阅读说明：本技术 一种对甲基苯乙烯/1-辛烯共改性含氢硅油脱模剂的制备方法 (Preparation method of p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent ) 是由 欧阳密 秦超 胡旭明 陈璐 张�诚 于 2020-04-08 设计创作，主要内容包括：一种对甲基苯乙烯/1-辛烯共改性含氢硅油脱模剂的制备方法,将含氢硅油投入反应釜中,搅拌下升温至80～90℃后,滴加对甲基苯乙烯与铂催化剂的混合物,滴加完毕后在80～90℃下反应3～6h,升温至100～120℃后,滴加1-辛烯与铂催化剂的混合物,滴加完毕后在100～120℃下反应3～6h,冷却至室温,抽真空脱低沸得到对甲基苯乙烯/1-辛烯共改性含氢硅油脱模剂。本发明工艺制备的脱模剂具有过程简单、易操作、效率高、质量好等优点。(A preparation method of a p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent comprises the steps of putting hydrogen-containing silicone oil into a reaction kettle, heating to 80-90 ℃ under stirring, dropwise adding a mixture of p-methylstyrene and a platinum catalyst, reacting at 80-90 ℃ for 3-6 hours after dropwise adding, heating to 100-120 ℃, dropwise adding a mixture of 1-octene and a platinum catalyst, reacting at 100-120 ℃ for 3-6 hours after dropwise adding, cooling to room temperature, vacuumizing and removing low boiling to obtain the p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent. The release agent prepared by the process has the advantages of simple process, easy operation, high efficiency, good quality and the like.)

1. A preparation method of a p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent is characterized in that hydrogen-containing silicone oil is put into a reaction kettle, the temperature is raised to 80-90 ℃ under stirring, then a mixture of p-methylstyrene and a platinum catalyst is dripped, and the reaction lasts for 3-6 hours at 80-90 ℃ after the dripping is finished; heating to 100-120 ℃, dropwise adding a mixture of 1-octene and a platinum catalyst, and reacting at 100-120 ℃ for 3-6 h after dropwise adding; cooling to room temperature, vacuumizing and removing low boiling to obtain the p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent.

2. The preparation method of the p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil mold release agent according to claim 1, wherein the platinum catalyst is Karstedt catalyst, the mass concentration of Pt is 2%, and the input amount is 1-10 ppm of the addition raw material; the raw material adopts p-methylstyrene with the purity of 99 to 99.9 percent; 1-octene with a purity of 99-99.9%; the hydrogen content of the hydrogen-containing silicone oil is 0.4-1.6 wt%; the viscosity of the hydrogen-containing silicone oil is 90-170 mpa.s; the molar ratio of the hydrogen-containing silicone oil to the p-methylstyrene is 1:0.5 to 0.6; the molar ratio of the hydrogen-containing silicone oil to the 1-octene is 1: 0.4-0.5; the vacuum degree of the reduced pressure distillation is-0.0998 to-0.1 Mpa; the reduced pressure distillation temperature is 140-180 ℃.

3. The process for producing a p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent according to claim 2, wherein the amount of the platinum catalyst added is 5ppm based on the addition raw material.

4. The method for preparing the p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil mold release agent according to claim 2, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.5% wt, the viscosity of the hydrogen-containing silicone oil is 120mpa.s, the molar ratio of the hydrogen-containing silicone oil to the p-methylstyrene is 1:0.6, the molar ratio of the hydrogen-containing silicone oil to the 1-octene is 1:0.5, the vacuum degree of reduced pressure distillation is-0.1 Mpa, and the temperature of reduced pressure distillation is 150 ℃.

Technical Field

The invention relates to a preparation method of a p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent.

Background

The p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent is bifunctional modified silicone oil. The modified silicone oil has new characteristics on the basis of keeping the characteristics of the dimethyl silicone oil, has the advantages of good heat resistance, oxidation resistance, lubricity, good compatibility with organic matters and the like, and is widely applied to the fields of metal die casting demoulding, plastic demoulding, defoaming agents and the like. When the release agent is used as a release agent, the release agent does not generate chemical reaction with a finished product, is adhered to a mould without being transferred to a processed product, and does not interfere with the painting or secondary processing of the finished product.

Disclosure of Invention

In order to overcome the defects of the prior art, the invention provides a preparation method of a p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent, which has the advantages of lower raw material cost, higher reaction efficiency, no gel generation and better finished product quality; strong acid and strong alkali are not needed, post-treatment such as water washing, neutralization and the like is not needed, and reaction steps and time are saved.

In order to solve the technical problems, the invention provides the technical scheme that:

a preparation method of a p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent comprises the steps of putting hydrogen-containing silicone oil into a reaction kettle, heating to 80-90 ℃ under stirring, dropwise adding a mixture of p-methylstyrene and a platinum catalyst, controlling the dropwise adding time to be 40-120 min, reacting at 80-90 ℃ for 3-6 h after the dropwise adding is finished, heating to 100-120 ℃, dropwise adding a mixture of 1-octene and a platinum catalyst, controlling the dropwise adding time to be 40-120 min, reacting at 100-120 ℃ for 3-6 h after the dropwise adding is finished, cooling to room temperature, carrying out vacuum reduced pressure distillation on the obtained product, and removing low boiling points to obtain the p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent.

Further, the platinum catalyst is Karstedt catalyst, the mass concentration of Pt is 2%, and the input amount is 1-10 ppm of the addition raw material; the raw material adopts p-methylstyrene with the purity of 99 to 99.9 percent; 1-octene with a purity of 99-99.9%; the hydrogen content of the hydrogen-containing silicone oil is 0.4-1.6 wt%; the viscosity of the hydrogen-containing silicone oil is 90-170 mpa.s; the molar ratio of the hydrogen-containing silicone oil to the p-methylstyrene is 1:0.5 to 0.6; the molar ratio of the hydrogen-containing silicone oil to the 1-octene is 1: 0.4-0.5; the vacuum degree of the reduced pressure distillation is-0.0998 to-0.1 Mpa; the reduced pressure distillation temperature is 140-180 ℃.

Preferably, the amount of the platinum catalyst to be charged is 5ppm based on the addition raw material.

Still further, the hydrogen content of the hydrogen-containing silicone oil is 0.5 wt%, the viscosity of the hydrogen-containing silicone oil is 120mpa.s, the molar ratio of the hydrogen-containing silicone oil to p-methylstyrene is 1:0.6, the molar ratio of the hydrogen-containing silicone oil to 1-octene is 1:0.5, the vacuum degree of reduced pressure distillation is-0.1 Mpa, and the temperature of reduced pressure distillation is 150 ℃.

According to the invention, the p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent is characterized by nuclear magnetic resonance and infrared spectroscopy, and the result shows that the p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent prepared by the preparation method has a single structure and high purity.

Compared with the prior art, the invention has the beneficial effects that: the raw material cost is low, the Karstedt catalyst with high efficiency is used, the reaction efficiency is higher, no gel is generated, and the quality of a finished product is better; strong acid and strong alkali are not needed, post-treatment such as water washing, neutralization and the like is not needed, and reaction steps and time are saved.

Drawings

FIG. 1 is a nuclear magnetic hydrogen spectrum of modified silicone oil prepared by the method for preparing a p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent of example 1.

FIG. 2 is an infrared spectrum of a modified silicone oil prepared by the method for preparing a p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent of example 1.

Detailed Description

The invention is further described below with reference to the accompanying drawings.