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Preparation method of cyclic carbonates

A technology of cyclic carbonate and carbon dioxide, applied in the field of preparation of cyclic carbonate, can solve the problems of high temperature, high reaction pressure, high toxicity of acetonitrile, etc., and achieve the effects of less species, low reaction temperature and pressure, and large adsorption capacity

Inactive Publication Date: 2017-07-21
NANYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the patent raw material acetonitrile is highly toxic, the reaction pressure is high, and the temperature is very high, requiring special reaction equipment

Method used

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  • Preparation method of cyclic carbonates
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  • Preparation method of cyclic carbonates

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A kind of preparation method of cyclocarbonate, utilize epoxy compound and carbon dioxide as reactant, with the WO with oxygen hole 3 For catalyst, comprising the following steps:

[0036] Add 100 mg of WO with oxygen vacancies to the reaction kettle 3 Catalyst, 10 mg tetrabutylammonium bromide, 0.8 mL propylene oxide, and then use carbon dioxide to replace the gas three times. Under the condition of 1.0 MPa carbon dioxide atmosphere and 30 °C, the reaction was stirred for 10 h, and the reaction mixture was passed through a tube about 1 cm long. Silica gel chromatography column to remove the catalyst, that is. Reaction conversion rate 95%, selectivity 99%, 1H NMR (400 MHz, CDCl 3 ): δ 1.50 (d, 3H); 4.03 (t, 1H); 4.56 (t, 1H); 4.84 (m, 1H).

[0037] Among them, the WO with oxygen vacancies 3 The preparation method of catalyst comprises the following steps:

[0038] Put 0.5 g of yellow tungsten oxide nanosheets (average thickness 7 nm, average length 50 nm) in a t...

Embodiment 2

[0041] A kind of preparation method of cyclocarbonate, utilize epoxy compound and carbon dioxide as reactant, with the WO with oxygen hole 3 For catalyst, comprising the following steps:

[0042] Add 80 mg of WO with oxygen holes in the reaction kettle 3 Catalyst, 10mg tetrabutylammonium bromide, 2mL dichloromethane, 0.6mL epichlorohydrin, and then use carbon dioxide to replace the gas 3 times, under the condition of 0.3MPa carbon dioxide atmosphere and 50℃ temperature, stir the reaction for 8h, and the reaction mixture passes A silica gel chromatography column with a length of about 1 cm was used to remove the catalyst, and the reaction conversion rate was 96%, and the yield was 99%.

[0043] Among them, the WO with oxygen vacancies 3 The preparation method of the catalyst is shown in Example 1.

[0044] The WO with oxygen vacancies in Example 2 3 The catalyst can be recycled for 7 times, the conversion rate of the 7th time is 93%, and the selectivity is 96%.

Embodiment 3

[0046] A kind of preparation method of cyclocarbonate, utilize epoxy compound and carbon dioxide as reactant, with the WO with oxygen hole 3 For catalyst, comprising the following steps:

[0047] Add 30 mg of WO with oxygen vacancies to the reaction kettle 3 Catalyst, 10mg sodium bromide, 5mL tetrahydrofuran, 0.1mL tetradecane oxide, and then use carbon dioxide to replace the gas 4 times. Under the condition of 0.8 MPa carbon dioxide atmosphere and 80℃ temperature, stir the reaction for 5h, and the reaction mixture passes through a tube about 1 cm long Silica gel chromatography column to remove the catalyst, namely. The reaction conversion rate is 95%, and the yield is 98%.

[0048] Among them, the WO with oxygen vacancies 3 The preparation method of catalyst comprises the following steps:

[0049] Put 0.5g of yellow tungsten oxide nanorods (average diameter 200 nm) into the reaction bottle, add 30mL of water, ultrasonically disperse evenly, pass in a mixed atmosphere of h...

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Abstract

The invention belongs to the technical field of chemical synthesis, and more specifically relates to a preparation method of cyclic carbonates. The preparation method comprises following steps: 10 to 100mg of WO3 catalyst with oxygen vacancy, 10 to 50mg of a co-catalyst, 0 to 10ml of a solvent, and 0.05 to 1.0ml of an epoxy compound are delivered into a reaction kettle; carbon dioxide is used for replacing gas for 3 to 4 times, and stirring reaction is carried out for 3 to 15h at 20 to 130 DEG C under 0.1 to 1.0MPa carbon dioxide atmosphere so as to obtain a finished product. According to the preparation method, few kinds of raw materials are used; toxicity is low; chemical structure is simple; no pollution is caused; catalytic activity is high; reaction conversion rate is as high as 96%; selectivity is as high as 99%; the catalyst can be recycled for at least 7 times; reaction temperature and pressure are both low; conditions are mild; one-step synthesis is realized; and the preparation method is suitable to be popularized.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of cyclocarbonate. Background technique [0002] Carbon dioxide is one of the main causes of the greenhouse effect, and it is also the most important inexhaustible carbon resource. It is of great significance to use carbon dioxide as a raw material to prepare industrial products with high added value. Cyclic carbonates can be prepared by direct reaction of carbon dioxide and epoxy compounds in one step, without any waste, with 100% atom economy. Cyclocarbonate, as an important organic synthesis intermediate, excellent electrolyte, and aprotic solvent, has important applications in organic synthesis, lithium-ion batteries, engineering plastics, textile industry, dyes, and other fields. At present, the research on the synthesis of epoxy compounds from carbon dioxide and epoxy compounds mainly adopts the strategy of activating epoxy compo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/36C07D317/44C07D317/46
CPCY02P20/584C07D317/36C07D317/44C07D317/46
Inventor 毛武涛鲍克燕陈宝宽李娜单晨希刘正阳
Owner NANYANG NORMAL UNIV
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