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Polycarbonate preparation method

A technology of polycarbonate and acid-binding agent, which is applied in the field of polycarbonate preparation to achieve the effects of mild reaction conditions, avoiding side reactions, and mild conditions

Inactive Publication Date: 2018-10-09
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In addition, the above-mentioned existing ring-opening polymerization (Wang L, et al. Chemistry-A European Journal, 2013, 19 (40): 13463-13478; Vogdanis L, et al. Macromolecular Chemistry and Physics, 1990, 191 (3): 465-472) and alternating polymerization (Sugimoto Y, Inoue SJ. PolymSci Part APolymChem 2004; 42:5561) methods, both need to be carried out under high temperature and pressure and the presence of heavy metal catalysts (such as Cr and Co, etc.)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Embodiment 1: the preparation method of polyvinyl carbonate

[0065] The reaction formula is as follows:

[0066]

[0067] Add triphosgene (0.1mol) and 200mL o-dichlorobenzene into a three-neck flask equipped with a mechanical stirrer, a condenser, and a constant pressure dropping funnel, and stir to dissolve the triphosgene. Add ethylene glycol (0.40 mol), dipotassium hydrogen phosphate (0.60 mol), and triethylamine (catalytic amount) into the bottle, and reflux for 16 hours after the addition is complete. Remove insoluble impurities by filtration, extract impurities and by-products dissolved in the solvent with water, and concentrate under reduced pressure to remove the solvent to obtain an intermediate product.

[0068] Add the intermediate product and 200 mL o-dichlorobenzene into the three-necked flask, and stir to dissolve it. Ethyl chloroformate (0.1mol) was added to the bottle, and the reaction was refluxed for 2h to stop the reaction. Remove insoluble impur...

Embodiment 2

[0071] Add ethylene glycol (0.40mol), dipotassium hydrogen phosphate (0.60mol), and triethylamine (catalytic amount) in the there-necked flask equipped with mechanical stirring, condenser, and constant pressure dropping funnel, and start stirring to make it well mixed. Then add triphosgene (0.1 mol) o-dichlorobenzene solution into the bottle through a constant pressure dropping funnel, and reflux for 16 hours after the addition is complete. The insoluble impurities were removed by filtration, the impurities dissolved in the solvent were extracted with water, and the solvent was removed by concentration under reduced pressure to obtain an intermediate product.

[0072] Add the intermediate product and 200 mL o-dichlorobenzene into the three-necked flask, and stir to dissolve it. Ethyl chloroformate (0.1mol) was added to the bottle, and the reaction was refluxed for 2h to stop the reaction. Remove insoluble impurities by filtration, wash with water three times, and collect the...

Embodiment 3

[0076] The product obtained in embodiment 3-8 is polyvinyl carbonate, and reaction device used is identical with embodiment 1, other experimental conditions (solvent, catalyzer, acid-binding agent, end-capping agent, feeding amount, reaction time and temperature of reaction) and The product yields are shown in Table 1 below.

[0077] Table 1. Synthesis results of polyvinyl carbonate:

[0078]

[0079]

[0080] The results of Examples 3-8 show that the molecular weight of the product can be changed by changing the time of the polycondensation reaction, the reaction temperature, the type of catalyst and the type of acid-binding agent, so that the molecular weight of the product can be controlled.

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Abstract

The invention discloses a polycarbonate preparation method, wherein triphosgene and a dihydroxy-based compound are used as raw materials and are subjected to a normal pressure condensation polymerization reaction in the presence of an appropriate amount of a catalyst and an acid binding agent to obtain polycarbonate. According to the present invention, the method has advantages of mild reaction condition, easy operation, high product purity and controllable molecular weight, can avoid the decarboxylation reaction induced ether chain introduction in the product, and can meet the high-purity requirements of the lithium battery industry.

Description

technical field [0001] The invention belongs to a preparation method of polycarbonate, in particular to a synthesis method of polycarbonate compounds such as polyethylene carbonate and polytrimethylene carbonate. Background technique [0002] Polycarbonate is a kind of polymer containing carbonate groups in the molecular chain. Aromatic polycarbonate has the advantages of high strength and elastic modulus, high impact strength, fatigue resistance and weather resistance, etc. It is widely used in glass assembly industry and automobile industry It has been widely used (Zhang Ye et al., Liaoning Chemical Industry, 2010,39(6):640-643). In recent years, the research and development of using polycarbonate and its derivatives as the polymer matrix to prepare all-solid polymer electrolytes for lithium batteries has gradually attracted people's attention. Among them, polyethylene carbonate (Tominaga Y. Polymer Journal, 2012, 44 (12): 1155-1158) and polytrimethylene carbonate (Sun B,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/42C08G64/26C08G64/28
CPCC08G64/42C08G64/266C08G64/28
Inventor 周志彬王鹏冯文芳聂进
Owner HUAZHONG UNIV OF SCI & TECH
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