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Method for preparing fluorosilicone rubbers by using screw extruder

A technology of screw extruder and fluorosilicone raw rubber is applied in the field of preparing fluorosilicone raw rubber, which can solve the problems of difficulty in ensuring product quality, and achieve the effects of stable product quality, good mass transfer and heat transfer effect, and strong continuity.

Active Publication Date: 2012-07-04
ZHEJIANG HUANXIN FLUORO MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the polymerization, the neutralizing agent cannot be used to neutralize the polymerization catalyst silanol base. After the polymerization time is up, it is difficult to quickly cool down the polymerization kettle to terminate the reaction for high-viscosity materials. During the process of devolatilization, the polymerization balance of materials will also change at the same time, and it is difficult to ensure the quality of products between batches

Method used

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  • Method for preparing fluorosilicone rubbers by using screw extruder
  • Method for preparing fluorosilicone rubbers by using screw extruder
  • Method for preparing fluorosilicone rubbers by using screw extruder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 50kg D to dehydration kettle 1 3 F, the purity is 99.5%, D 4 Vi90g, temperature 100℃, nitrogen flow rate 10 m1 / min, 30mmHg vacuum dehydration for 2 hours, then put into prepolymerization kettle 2, add 250g alkali silicon alkoxide catalyst, capping agent hexamethyldisiloxane 10g, dehydration kettle 1 the temperature is controlled at 100 o C. The prepolymerization temperature is controlled at 80°C. When the viscosity of the material gradually increases and the output power of the micro-agitator is 8W, the material is fed into the mixing section 4 of the screw extruder 3. ①Pass the catalytic accelerator DMF (N,N-dimethylformamide) into the mixing section 4, the flow rate is 0.02m1 / min, and the temperature is controlled at 100℃; ②The materials treated by ① enter the condensation section 5, condensation section The vacuum degree of 5 is 10mmHg, and the temperature is controlled at 130°C; ③The polymer treated by ② enters the neutralization section 6, and a carbon dioxide ga...

Embodiment 2

[0049] Add 50kg D to dehydration kettle 1 3 F, the purity is 99.5%, D 4 Vi90g, temperature 130℃, nitrogen flow rate 20 m1 / min, 50mmHg vacuum dehydration for 1 hour, then put it into pre-polymerization kettle 2, add 200g alkali silicon alkoxide catalyst, 15g blocking agent divinyltetramethyldisiloxane , The temperature in dehydration kettle 1 is controlled at 130 o C. The prepolymerization temperature is controlled at 100°C. When the viscosity of the material gradually increases and the output power of the micro-agitator is 8W, the material is fed into the mixing section 4 of the screw extruder 3. ①In the mixing section 4, use the micro metering pump 9 to pass the catalytic accelerator tetrahydrofuran with the flow rate of 0.05m1 / min and the temperature control at 120℃; ②The material treated by ① enters the condensation section 5, and the vacuum degree of the condensation section 5 is 15mmHg , The temperature is controlled at 140°C; ③The polymer treated by ② enters the neutraliza...

Embodiment 3

[0053] Add 50kg D to dehydration kettle 1 3 F, the purity is 99.5%, D 4 Vi90g, temperature 120℃, nitrogen flow rate 30 m1 / min, 60mmHg vacuum dehydration for 4 hours, then put it into pre-polymerization kettle 2, add 200g alkali silicon alkoxide catalyst, capping agent hydroxyfluorosilicone 25g, temperature control in dehydration kettle 1. At 115 o C. The prepolymerization temperature is controlled at 90°C and reacts at 100°C. When the viscosity of the material gradually increases and the output power of the micro agitator is 8W, the material is fed into the mixing section 4 of the screw extruder 3. ①Put the accelerator DMF into the mixing section 4, the flow rate is 0.1m1 / min, and the temperature is controlled at 130℃; ②The material treated by ① enters the condensation section 5, the vacuum degree of the condensation section 5 is 30mmHg, and the temperature is controlled at 160℃ ③Put the polymer treated by ② into the neutralization section 6, add organosilicon phosphate in the n...

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Abstract

The invention discloses a method for preparing fluorosilicone rubbers by using a screw extruder. The method comprises the following steps: (1) dehydration; (2) prepolymerization; and (3) feeding the prepolymer into the screw extruder, wherein the screw extruder has five sections, namely a mixing section, a condensation section, a neutralization section, a volatile matter-removing section and a cooling section, cooling the polymer to below 100 DEG C by the cooling section, and extruding to obtain the fluorosilicone rubbers. In the invention, the screw extruder is used as a reactor, so that the temperature can be controlled by sections, and the polymerization catalyst is used for neutralization, so that the polymerization balance can not change; and the mass transferring effect is good, the continuity is strong, the quality of the product is stable and is beneficial to the industrial production of rubbers.

Description

Technical field [0001] The invention relates to a method for preparing fluorosilicone raw rubber, in particular to a method for preparing fluorosilicone raw rubber by using a screw extruder. Background technique [0002] Fluorine-containing silicon polymer is a new type of special material developed for the needs of the aerospace and automotive industries. It has excellent resistance to high and low temperature, fuel oil, and solvent resistance. It is widely used in automobiles, aerospace, machinery and electronics, and petroleum Chemical, medical machinery and other fields. The main chain is a silica structure, and the side chain contains trifluoropropyl groups. In the process of synthesizing raw rubber, a small amount of vinyl siloxane chain links are introduced at the same time as the vulcanization point of rubber vulcanization. [0003] The preparation of fluorosilicone raw rubber is generally based on a tank reactor, but due to the too fast polymerization rate, the polymer m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/24C08G77/20C08G77/06C08G77/32B29C47/92B29C48/92
CPCB29C48/92B29C2948/92895
Inventor 方海滔应永安王志强吴志筐陈伟杨新华谢福钦李国杰倪一峰
Owner ZHEJIANG HUANXIN FLUORO MATERIAL