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Vinylene carbonate preparation method

The technology of vinylene carbonate and ethylene carbonate is applied in the field of preparation of vinylene carbonate, which can solve the problems of high equipment and process requirements, and achieve the effects of good economic and social benefits, simple process flow and strong operability.

Inactive Publication Date: 2015-02-04
RONGCHENG QINGMU CHEM MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN199360, which adopts photochlorination reaction, requires industrial production, and has high requirements for equipment and technology

Method used

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preparation example Construction

[0023] A kind of preparation method of vinylene carbonate, it comprises the following steps:

[0024] (1) Synthesis of monochloroethylene carbonate (ClEC): using ethylene carbonate (EC) as raw material, azo compound as initiator, and sulfonyl chloride as chlorinating agent, free radical substitution reaction occurs to obtain monochlorocarbonic acid Vinyl esters (ClEC).

[0025] The main reaction equation is:

[0026]

[0027] Specifically: Add ethylene carbonate (EC) into the reactor, add azo compounds according to the oil-soluble initiator azo compound: EC=2-3:100 (weight ratio), and the molar ratio of sulfuryl chloride and EC is 1.1 -1.2:1 Add sulfuryl chloride dropwise, the dropwise addition temperature is 55~80°C, the dropwise addition time is 5~6 h, and then keep warm for 1 h, and the tail gas is removed in vacuum to obtain the crude ClEC.

[0028] (2) In the presence of dimethyl carbonate (DMC), bimolecular elimination reaction (E-2 reaction process) occurs between ...

Embodiment 1

[0043] Example 1: Press figure 1 The steps shown: (1) Add 500 kg (5.68 kmol) of ethylene carbonate (EC) to the chlorination kettle, raise the temperature to 70~80 ℃ and add 13 kg of azobisisobutyronitrile (AIBN) (2.6% of the amount of EC) , and at 70~80 ℃, 843 kg (6.25 kmol) of sulfuryl chloride was added dropwise within 4.5~6 hours, and at the same time, 1.3 kg of AIBN was added every 30 minutes, and AIBN was added 10 times in total. Insulate at 80°C for 1 h, remove the tail gas in vacuum, and cool down to obtain 668 kg (about 5.45 kmol) of crude monochloroethylene carbonate. The conversion rate from EC to ClEC is 91%. (2) Add 668 kg of the ClEC crude product obtained in step (1), 2000 kg of dimethyl carbonate, and 3.3 kg of the polymerization inhibitor p-hydroxyanisole to the dehydrochlorination kettle. Raise the temperature to 55-59 °C, add 668 kg (6.6 kmol) of triethylamine dropwise in 5-8 h, and keep the temperature for 12 h after the dropping. A mixture containing vin...

Embodiment 2

[0044] Example 2: Press figure 1 Shown: Step (1) Add 500 kg (5.68 kmol) of ethylene carbonate (EC) to the chlorination tank and heat up to 55~60 °C, then add 12.5 kg of azobisisoheptanonitrile (ABVN) at one time, and At ~60°C, 882 kg (6.53kmol) of sulfuryl chloride was added dropwise within 4~5 hours. After the drop was completed, the temperature was kept at 55~60°C for 1 hour, the tail gas was removed in vacuum, and the crude product of chloroethylene carbonate (ClEC) 675 kg (about 5.51 kmol). The conversion rate from EC to ClEC is 96.3%. GC analysis contained EC 3.7 %, ClEC 87.3 %, dichloroethylene carbonate Cl 2 EC 6.3%, undetected substance 2.7%. Step (2) Add 675 kg of crude ClEC obtained in step (1) to the dehydrochlorination kettle, add 2025 kg of dimethyl carbonate, and 3.4 kg of p-hydroxyanisole as a polymerization inhibitor. 675 kg (6.68 kmol) of triethylamine was added dropwise within 5-8 h, and after the drop was completed and kept for 12 h, a mixture containing...

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Abstract

The invention relates to a vinylene carbonate preparation method, which comprises the following steps: synthesizing monochloroethylene carbonate (C1EC), adding sulfonyl chloride drop by drop on ethylene carbonate (EC) under existence of an initiator azo, wherein mol ratio of sulfonyl chloride to EC is 1.1-1.2: 1, adding temperature is 55-80 DEG C, adding time is 5-6 hours, insulating for 1 hour, adding trialkylamine for 6-7 hours in a solution of dimethyl carbonate (DMC) and ClEC crude product according to weight ratio of 2.5-2.5: 1, wherein the addition temperature is 50-59 DEG C, insulating for 10-12 hours, wherein weight ratio of trialkylamine to ClEC is 1:1-1.1, and performing vacuum rectification and toluene recrystallization for purifiying VC. According to the invention, EC conversion rate can reach more than 94%, VC yield can reach 44%, and purity can reach more than 99.9%. The method has the advantages of simple process flow, mild technology condition, low reaction temperature and increased production security. In the invention, DMC is especially employed as solvent product which is easy to be separated.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and in particular relates to a preparation method of vinylene carbonate. Background technique [0002] Vinylene carbonate (VC for short) is a colorless and transparent liquid. It is an organic synthesis intermediate and an electrolyte additive for lithium-ion batteries. It can significantly prolong the cycle life of lithium-ion batteries. It is a non-aqueous electrolyte. solvent. It can also be used as a surface coating component or as a monomer for preparing polyvinylene carbonate, and has a broad market prospect. [0003] At present, the main methods of producing vinylene carbonate are as follows: ethylene carbonate and chlorine are chlorinated under photoinitiation to generate ethylene carbonate (ClEC), and then inorganic bases are used: sodium hydroxide, potassium hydroxide, sodium carbonate, carbonic acid Potassium, or organic bases: N, N-dimethylaniline, triethylamine, etc...

Claims

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Application Information

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IPC IPC(8): C07D317/40
CPCC07D317/40
Inventor 任相忠刘玉美宋春凤曲泽嵩程玉强刘学松于莹莹
Owner RONGCHENG QINGMU CHEM MATERIALS
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