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A method for cracking polysiloxane oligomers containing long-chain fluoroalkyl groups

A chain fluoroalkyl and polysiloxane technology, which is applied in the field of polysiloxane oligomer cracking devices, can solve the problems of long duration of rectification process, reduced product yield, high boiling point of cyclic compounds, etc., and achieves improvement Effect of mass transfer and heat transfer, improvement of production efficiency, effect of shortening the rectification process

Active Publication Date: 2019-01-22
宁夏胜佳环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, due to the high boiling point of the above-mentioned cyclic compounds, it is not easy to evaporate, and it is also slow to evaporate even under high vacuum conditions; in addition, the viscosity of the polymer is high, resulting in slow mass transfer and heat transfer; these reasons lead to the duration of the rectification process Often longer and less productive
On the other hand, the strong base catalyst added in the cracking process will cause the fluoroalkyl group to remove fluorine atoms during the high temperature cracking process, and may further generate crosslinking, reducing the product yield

Method used

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  • A method for cracking polysiloxane oligomers containing long-chain fluoroalkyl groups

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1) put R F for CF 3 CF 2 CF 2 CF 2 CH 2 CH 2 1000 mass parts of polysiloxane oligomers containing long-chain fluoroalkyl groups, 5 mass parts of potassium hydroxide, and 20 mass parts of stearyl alcohol are added in the cracking container, and the stirring is started, and vacuumization is started simultaneously, and the cracking container is gradually raised. Internal material temperature, before distilling out the distillate;

[0045] 2) After the former fraction is separated, start to continuously feed inert gas into the cracking vessel while keeping the vacuum in the cracking vessel at -0.95MPa, and continue to gradually increase the temperature of the material in the cracking vessel to extract cracked products until there is no product to continue mining out. The rectification time (the rectification time in the present invention refers to the time elapsed from the beginning of the separation of the front fraction to the end when no product continues to be ex...

Embodiment 2

[0047] 1) put R F for CF 3 CF 2 CF 2 CF 2 CH 2 CH 2 1000 mass parts of polysiloxane oligomers containing long-chain fluoroalkyl groups, 0.5 mass parts of potassium hydroxide, and 15 mass parts of stearyl alcohol are added in the cracking container, and the stirring is started, and vacuumization is started simultaneously, and the cracking container is gradually raised. Internal material temperature, before distilling out the distillate;

[0048] 2) After separating the previous fraction, start to continuously feed inert gas into the cracking vessel, keep the vacuum in the cracking vessel at -0.97MPa, and continue to gradually increase the temperature of the material in the cracking vessel to extract cracked products until there is no product to continue mining out. The rectification time was 3.5 hours, and a total of 926 g of cyclization cracking products were obtained.

Embodiment 3

[0050] 1) put R F for CF 3 CF 2 CF 2 CF 2 CH 2 CH 2 1000 mass parts of polysiloxane oligomers containing long-chain fluoroalkyl groups, 10 mass parts of potassium hydroxide, and 35 mass parts of stearyl alcohol are added in the cracking container, and the stirring is started, and vacuumizing is started simultaneously, and the cracking container is gradually raised. Internal material temperature, before distilling out the distillate;

[0051] 2) After the former fraction is separated, start to continuously feed inert gas into the cracking vessel while keeping the vacuum in the cracking vessel at -0.93MPa, and continue to gradually increase the temperature of the material in the cracking vessel to extract cracked products until there is no product to continue mining out. The rectification time was 4.0 h, and a total of 914 g of cyclization cracking products were obtained.

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Abstract

The invention discloses a cracking device and method for a polysiloxane oligomer containing long-chain fluoroalkyl. The device comprises a cracking reaction kettle, an insertion pipe and a condensation pipe, and is characretzied in that a stirrer is arranged in the cracking reaction kettle, one end of the insertion pipe is inserted in the cracking reaction kettle through an insertion opening and communicated with a gas disperser, the other end of the insertion pipe is communicated with an inert gas tank, one end of the condensation pipe is connected with a vacuum pump through a vacuum pipeline, the other end of the condensation pipe is connected with a product receiving vessel and the upper end of a rectifying column, and the lower end of the rectifying column is communicated with the cracking reaction kettle through a gas phase opening. The cracking method includes the steps that 1, the oligomer, a catalyst and octadecanol are added into the reaction kettle, stirring is performed, vacuumizing is performed, the temperature is increased step by step, and front cut fraction is distilled out; 2, after the front cut fraction is separated out, inert gas is introduced into the reaction kettle, the vacuum degree is kept being -0.9 MPa or above, the temperature is increased step by step, and the cracked product is extracted out. The cracking device and method are mainly used for cracking the polysiloxane oligomer containing long-chain fluoroalkyl.

Description

technical field [0001] The invention relates to a cracking device and a cracking method, in particular to a cracking device and a cracking method for polysiloxane oligomers containing long-chain fluoroalkyl groups. Background technique [0002] Due to its low surface tension, non-flammability and oil-repellent properties, fluorine-containing polysiloxane is widely used in various fields such as defoamers, strippers, and anti-graffiti coatings. However, common fluorine-containing polysiloxanes (such as poly(3,3,3-trifluoropropylmethylsiloxane)) are difficult to achieve in terms of oil and dirt resistance due to their short fluorine-containing chains. satisfactory effect. We know that with the growth of fluorine-containing chains, the above properties of fluorine-containing polysiloxane macromolecular polymers will be further improved. [0003] Ring-opening polymerization of siloxane cyclic compounds is an important method for preparing polysiloxane macromolecular polymers. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J8/10
CPCB01J8/087B01J8/10B01J2208/00212B01J2208/00946
Inventor 向德轩梁春华李元祥胡杨剑梁长旺
Owner 宁夏胜佳环保科技有限公司
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