CN1648120A

CN1648120A - Zineb synthesizing process

Info

Publication number: CN1648120A
Application number: CN 200410103252
Authority: CN
Inventors: 黄志刚
Original assignee: Individual
Current assignee: Individual
Priority date: 2004-12-30
Filing date: 2004-12-30
Publication date: 2005-08-03

Abstract

The new zineb synthesizing process features that ambam is first synthesized with ethylenediamine, carbon disulfide and ammonia water, and then reacted with zinc chloride to synthesize zineb. The present invention has the useful effects of simple preparation process, zineb product reaching ideal state in zinc content, false specific weight, water content, stability, etc., easy crushing of zineb product in producing into wettable powder, and suspension rate over 80 %.

Description

New zineb synthesizing process

The technical field is as follows:

the invention relates to a pesticide technology, in particular to a synthesis method of a plant bactericide, and specifically relates to a new synthesis process of zineb.

Background art:

zineb is a high-efficiency, low-toxicity, broad-spectrum and protective organic sulfur bactericide and is used for preventing and treating a plurality of diseases of various crops, such as wheat rust, gibberellic disease, rice blast and leaf blight, apple and pear scab, black spot disease, flower rot, grape downy mildew, anthracnose of peach trees, cucumber downy mildew, tobacco damping-off, beet brown spot and the like. In 1943, Rhom and Haas co. was successfully developed, and China began to put into production and use in 1965.

The traditional production method comprises the following steps:

1. synthesis of sodium metiram

2. Synthesis of zineb

The zineb produced by the method is superficially higher in content, yellowish in color and free of abnormal other indexes, but further analysis shows that the content of zinc in the zineb is possibly lower than the theoretical zinc content in the molecular structure, namely, sodium zineb and zinc chloride cannot fully react to form real zineb, while the analysis of the zineb is a chemical analysis method, carbon disulfide is released by acidolysis, the content of the zineb is measured and calculated according to two carbon disulfides, namely, as long as substances in a sample can be acidolyzed to release the carbon disulfide, effective components are calculated, and the situation of high content exists, when the zineb is stored, the stability is poor, 85% of original medicine produced by manufacturers in China is exported abroad, after a period of time, the content is greatly reduced due to decomposition, foreign claims are frequently found, and the original medicine is processed into wettable powder, the suspension rate and the fineness can hardly reach an ideal target, and the suspension rate after processing is only 30-40% generally, so that the suspension rate of the zineb wettable powder specified by the national standard is only 60%, the FAO is also only 70%, and the domestic zineb hardly reaches the national standard and the international standard. Many manufacturers crush the original drug by adopting airflow, the energy consumption is very large, or import auxiliary agents are adopted to improve the suspension rate, the processing cost is greatly improved, the inherent quality of the original drug cannot be changed by a physical method, and the drug effect is still thesame.

The invention content is as follows:

the invention aims to provide a novel zineb synthesis process which is simple in method, high in zinc content, good in stability, especially high in suspension rate and can be greatly higher than the FAO standard.

The technical solution of the invention is as follows: a new zineb synthesis process is characterized in that: firstly, synthesizing ambam by using ethylenediamine, carbon disulfide and ammonia water, and then synthesizing zineb by using the ambam and zinc chloride.

In the synthesis of ambam, the amounts of ethylenediamine, carbon disulfide and 40% ammonia water are respectively as follows: 150-210Kg, 441-541Kg and 500-590Kg or in the same proportion; when synthesizing zineb, the dosage of the zineb and the zinc chloride are respectively as follows: 1000-1400Kg, 200-250Kg or the same ratio. When synthesizing ambam, the dosage of ethylenediamine, carbon disulfide and 40% ammonia water is respectively: 180Kg, 491Kg and 540Kg or in the same proportion; in the synthesis of zineb, dysonThe dosage of ammonium and zinc chloride is respectively: 1200Kg, 225Kg or in the same proportion. And adding a stabilizer in the process of synthesizing the ambam. The added stabilizer is sodium pyrosulfite, sodium sulfite or sodium hydrosulfite. Adding a catalyst in the process of synthesizing zineb. The added catalyst is Bi₂(MoO₄)₃、Ni/Al₂O₃Or Pol₆(CO)_X。

The invention has the beneficial effects that: the method is simple, the zineb technical can reach an ideal state from zinc content, bulk specific gravity, moisture content, stability and the like, when the zineb technical is processed into wettable powder, the index of jet milling can be reached only byordinary mechanical processing and milling, particularly, the suspension rate can reach more than 80 percent and is greatly higher than the FAO standard.

The invention is further illustrated by the following examples:

the specific implementation mode is as follows:

the first embodiment is as follows:

1. synthesis of amobam

2. Synthesis of zineb

Wherein, when synthesizing ambam, the dosage of ethylenediamine, carbon disulfide and 40% ammonia water is respectively: 180Kg, 491Kg, 540Kg or similar ratios; when synthesizing zineb, the dosage of the zineb and the zinc chloride are respectively as follows: 1200Kg, 225Kg or similar. And adding a stabilizer in the process of synthesizing the ambam (the addition amount can be according to the conventional method). The stabilizer added is sodium pyrosulfite (or sodium sulfite, sodium hydrosulfite, etc.), or other suitable stabilizers. The catalyst is added in the process of synthesizing zineb (the addition amount is according to the similar synthesis reaction). Catalyst of additionThe oxidant is Bi₂(MoO₄)₃(or is Ni/Al)₂O₃、Pol₆(CO)_XEtc.), or other suitable catalysts.

