CN102432504A - Preparation method of alpha-type crystal lattice chlorothalonil - Google Patents
Preparation method of alpha-type crystal lattice chlorothalonil Download PDFInfo
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- CN102432504A CN102432504A CN2010102956717A CN201010295671A CN102432504A CN 102432504 A CN102432504 A CN 102432504A CN 2010102956717 A CN2010102956717 A CN 2010102956717A CN 201010295671 A CN201010295671 A CN 201010295671A CN 102432504 A CN102432504 A CN 102432504A
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- tetrachlorophthalodinitrile
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Abstract
The invention discloses a preparation method of alpha-type crystal lattice chlorothalonil, which belongs to the field of the manufacturing of agricultural bactericides. Chlorothalonil is an efficient and safe broad-spectrum bactericide; crystal lattices of the chlorothalonil have three kinds of distribution, which are generally called as an alpha type, a beta type and a gamma type; due to the reasons of a current production process, alpha-type crystal lattice chlorothalonil obtained in an industrial product is less; beta-type crystal lattice chlorothalonil is the most; and gamma-type crystal lattice chlorothalonil is extremely few, wherein the alpha-type crystal lattice chlorothalonil is the most stable at a normal temperature; and the bactericidal activity of a preparation after being processed is the best. The preparation method of the alpha-type crystal lattice chlorothalonil comprises the following steps: crushing mixed crystal lattice chlorothalonil particles, sending the crushed particles into a warehouse, hermetically heating to a temperature between 80 DEG C and 120 DEG C, preserving heat for 6-10 days, and then, making the alpha-type crystal lattice chlorothalonil once on a large scale. The method has the advantages that the emission is zero, the pollution is free, the one-time conversion quantity is large, a crystal seed is not necessary to be added, and the like.
Description
Technical field:
The invention belongs to disinfectant use in agriculture and make the field, it is characterized in that relating to a kind of α type lattice m-tetrachlorophthalodinitrile.
Background technology:
M-tetrachlorophthalodinitrile, chemical name: 2,4,5,6-tetrachloro-1,3-dicyanobenzenes, molecular formula: C
8N
2Cl
4Molecular weight: 265.91, fusing point: 250 ℃-251 ℃, boiling point: 350 ℃; Pure article are white tasteless powder, solubleness (25 ℃): 0.0006g/L in the water, 80g/L in the YLENE; Acetone 2g/L, 30g/L in pimelinketone, the N, in the kerosene≤10g/L; Stable under the storage at normal temperature condition, to weak base or weak acidic medium and stable, decompose in highly basic medium first to illumination.M-tetrachlorophthalodinitrile at first by the exploitation of U.S. diamond system alkali company, was introduced China in 1963 then.M-tetrachlorophthalodinitrile is a kind of efficient, safe wide-spectrum bactericide; Its mechanism of action is: can have an effect with the glyceraldehyde 3-phosphate dehydrogenase among the fungal cell; Combine with the protein that contains halfcystine in this enzyme; Thereby destroy this enzymic activity, fungal cell's metabolism is damaged and loses one's life power.Inhale conduction in m-tetrachlorophthalodinitrile does not have, but after being sprayed onto on the plant materials, good tackiness can be arranged on body surface, be difficult for being fallen, so the drug effect phase is longer by rain drop erosion.M-tetrachlorophthalodinitrile belongs to the low toxicity sterilant, and former powder rat acute per os and rabbit are acute through skin LD50＞10000mg/kg, and lagophthalmos is had the intense stimulus effect, with some human eye tangible hormesis are arranged, and be big to toxicity of fish.M-tetrachlorophthalodinitrile is mainly used in the control of rust, anthrax, Powdery Mildew, oidium on fruit tree, the vegetables.The lattice of m-tetrachlorophthalodinitrile has three kinds of distributions, is commonly referred to α type (I type), β type (II type); γ type (III type), because present production technique, α type lattice is less in the m-tetrachlorophthalodinitrile that industrial goods obtain; β type lattice at most; γ type lattice is few, and wherein α type lattice m-tetrachlorophthalodinitrile is the most stable at normal temperatures, and the fungicidal activity of processing back preparation is best.But wet-milling and suspension concentrate like the processing of α type lattice m-tetrachlorophthalodinitrile are very big with the direct product processed difference of industrial goods mixing lattice m-tetrachlorophthalodinitrile on suspensibility, and the agricultural chemicals finished product of α type lattice m-tetrachlorophthalodinitrile processing is with the obvious advantage in each item index.How the m-tetrachlorophthalodinitrile (its staple is a β type lattice m-tetrachlorophthalodinitrile) of industrial goods mixing lattice is transformed α type lattice m-tetrachlorophthalodinitrile for this reason and just seem very urgent.In Chinese patent 200510095077.2, introduced a kind of method that industrial goods mixing lattice m-tetrachlorophthalodinitrile is converted into α type lattice m-tetrachlorophthalodinitrile in detail; This method is with industrial goods mixing lattice m-tetrachlorophthalodinitrile method of separating out of crystallisation by cooling again after the heating for dissolving in the organic solvent of low carbon chain; This method effect is better, but solvent consumption is bigger, and needs to add crystal seed; Unit cost is very high, has limited use range.Therefore seek a kind of method that cheaply industrial goods mixing lattice m-tetrachlorophthalodinitrile is converted into α type lattice m-tetrachlorophthalodinitrile and seem very urgent.
