A kind of fluorosilicone copolymer and preparation method thereof

A technology of fluorosilicon copolymer and methyltrifluoropropylcyclotrisiloxane, which is 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, broad application prospects, and the effect of expanding the scope of application

Active Publication Date: 2017-01-04
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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  • A kind of fluorosilicone copolymer and preparation method thereof
  • A kind of fluorosilicone copolymer and preparation method thereof
  • A kind of fluorosilicone copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] To prepare a copolyfluorosilicone rubber with a molar ratio of methylphenylsiloxane chain links of 3.7%:

[0041] (1) 4.41g methyl phenyl cyclosiloxane, 94.32 g methyl trifluoropropyl cyclotrisiloxane, and 1.27 g tetramethyl tetravinyl cyclosiloxane (D 4 Vi ) Was added to the reactor one by one, and kept at a constant temperature of 60°C for 30 minutes under vacuum to remove moisture and CO 2 Impurities

[0042] (2) Raise the temperature to 130°C, add 0.01% of the total mass of the reactants (denoted by alkali metal hydroxide) sodium siliconate and 0.01% mass fraction of tributyl phosphate. Under normal pressure, N 2 In the atmosphere, under the action of mechanical stirring, after the system starts to wrap around the shaft, stop stirring and continue the equilibrium reaction for 2.5h;

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

Embodiment 2

[0047] To prepare a copolyfluorosilicone rubber with a molar ratio of methylphenylsiloxane chain links of 7.2%:

[0048] By changing the ratio of methyl phenyl siloxane ring body and methyl trifluoropropyl siloxane ring body, copolymerized fluorosilicone rubber with different molar ratios of methyl phenyl siloxane chain links can be prepared.

[0049] In this embodiment, a copolyfluorosilicone rubber with a molar ratio of methyl phenylsiloxane chain links of 7.2% was selected for the preparation. The quality of raw materials required to prepare 100g of copolyfluorosilicone rubber is given in Table 1 below.

[0050] Table 1 The quality of raw materials required to prepare 100g of methylphenylsiloxane chain link molar ratio of 7.2% copolyfluorosilicone rubber

[0051]

[0052] The preparation process is to keep the temperature at 60℃ for 30min under vacuum condition, after removing the water, N 2 Replace three times to remove residual O 2 , CO 2 . After the water is removed, add 0.01% ...

Embodiment 3

[0055] A copolyfluorosilicone rubber with a molar ratio of methyl phenylsiloxane segments of 9.6% was prepared.

[0056] Through this embodiment, a copolyfluorosilicone rubber with a molar ratio of methyl phenyl siloxane chain links of 9.6% was selected to prepare. Table 2 below shows the quality of raw materials required to prepare 100 g of copolyfluorosilicone rubber.

[0057] Table 2 The quality of raw materials needed to prepare 100g of methylphenylsiloxane chain link molar ratio of 9.6% copolyfluorosilicone rubber

[0058]

[0059] The preparation process is to keep the temperature at 60℃ for 30min under vacuum condition, after removing the water, N 2 Replace three times to remove residual O 2 , CO 2 . After the moisture is removed, at 130°C, 0.01% of the total mass of the reactants and 0.01% of the total mass of the reactants are added with tributyl phosphate. In this example, NaOH is used (the mass fraction is prepared as 2% sodium siloxanol alkali gel 0.5g), under the actio...

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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 fluorosilicon copolymer and a preparation method thereof, in particular to a copolymer of methylphenylcyclosiloxane and methyltrifluoropropylcyclosiloxane (that is, containing phenylsiloxane chain link Copolyfluorosilicone rubber) and its preparation method belong to the field of organic silicon synthetic chemistry. Background technique [0002] Fluorosilicone rubber is based on -Si-O- chain links as the main chain, with trifluoropropyl (CF 3 CH 2 CH 2 -) and methyl (CH 3 -) High molecular polymers. Due to the relatively large electronegativity of fluorine atoms, it has a great electron-attracting effect, which reduces the swelling degree of fluorosilicone rubber to fuel oil and organic solvents, and has good oil resistance and solvent resistance. For the preparation of fluorosilicone rubber with larger molecular weight, Guangdong Xinli Special Rubber Products Co., Ltd. discloses in the patent CN101177486 "The Polymerization Meth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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