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Preparing method for synthesizing sanmate from calcium cyanamide

A technology of lime nitrogen and carbendazim, which is applied in the field of preparation of carbendazim by using lime nitrogen, can solve the problems of low yield and excessive waste water, and achieve the effects of high waste water concentration, increased concentration, and reduced energy consumption

Inactive Publication Date: 2011-05-25
XINYI AGRI CHEM PLANT JIANGSU PROV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] In order to solve the problem of excessive waste water and low yield in the production of carbendazim by using lime nitrogen as raw material in the prior art, the present invention aims to provide a synthetic cyanamide aqueous solution using industrial lime nitrogen as raw material to produce carbendazim , Compared with the traditional process, it improves the yield, reduces the discharge of three wastes, and reduces the cost of the process

Method used

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  • Preparing method for synthesizing sanmate from calcium cyanamide
  • Preparing method for synthesizing sanmate from calcium cyanamide
  • Preparing method for synthesizing sanmate from calcium cyanamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] 1) Put 1350ml of water or the last batch of washing liquid (need to make up if less than 1350ml) into a 2000ml four-necked bottle equipped with a thermometer, carbon dioxide ventilation device, condenser, and stirrer. The washing liquid is mentioned in step 3) below washing liquid;

[0063] 2) The temperature is controlled at 0°C, and 250g of lime nitrogen (effective nitrogen content 21%) is slowly added, and 82.5g of carbon dioxide gas is introduced during the feeding process to keep the pH value of the solution at 6;

[0064] 3) After feeding, vacuum filter, the filtrate is to adjust the pH value, wash the filter cake 4 times with 800ml of water, and collect the washing liquid to be used in the next batch of feeding;

[0065] 4) The filtrate is adjusted to pH 4 with an appropriate amount of 10% phosphoric acid, and then suction filtered to remove a small amount of solid impurities;

[0066] 5) The filtrate is concentrated in a rotary evaporator under reduced pressure...

Embodiment 2

[0072] 1) Put 500ml of water or the last batch of washing liquid (less than 500ml needs to be supplemented) into a 2000ml four-necked bottle equipped with a thermometer, carbon dioxide ventilation device, condenser, and stirrer. The washing liquid is mentioned in step 3) below. washing liquid;

[0073] 2) The temperature is controlled within the range of 50°C, and 250g of lime nitrogen (effective nitrogen content 21%) is slowly added, and 123.75g of carbon dioxide gas is introduced during the feeding process to keep the pH value of the solution at 9;

[0074] 3) After feeding, vacuum filter, the filtrate is to adjust the pH value, wash the filter cake with 500ml of water 4 times, and collect the washing liquid to be used in the next batch of feeding;

[0075] 4) The filtrate is adjusted to pH 6 with an appropriate amount of 80% phosphoric acid, and then suction filtered to remove a small amount of solid impurities;

[0076] 5) The filtrate is concentrated in a rotary evaporat...

Embodiment 3

[0082] 1) Put 800ml of water or the last batch of washing liquid (need to make up if less than 800ml) into a 2000ml four-necked bottle equipped with a thermometer, carbon dioxide ventilation device, condenser, and stirrer. The washing liquid is mentioned in step 3) below washing liquid;

[0083] 2) The temperature is controlled at 30°C, and 250g of lime nitrogen (effective nitrogen content 21%) is slowly added, and 91.67g of carbon dioxide gas is introduced during the feeding process to keep the pH value of the solution at 7;

[0084] 3) After feeding, vacuum filter, the filtrate is to adjust the pH value, wash the filter cake 4 times with 800ml of water, and collect the washing liquid to be used in the next batch of feeding;

[0085] 4) The filtrate is adjusted to a pH value of 5 with an appropriate amount of 60% phosphoric acid, and then suction filtered to remove a small amount of solid impurities;

[0086] 5) The filtrate is concentrated in a rotary evaporator under reduced...

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Abstract

The invention relates to a preparing method for synthesizing sanmate from calcium cyanamide, in particular to the preparing method for synthesizing the sanmate and generating single-cyanamide water solution from the calcium cyanamide through hydrolytic decalcification. The process flow in the preparing method disclosed by the invention comprises the following steps: 1. hydrolytic decalcification work procedures; 2. amination work procedures; and 3. condensation work procedures and the like. Auxiliary steps such as acid regulation work procedures, exsolution work procedures, cooling work procedures and the like are also included between the hydrolytic decalcification work procedures and the amination work procedures. In the sanmate preparing process, the preparing method disclosed by the invention has high yield, the quantity of generated three-wastes is decreased, consumed raw materials are reduced through being compared with that of the traditional process, the environment protection treatment cost is reduced, and good economic benefits and social benefits are realized.

Description

technical field [0001] The invention relates to a production process of the original drug of carbendazim, in particular to a process for generating cyanamide aqueous solution and synthesizing carbendazim by hydrolysis and decalcification of lime nitrogen. Background technique [0002] Carbendazim is a systemic fungicide of benzimidazoles, whose scientific name is 2-methyl benzimidazole carbamate, referred to as MBC. The industrial product is white or taupe powder. The pure product has a melting point of 330-335°C. It is slightly soluble in water and organic solvents. It can be dissolved in acid to form a salt. It is stable in nature, but it is easy to decompose when it meets alkali. Its toxicity is low, and the half-lethal dose of acute toxicity is LD50 value: it is greater than 15g / kg for rats orally. Carbendazim can be absorbed by plants and transferred to other parts through conduction, interfering with the mitosis of pathogen cells and inhibiting their growth. It is ef...

Claims

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Application Information

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IPC IPC(8): C07D235/32
Inventor 郑善龙纪传武巩绪干骆志才王子成
Owner XINYI AGRI CHEM PLANT JIANGSU PROV
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