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Synthesis method of high-purity p-tert-butylcatechol

A technology of tert-butylcatechol and synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, chemical recovery, etc., to achieve the effects of low production cost, reduced loss of raw materials, and mild reaction conditions

Active Publication Date: 2012-07-25
辽宁凯迪化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of this invention is to provide a kind of synthetic method of high-purity p-tert-butylcatechol, to overcome many deficiencies of existing synthetic methods

Method used

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  • Synthesis method of high-purity p-tert-butylcatechol
  • Synthesis method of high-purity p-tert-butylcatechol
  • Synthesis method of high-purity p-tert-butylcatechol

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Embodiment 1

[0016] Embodiment 1: 200kg pyrocatechol is added in the synthetic kettle 6 through raw material warehouse 5, 40kg methyl tert-butyl ether is also added in the synthetic kettle 6 from storage tank 1, elevated tank 2 by negative pressure, simultaneously from catalyst material Add 10kg of NKC-99 catalyst to bin 4, heat the synthesis kettle 6 to 70-100°C, start stirring, raise the temperature to 100-110°C, control the reaction pressure to less than 0.04MPa, react for 3-5 hours, cool down to 85°C, and condense The reaction by-product methanol is flashed out by the device 17, and enters the methanol recovery tank 3. Heat the synthesis liquid in the synthesis kettle 6 to 130-160°C, control the reaction pressure to be less than 0.04MPa, stir for 2-4 hours, cool down to 100°C, send it to the filter 7 to filter out the NKC-99 catalyst, and the synthesis liquid enters a stable state. Kettle 10. After the filtered NKC-99 catalyst is regenerated by the regeneration kettle 8 and the regene...

Embodiment 2

[0017] Embodiment 2: 200kg catechol is added in the synthetic kettle 6 through raw material bin 5, will go out 60kg methyl tertiary butyl ethers also add in the synthetic kettle 6 from storage tank 1, head tank 2 by negative pressure, simultaneously from catalyst Add 15kg of NKC-99 catalyst to silo 4, heat the synthesis kettle 6 to 70-100°C, start stirring, raise the temperature to 100-110°C, control the reaction pressure to less than 0.04MPa, react for 3-5 hours, cool down to 85°C, and The condenser 17 flashes methanol as a by-product of the reaction, and enters the methanol recovery tank 3 . Heat the synthesis liquid in the synthesis kettle 6 to 130-160°C, control the reaction pressure to be less than 0.04MPa, stir for 2-4 hours, cool down to 100°C, send it to the filter 7 to filter out the NKC-99 catalyst, and the synthesis liquid enters a stable state. Kettle 10. After the filtered NKC-99 catalyst is regenerated by the regeneration kettle 8 and the regenerator 9, it is se...

Embodiment 3

[0018] Embodiment 3: 250kg pyrocatechol is added in the synthetic kettle 6 through raw material warehouse 5, 120kg methyl tert-butyl ether is also added in the synthetic kettle 6 from storage tank 1, elevated tank 2 by negative pressure, simultaneously from catalyst material Add 17kg of NKC-99 catalyst to bin 4, heat the synthesis kettle 6 to 70-100°C, start stirring, raise the temperature to 100-110°C, control the reaction pressure to less than 0.04MPa, react for 3-5 hours, cool down to 85°C, and condense The reaction by-product methanol is flashed out by the device 17, and enters the methanol recovery tank 3. Heat the synthesis liquid in the synthesis kettle 6 to 130-160°C, control the reaction pressure to be less than 0.04MPa, stir for 2-4 hours, cool down to 100°C, send it to the filter 7 to filter out the NKC-99 catalyst, and the synthesis liquid enters a stable state. Kettle 10. After the filtered NKC-99 catalyst is regenerated by the regeneration kettle 8 and the regen...

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Abstract

The invention discloses a synthesis method of high-purity p-tert-butylcatechol (TBC). The product is prepared by the steps of reacting pyrocatechol and methyl tert-butyl ether as raw materials in the present of NKC-99 (dry hydrogen) as a catalyst for 3-9 hours under the conditions that the temperature is 100-160 DEG C and the reaction pressure is less than 0.04MPa while separating out byproducts. The synthesis method provided by the invention has the advantages that (1) compared with isobutylene used as the raw material, the used raw material has no safety problem during isobutylene storage and the transportation or production process; (2) the use amount of the catalyst is less, which is only 0.5-5% of pyrocatechol by weight, and the catalyst can be recycled, so as to reduce the loss of raw materials; (3) the reaction liquid does not contain 3-TBC and 3,5-TBC, the product purity is high and can be up to above 99%, only a small amount of residue is left in a kettle, neutralization and washing processes are not needed, and no wastewater is discharged; and (4) the synthesis method provided by the invention is mild in reaction conditions, simple in process and low in production cost.

Description

1. Technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for synthesizing high-purity p-tert-butylcatechol. 2. Background technology [0002] P-tert-butylcatechol is referred to as TBC. It is white or light yellow crystal. It is mainly used as a high-efficiency polymerization inhibitor in the distillation, storage and transportation of styrene, butadiene and other vinyl monomers. It is also used as an antioxidant and insecticide for polyethylene, polybutadiene and synthetic rubber products. stabilizers, etc. At present, the method of synthesizing TBC at home and abroad is mainly the phosphoric acid method or sulfuric acid method catalytic synthesis of catechol. Among them, JP 49-127932 and JP 2-132939 respectively disclose the method for preparing TBC by reacting catechol and isobutylene in the presence of sulfuric acid. That is, using sulfuric acid as a catalyst, controlling the amount of sulfuric...

Claims

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Application Information

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IPC IPC(8): C07C39/08C07C37/16
CPCY02P20/584
Inventor 周少瑛周子翘
Owner 辽宁凯迪化工有限公司
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