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Method for manufacturing cyclic carbonate

一种制造方法、碳原子数的技术，应用在化学仪器和方法、物理/化学过程催化剂、有机化合物/氢化物/配位配合物催化剂等方向，能够解决不能得到充分满足、经时收率降低、催化剂量减少等问题，达到抑制催化剂更新成本、高转化率、有利制造的效果

Active Publication Date: 2016-03-02
NAT INST OF ADVANCED IND SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, these heterogeneous catalysts have the problem that the immobilized quaternary The salt seeps out slowly during the reaction, so that the amount of catalyst participating in the reaction is substantially reduced, and the yield decreases over time
Especially when the above-mentioned catalyst is used in a continuous process, the catalyst needs to be frequently exchanged due to the deterioration of the catalyst, which cannot be fully satisfied in terms of production efficiency and catalyst cost.

Method used

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  • Method for manufacturing cyclic carbonate
  • Method for manufacturing cyclic carbonate
  • Method for manufacturing cyclic carbonate

Examples

Experimental program
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Embodiment

[0112] Hereinafter, although an Example is given and this invention is demonstrated in detail, this invention is not limited to these Examples.

[0113] The analysis methods used in the respective examples and comparative examples are as follows.

[0114] (1) Fluorescence X-ray analysis

[0115] The amount of bromine, chlorine, and phosphorus modification of the catalyst was measured using fluorescent X-ray analysis (device: product name "System 3270" (manufactured by Rigaku Denki Kogyo Co., Ltd.), measurement conditions: Rh tube bulb, tube voltage 50kV, tube current 50mV, vacuum environment, Detector: SC, F-PC).

[0116] (2) Gas chromatography analysis

[0117] Compositional analysis of the reaction solution and the like used gas chromatography. The analysis conditions are as follows.

[0118] Device: Product name "GC-2010Plus" (manufactured by Shimadzu Corporation)

[0119] Detector: FID

[0120] INJ temperature: 150°C

[0121] DET temperature: 260°C

[0122] Sample ...

Synthetic example 1

[0126] Catalyst Synthesis Example 1: Tributyl Bromide Synthesis of Surface Modified Silica Catalyst (Catalyst A)

[0127] Bead silica gel (CARiACTQ-10 manufactured by Fuji Silysia Chemical (average pore diameter 10nm, particle diameter 1.2-2.4mm, specific surface area 300m 2 / g)) 20g and 50mL of 2N hydrochloric acid were put into a 200mL three-necked flask with stirring blades, and the inside of the flask was replaced with nitrogen and heated to reflux for 4 hours, thereby demetallizing the silica gel. Thereafter, the silica gel was separated by filtration, and sufficiently washed with ion-exchanged water. In addition, when 1N silver nitrate aqueous solution was dripped at the liquid after washing|cleaning, it did not become cloudy, and it was confirmed that it does not contain chlorine and that washing|cleaning was sufficient.

[0128] Put the acid-treated silica gel and 50 mL of toluene into a 200 mL three-neck flask with stirring blades equipped with Dean-Stark, and perf...

Synthetic example 2

[0132] Catalyst Synthesis Example 2: Tributyl Bromination Synthesis of Surface Modified Silica Catalyst (Catalyst B)

[0133] Bead silica gel (CARiACTQ-10 manufactured by Fuji Silysia Chemical (average pore diameter 10nm, particle diameter 1.2-2.4mm, specific surface area 300m 2 / g)) 2000g and 5000mL of xylene were put into a 10L three-necked flask with stirring blades equipped with a Dean-Stark separator, and azeotropic dehydration of xylene-water was carried out at 140°C for 2 hours to remove the moisture in the silica gel . Next, the Dean-Stark separator was removed, and after replacing the inside of the flask with nitrogen, 219 g (0.846 mol) of 3-bromopropyltrimethoxysilane was added dropwise. The silanization reaction was carried out by directly heating it to reflux at 135° C. for 7 hours. Next, the obtained reactant was separated by filtration, washed twice with xylene, and 3810 g of a catalyst precursor (bromopropylated silica gel) containing xylene was obtained. N...

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Abstract

Provided is a method for manufacturing a cyclic carbonate which is a method for manufacturing a cyclic carbonate by reacting epoxide and carbon dioxide, the method being capable of efficiently manufacturing a cyclic carbonate at a high conversion percentage and high yield, and in which degradation of the catalyst over time is inhibited and catalytic activity is unlikely to occur. A method for manufacturing a cyclic carbonate for reacting epoxide and carbon dioxide in the presence of a quaternary onium salt selected from quaternary ammonium salt having a halogenated anion as a counter ion and a quarternary phosphonium salt having a halogenated anion as a counter ion, or in the presence of a solid catalyst in which the quarternary onium salt has been immobilized on a carrier, wherein a halogenated organic containing at least one halogen atom in one molecule is added to the reaction system.

Description

technical field [0001] The present invention relates to a method for producing cyclic carbonates. Background technique [0002] Cyclic carbonates can be used as organic solvents, synthetic fiber processing agents, raw materials for pharmaceuticals, cosmetic additives, electrolyte solvents for lithium batteries, and are also used in the synthesis of alkylene glycols and dialkyl carbonates, etc. (Patent Document 1) , is one of the important compounds with a wide range of uses. [0003] Conventionally, this cyclic carbonate has been synthesized by reacting an epoxide with carbon dioxide in the presence of a homogeneous catalyst under appropriate pressure conditions. As such a homogeneous catalyst, halides such as alkali metals, quaternary ammonium salts, etc. have been known conventionally. Salt (Patent Document 2) is also used industrially. [0004] However, when such a homogeneous catalyst is used, separation operations such as distillation of the reaction mixture and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/36B01J31/02C07D317/38
CPCB01J31/0239B01J31/0254B01J31/0268B01J31/0269B01J2231/341C07D317/36C07D317/38Y02P20/141
Inventor 高桥利和安田弘之山本昭治何木隆史林泰宪春名健志古川拓郎
Owner NAT INST OF ADVANCED IND SCI & TECH
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