The invention adopts ammonia water to replace caustic soda when synthesizing the sodium metiram, so as to control the pH value of the synthesis and produce the ammonium metiram, a stabilizing agent is added in the synthesis process to improve the actual ammonium metiram, an accessory product with acarbon disulfide group is removed, the decomposition of the ammonium metiram is reduced, a catalyst is added in the reaction of the ammonium metiram and a zinc salt solution, the double decomposition reaction can be accelerated, so as to ensure that the zinc ions in the ammonium metiram and the zinc salt are carried out with theoretical reaction equivalent, and an intermediate product is removed, so that the zinc metiram is uniformly distributed in the reaction solution, particles are reduced, and hard particles generated due to high temperature when drying are reduced. By the measures, the zineb technical can reach an ideal state from zinc content, bulk specific gravity, moisture content, stability and the like, when the zineb technical is processed into wettable powder, the index of jet milling can be reached only by ordinary mechanical processing and milling, particularly the suspension rate can reach more than 80 percent and is greatly higher than the FAO standard. The invention improves the condensation and replacement in the production process, so that the quality of the zineb technical reaches a qualitative leap.

Example two:

1. synthesis of amobam

2. Synthesis of zineb

Wherein, when synthesizing ambam, the dosage of ethylenediamine, carbon disulfide and 40% ammonia water is respectively: 150Kg, 441Kg, 500Kg or in the same proportion; when synthesizing zineb, the dosage of the zineb and the zinc chloride are respectively as follows: 1000Kg, 200Kg or the same ratio. And adding a stabilizer in the process of synthesizing the ambam (the addition amount can be according to the conventional method). The stabilizer added is sodium sulfite (or other stabilizer with similar effect). The catalyst is added in the process of synthesizing zineb (the addition amount can be according to the conventional method). The added catalyst is Ni/Al₂O₃(or other catalysts with similar action).

Example three:

1. synthesis of amobam

2. Synthesis of zineb

Wherein, when synthesizing ambam, the dosage of ethylenediamine, carbon disulfide and 40% ammonia water is respectively: 210Kg, 541Kg, 590Kg or the same proportion; when synthesizing zineb, the dosage of the zineb and the zinc chloride are respectively as follows: 1400Kg, 250Kg or the same ratio. And adding a stabilizer in the process of synthesizing the ambam (the addition amount can be according to the conventional method). The added stabilizer is sodium hydrosulfite (or other stabilizers with similar functions). The catalyst is added in the process of synthesizing zineb (the addition amount can be according to the conventional method). The added catalyst is or Pol₆(CO)_x(or other catalysts with similar action).

Example four:

1. synthesis of amobam

2. Synthesis of zineb

Wherein, when synthesizing ambam, the dosage of ethylenediamine, carbon disulfide and 40% ammonia water is respectively: 160Kg, 530Kg, 550Kg or the same ratio; when synthesizing zineb, the dosage of the zineb and the zinc chloride are respectively as follows: 1100Kg, 240Kg or in the same proportion. The stabilizer is added during the synthesis of amobam (the amount added may be in accordance with the amount added in a generally similar synthesis reaction). The stabilizer added is sodium metabisulfite (or other stabilizer with similar effect). The catalyst is added during the synthesis of zineb (the amount added can be in accordance with the amount added in a generally similar synthesis reaction). The added catalyst is Bi₂(MoO₄)₃(or other catalysts with similar action).

Example five:

1. synthesis of amobam

2. Synthesis of zineb

Wherein, when synthesizing ambam, the dosage of the ethylenediamine, the carbon disulfide and the 40 percent ammonia water is divided intoRespectively, the following steps: 200Kg, 461Kg, 560Kg or in the same proportion; when synthesizing zineb, the dosage of the zineb and the zinc chloride are respectively as follows: 1300Kg, 210Kg or the same ratio. The stabilizer is added during the synthesis of amobam (the amount added may be in accordance with the amount added in a generally similar synthesis reaction). The stabilizer added is sodium sulfite (or other stabilizer with similar effect). The catalyst is added during the synthesis of zineb (the amount added can be in accordance with the amount added in a generally similar synthesis reaction). The added catalyst is Ni/Al₂O₃(or other catalysts with similar action).

Claims

1. A new zineb synthesis processis characterized in that: firstly, synthesizing ambam by using ethylenediamine, carbon disulfide and ammonia water, and then synthesizing zineb by using the ambam and zinc chloride.

2. The new zineb synthesis process as set forth in claim 1, characterized in that: when synthesizing ambam, the dosage of ethylenediamine, carbon disulfide and 40% ammonia water are respectively: 150-210Kg, 441-541Kg and 500-590Kg or in the same proportion; when synthesizing zineb, the dosage of the zineb and the zinc chloride are respectively as follows: 1000-1400Kg, 200-250Kg or the same ratio.

3. The new zineb synthesis process as set forth in claim 1, characterized in that: when synthesizing ambam, the dosage of ethylenediamine, carbon disulfide and 40% ammonia water are respectively: 180Kg, 491Kg and 540Kg or in the same proportion; when synthesizing zineb, the dosage of the zineb and the zinc chloride are respectively as follows: 1200Kg, 225Kg or in the same proportion.

4. The new zineb synthesis process according to claim 1, 2 or 3, characterized by: and adding a stabilizer in the process of synthesizing the ambam.

5. The new zineb synthesis process as set forth in claim 4, wherein: the added stabilizer is sodium pyrosulfite, sodium sulfite or sodium hydrosulfite.

6. The new zineb synthesis process according to claim 1, 2 or 3, characterized by: adding a catalyst in the process of synthesizing zineb.

7. The new zineb synthesis process as set forth in claim 6, wherein: the added catalyst is Bi₂(MoO₄)₃、Ni/Al₂O₃Or Pol₆(CO)_X。