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Preparation method for heat-conducting methylphenyl silicone oil

A heat-conducting silicone oil, methyl phenyl technology, applied in the field of preparation of methyl phenyl heat-conducting silicone oil, can solve the problems of expensive graphene oxide, easy agglomeration of graphene oxide nanosheets, and difficulty in industrialization, etc., to achieve excellent heat resistance sexual effect

Active Publication Date: 2016-04-27
浙江乾晟科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, graphene oxide nanosheets are very easy to agglomerate, and graphene oxide is relatively expensive, making it difficult to realize industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Make 5g of lanthanum oxide into an ethanol suspension with a mass percent concentration of 1%, and after ultrasonication at 25°C for 0.5h, add 0.1wt% orthosilicate methyl ester and 0.5wt% deionized water in ethanol, Under stirring, react at 30°C for 24h. Then distill at a vacuum degree of 0.06 MPa to obtain surface-modified rare earth oxides.

[0024] (2) Add 3.0g of the surface-modified rare earth oxide obtained in (1) to 150g of D3, 50g of methylphenylcyclotrisiloxane, 1.62g of capping agent Me 3 SiOSiMe 3 and 3g of tetramethylammonium hydroxide silicon alkoxide, in-situ ring-opening polymerization at 80°C for 24h, and decomposing the catalyst at 140°C for 2h, and finally decompression at 200°C with a vacuum of 0.07MPa to remove low boilers to obtain Methylphenyl thermally conductive silicone oil 1 with a viscosity of 320mpa·s and excellent heat resistance.

[0025] The methyl phenyl thermally conductive silicone oil 1 obtained in Example 1 has basically no cha...

Embodiment 2

[0027] (1) Make 5g of neodymium oxide into an ethanol solution with a concentration of 10% by mass, and after ultrasonication at 45°C for 4 hours, add 1 wt% ethyl orthosilicate and 1 wt% deionized water under stirring. React at 60°C for 2h. Then distill at a vacuum degree of 0.09MPa to obtain surface-modified rare earth oxides.

[0028] (2) Add 4g of the surface-modified rare earth oxide obtained in (1) to 100g D4, 120g methyl phenyl mixed ring, 1.86g end-capping agent Me 2 ViSiOSiMe 2 In Vi and 3g of tetramethylammonium hydroxide silicon alkoxide, in-situ ring-opening polymerization was carried out at 100°C for 4h, and the catalyst was decomposed at 150°C for 1h, and finally the low boilers were removed under reduced pressure at 220°C with a vacuum degree of 0.08MPa. A methyl phenyl thermally conductive silicone oil 2 with a viscosity of 1500 mpa·s and excellent heat resistance was obtained.

[0029] The methyl phenyl thermally conductive silicone oil 2 obtained in Example...

Embodiment 3

[0031] (1) Mix 2g of neodymium oxide and 3g of lanthanum oxide into an isopropanol solution with a concentration of 5% by mass, and after ultrasonication at 70°C for 1 hour, add 3wt% methyltrimethoxysilane and 2wt% of isopropanol KH-570, 5wt% deionized water, reacted at 70°C for 0.5h under stirring. Then distill at a vacuum degree of 0.09 MPa to obtain a surface-modified rare earth oxide mixture.

[0032] (2) Add 5g of the surface-modified rare earth oxide mixture obtained in (1) to 100g of DMC, 350g of octaphenylcyclotetrasiloxane, 0.186g of capping agent Me 2 ViSiOSiMe 2 In Vi and 15g of tetramethylammonium hydroxide silicon alkoxide, in-situ ring-opening polymerization was carried out at 90°C for 18 hours, and the catalyst was decomposed at 130°C for 4 hours, and finally the low boilers were removed under reduced pressure at 180°C with a vacuum degree of 0.09MPa , to obtain methyl phenyl thermally conductive silicone oil 3 with a viscosity of 5800mpa·s and excellent heat ...

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Abstract

The invention relates to the technical field of organosilicon and discloses a preparation method for heat-conducting methylphenyl silicone oil to overcome the problem of heat resistance of silicone oil. The method comprises the following steps: adding rare earth oxide having undergone surface silane modification into phenylcyclosiloxane and dimethylcyclosiloxane monomers; carrying out in-situ ring-opening polymerization in the presence of a catalyst (CH3)4NOH silicon alkoxide and an end-capping reagent; decomposing the catalyst at 130 to 150 DEG C for 1 to 4 h; and then carrying out pressure reduction to remove low-boiling-point substances so as to obtain the heat-conducting methylphenyl silicone oil. The obtained methylphenyl silicone oil has silicone oil viscosity of 25 MPa.s to 12000 MPa.s and has excellent heat resistance.

Description

technical field [0001] The invention relates to the technical field of organosilicon, in particular to a method for preparing methylphenyl heat-conducting silicone oil. Background technique [0002] Heat transfer oil has very important uses in industry. With the advancement of science and technology, higher requirements are placed on the heat resistance of heat transfer oil. The use temperature of mineral oil type heat transfer oil is relatively low, but its high temperature thermal stability is poor. Synthetic heat transfer oils are mostly aromatic hydrocarbons, biphenyls or diphenyl ether compounds. Although their thermal conductivity and thermal stability are excellent, they have relatively large toxic and side effects. [0003] Silicone oil is an organosiloxane polymer with Si-O-Si main chain structure and various substituents in side chains, and has the properties of both organic and inorganic compounds. For example, simethicone hardly oxidizes below 150°C, and its v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/08C08G77/04C08K9/06C08K3/22
Inventor 华西林杨雄发蒋剑雄罗蒙贤邬继荣
Owner 浙江乾晟科技有限公司
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