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Method and device for improving yield by effectively utilizing buprofezin intermediate 1-isopropyl-3-tert-butyl thiourea mother liquor

A technology of tert-butylthiourea and isopropyl, which is applied in the field of preparation of buprofezin intermediates, can solve the problems of inability to degrade organic matter, reduce product quality and yield, and reduce the biodegradability of mother liquor wastewater, so as to improve the biochemical Sexuality, reduced processing costs, and reduced consumption

Pending Publication Date: 2021-04-30
JIANGSU ANPON ELECTROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method and device for effectively utilizing the mother liquor of buprofezin intermediate 1-isopropyl-3-tert-butylthiourea to increase the yield, aiming to solve the problem that the process in the prior art can increase the consumption of raw materials , reduce the quality and yield of the product, reduce the biodegradability of the mother liquor wastewater, and fail to effectively degrade the organic matter in the subsequent process.

Method used

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  • Method and device for improving yield by effectively utilizing buprofezin intermediate 1-isopropyl-3-tert-butyl thiourea mother liquor
  • Method and device for improving yield by effectively utilizing buprofezin intermediate 1-isopropyl-3-tert-butyl thiourea mother liquor
  • Method and device for improving yield by effectively utilizing buprofezin intermediate 1-isopropyl-3-tert-butyl thiourea mother liquor

Examples

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Effect test

Embodiment 1

[0031] Example 1, see figure 1 , the present invention also provides a method for effectively utilizing the mother liquor of buprofezin intermediate 1-isopropyl-3-tert-butylthiourea as described above to increase the yield, comprising the steps of:

[0032] S1: Add 1,000 g of 1-isopropyl-3-tert-butylthiourea mother liquor into the reaction flask, and raise the temperature to 80°C;

[0033] S2: put hydrochloric acid into the reaction bottle, and stir, adjust the pH value to 7, and then keep stirring at 80°C for 1 hour;

[0034] S3: After heat preservation and stirring for 1 hour, let stand and cool down to 10°C to crystallize, obtain sediment and supernatant, and stir for half an hour;

[0035] S4: After the sediment is stirred, centrifuge the sediment with a 300-mesh filter bag to obtain a wet product; dry the wet product at 110°C for 2 hours to obtain the intermediate 1-isopropyl-3-tert-butyl Dithiourea dry product, 24.3g.

[0036] In this embodiment, in step S1, the speci...

Embodiment 2

[0037] Example 2, see figure 2 , the present invention also provides a method for effectively utilizing the mother liquor of buprofezin intermediate 1-isopropyl-3-tert-butylthiourea as described above to increase the yield, comprising the steps of:

[0038]S1: Add 1000 g of 1-isopropyl-3-tert-butylthiourea mother liquor into the reaction flask, and raise the temperature to 50°C;

[0039] S2: put hydrochloric acid into the reaction bottle, and stir to adjust the pH value to 7.5, and then keep stirring at 80°C for 2 hours;

[0040] S3: After heat preservation and stirring for 2 hours, let stand and cool down to 10°C to crystallize, obtain sediment and supernatant, and stir for half an hour;

[0041] S4: After the sediment is stirred, centrifuge the sediment with a 300-mesh filter bag to obtain a wet product; dry the wet product at 110°C for 2 hours to obtain the intermediate 1-isopropyl-3-tert-butyl Dithiourea dry product, 23.6g.

[0042] In this embodiment, in step S1, the ...

Embodiment 3

[0043] Example 3, see image 3 , the present invention also provides a method for effectively utilizing the mother liquor of buprofezin intermediate 1-isopropyl-3-tert-butylthiourea as described above to increase the yield, comprising the steps of:

[0044] S1: Add 1,000 g of 1-isopropyl-3-tert-butylthiourea mother liquor into the reaction flask, and raise the temperature to 80°C;

[0045] S2: put hydrochloric acid into the reaction bottle, and stir, adjust the pH value to 9, and then keep stirring at 80°C for 1 hour;

[0046] S3: After heat preservation and stirring for 1 hour, let stand and cool down to 10°C to crystallize, obtain sediment and supernatant, and stir for half an hour;

[0047] S4: After the sediment is stirred, centrifuge the sediment with a 300-mesh filter bag to obtain a wet product; dry the wet product at 110°C for 2 hours to obtain the intermediate 1-isopropyl-3-tert-butyl Thiourea dry product, 21.7g.

[0048] In this embodiment, in step S1, the specifi...

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Abstract

The invention discloses a method and a device for improving yield by effectively utilizing buprofezin intermediate 1-isopropyl-3-tert-butylthiourea mother liquor, and the method comprises the following steps: adding the 1-isopropyl-3-tert-butylthiourea mother liquor into a heating box, and raising the temperature in the heating box to a certain temperature; feeding hydrochloric acid in the feeding bin into the heating box through the feeding pipe, adjusting the PH value, and performing heat preservation and stirring for a period of time; placing the obtained solution in the heat preservation box to be precipitated for a period of time, performing standing, cooling and crystallization to obtain precipitate and supernatant, and then stirring the precipitate for half an hour; and placing the filter cloth bag in the filter box to be centrifuged, obtaining a wet product, and then drying the wet product to obtain a 1-isopropyl-3-tert-butyl thiourea dry product, so that the consumption of raw materials can be reduced, and the quality and the yield of the product can be improved.

Description

technical field [0001] The invention relates to the technical field of preparation of buprofezin intermediates, in particular to a method and device for effectively utilizing the mother liquor of buprofezin intermediate 1-isopropyl-3-tert-butylthiourea to increase yield. Background technique [0002] Buprofezin is a new insect growth regulator with high efficiency, long duration, strong selectivity and safety. It is mainly used for the control of leafhoppers, planthoppers, whiteflies and scale insects in crops such as rice, vegetables, tea and citrus. It is currently the leading variety for the control of rice planthoppers. [0003] At present, the synthesis of Buprofezin is based on the reaction of ammonium thiocyanate as raw material and tert-butanol in the presence of hydrochloric acid to obtain a mixture of tert-butyl thiocyanate and tert-butyl isocyanate (mixed ester for short), which is obtained by transposition Butyl isothiocyanate (abbreviated as isoester), reacted...

Claims

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Application Information

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IPC IPC(8): C07C335/08B01J19/18
CPCC07C335/08B01J19/18
Inventor 姚修宇范锦龙杨玉坤李卫徐晓东陈建国姜育田朱学军唐素荣万金方于同锋
Owner JIANGSU ANPON ELECTROCHEM