Summary of the invention:
In order to overcome the method complex process that solvent method transition transforms α type lattice m-tetrachlorophthalodinitrile; Production cost is high; Need to add the defective of crystal seed, the problem that the present invention mainly solves provides the method that also can in enormous quantities industrial goods mixing lattice m-tetrachlorophthalodinitrile be converted into α type lattice m-tetrachlorophthalodinitrile that a kind of technology is simple, production cost is extremely low.This method has zero release, and is pollution-free, and one time formation number is big, need not add advantages such as crystal seed.
The present invention can realize through following technical scheme:
A kind of industrial goods mixing lattice m-tetrachlorophthalodinitrile is converted into the method for α type lattice m-tetrachlorophthalodinitrile, it is characterized in that constituting by following steps:
1. earlier industrial goods mixing lattice m-tetrachlorophthalodinitrile is pulverized with micronizer mill or mechanical crusher, the granularity after the pulverizing is greater than 200 orders.
2. be provided with one and can heat the sealing warehouse that also can be incubated; A plurality of open containers (the container number is confirmed by warehouse size) are set in the warehouse, and the characteristics of open container are mouthful big but the degree of depth is more shallow, and the degree of depth generally is no more than 0.3m; The postindustrial article mixing of above-mentioned pulverizing lattice m-tetrachlorophthalodinitrile is put into open container; With warehouse sealing, through steam or other thermal source in the warehouse air heating, and the air in the warehouse is constantly circulated through interchanger; Keep uniform heat distribution and temperature in the warehouse to be controlled between 80 ℃ of-120 ℃ of degree soaking time 6-10 days.
3.6-10 after it, stop heating, be cooled to normal temperature, open the sealing warehouse, the m-tetrachlorophthalodinitrile of the former mixing lattice in the open container has been converted into α type lattice m-tetrachlorophthalodinitrile at this moment, and transformation efficiency is 95%-99%.
Granularity after mixing lattice m-tetrachlorophthalodinitrile described in the above-mentioned steps 1 is pulverized should be greater than 200 orders.
Temperature in the above-mentioned steps 2 in the warehouse should be controlled between 80 ℃ of-120 ℃ of degree, soaking time 6-10 days.
The present invention compared with prior art has the following advantages:
1. industriallization will mix the lattice m-tetrachlorophthalodinitrile and be converted into α type lattice m-tetrachlorophthalodinitrile, and will be big, pollution-free in batches;
2. production cost is low, and social benefit is good;
3. production technique is simple, need not to increase visual plant, and is easy to operate, is easy to promote.
Embodiment:
Embodiment 1
Industrial goods mixing lattice m-tetrachlorophthalodinitrile is pulverized with micronizer mill or mechanical crusher, and the granularity after the pulverizing is greater than 200 orders; Be provided with one and can heat the sealing warehouse that also can be incubated; A plurality of open containers (number is confirmed by warehouse size) are set in the warehouse, and the characteristics of open container are mouthful big but the degree of depth is more shallow, and the degree of depth generally is no more than 0.3m; The postindustrial article mixing of above-mentioned pulverizing lattice m-tetrachlorophthalodinitrile is put into open container; With warehouse sealing, through steam or other thermal source in the warehouse air heating, and the air in the warehouse is constantly circulated through interchanger; Keep uniform heat distribution and temperature in the warehouse to be controlled at 80 ℃ of degree, soaking time 10 days; After 10 days, stop heating, be cooled to normal temperature, open the sealing warehouse, the former mixing lattice m-tetrachlorophthalodinitrile in the open container has been converted into α type lattice m-tetrachlorophthalodinitrile at this moment, and transformation efficiency is 95%-99%.
