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Method for synthesizing herbicide raw medicine

A synthesis method and herbicide technology, which is applied in the field of synthesis of herbicide technical materials, can solve the problems of inability to industrialize production, large amount of ethanol, and large investment in industrialization, and achieve the effects of simple and reliable production process, high yield and product purity

Inactive Publication Date: 2017-03-15
枣阳市先飞高科农药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The amount of ethanol used is large, and at the same time, the loss is large, the industrialization investment is large, and the economic benefit is poor, so it cannot be industrialized so far.
Another example: Toluene and xylene are used as auxiliary agents for crystallization and purification. In industrialization, the crystallization and auxiliary agents cannot be separated, and the purpose of purification cannot be achieved, resulting in failure.

Method used

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  • Method for synthesizing herbicide raw medicine

Examples

Experimental program
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Effect test

Embodiment 1

[0020] like figure 1 As shown, the synthetic method of a kind of herbicide former drug of the present embodiment comprises the following processing steps:

[0021] (1) Preparation of raw materials: the raw materials for the production of the herbicide technical drug include the following components (parts by weight): 30 parts of sec-butylamine, 80 parts of 2,6-dinitro-p-tertiary chlorobenzene, 40 parts of NaOH solution, clear water 100 parts, 15 parts of sodium metabisulfite, wherein the purity of sec-butylamine is 99%, and the concentration of NaOH solution is 40%;

[0022] (2) Mixing and preheating of the reaction kettle: add 2,6-dinitro-p-tertiary chlorobenzene and water into the reaction kettle, heat and stir, and the heating temperature is 80°C. After stirring, let stand for a period of 15min, the upper layer waste liquid is separated after standing, and the stirring time is 20min;

[0023] (3) solution neutralization treatment: add NaOH solution to the solution after s...

Embodiment 2

[0027] Example 2: The rest are the same as Example 1, except that the production raw materials in the step (1) include the following components (parts by weight): 25 parts of sec-butylamine, 2,6-dinitro-p-tertyl 70 parts of chlorobenzene, 35 parts of NaOH solution, 90 parts of clear water, and 12 parts of sodium metabisulfite, wherein the purity of sec-butylamine is 98%, the concentration of NaOH solution is 38%, the stirring time in the step (2) is 18min, heating The temperature is 70°C, the standing time is 12min, the heating temperature in the step (4) is 80°C, the stirring time is 20min, and the standing time is 25min. The addition time is 1.2h, the reaction temperature is 45°C, the reaction time is 1.2h, and the heating temperature in the step (6) is 95°C.

Embodiment 3

[0028] Example 3: the rest are the same as Example 1, except that the production raw materials in the step (1) include the following components (parts by weight): 30 parts of sec-butylamine, 2,6-dinitro-p-tertyl 80 parts of chlorobenzene, 40 parts of NaOH solution, 100 parts of clear water, and 15 parts of sodium metabisulfite, wherein the purity of sec-butylamine is 99%, the concentration of NaOH solution is 40%, the stirring time in the step (2) is 20min, heating The temperature is 80°C, the standing time is 15min, the heating temperature in the step (4) is 90°C, the stirring time is 25min, and the standing time is 30min. The addition time is 1.2h, the reaction temperature is 50°C, the reaction time is 1.5h, and the heating temperature in the step (6) is 100°C.

[0029] After the above process steps, take out the herbicide technical sample, and obtain the following data:

[0030] serial number purity yield Example 1 95.6％ 92％ Example 2 96.4％ 92.5...

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Abstract

The invention discloses a method for synthesizing a herbicide raw medicine, and relates to the pesticide production field. The method includes six technological processes of raw material preparation, reaction kettle mixing preheating, solution neutralizing treatment, sulfonation reaction, amination reaction and washing layering treatment; with use of the sulfonation reaction of 2,6-dinitro p-tert chlorobenzene and sodium pyrosulfite and the amination reaction of 2,6-dinitro p-tert chlorobenzene and sec-butylamine, the herbicide raw medicine with relatively high purity can be prepared; moreover, with multiple use of clear water for washing, the production process is simple and reliable, recrystallization is not needed, the high-purity product can be obtained, the yield and the product purity are high, an efficient herbicide product can be obtained, and the method is worthy of promotion.

Description

technical field [0001] The invention relates to the field of pesticide production, in particular to a method for synthesizing a herbicide original drug. Background technique [0002] Herbicides are agents that can kill weeds completely or selectively, also known as herbicides, and are a class of substances used to eliminate or inhibit plant growth. Among them, sodium chlorate, borax, arsenate, and trichloroacetic acid have the effect of withering on any kind of plants, and their effects are affected by three factors: herbicides, plants and environmental conditions. Although, in the prior art, there is a crystallization method to purify the herbicide original drug, and domestic counterparts have also carried out a lot of work. If anhydrous ethanol is used as an auxiliary agent for crystallization, the final product content can also reach more than 95%, but three steps of recrystallization are required to achieve this. The amount of ethanol used is large, and at the same tim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/22C07C309/48
CPCC07C303/04C07C303/22C07C309/40C07C309/48
Inventor 李建新
Owner 枣阳市先飞高科农药有限公司
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