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Fluorosiloxane copolymer and preparing method thereof

A technology of fluorosilicon copolymer and methyl trifluoropropyl cyclotrisiloxane, applied in the field of organosilicon synthesis chemistry, can solve the problems of insufficient temperature resistance and solvent resistance, and achieve good high temperature resistance and low temperature resistance. performance, improved stability, effect of high content of methyltrifluoropropylsiloxane segments

Active Publication Date: 2014-08-27
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problems of insufficient temperature resistance and solvent resistance of existing fluorosilicone rubber, the object of the present invention is to provide a Trisiloxane, a fluorosilicon copolymer containing methylphenylsiloxane or diphenylsiloxane chains and methyltrifluoropropylsiloxane chains prepared in the presence of an anionic initiator , the content of methyltrifluoropropylsiloxane chain in the fluorosilicone copolymer is high, and the polymer has excellent solvent resistance; at the same time, the introduction of methylphenyl chain improves the temperature resistance of the polymer

Method used

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  • Fluorosiloxane copolymer and preparing method thereof
  • Fluorosiloxane copolymer and preparing method thereof
  • Fluorosiloxane copolymer and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of copolymerized fluorosilicone rubber with a molar ratio of methylphenylsiloxane chains of 3.7%:

[0041] (1) 4.41g methylphenylcyclosiloxane, 94.32g methyltrifluoropropylcyclotrisiloxane, and 1.27g tetramethyltetravinylcyclosiloxane (D 4 Vi ) into the reactor in turn, and keep the temperature at 60°C for 30min under vacuum conditions to remove moisture and CO 2 impurities;

[0042] (2) Warming up to 130°C, adding 0.01% (in terms of alkali metal hydroxide) sodium silanolate and 0.01% mass fraction of tributyl phosphate, accounting for the total mass of the reactants, under normal pressure conditions, N 2 In the atmosphere, under the action of mechanical stirring, after the reaction until the system begins to wrap around the shaft, stop stirring and continue the equilibrium reaction for 2.5h;

[0043] (3) Add 0.1 g of glacial acetic acid, mix evenly on a mixer, heat up to 160°C to remove small molecules in a vacuum, cool down and discharge. The raw rubbe...

Embodiment 2

[0047] Preparation of copolymerized fluorosilicone rubber with a methylphenylsiloxane chain segment molar ratio of 7.2%:

[0048] Copolymerized fluorosilicone rubbers with different molar ratios of methylphenylsiloxane chains can be prepared by changing the proportion of methylphenylsiloxane ring body and methyltrifluoropropylsiloxane ring body.

[0049] This embodiment selects the preparation of copolyfluorosilicone rubber with the molar ratio of methylphenylsiloxane chains being 7.2%. Table 1 below shows the mass of raw materials required to prepare 100 g of copolymerized fluorosilicone rubber.

[0050] Table 1 The mass of raw materials required to prepare 100g of methylphenylsiloxane chain segment molar ratio of 7.2% copolymerized fluorosilicone rubber

[0051]

[0052] The preparation process is to keep the temperature at 60 ° C for 30 min under vacuum conditions, and after removing moisture, N 2 Replaced three times to remove residual O 2 , CO 2 . After removing t...

Embodiment 3

[0055] A copolymerized fluorosilicone rubber with a molar ratio of methylphenylsiloxane chains of 9.6% was prepared.

[0056] According to this embodiment, the preparation of copolyfluorosilicone rubber with the molar ratio of methylphenylsiloxane chains being 9.6% is selected. Table 2 below shows the mass of raw materials required to prepare 100 g of copolyfluorosilicone rubber.

[0057] Table 2 The mass of raw materials required to prepare 100g of methylphenylsiloxane chain segment molar ratio of 9.6% copolymerized fluorosilicone rubber

[0058]

[0059] The preparation process is to keep the temperature at 60 ° C for 30 min under vacuum conditions, and after removing moisture, N 2 Replaced three times to remove residual O 2 , CO 2 . After moisture is removed, add the tributyl phosphate that accounts for the alkali metal hydroxide of reactant gross mass 0.01% and reactant gross mass 0.01% at 130 DEG C, select NaOH for use in this example (it is prepared into mass frac...

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Abstract

The invention discloses a fluorosiloxane copolymer and a preparing method thereof. The method includes the following steps that 0.1-50 parts of methylphenyldichlorosilane or diphenyl cyclosiloxane, 45-99.8 parts of 1,3,5-tris(3,3,3-trifluoropropyl)methylcyclotrisiloxane and 0.1-5 parts of polymethylphenylsiloxane are sequentially added into a reactor and dried under the heating condition of 60- 90 DEG C, and water and CO2 in a reactant are removed, wherein the total number of the methylphenyldichlorosilane or diphenyl cyclosiloxane, the 1,3,5-tris(3,3,3-trifluoropropyl)methylcyclotrisiloxane and the polymethylphenylsiloxane are 100 parts; an initiator and an accelerant are added, the use quantity of the initiator accounts for 0.001-1% the mass of the reactant, the use quantity of the accelerant accounts for 0.01-1% the mass of the reactant, at the temperature of 90-200 EDG C, preferentially 130-150 DEG C, stirring reaction is carried out until a shaft is wrapped in a N2 atmosphere under a normal-pressure condition, balanced reaction continues being carried out for 2-3 h, and raw rubber is manufactured; an acidoid neutralization initiator is added into the raw rubber manufactured in the step (2), extraction or high-vacuum processing is carried out on the neutralized raw rubber, and low-molecular matter is removed. Heat resistance of the fluorosiloxane copolymer is improved by about 80 DEG C compared with fluorosiloxane raw rubber with 100% of methyl trifluoropropyl.

Description

technical field [0001] The invention relates to a fluorosilicone copolymer and a preparation method thereof, in particular to a copolymer of methylphenylcyclosiloxane and methyltrifluoropropylcyclosiloxane (that is, containing phenylsiloxane chain link Copolymerized fluorosilicone rubber) and a preparation method thereof belong to the field of organosilicon synthesis chemistry. Background technique [0002] Fluorosilicone rubber is based on -Si-O-links as the main chain, with trifluoropropyl (CF) on the silicon atom 3 CH 2 CH 2 -) and methyl (CH 3 -) polymers. Due to the high electronegativity of fluorine atoms, it has a great electron-withdrawing effect, which makes fluorosilicone rubber less swellable to fuel oil and organic solvents, and has good oil resistance and solvent resistance. For the preparation of fluorosilicone rubber with relatively large molecular weight, Guangdong Xinli Special Rubber Products Co., Ltd. disclosed a kind of fluorosilicone structural unit...

Claims

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Application Information

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IPC IPC(8): C08G77/24C08G77/20C08G77/34
Inventor 周传健王帅王云凤龙腾马琳
Owner SHANDONG UNIV
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