Preparation method of fluorosilicone rubber with controllable molecular weight

A technology of fluorosilicone raw rubber and molecular weight, which is applied in the field of preparation of molecular weight controllable fluorosilicone raw rubber, which can solve the problems of wide molecular weight distribution, affecting the quality and performance of fluorosilicone raw rubber, and large amount of catalyst.

Active Publication Date: 2013-04-03
新元化学(山东)股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In short, the existing fluorosilicone raw rubber preparation process uses a large amount of catalyst, the polymerization speed and raw rubber molecular weight are not easy to control, and the molecular weight distribution is wide, which directly affects the quality and performance of fluorosilicone raw rubber.

Method used

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  • Preparation method of fluorosilicone rubber with controllable molecular weight
  • Preparation method of fluorosilicone rubber with controllable molecular weight
  • Preparation method of fluorosilicone rubber with controllable molecular weight

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] According to the above formula, calculate the feeding amount, and prepare fluorosilicone raw rubber with an average molecular weight of 800,000 and a vinyl molar content of 0.04%.

[0040] Add 100KgD to the reactor 3 F and 22.1gD 3 Vi , heated to 55~60°C, dehydrated under 130Pa pressure for 1.5h, added 46.2g sodium silanolate catalyst (3.25% sodium hydroxide content, accounting for 0.0015% of the total mass of raw materials) and 66.9g 1,1,1,3, 5,7,9,9,9-nonamethyl-3,5,7-tris(3,3,3-trifluoropropyl)pentasiloxane, with high purity N 2 Replace the air in the reactor, raise the temperature to 90°C, start the reaction, raise the temperature to 130°C at a rate of 1.5°C / min, maintain the temperature for 0.5h, reduce the system pressure to 26Pa for 1.5h, add 51.8g of fluorine-containing silicon base Phosphoric acid ester (phosphoric acid content 3.55%), neutralized under normal pressure for 2 hours, finally raised the temperature to 180~200°C, kept it under ultimate vacuum fo...

Embodiment 2

[0042] Preparation of fluorosilicone raw rubber with an average molecular weight of 600,000 and a vinyl content of 0.1%

[0043] Add 100KgD to the reactor 3 F and 55.3gD 3 Vi , heated to 55~60°C, dehydrated under 130Pa pressure for 1.5h, added 61.6g sodium silanolate catalyst (3.25% sodium hydroxide content, accounting for 0.002% of the total mass of raw materials) and 102.6g 1,1,3,5, 7,9,9-Heptamethyl-1,3,5,7,9-penta(3,3,3-trifluoropropyl)pentasiloxane, with high purity N 2 Replace the air in the reactor, raise the temperature to 90°C, start the reaction, program the temperature to 130°C at a rate of 2°C / min, maintain the temperature for 0.5h, reduce the system pressure to 26Pa for 1.5h, add 69.2g of fluorine-containing silicon Phosphoric acid ester (phosphoric acid content: 3.55%), neutralized under normal pressure for 2 hours, and finally heated to 180~200°C, maintained for 2 hours under ultimate vacuum, removed low boiling matter, cooled to obtain raw rubber. Eight par...

Embodiment 3

[0045] Preparation of fluorosilicone raw rubber with an average molecular weight of 1 million and a vinyl content of 0.08%

[0046] Add 100KgD to the reactor 3 F and 44.2gD 3 Vi , heated to 55~60°C, dehydrated under 130Pa pressure for 1.5h, added 30.8g sodium silanolate catalyst (3.25% sodium hydroxide content, accounting for 0.001% of the total mass of raw materials) and 57.2g 1,1,3,5, 7,9,9-Heptamethyl-1,9-divinyl-3,5,7-tris(3,3,3-trifluoropropyl)pentasiloxane, with high purity N 2 Replace the air in the reactor, raise the temperature to 90°C, start the reaction, program the temperature to 130°C at a rate of 1°C / min, maintain the temperature for 0.5h, reduce the system pressure to 26Pa for 1.5h, add 34.5g of fluorine-containing silicon Phosphoric acid ester (phosphoric acid content: 3.55%), neutralized under normal pressure for 2 hours, and finally heated to 180~200°C, maintained for 2 hours under ultimate vacuum, removed low boiling matter, cooled to obtain raw rubber. ...

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Abstract

The invention relates to a preparation method of fluorosilicone rubber with the controllable molecular weight. According to the method, catalyst consumption is reduced, and the molecular weight is adjusted by a special end capping reagent, so that the molecular weight of the prepared fluorosilicone rubber is controllable, and the distribution is narrow. The method comprises the steps of (1) adding D3F and methyl-vinyl-cyclosiloxane to a reactor for dehydration, (2) adding a silanolate catalyst and the end capping reagent with the mass accounting for 0.0005-0.003% of the mass of D3F to the reactor, heating and starting reaction, (3) conducting temperature programming to about 130 DEG C after reaction starting, and polymerizing for 0.5h at a normal pressure, (4) dropping the pressure in the reactor to 26Pa-26000Pa, and reacting for 0.5h-3h, (5) adding fluorosilicone-base phosphate to neutralize, and (6) rising temperature to 180-200 DEG C, removing low-boiling-point substances at vacuum, cooling, and obtaining the rubber.

Description

technical field [0001] The invention relates to a method for preparing fluorosilicone raw rubber with controllable molecular weight, in particular to a method for preparing fluorosilicone raw rubber used in the automotive industry and aerospace fields. technical background [0002] Fluorosilicone rubber is a special synthetic rubber material whose main chain is a silicon-oxygen structure and the side chain is a fluorine-containing alkyl structure. It combines the high and low temperature resistance of silicone rubber with the advantages of oil resistance and solvent resistance of fluororubber, and can be widely used in important fields such as automobiles, aircrafts, petrochemicals, machinery, electronics, etc. Fluorosilicone raw rubber is used to produce fluorosilicone rubber main raw material. [0003] At present, fluorosilicone raw rubber mainly passes through D 3 F is prepared by anionic ring-opening polymerization under the action of a catalyst. Used catalyzer is gen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/395C08G77/24
Inventor 张翚鹰张殿松田志钢于鹏飞解承钢王爱卿
Owner 新元化学(山东)股份有限公司
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