Preparation method of unilateral reaction type functional group terminated silicone oil

A reactive, functional group technology, applied in the field of preparation of unilateral reactive functional group-terminated silicone oil, can solve the problems of long equilibrium reaction time, affecting the use effect, and complicated solvent recovery.

Pending Publication Date: 2022-08-05
希立科高新材料科技(苏州)有限公司
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  • Abstract
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Problems solved by technology

[0004] The invention discloses a preparation method of unilaterally reactive functional group-terminated silicone oil, aiming to solve the problem that the grafting rate of the current type of products is not high due to technological reasons, and contains double-terminal reactive functional group-terminated silicone oil and Inert group-capped silicone oil leads to low product quality and seriously affects the use effect. In order to obtain high-quality products, it is necessary to use butyllithium as a ring-opening reagent and inert group-capped agent. The reaction requires low temperature and a long equilibrium reaction time. Handle complex, complex technical issues with solvent recovery

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  • Preparation method of unilateral reaction type functional group terminated silicone oil
  • Preparation method of unilateral reaction type functional group terminated silicone oil
  • Preparation method of unilateral reaction type functional group terminated silicone oil

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Embodiment Construction

[0029] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments.

[0030] refer to figure 1 , a preparation method of unilateral reactive functional group-terminated silicone oil, which specifically comprises the following steps:

[0031] S1: Hexamethylcyclotrisiloxane (D3) 884g dissolved in 800g THF under nitrogen protection, set the flow rate of quantitative pump B to 28.06g / min, butyllithium 400mL nitrogen protection, set the flow rate of quantitative pump A to 4.53g / min, At the same time, turn on the two pumps A and B to pump the material into the premixer and then enter the microchannel reactor, set the reaction temperature to 0-5 degrees Celsius, enter the reactor B through the quantitative pump C, a...

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Abstract

The invention discloses a preparation method of unilateral reaction type functional group end-capped silicone oil, which specifically comprises the following steps: S1, dissolving hexamethylcyclotrisiloxane in THF (tetrahydrofuran) under the protection of nitrogen, setting the flow rate of a metering pump B to be 28.06 g / min, setting the flow rate of a metering pump A to be 4.53 g / min under the protection of 400mL of butyl lithium and nitrogen, simultaneously starting the pumps A and B to pump materials into a premixer and then enter a microchannel reactor, the reaction temperature is set to be 0-5 DEG C, and the mixture enters the reactor through a metering pump C; the preparation method of the unilateral reaction type functional group end-capped silicone oil disclosed by the invention comprises the following steps: carrying out ring-opening polymerization reaction on butyl lithium and hexamethylcyclotrisiloxane cations by using a microchannel reactor, and then reacting with monochlorosilane to generate single-end hydrogen-containing or single-end functional group end-capped silicone oil. The equilibrium reaction time is shortened, the molecular weight distribution width of the silicone oil is reduced, and the high-quality monoreactive functional group terminated silicone oil is obtained.

Description

technical field [0001] The invention relates to the technical field of silicone oil preparation, in particular to a preparation method of a unilateral reactive functional group-terminated silicone oil. Background technique [0002] The single-end reactive functional group-terminated silicone oil has good powder dispersibility, hydrophobicity, antifouling, and non-adhesion. Heat resistance, wear resistance, biocompatibility, good oxygen permeability. Widely used in medical, electronic, biological and other special materials. [0003] At present, due to technological reasons, the grafting rate of these products is not high, and they contain double-end reactive functional group-terminated silicone oil and inert group-terminated silicone oil, which leads to low product quality and seriously affects the use effect. In order to obtain high-quality products, it is necessary to use Butyllithium is used as a ring-opening reagent and an inert group end-capping agent, and the reactio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/10C08G77/08C08G77/12C08G77/14C08G77/20C08G77/34C08G77/38C08G77/388
CPCC08G77/10C08G77/08C08G77/12C08G77/14C08G77/20C08G77/34C08G77/38C08G77/388
Inventor 李杰张建平余敏
Owner 希立科高新材料科技(苏州)有限公司
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