Embodiment 2
Industrial goods mixing lattice m-tetrachlorophthalodinitrile is pulverized with micronizer mill or mechanical crusher, and the granularity after the pulverizing is greater than 200 orders; Be provided with one and can heat the sealing warehouse that also can be incubated; A plurality of open containers (number is confirmed by warehouse size) are set in the warehouse, and the characteristics of open container are mouthful big but the degree of depth is more shallow, and the degree of depth generally is no more than 0.3m; The postindustrial article mixing of above-mentioned pulverizing lattice m-tetrachlorophthalodinitrile is put into open container; With warehouse sealing, through steam or other thermal source in the warehouse air heating, and the air in the warehouse is constantly circulated through interchanger; Keep uniform heat distribution and temperature in the warehouse to be controlled at 90 ℃ of degree, soaking time 9 days; After 9 days, stop heating, be cooled to normal temperature, open the sealing warehouse, the former mixing lattice m-tetrachlorophthalodinitrile in the open container has been converted into α type lattice m-tetrachlorophthalodinitrile at this moment, and transformation efficiency is 95%-99%.
Embodiment 3
Industrial goods mixing lattice m-tetrachlorophthalodinitrile is pulverized with micronizer mill or mechanical crusher, and the granularity after the pulverizing is greater than 200 orders; Be provided with one and can heat the sealing warehouse that also can be incubated; A plurality of open containers (number is confirmed by warehouse size) are set in the warehouse, and the characteristics of open container are mouthful big but the degree of depth is more shallow, and the degree of depth generally is no more than 0.3m; The postindustrial article mixing of above-mentioned pulverizing lattice m-tetrachlorophthalodinitrile is put into open container; With warehouse sealing, through steam or other thermal source in the warehouse air heating, and the air in the warehouse is constantly circulated through interchanger; Keep uniform heat distribution and temperature in the warehouse to be controlled at 100 ℃ of degree, soaking time 8 days; After 8 days, stop heating, be cooled to normal temperature, open the sealing warehouse, the former mixing lattice m-tetrachlorophthalodinitrile in the open container has been converted into α type lattice m-tetrachlorophthalodinitrile at this moment, and transformation efficiency is 95%-99%.
Embodiment 4
Industrial goods mixing lattice m-tetrachlorophthalodinitrile is pulverized with micronizer mill or mechanical crusher, and the granularity after the pulverizing is greater than 200 orders; Be provided with one and can heat the sealing warehouse that also can be incubated; A plurality of open containers (number is confirmed by warehouse size) are set in the warehouse, and the characteristics of open container are mouthful big but the degree of depth is more shallow, and the degree of depth generally is no more than 0.3m; The postindustrial article mixing of above-mentioned pulverizing lattice m-tetrachlorophthalodinitrile is put into open container; With warehouse sealing, through steam or other thermal source in the warehouse air heating, and the air in the warehouse is constantly circulated through interchanger; Keep uniform heat distribution and temperature in the warehouse to be controlled at 110 ℃ of degree, soaking time 7 days; After 7 days, stop heating, be cooled to normal temperature, open the sealing warehouse, the former mixing lattice m-tetrachlorophthalodinitrile in the open container has been converted into α type lattice m-tetrachlorophthalodinitrile at this moment, and transformation efficiency is 95%-99%.
