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Process of producing diphenyl carbonate by non-solvent method

A technology of diphenyl carbonate and non-solvent method, which is applied in the field of production technology of diphenyl carbonate, can solve the problems of unstable appearance color, weak market competitiveness, cumbersome synthesis process, etc., so as to avoid sodium chloride mother liquor water and waste water, improving safety and productivity, and reducing production costs

Active Publication Date: 2015-03-25
CHONGQING CHANGFENG CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this process are: the synthesis process is cumbersome, a large amount of sodium chloride mother liquor water is produced, and it is difficult to handle; Time-consuming, high cost, low production capacity, weak market competitiveness

Method used

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  • Process of producing diphenyl carbonate by non-solvent method
  • Process of producing diphenyl carbonate by non-solvent method
  • Process of producing diphenyl carbonate by non-solvent method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Put 282g of phenol into a 500ml reaction bottle, heat up and melt, and when it reaches 115°C, add an appropriate amount of catalyst DMF according to 1% of the weight of phenol. Under stirring conditions, the flow rate is controlled to slowly feed phosgene to ensure that the phosgene reaction is complete; after 12 hours of photochemistry, sampling analysis: phenol 2.1%, phenyl chloroformate 0.9%, diphenyl carbonate 96.3%, the reaction is over; phenol and The molar ratio of phosgene actually used is 1:0.8. Raise the temperature to 150°C and keep it warm for 3 hours, and the measured phenyl chloroformate content is <0.1% as the end point. Using oil bath heating distillation process, the oil temperature is 180°C, the internal temperature is 150°C, and the vacuum degree is 0.085Mpa, and the phenol is distilled and separated; the oil temperature is 220°C, the internal temperature is 190°C, and the vacuum degree is 0.096Mpa, and the product is obtained by distillation. The qu...

Embodiment 2

[0038] Put 282g of phenol into a 500ml reaction bottle, heat up and melt, and when it reaches 115°C, add an appropriate amount of catalyst N,N-dimethylaniline according to 1.1% of the weight of phenol. Under stirring conditions, control the flow rate and slowly feed phosgene to ensure that the phosgene reaction is complete; the photochemical time is 13 hours, and the sampling analysis: 3.7% phenol, 3.3% phenyl chloroformate, and 92.3% diphenyl carbonate; add 20g of phenol to carry out After heat preservation, keep heat at 170°C for 4 hours, and measure the content of phenyl chloroformate <0.1% as the end point. The actual molar ratio of phenol to phosgene used is 1:0.9. Using oil bath heating distillation process, the oil temperature is 180°C, the internal temperature is 150°C, and the vacuum degree is 0.086Mpa, and the phenol is distilled and separated; the oil temperature is 220°C, the internal temperature is 190°C, and the vacuum degree is 0.096Mpa, and the product is obtai...

Embodiment 3

[0042] Put 282g of phenol into a 500ml reaction bottle, heat up and melt, and when it reaches 115°C, add an appropriate amount of catalyst DMF according to 1.1% of the weight of phenol. Under stirring conditions, the flow rate is controlled to slowly feed phosgene to ensure that the phosgene reaction is complete; the photochemical time is 11 hours, sampling analysis: phenol 5.8%, phenyl chloroformate 0.3%, diphenyl carbonate 92.3%, the reaction is over; phenol and The actual molar ratio of phosgene used is 1:0.6. Raise the temperature to 160°C and keep it warm for 4 hours, and the measured phenyl chloroformate content is <0.1% as the end point. Using oil bath heating distillation process, the oil temperature is 180°C, the internal temperature is 150°C, and the vacuum degree is 0.083Mpa, and the phenol is distilled and separated; the oil temperature is 220°C, the internal temperature is 190°C, and the vacuum degree is 0.097Mpa, and the product is obtained by distillation. The ...

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Abstract

The invention aims to provide a process of producing diphenyl carbonate by non-solvent method. The process can improve the quality of proeducts and also reduce the production cost of products and the waste discharge. The method comprises the following steps: melting phenol, and heating up to 110-130 DEG C; adding DMF or N,N-dimethylaniline or analogs thereof as catalyst in an amount of 0.03-3% of phenol; maintaining the temperature, and introducing phosgene for photochemical reaction while stirring; heating up to 140-180 DEG C and maintaining for 1-5 hours; and performing reduced pressure distillation to obtain the final product. The new process provided by the invention improves the quality and yield of products, completely eliminates sodium chloride mother liquid and waste water and reduces distillation residues, reduces the production cost, and achieves the purpose of clean production. The operation of phenol system recovery and the procedure of ingredients are reduced, the production efficiency is greatly increased, the operation is more stable, and the safety of production is improved.

Description

technical field [0001] The present invention relates to the production technology of diphenyl carbonate. Background technique [0002] Diphenyl carbonate (DPC) is a white crystalline solid that is insoluble in water but soluble in hot ethanol, benzene, ether, carbon tetrachloride, glacial acetic acid and other organic solvents. It is mainly used as a synthetic raw material for engineering plastics such as polycarbonate and polyparaben, and can also be used as a plasticizer and solvent for nitrocellulose. In pesticides, it is mainly used to synthesize methyl isocyanate, and then to prepare carbamate insecticide carbofuran. In addition, it is mainly used in the plastics industry to manufacture polyaryl carbonate and p-hydroxybenzoic acid polyester, monoisocyanate and diisocyanate. Plasticizers can also be prepared. It is used as solvent and heat carrier in chemical production. [0003] The production of diphenyl carbonate in the prior art is mainly to be raw material with ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/96C07C68/02
Inventor 李定山杜祥伦周树新
Owner CHONGQING CHANGFENG CHEM IND
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