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Process for producing deiphenyl carbonate by using non-solvent method

A technology of diphenyl carbonate and non-solvent method, applied in the field of production technology of diphenyl carbonate, can solve the problems of unstable appearance and color, complicated synthesis procedures, low product quality, etc., and avoids sodium chloride mother liquor and waste water. , the effect of reducing production costs and simplifying operations

Inactive Publication Date: 2018-04-03
青岛九洲千和机械有限公司
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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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 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, control the flow rate and slowly feed phosgene to ensure that the phosgene reaction is complete; after 12 hours of photochemistry,

[0036] Sampling analysis: 2.1% phenol, 0.9% phenyl chloroformate, 96.3% diphenyl carbonate, the reaction is over; the actual molar ratio of phenol to phosgene 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.

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, sampling analysis: 3.7% phenol, 3.3% phenyl chloroformate, 92.3% diphenyl carbonate; add 20g of phenol to carry out After the heat preservation, the temperature was kept at 170° C. for 4 hours, and the measured phenyl chloroformate content was less than 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 ...

Embodiment 3

[0040] 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 the condition of stirring, control the flow rate and 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 less than 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 distill...

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Abstract

The purpose of the present invention is to provide a process for producing diphenyl carbonate by non-solvent method, which can improve product quality and reduce product production cost and waste discharge; the steps of the process include: melting phenol and heating up to 110-130°C ; Use DMF or N, N-dimethylaniline or the analogue of the two as a catalyst, the charging amount is 0.03-3% of phenol; keep the temperature, feed phosgene under stirring conditions and carry out photochemical reaction; then be warming up to 140 ‑180°C for 1‑5 hours; then distilled under reduced pressure to obtain the product. The new process of the invention improves product quality and output, completely avoids sodium chloride mother liquor water and waste water, reduces distillation residue, reduces production cost, and achieves clean production. The operation of phenol system recovery and the special batching process are reduced, which greatly improves the production efficiency; the operation is more stable, and the safety and productivity are improved.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a production process 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 ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/02C07C69/96
CPCC07C68/02C07C69/96
Inventor 李辉
Owner 青岛九洲千和机械有限公司
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