Embodiment 5
Industrial goods mixing lattice m-tetrachlorophthalodinitrile is pulverized with micronizer mill or mechanical crusher, and the granularity after the pulverizing is greater than 200 orders; Be provided with one and can heat the sealing warehouse that also can be incubated; A plurality of open containers (number is confirmed by warehouse size) are set in the warehouse, and the characteristics of open container are mouthful big but the degree of depth is more shallow, and the degree of depth generally is no more than 0.3m; The postindustrial article mixing of above-mentioned pulverizing lattice m-tetrachlorophthalodinitrile is put into open container; With warehouse sealing, through steam or other thermal source in the warehouse air heating, and the air in the warehouse is constantly circulated through interchanger; Keep uniform heat distribution and temperature in the warehouse to be controlled at 120 ℃ of degree, soaking time 6 days; After 6 days, stop heating, be cooled to normal temperature, open the sealing warehouse, the former mixing lattice m-tetrachlorophthalodinitrile in the open container has been converted into α type lattice m-tetrachlorophthalodinitrile at this moment, and transformation efficiency is 95%-99%.
Claims (6)
1. the preparation method of a α type lattice m-tetrachlorophthalodinitrile, it is characterized in that: with industrial goods mixing lattice m-tetrachlorophthalodinitrile is raw material, obtains finished product through following steps.
2. the preparation method of a kind of α type lattice m-tetrachlorophthalodinitrile according to claim 1, the characteristic of its first step is: earlier industrial goods mixing lattice m-tetrachlorophthalodinitrile is pulverized with micronizer mill or mechanical crusher, the granularity after the pulverizing is greater than 200 orders.
3. the preparation method of a kind of α type lattice m-tetrachlorophthalodinitrile according to claim 1; The characteristic in its second step is: be provided with one and can heat the sealing warehouse that also can be incubated; A plurality of open containers (the container number is confirmed by warehouse size) are set in the warehouse, and the characteristics of open container are mouthful big but the degree of depth is more shallow, and the degree of depth generally is no more than 0.3m; Industrial goods mixing lattice m-tetrachlorophthalodinitrile after the above-mentioned pulverizing is put into open container; With warehouse sealing, through steam or other thermal source in the warehouse air heating, and the air in the warehouse is constantly circulated through interchanger; Keep uniform heat distribution and temperature in the warehouse to be controlled between 80 ℃ of-120 ℃ of degree soaking time 6-10 days.
4. the preparation method of a kind of α type lattice m-tetrachlorophthalodinitrile according to claim 1; The characteristic in its 3rd step is: after 6-10 days; Stop heating, be cooled to normal temperature, open the sealing warehouse; The m-tetrachlorophthalodinitrile of the former mixing lattice in the open container has been converted into α type lattice m-tetrachlorophthalodinitrile at this moment, and transformation efficiency is 95%-99%.
5. the granularity after the mixing lattice m-tetrachlorophthalodinitrile described in the aforesaid right requirement 2 is pulverized should be greater than 200 orders.
6. the temperature in the warehouse should be controlled between 80 ℃ of-120 ℃ of degree soaking time 6-10 days in the aforesaid right requirement 3.
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| CN2010102956717A CN102432504A (en) | 2010-09-29 | 2010-09-29 | Preparation method of alpha-type crystal lattice chlorothalonil |
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| CN2010102956717A CN102432504A (en) | 2010-09-29 | 2010-09-29 | Preparation method of alpha-type crystal lattice chlorothalonil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265366A (en) * | 2018-12-06 | 2019-01-25 | 江苏新河农用化工有限公司 | A kind of Bravo lattice transition device and method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4942250A (en) * | 1985-04-17 | 1990-07-17 | S.I.P.C.A.M. - Societa Italiana Prodotti Chimici E Per L'agricoltura Milano S.P.A. | Process for the production of chlorothalonyl |
| CN1752069A (en) * | 2005-10-28 | 2006-03-29 | 江苏工业学院 | Method of preparing alpha-chlorothalonil |
-
2010
- 2010-09-29 CN CN2010102956717A patent/CN102432504A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4942250A (en) * | 1985-04-17 | 1990-07-17 | S.I.P.C.A.M. - Societa Italiana Prodotti Chimici E Per L'agricoltura Milano S.P.A. | Process for the production of chlorothalonyl |
| CN1752069A (en) * | 2005-10-28 | 2006-03-29 | 江苏工业学院 | Method of preparing alpha-chlorothalonil |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265366A (en) * | 2018-12-06 | 2019-01-25 | 江苏新河农用化工有限公司 | A kind of Bravo lattice transition device and method |
| CN109265366B (en) * | 2018-12-06 | 2023-10-03 | 江苏新河农用化工有限公司 | Chlorothalonil lattice transformation device and method |
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Application publication date: 20120502 |