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Preparation method of allyl-1,3-sultone

A technology of sultone and propane sultone, which is applied in the field of organic compound preparation, can solve the problems of high equipment requirements, difficult industrialization, and more three wastes, and achieve the effect of low equipment requirements, less three wastes, and good reaction selectivity

Active Publication Date: 2017-01-04
吉和昌新材料(荆门)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0017] Due to the special structural characteristics of propenyl-1,3-sultone, it can be widely used in electroplating, medicine and lithium battery industries. Especially in recent years, the demand for lithium batteries in the new energy industry has given birth to propenyl-1,3-sultone -Synthesis and application development of sultone, patents CN101456856B and CN101659653A use propynyl alcohol as raw material, through addition, acidification, dehydration ring closure process, patent CN104610221A also use propynyl alcohol as raw material, add anion in the addition process Exchange resin, the above synthesis methods all have disadvantages such as low yield, many wastes, and high equipment requirements, and to a certain extent, they are difficult to industrialize

Method used

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  • Preparation method of allyl-1,3-sultone
  • Preparation method of allyl-1,3-sultone
  • Preparation method of allyl-1,3-sultone

Examples

Experimental program
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Effect test

Embodiment 1

[0050] The synthetic route of preparation method of the present invention is as Image 6 Shown: Weigh 10kg of electronic grade 1,3-propane sultone into a jacketed metering tank, heat it at 50°C after dissolving with steam, dissolve 15kg of NBS and 0.05kg of AIBN with 10kg of dichloromethane, and put the microchannel reactor or tubular Preheat the reactor to a certain temperature, pump 1,3-propane sultone at a rate of 2kg / h, pump a mixture of NBS, AIBN, and methylene chloride at a rate of 5kg / h, and simultaneously adjust the outlet back pressure valve to control The reaction pressure was 0.6MPa, the collected reaction solution was filtered to remove succinimide, and the solvent dichloromethane was evaporated under normal pressure to obtain 15kg of 2-bromo-1,3-propane sultone, which was recovered and used mechanically. The rate reached 89.4%.

[0051] Weigh 2kg of 2-bromo-1,3-propane sultone obtained from the above reaction, 0.01kg of polymerization inhibitor, and 30kg of dichl...

Embodiment 2

[0053] Weigh 1.20kg of electronic grade 1,3-propane sultone into a jacketed metering tank, turn on steam to dissolve and keep warm at 50°C, dissolve 30kg of NBS and 1kg of AIBN with 30kg of dichloromethane, preheat the microchannel reactor or tubular reactor Heat to a certain temperature, pump 1,3-propane sultone at a rate of 2kg / h, pump a mixture of NBS, AIBN, and methylene chloride at a rate of 6.1kg / h, and adjust the outlet back pressure valve to control the reaction pressure 1.2MPa, collect the reaction liquid and filter to remove succinimide, evaporate the solvent dichloroethane under normal pressure to get 32kg of 2-bromo-1,3-propane sultone, recover the dichloromethane and apply it mechanically, the bromination reaction yield up to 95%.

[0054] Weigh 2.2kg of 2-bromo-1,3-propane sultone obtained from the above reaction, 0.02kg of polymerization inhibitor, and 30kg of dichloroethane into a 50L enamel reactor with a reflux condenser and heat up to reflux, slowly drop 1k...

Embodiment 3

[0056] Weigh 10kg of electronic grade 1,3-propane sultone into a jacketed metering tank, turn on steam to dissolve and keep warm at 50°C, 15kg of Br 2 , Dissolve 0.05kg BPO with 10kg carbon tetrachloride, preheat the microchannel reactor or tubular reactor to a certain temperature, pump 1,3-propane sultone at a speed of 2kg / h, and pump at a speed of 5kg / h Into Br 2 , BPO, carbon tetrachloride mixture, at the same time adjust the outlet back pressure valve, control the reaction pressure 1.5MPa, collect the reaction liquid and filter to remove succinimide, evaporate the solvent under normal pressure to get 15kg2-bromo-1,3-propane The sultone and solvent recovery are applied mechanically, and the bromination reaction yield reaches 89.4%.

[0057] Weigh 2kg of 2-bromo-1,3-propane sultone obtained from the above reaction, 0.01kg of polymerization inhibitor (BHT), and 30kg of dichloromethane into a 50L enamel reactor with a reflux condenser and heat up to reflux, slowly drop Add 1...

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Abstract

The invention discloses a preparation method of allyl-1,3-sultone. The method comprises the following steps: 1) halogenation reaction: in a condition of catalyst or illumination, enabling 1,3-propane sultone and a brominating agent to react in a micro-channel reactor or a tubular reactor to obtain 2-bromo-1,3-propane sultone; 2) elimination reaction: in a reflux reaction device, removing hydrogen bromide of the 2-bromo-1,3-propane sultone obtained in the step 1) under the effect of a dehalogenation agent and a polymerization inhibitor till reaction is completed; and 3) concentration and crystallization: adding active carbon into the reaction system of the step 2) for decoloration; after the decoloration, filtering out the active carbon; and performing concentration and crystallization to obtain the allyl-1,3-sultone. According to the preparation method disclosed by the invention, electronic-grade 1,3-propane sultone is used as a raw material, and the allyl-1,3-sultone is synthesized through halogenation and elimination reactions; and the reaction process is in stable control, the requirements on equipment are not high, the reaction selectivity is good, the product yield is high, few three wastes are produced, the cost is low, and the method is suitable for industrial production.

Description

Technical field [0001] The invention belongs to the technical field of organic compound preparation, and specifically relates to a preparation method of propenyl-1,3-sultone. Background technique [0002] Because propenyl-1,3-sultone contains unsaturated bonds and heteroatoms in its structure, it can synthesize a variety of products with special properties, such as sulfonamide herbicides and sulfonamide drugs used in pesticides. It can also be used as an electrolyte additive for lithium batteries to improve battery performance, reduce battery expansion, greatly extend the rechargeable life of the battery, and greatly improve safety. In recent years, the demand for lithium-ion batteries in the new energy field has increased dramatically. As a lithium-ion battery electrolyte additive with excellent performance, the industrial production of propenyl-1,3-sultone is particularly important. [0003] In the existing technology, there are currently five synthesis methods for propen...

Claims

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Application Information

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IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 冯庆诚杨威周世骏明瑞涛肖忠新郭新乐胡哲黄开伟
Owner 吉和昌新材料(荆门)有限公司
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