阅读说明：本技术 一种201甲基硅油的生产工艺 (Production process of 201 methyl silicone oil ) 是由 黄立忠 陶明海 李海成 黄金龙 童红梅 于 2019-11-29 设计创作，主要内容包括：本发明公开了一种201甲基硅油的生产工艺,包括以下步骤：无氧条件下,利用真空泵将100重量份二甲基环硅氧烷混合物和2-3重量份封头剂抽入反应釜内,接着升温至55-65℃；搅拌条件下,向反应釜内加入5-8重量份活性白土作为催化剂,充分混匀后,于125-130℃条件下聚合0.5-1.5小时；以25-30℃/h的速度加热反应釜,当反应釜升温至170℃时,恒温恒压维持0.5-1.5小时；以25-30℃/h的速度使反应釜降温至90-100℃后关闭真空泵,打开真空阀,放料,冷却至室温,即得到无色透明状的201甲基硅油。本发明使用少量活性白土作为催化剂,能吸附杂质颜色,过滤后可重复使用,降低了生产成本,且对空气污染小。(The invention discloses a production process of 201 methyl silicone oil, which comprises the following steps: pumping 100 parts by weight of dimethyl cyclosiloxane mixture and 2-3 parts by weight of end sealing agent into a reaction kettle by using a vacuum pump under an anaerobic condition, and then heating to 55-65 ℃; under the condition of stirring, adding 5-8 parts by weight of activated clay serving as a catalyst into the reaction kettle, fully and uniformly mixing, and polymerizing for 0.5-1.5 hours at the temperature of 125-130 ℃; heating the reaction kettle at the speed of 25-30 ℃/h, and maintaining the constant temperature and the constant pressure for 0.5-1.5 hours when the temperature of the reaction kettle is raised to 170 ℃; cooling the reaction kettle to 90-100 ℃ at the speed of 25-30 ℃/h, then closing the vacuum pump, opening the vacuum valve, discharging, and cooling to room temperature to obtain the colorless transparent 201 methyl silicone oil. The invention uses a small amount of activated clay as a catalyst, can adsorb impurity colors, can be repeatedly used after filtration, reduces the production cost and has little pollution to air.)

1. A production process of 201 methyl silicone oil is characterized by comprising the following steps:

(1) introducing nitrogen into the reaction kettle to remove oxygen, starting a vacuum pump, pumping 100 parts by weight of the dimethylcyclosiloxane mixture and 8-12 parts by weight of the end sealing agent into the reaction kettle, and then heating to 55-65 ℃;

(2) under the condition of stirring, adding 5-8 parts by weight of activated clay serving as a catalyst into the reaction kettle, fully and uniformly mixing, and polymerizing for 0.5-1.5 hours at the temperature of 125-130 ℃;

(3) heating the reaction kettle at the speed of 25-30 ℃/h, and maintaining the constant temperature and the constant pressure for 0.5-1.5 hours when the temperature of the reaction kettle is raised to 170 ℃;

(4) cooling the reaction kettle to 90-100 ℃ at the speed of 25-30 ℃/h, then closing the vacuum pump, opening the vacuum valve, discharging, and cooling to room temperature.

2. The process for producing 201 simethicone as claimed in claim 1, wherein: in the dimethyl cyclosiloxane mixture, the weight percentage of D3, D4, D5 and D6 is more than or equal to 99.8 percent, and the weight percentage of D4 is more than or equal to 80 percent.

3. The process for producing 201 simethicone according to claim 1 or 2, wherein: the total water content of the dimethyl cyclosiloxane mixture and the end sealing agent is less than or equal to 0.1 wt%.

4. The process for producing 201 simethicone as claimed in claim 1, wherein: the reaction kettle is a reaction kettle with an inner lining made of an anticorrosive material.

5. The process for producing 201 simethicone according to claim 1 or 4, wherein: the reaction kettle is an enamel reaction kettle.

6. The process for producing 201 simethicone as claimed in claim 1 or 3, wherein: firstly introducing nitrogen into a reaction kettle to remove oxygen, and then pumping the dimethyl cyclosiloxane mixture and the end sealing agent into the reaction kettle.

