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Method for preparing full-fluoride methyl vinyl ether by using fluidized bed

A perfluoromethyl vinyl ether, fluidized bed technology, applied in ether preparation, organic chemistry, ether separation/purification and other directions, can solve problems such as low overall yield, achieve high purity, be conducive to industrial production, save money cost effect

Active Publication Date: 2018-03-20
陕西中化蓝天化工新材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the yield of the first step reaction of this method has been improved, the overall yield is still low in the second step because the cracking furnace is still used for cracking.

Method used

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  • Method for preparing full-fluoride methyl vinyl ether by using fluidized bed

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] After passing 6.0Kg of self-made perfluoro 2-methoxypropionyl fluoride (purity ≥ 99%) through a preheater at a temperature of 200 to 230°C, it is divided into three streams, with different flow rates of 0.1m / s and 0.2m / s respectively , 0.5m / s through the fluidized bed corresponding to the design of the three areas. At the same time, 4.0Kg of excess potassium carbonate with an average particle size of 0.1-0.5mm enters the fluidized bed from top to bottom at a flow rate of 0.5m / s, and flows through the distributor with perfluoro 2-methoxypropionyl fluoride. Chemical contact cracking fast reaction, cracking temperature 200 ℃. The fluidized bed selected in this test has a diameter of 1.2m and a bed height of 1.5m. After the reacted mixed product is separated by cyclone separation B, unreacted solid potassium carbonate and stream 5 containing perfluoromethyl vinyl ether are obtained, wherein the unreacted solid potassium carbonate is recycled to the fluidized Bed, continue...

Embodiment 2

[0041]After 3.0Kg of self-made perfluoro 2-methoxypropionyl fluoride (purity ≥ 99%) passed through a preheater at a temperature of 180-230°C, it was divided into three streams, with different flow rates of 0.1m / s and 0.2m / s respectively , 0.3m / s through the fluidized bed corresponding to the design of the three areas. At the same time, 2.1Kg of excess potassium carbonate with an average particle size of 0.1-0.5mm enters the fluidized bed from top to bottom at a flow rate of 0.3m / s, and flows through the distributor with perfluoro 2-methoxypropionyl fluoride. Chemical contact cracking rapid reaction, cracking temperature 190 ℃. The fluidized bed selected in this test has a diameter of 1.5m and a bed height of 1m. After the reacted mixed product is separated by cyclone separator B, unreacted solid potassium carbonate and stream 5 containing perfluoromethyl vinyl ether are obtained, wherein unreacted solid potassium carbonate is circulated to the fluidized bed through the carbon...

Embodiment 3

[0044] After the self-made perfluoro 2-methoxypropionyl fluoride 3.0Kg (purity ≥ 99%) passes through the preheater at a temperature of 180-200°C, it is divided into three streams, respectively with different flow rates of 0.1m / s and 0.2m / s , 0.5m / s through the fluidized bed corresponding to the design of the three regions. At the same time, 2Kg of excess sodium carbonate with an average particle size of 0.1-0.5mm enters the fluidized bed from top to bottom at a flow rate of 0.5m / s, and fluidizes with perfluoro 2-methoxypropionyl fluoride after passing through the distributor. Rapid reaction of contact cracking, cracking temperature 190°C. The fluidized bed selected in this test has a diameter of 1.5m and a bed height of 1m. After the reacted mixed product is separated by cyclone separator B, unreacted solid sodium carbonate and stream 5 containing perfluoromethyl vinyl ether are obtained, wherein unreacted solid sodium carbonate is circulated to the fluidized bed through the ...

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Abstract

The invention discloses a method for preparing full-fluoride methyl vinyl ether by using a fluidized bed. The method comprises the following steps: firstly, enabling solid alkali carbonate and full-fluoride-2-methoxy propionyl fluoride to contact and react so as to obtain a full-fluoride-2-methoxy propionyl alkali metal salt, and further enabling the full-fluoride-2-methoxy propionyl alkali metalsalt to crack at 180-250 DEG C, thereby obtaining full-fluoride methyl vinyl ether. With the method disclosed by the invention, the yield and purity of full-fluoride methyl vinyl ether are high, the cost is low and industrial production is facilitated.

Description

technical field [0001] The invention relates to a preparation method of perfluoromethyl vinyl ether. Background technique [0002] Perfluoromethyl vinyl ether, abbreviated PMVE, chemical formula CF 3 OCF=CF 2 , is an important monomer, which can be used to synthesize new high-efficiency pesticides and new-type fluoroplastics and fluororubbers with excellent performance, such as the synthesis of new non-toxic and high-efficiency insecticide difenfluramide as an intermediate, and the synthesis of low-temperature resistant , Perfluoroether rubber with acid and alkali resistance and corrosion resistance, as a comonomer and tetrafluoroethylene copolymerized to prepare melt-processable fluororesin, etc. [0003] For the preparation method of perfluoromethyl vinyl ether, the prior art has the following reports: [0004] U.S. Patent US3114778 reports a two-step method for preparing perfluoromethyl vinyl ether. First, under the action of activated carbon catalyst, carbonyl fluorid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/01C07C41/34C07C41/42C07C43/17
CPCC07C41/01C07C41/34C07C41/42C07C43/17
Inventor 马亚锋齐仲龙杨会娥魏攀
Owner 陕西中化蓝天化工新材料有限公司
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