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Catalyst and preparation process of tert-butyl isothiocyanate

A technology of tert-butyl isothiocyanate and isothiocyanate, which is applied in the field of preparation of tert-butyl isothiocyanate, can solve problems such as high viscous substances, production environment impact, etc., and achieves the effects of easy separation and improved preparation environment

Active Publication Date: 2020-07-28
江苏再拓生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is in order to solve above-mentioned deficiencies in the prior art, will produce highly viscous substance in the process of converting zinc chloride isomeric tert-butyl thiocyanate into tert-butyl isothiocyanate in the traditional process, which is harmful to the production environment Influenced problems, a catalyst for the preparation of tert-butyl isothiocyanate and a preparation process for tert-butyl isothiocyanate are proposed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0018] The preparation technique of tert-butyl isothiocyanate is described in detail:

[0019] According to the parts by mass, 70-85 parts of ammonium thiocyanate, 200 parts of water, 65-90 parts of 85% tert-butanol and 200-250 parts of 30% hydrochloric acid are taken.

[0020] Add ammonium thiocyanate into water and stir to obtain ammonium thiocyanate solution, add 85% tert-butanol to the ammonium thiocyanate solution and raise the temperature to 45°C-50°C to obtain a mixed solution, add dropwise to the mixed solution 30% hydrochloric acid, the dropwise addition time is 30±5min, and the stirring is continued during the dropping process, and the stirring is continued for 30min~90min after the 30% hydrochloric acid is added dropwise. Stop stirring and let stand to stratify, and take the upper layer material.

[0021] Transfer the upper material to the drying container, the volume of the drying container is 1 to 1.5 times the water volume, raise the temperature to 50 ° C ~ 60 °...

Embodiment 1

[0023] Add 76.1 grams of ammonium thiocyanate into 200 g of water, stir and dissolve, add 87 grams of 85% tert-butanol, heat up to 45°C, add 220 g of 30% hydrochloric acid within 30 minutes, keep the reflux state for 2 hours, stop stirring and divide Lower floor water, supernatant material obtains 96 grams, detects that tert-butyl thiocyanate content is 54%, and tert-butyl isothiocyanate is 46%.

[0024] The material was transferred to a dry 250 ml flask, heated up to 50°C, the flask was evacuated to 0.09MPa, the glass tube inserted into the material was connected to the hydrogen chloride cylinder, the valve was opened, and the pressure in the flask was returned to normal pressure. After keeping for 30 minutes, nitrogen replacement. Sampling was carried out to detect that the content of tert-butyl isothiocyanate was 98.3%.

Embodiment 2

[0026] Add 95 grams of ammonium thiocyanate into 250 g of water, stir and dissolve, add 87 grams of 85% tert-butanol, raise the temperature to 45-50°C, add 250 g of 30% hydrochloric acid within 30 minutes, keep the reflux state for 1.5 hours, stop stirring and divide The lower layer of water is removed, and the upper layer material obtains 105 grams, and the detection content of tert-butyl thiocyanate is 51%, and the content of tert-butyl isothiocyanate is 48%.

[0027] The material was transferred to a dry 250 ml flask, the temperature was raised to 55° C., the flask was evacuated to 0.08 MPa, the glass tube inserted into the material was connected to the hydrogen chloride cylinder, the valve was opened, and the pressure in the flask was returned to normal pressure. After keeping for 25 minutes, nitrogen replacement. Sampling was carried out to detect that the content of tert-butyl isothiocyanate was 98.5%.

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Abstract

The invention discloses a catalyst and a preparation process of tert-butyl isothiocyanate. The catalyst is dry hydrogen chloride gas. The preparation method comprises the following steps: taking 70-85parts by mass of ammonium thiocyanate, 200 parts by mass of water, 65-90 parts by mass of 85% tert-butyl alcohol and 200-250 parts by mass of 30% hydrochloric acid, dissolving ammonium thiocyanate inwater, adding 85% tert-butyl alcohol, heating, dropwise adding 30% hydrochloric acid, standing for layering, taking an upper-layer material, transferring the upper-layer material into a drying container, heating to 50-60 DEG C, carrying out vacuumizing operation, introducing dry hydrogen chloride gas into a vacuumizing drying container, closing a valve until the drying container returns to normalpressure, maintaining for 30+ / -5 minutes, and carrying out nitrogen replacement to obtain tert-butyl isothiocyanate. According to the method, the dried hydrogen chloride gas is used as the catalyst for preparing tert-butyl isothiocyanate, hydrogen chloride is easy to separate, no by-product is generated, the prepared tert-butyl isothiocyanate reaches 98% or above, and meanwhile, the preparation environment of tert-butyl isothiocyanate can be effectively improved.

Description

technical field [0001] The invention relates to a catalyst for preparing tert-butyl isothiocyanate and a preparation process of tert-butyl isothiocyanate, belonging to the technical field of tert-butyl isothiocyanate preparation. Background technique [0002] The chemical name of buprofezin is 2-t-butylimino-3-isopropyl-5-phenyl-1,3,5-thiadiazin-4-one, and the molecular formula is C 16 h 23 N 3 OS, first successfully developed by a Japanese pesticide company, is a new type of selective insecticide that inhibits the growth and development of insects. It has a strong contact effect and stomach toxicity. The mechanism of action is to inhibit the synthesis of insect chitin and interfere with metabolism, causing nymphs to peel off Post-deformation or malformation of adult wings and slow death. Generally, it will take 3 to 7 days after the application of the pesticide to be effective. It has no direct lethality to adults, but it can shorten the life span and reduce the amount o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/10C07C331/20
CPCB01J27/10C07C331/20Y02P20/584
Inventor 任天瑞陈福勇
Owner 江苏再拓生物科技有限公司
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