ESH.