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A preparation method for improving the ratio of 1,3-position normal form dimehypo

A technology of dimehypo and normal form, which is applied in the field of chemical chemistry, can solve the problems of many internal isomers of dimehypo and product quality not up to standard, and achieve the goal of reducing production costs, improving effectiveness, and increasing process yield Effect

Active Publication Date: 2017-02-22
HUNAN HAOHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The domestic production of cartap is based on the monosultap obtained from the crystallization of the sulfonated liquid dimehypo as the raw material, mainly because the sulfonated liquid dimehypo is too many endoisomers, and the product quality cannot meet the standard

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In the embodiment of the present invention, a preparation method for increasing the ratio of the 1,3-position normal form in the sulfonated liquid dimehypo, the specific steps are as follows:

[0025] (1) Take by weighing 280g60% chloride and put it into a 1000mL four-necked flask equipped with stirring;

[0026] (2) Add methanol 200mL;

[0027] (3) Lower the temperature to 0°C, add 32g of caustic soda to the four-necked bottle, and adjust the pH value of the chloride to 7;

[0028] (4) Add 1 g of benzyltrimethylammonium bromide to the four-necked flask;

[0029] (5) Add 406 g of sodium thiosulfate to the four-necked flask, and perform sulfonation reaction at a temperature of 80° C. for 1.5 hours;

[0030] (6) remove and reclaim methanol;

[0031] (7) desalting by centrifugation to obtain sulfonated liquid insecticidal double product;

[0032] (8) Measure the mass percentage of the dimehypo normal isomer of the sulfonated liquid with high performance liquid chromato...

Embodiment 2

[0034] In the embodiment of the present invention, a preparation method for increasing the ratio of the 1,3-position normal form in the sulfonated liquid dimehypo, the specific steps are as follows:

[0035] (1) Take by weighing 300g52% chloride and put it into a 1000mL four-necked flask equipped with stirring;

[0036] (2) Add methanol 220mL;

[0037] (3) Lower the temperature to 20°C, add 25g of soda ash to the four-necked bottle, and adjust the pH value of the chloride to 6.5;

[0038] (4) Add cetyltrimethylammonium bromide 6g in the four-necked bottle;

[0039] (5) Add 390 g of sodium thiosulfate to the four-necked flask, and perform sulfonation reaction at a temperature of 70° C. for 2 hours;

[0040] (6) remove and reclaim methanol;

[0041] (7) desalting by centrifugation to obtain sulfonated liquid insecticidal double product;

[0042] (8) Measure the mass percent of the dimehypo normal isomer of the sulfonated liquid with high performance liquid chromatography, 1,...

Embodiment 3

[0044] In the embodiment of the present invention, a preparation method for increasing the ratio of the 1,3-position normal form in the sulfonated liquid dimehypo, the specific steps are as follows:

[0045] (1) Take by weighing 312g50% chloride and put it into a 1000mL four-necked flask equipped with stirring;

[0046] (2) Add methanol 260mL;

[0047] (3) Lower the temperature to -3°C, add 67g of ammonia water to the four-necked bottle, and adjust the pH value of the chloride to 8.0;

[0048] (4) Add tetrabutylammonium bisulfate 10g in the four-necked bottle;

[0049] (5) Add 447 g of sodium thiosulfate to the four-necked flask, and perform sulfonation reaction at a temperature of 65° C. for 4 hours;

[0050] (6) remove and reclaim methanol;

[0051] (7) desalting by centrifugation to obtain sulfonated liquid insecticidal double product;

[0052] (8) Measure the mass percent of the dimehypo normal isomer of the sulfonated liquid with high performance liquid chromatography...

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Abstract

The invention discloses a preparation method capable of increasing a proportion of 1,3-bit normal compound in bisultap. The preparation method comprises the following steps: using chloride, thiosulfate and alkali as raw materials, in the existence of a catalyst and at the temperature of 40-90 DEG C, taking a reaction for 1-8 hours, and preparing bisultap. According to the bisultap produced by the preparation method, the proportion of the 1,3-bit normal compound in a sulfonated liquid bisultap is high; compared with the bisultap prepared by the conventional process, the 1,3-bit normal compound is higher than 3-5%; the sulfonated liquid bisultap can be directly used for producing cartap, so that the production cost of cartap is lowered; the problem that in the method of utilizing the bisultap crystal to produce monosultap, bisultap can be still generated; a novel technology and a novel method of using the sulfonated liquid bisultap to directly produce cartap and preparing high-quality raw materials are provided; the preparation method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of chemical engineering, in particular to a preparation method for increasing the ratio of 1,3-position orthomorph dimehypo. Background technique [0002] Dimehypo is a nereistoxins insecticide. It is a broad-spectrum, safe and economical insecticide with high efficiency, moderate toxicity, contact and systemic conduction of gastric poisoning and certain ovicidal efficacy. It is a pesticide variety independently developed by our country. It can control rice, wheat, sugar cane, vegetables, cotton, fruit trees and other pests. It is produced from allyl chloride, dimethylamine, sodium bicarbonate and other raw materials through amination, acidification, dehydration, chlorination, sulfonation and other processes. Sulfonated liquid dimehypo is a crude product, and the crude product of sulfonated liquid dimehypo has normal form and isomer, namely 2-N,N-dimethylamino-1,3-dithiosulfonic acid X propane (normal form), 3-N,N-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C381/02
Inventor 袁美和
Owner HUNAN HAOHUA CHEM
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