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Ethylene-alpha olefin-polyfluorosiloxane ternary graft copolymer and preparation method thereof

A ternary grafting, alpha olefin technology, applied in the field of graft copolymers, can solve the problems of reducing the strong polarity of siloxane, decreasing the content of polysiloxane, increasing the content of alkyl groups, etc. The effect of tensile strength and elongation at break, optimal mechanical properties

Active Publication Date: 2020-07-03
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The preparation method uses dihydrogen-terminated siloxane as the initial raw material, respectively connects long-chain alkyl groups to both ends of the dihydrogen-terminated siloxane through two hydrosilylation reactions, and adds double bond-terminated alkane The content of the alkyl group in the base siloxane is used to reduce the strong polarity of the siloxane, thereby improving the poisoning effect of the strong polarity of the polysiloxane on the transition metal catalysts commonly used in olefin polymerization. At the same time, due to the high alkyl content , also increases the compatibility with carbon-based materials; but because the content of the alkyl group is greatly increased, the content of polysiloxane is bound to be greatly reduced. In order to ensure that the polysiloxane in the olefin-polysiloxane random copolymer The high content of alkane can only be solved by greatly increasing the grafting density of polysiloxane branched chains, but this is at the expense of the molecular weight and mechanical properties of the product alkylsiloxane-olefin random copolymer

Method used

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  • Ethylene-alpha olefin-polyfluorosiloxane ternary graft copolymer and preparation method thereof
  • Ethylene-alpha olefin-polyfluorosiloxane ternary graft copolymer and preparation method thereof
  • Ethylene-alpha olefin-polyfluorosiloxane ternary graft copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] (1) Vacuumize a 50mL flask equipped with a magnetic stirrer and fill it with nitrogen three times to fill it with an inert atmosphere, add 27.5g (0.25mol) of 1,7-octadiene and 0.3g (50ppm) of Karstedt catalyst solution (the mass concentration of platinum is 2%), the temperature is controlled at 20°C and the reaction is stirred for 2h. Then slowly add 4.7g (0.05mol) dimethylchlorosilane, and continue to stir the reaction for 24h. The obtained product was distilled under reduced pressure to remove unreacted excess 1,7-octadiene, and then rectified to obtain 7.6 g of a colorless oily liquid product, namely 7-octenyldimethylchlorosilane. The yield was 74%.

[0064] (2) A 100mL flask equipped with a magnetic stirrer was vacuum-filled with nitrogen for three times, so that it was filled with an inert atmosphere, and 10.5g (0.0225mol) of trifluoropropylmethylcyclotrisiloxane and 10mL of tetrahydrofuran were added. Then 9 mL of n-butyllithium / hexane solution (2.5M) was added ...

Embodiment 2

[0072] The preparation process was the same as in Example 1, except that the amount of polyfluorosiloxane macromonomer added in step (3) was 5.6 g (80 mmol / L), and 1.6 g of the product was obtained. It is confirmed by hydrogen nuclear magnetic spectrum that it is ethylene-octene-polyfluorosiloxane ternary graft copolymer. According to nuclear magnetic analysis, it can be seen that the mass content of 1-octene in the copolymer is 6.2%, and the mass content of polyfluorosiloxane macromonomer is 20.7%. The copolymer had a weight average molecular weight of 25.9 kg / mol as determined by GPC analysis.

Embodiment 3

[0074] (1) Repeat step (1) in Example 1.

[0075] (2) A 100mL flask equipped with a magnetic stirrer was vacuum-filled three times with nitrogen to make it filled with an inert atmosphere, and 31.5g (0.0675mol) of trifluoropropylmethylcyclotrisiloxane and 10mL of tetrahydrofuran were added. Then 9 mL of n-butyllithium / hexane solution (2.5M) was added to initiate ring-opening polymerization. The temperature was controlled at 0°C and the reaction was stirred for 2 hours, and then 4.6 g of 7-octenyldimethylchlorosilane prepared in step (1) was added, and the capping time was 24 hours. After washing with deionized water and n-hexane three times, drying with anhydrous magnesium sulfate and rotary evaporation to remove the solvent, 33.3 g of a colorless liquid product was obtained, which was the octenyl-terminated polyfluorosiloxane macromonomer. The yield is 90%. It can be seen from the characterization of the hydrogen NMR spectrum that in the polyfluorosiloxane macromonomer, a=4...

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Abstract

The invention discloses an ethylene-alpha olefin-polyfluorosiloxane ternary graft copolymer, the structural general formula of the ethylene-alpha olefin-polyfluorosiloxane ternary graft copolymer is shown as the following formula (I-1) or (I-2), in the formula, R1 is selected from C1-C8 fluorine-containing alkyl, R2 is selected from C1-C8 alkyl, x is a natural number ranging from 100 to 10000, y is a natural number ranging from 10 to 1000, z is a natural number ranging from 1 to 100, a is a natural number ranging from 2 to 8, b is a natural number ranging from 3 to 90, and c is a natural number ranging from 2 to 8. The preparation method comprises three steps of hydrosilylation, anionic ring-opening polymerization and coordination copolymerization. According to the preparation method, thetoxic action of strong polarity of polysiloxane on a transition metal catalyst commonly used in olefin polymerization is avoided under the condition of high polysiloxane content, and the polysiloxanecontent and the weight-average molecular weight in the prepared ethylene-alpha olefin-polyfluorosiloxane ternary graft copolymer are adjustable in a large range.

Description

technical field [0001] The invention relates to the technical field of graft copolymers, in particular to an ethylene-alpha olefin-polyfluorosiloxane ternary graft copolymer and a preparation method thereof. Background technique [0002] As the most widely used general-purpose plastic, polyolefin has the characteristics of abundant raw material sources, low price, and excellent mechanical properties. It has been widely used in human daily production and life, national defense and military affairs. However, its wear resistance and environmental stress cracking resistance are not good, and the processing fluidity of some grades is not good. With the development of society, the lack of functionalization of traditional polyolefins has become more and more obvious, making it difficult to meet increasingly sophisticated requirements. [0003] The polysiloxane segment is soft, and has extremely low surface tension, good chemical stability, excellent high and low temperature resist...

Claims

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Application Information

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IPC IPC(8): C08F283/12C08F210/16C08F210/14C08G77/24C08G77/20C08G77/06
CPCC08F283/124C08G77/06C08G77/20C08G77/24C08F210/16C08F210/14C08F2500/01
Inventor 范宏田保政蔡育铨
Owner ZHEJIANG UNIV