7. The process for producing 201 simethicone as claimed in claim 1, wherein: in the step (2), the addition amount of activated clay is 5 parts by weight.

8. The process for producing 201 simethicone as claimed in claim 1, wherein: in the step (2), the polymerization temperature is 125 ℃ and the polymerization time is 1 hour.

9. The process for producing 201 simethicone as claimed in claim 1, wherein: the capping agent is prepared by reacting dimethyl cyclosiloxane mixture, hexamethyldisiloxane and concentrated sulfuric acid in a weight ratio of 100:60:5 at 85-90 ℃ and hydrolyzing.

Technical Field

The invention belongs to the field of organic silicon, and particularly relates to a production process of 201 methyl silicone oil.

Background

201 methyl silicone oil is a linear polymethylsiloxane, is colorless transparent oily liquid and has a molecular formula of (CH)₃)₃SiO[(CH₃)₂SiO]_nSi(CH₃)₃. Due to excellent heat resistance and oxygen resistanceChemical conversion and low temperature resistance, the 201 dimethyl silicone oil can be used for a long time within the temperature range of-50 ℃ to +180 ℃; the anti-shearing property is strong, the compressibility is more than 20 times of that of common mineral oil, and the spring is an ideal liquid spring; and has low temperature viscosity coefficient, low vapor pressure, low surface tension, high water increasing property and lubricity; the 201 dimethyl silicone oil also has the advantages of high breakdown voltage resistance, electric arc resistance, corona resistance, small dielectric loss, good light transmittance, no toxic action on human bodies and the like, is widely applied to departments of industrial production, national defense, scientific research, medical health and the like, and is mainly used for aspects of electrical insulation, demoulding, defoaming, damping and shock resistance, hydraulic pressure, dust prevention, water prevention, high and low temperature lubrication and the like.

Disclosure of Invention

Aiming at the defects in the prior art, the invention aims to provide a production process of 201 methyl silicone oil, which solves the problems of low product transparency, high cost and the like in the prior art.

In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:

a production process of 201 methyl silicone oil comprises the following steps:

(1) introducing nitrogen into the reaction kettle to remove oxygen, starting a vacuum pump, pumping 100 parts by weight of the dimethylcyclosiloxane mixture and 8-12 parts by weight of the end sealing agent into the reaction kettle, and then heating to 55-65 ℃;

(2) under the condition of stirring, adding 5-8 parts by weight of activated clay serving as a catalyst into the reaction kettle, fully and uniformly mixing, and polymerizing for 0.5-1.5 hours at the temperature of 125-130 ℃;

(3) heating the reaction kettle at the speed of 25-30 ℃/h, and maintaining the constant temperature and the constant pressure for 0.5-1.5 hours when the temperature of the reaction kettle is raised to 170 ℃;

(4) cooling the reaction kettle to 90-100 ℃ at the speed of 25-30 ℃/h, then closing the vacuum pump, opening the vacuum valve, discharging, and cooling to room temperature.

On the basis of the technical scheme, the total water content of the dimethylcyclosiloxane mixture and the end sealing agent is less than or equal to 0.1 wt%.

On the basis of the technical scheme, the reaction kettle is a reaction kettle with an inner lining made of an anticorrosive material.

On the basis of the technical scheme, the reaction kettle is an enamel reaction kettle.

On the basis of the technical scheme, firstly introducing nitrogen into the reaction kettle to remove oxygen, and then pumping the dimethyl cyclosiloxane mixture and the end sealing agent into the reaction kettle.

In addition to the above technical means, in the step (2), the amount of activated clay added is 5 parts by weight.

On the basis of the technical scheme, in the step (2), the polymerization temperature is 95 ℃, and the polymerization time is 3 hours.

On the basis of the technical scheme, the end sealing agent is generated by hydrolyzing a dimethyl cyclosiloxane mixture, hexamethyldisiloxane and concentrated sulfuric acid in a weight ratio of 100:60:5 at 85-90 ℃.

Compared with the prior art, the invention uses a small amount of activated clay as a catalyst, can adsorb impurity colors, can be repeatedly used after filtration, reduces the production cost and has little pollution to air.

Detailed Description

The technical solution of the present invention will be described in further detail with reference to examples.

The reactors used in the following examples are all enamel reactors.