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Preparation method of p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent

A technology of p-methylstyrene and hydrogen-containing silicon is applied in the preparation field of p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil mold release agent, and can solve the problem of tetramethylhydrogencyclotetrasiloxane Expensive, cumbersome steps, high cost problems, to achieve the effect of saving reaction steps and time, low cost of raw materials, and good quality of finished products

Pending Publication Date: 2020-08-18
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. The raw material tetramethylhydrocyclotetrasiloxane is relatively expensive. Although the product can effectively control the molecular weight and high viscosity, and has good performance, the cost is high in large-scale production and sales, and it cannot form a price advantage
[0006] 2. In the purification process of the product, post-treatments such as washing with water and neutralization are required. The steps are cumbersome, and the residual active group Si-H is easy to dehydrogenate and cross-link under the action of the catalyst due to incomplete reaction, forming a gel, resulting in the product Yield and quality decline

Method used

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  • Preparation method of p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent
  • Preparation method of p-methylstyrene/1-octene co-modified hydrogen-containing silicone oil release agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] refer to figure 1 and figure 2 , a preparation method of a p-methylstyrene / 1-octene co-modified hydrogen-containing silicone oil release agent, pour 640g of hydrogen-containing silicone oil into a 2000ml three-hole flask at room temperature, stir, heat up to 80°C, drop Add 190g of p-methylstyrene and 0.5ppm Karstedt catalyst, dropwise time is 60min, then maintain at 80°C for 3h, after heating up to 100°C, add dropwise 144g octene and 0.5ppm Karstedt catalyst, dropwise time is 60min, Then maintain at 100°C for 3h, and finally cool to room temperature, vacuumize to remove low boiling, vacuum degree -0.0998MPa, maximum temperature 140°C, time 1.5h, to obtain a qualified product.

[0020] Product indicators:

[0021] Viscosity: 900~1400mpa.s;

[0022] Refractive index: 1.4500~1.4650;

[0023] Volatile content: 0.1~1%.

Embodiment 2

[0025] Pour 640g of hydrogen-containing silicone oil into a 2000ml three-hole flask at room temperature, stir, and after raising the temperature to 90°C, add 227g of p-methylstyrene and 5ppm Karstedt catalyst dropwise for 60min, and then maintain at 90°C for 6h. After the temperature was raised to 120°C, 180g of octene and 5ppm Karstedt catalyst were added dropwise for 60min, and then maintained at 120°C for 6h. Finally, cool to room temperature, vacuumize to remove low boiling, vacuum degree -0.1MPa, maximum temperature 180°C, time 1.5h, and obtain qualified product.

[0026] Product indicators:

[0027] Viscosity: 900~1400mpa.s;

[0028] Refractive index: 1.4500~1.4650;

[0029] Volatile content: 0.1~1%.

Embodiment 3

[0031] Pour 640g of hydrogen-containing silicone oil into a 2000ml three-hole flask at room temperature, stir, and after raising the temperature to 84°C, add 200g of p-methylstyrene and 2ppm Karstedt catalyst dropwise for 60min, and then maintain at 84°C for 4h. After the temperature was raised to 110°C, 150g of octene and 2ppm Karstedt catalyst were added dropwise for 60 minutes, and then maintained at 110°C for 4 hours. Finally, cool to room temperature, evacuate to remove low boiling, the vacuum degree is -0.099MPa, the highest temperature is 150°C, and the time is 1.5h, and a qualified product is obtained.

[0032] Product indicators:

[0033] Viscosity: 900~1400mpa.s;

[0034] Refractive index: 1.4500~1.4650;

[0035] Volatile content: 0.1~1%.

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Abstract

The invention discloses a preparation method of a p-methyl styrene / 1-octene co-modified hydrogen-containing silicone oil release agent. Putting the hydrogen-containing silicone oil into a reaction kettle; raising the temperature to 80-90 DEG C while stirring; dropwise adding a mixture of p-methyl styrene and a platinum catalyst; and after dropwise adding is finished, reacting for 3-6 hours at 80-90 DEG C, heating the reactants to 100-120 DEG C, dropwise adding a mixture of 1-octene and a platinum catalyst, reacting for 3-6 hours at 100-120 DEG C, cooling the reaction product to room temperature, vacuumizing the system and removing low boiling point to obtain the p-methyl styrene / 1-octene co-modified hydrogen-containing silicone oil release agent. The release agent prepared by the process has the advantages of simple process, easiness in operation, high efficiency, good quality and the like.

Description

technical field [0001] The invention relates to a preparation method of p-methylstyrene / 1-octene co-modified hydrogen-containing silicone oil release agent. Background technique [0002] P-methylstyrene / 1-octene co-modified hydrogen-containing silicone oil release agent is a kind of bifunctional modified silicone oil. On the basis of retaining the characteristics of dimethyl silicone oil, this modified silicone oil has added new characteristics. It has the advantages of good heat resistance, oxidation resistance, lubricity and good compatibility with organic substances, and is widely used. It is used in the fields of metal die-casting demoulding, plastic demoulding and defoaming agent. When it is used as a release agent, it does not chemically react with the finished product, and it adheres to the mold without transferring to the processed part, and does not hinder the painting or secondary processing of the finished product. [0003] The existing technical route: using te...

Claims

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Application Information

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IPC IPC(8): C08G77/38C08G77/08B29C33/64C08G77/12
CPCC08G77/38C08G77/08B29C33/64C08G77/12
Inventor 欧阳密秦超胡旭明陈璐张诚
Owner ZHEJIANG UNIV OF TECH
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