CN105732512A - Carbendazim production technology - Google Patents
Carbendazim production technology Download PDFInfo
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- CN105732512A CN105732512A CN201610219619.0A CN201610219619A CN105732512A CN 105732512 A CN105732512 A CN 105732512A CN 201610219619 A CN201610219619 A CN 201610219619A CN 105732512 A CN105732512 A CN 105732512A
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- Prior art keywords
- carbendazim
- solid
- water
- liquid
- sodium chloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D235/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings
- C07D235/02—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings condensed with carbocyclic rings or ring systems
- C07D235/04—Benzimidazoles; Hydrogenated benzimidazoles
- C07D235/24—Benzimidazoles; Hydrogenated benzimidazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
- C07D235/30—Nitrogen atoms not forming part of a nitro radical
- C07D235/32—Benzimidazole-2-carbamic acids, unsubstituted or substituted; Esters thereof; Thio-analogues thereof
Abstract
The invention relates to a carbendazim production technology.The production technology includes the steps that amination is conducted, wherein water, cyanamide, methyl chloroformate and a sodium hydroxide solution are put into an amination kettle for amination reaction; condensation is conducted, wherein a solution generated by the amination kettle is conveyed into a condensation kettle through a mother liquor pump, and o-phenylenediamine and hydrochloric acid are added into the condensation kettle for condensation reaction; solid-liquid separation is conducted, wherein the reacted solution is conveyed into a centrifugal machine for solid-liquid separation; drying is conducted to obtain a finished product, wherein the separated solid is dried to obtain the carbendazim finished product; secondary precipitation is conducted, wherein the separated liquid is subjected to secondary precipitation and separation; evaporation is carried out, wherein the liquid separated for the second time is evaporated; centrifugal washing is conducted, wherein remaining liquid is conveyed into the centrifugal machine for solid-liquid separation; drying is conducted, wherein the separated solid is dried to obtain a sodium chloride byproduct finished product.The technology has the advantages that energy consumption and material consumption are reduced, the output and the emission amount of three wastes are controlled and reduced, the byproduct sodium chloride is generated by reprocessing waste water, and energy conservation and emission reduction are achieved.
Description
Technical field
The present invention relates to the production field of carbendazim, specifically a kind of high-quality, pollution-free, without the production technology of the carbendazim of waste.
Background technology
Carbendazim is systemic fungicide efficient, wide spectrum, safety, can prevent and treat leaf spot of peanut, melasma, stem rot, the head blight of wheat, barley and highland barley, the melasma of Cereal, sclerotinia rot of colza, rice sheath blight disease, citrus bacterial canker disease, storage disease, cucurbits fusarium wilt, flowers root rot, stem rot etc..Additionally, carbendazim also has broad application prospects in weaving, printing and dyeing, papermaking, process hides, wood preservation etc..Carbendazim is efficient, low toxicity systemic fungicide, has interior inhale treatment and protective effect, to people and animals' low toxicity, toxicity in fish is also low.
At present, carbendazim energy consumption material consumption is high, yields poorly, and quality is also bad, also produces the substantial amounts of three wastes, and environmental pollution is serious.
Summary of the invention
In order to solve the problems referred to above, the present invention proposes the production technology of a kind of carbendazim, perfect technology, and energy and material consumption is low, and yield is high, and quality is good, reduces the three wastes, and environmental pollution is few.
In order to achieve the above object, the present invention proposes techniques below scheme:
The production technology of carbendazim, is characterized in particular in following steps:
1) amination: these raw materials of water, cyanamide, methylchloroformate and sodium hydroxide solution are put into amination still and carries out aminating reaction, have cyanogen amidocarbonic acid first sodium salt, water and sodium chloride after reaction in solution.
2) condensation: solution amination still generated by mother solution pump is transported in condensation kettle, in condensation kettle, add neck phenylenediamine simultaneously and hydrochloric acid carries out condensation reaction, solution has after reaction water, carbendazim, sodium chloride, neck phenylenediamine, carbendazim hydrochloride, hydrogen chloride, ammonium chloride.
3) solid-liquid separation: the 2nd) reacted solution is transported in centrifuge and carries out solid-liquid separation in step, mainly carbendazim and a small amount of water, sodium chloride, neck phenylenediamine, carbendazim hydrochloride, hydrogen chloride and ammonium chloride in isolated solid；Isolated liquid mainly contains water, sodium chloride, ammonium chloride and a small amount of carbendazim, neck phenylenediamine, carbendazim hydrochloride and hydrogen chloride.
4) dry finished product: the 3rd) isolated solid is dried in step, and moisture drying is gone out, obtains carbendazim finished product.
5) two-stage precipitation: the 3rd) isolated liquid carries out secondary precipitation separation in step, isolates a small amount of solid carbendazim, a small amount of carbendazim is transported to the 4th) step dries together.
6) evaporation: the 5th) secondary separation goes out in step liquid is evaporated, and after evaporation, liquid residual volume is the 1/3 of original volume, and the gas evaporated carries out cooling down recycling.
7) centrifuge washing: the 6th) remaining liquid is transported in centrifuge and carries out solid-liquid separation in step, separate and backward centrifuge is carried clear water centrifuge is carried out, containing a small amount of water, ammonium chloride and substantial amounts of sodium chloride in isolated solid, containing substantial amounts of water, the ammonium chloride of middle amount and sodium chloride, the carbendazim of trace, o-phenylenediamine, carbendazim hydrochloride and hydrogen chloride in isolated liquid.
8) dry: the 7th) isolated solid is dried in step, and make water and ammonium chloride volatilize away, obtain sodium chloride salt byproduct finished product.
By the 1st) chemical equation of the aminating reaction described in step is:
。
By the 2nd) chemical equation of the condensation reaction described in step is:
By the 1st) the raw material weight ratio described in step is water 120kg, concentration is 50.8% cyanamide 39.9kg, and concentration is 99% methylchloroformate 52.6kg, and concentration is the sodium chloride solution 57kg of 50%.
By the 2nd) concentration added in condensation reaction described in step is 50.8% neck phenylenediamine 43.2kg, concentration is 31% hydrochloric acid 75kg.
By the 4th) the carbendazim finished product concentration that obtains described in step is more than 98%.
By the 8th) the sodium chloride salt finished product concentration that obtains described in step is more than 98%.
It is an advantage of the invention that and adjust the product mix and yield, improve and promote production technology, reducing energy consumption and material consumption, control and reduce generation amount and the discharge capacity of " three wastes "；The processing method of improvement perfect " three wastes ", thoroughly solves to affect the environmental protection problem that enterprise develops further；Waste water reprocessing generates side product chlorinated sodium, energy-saving and emission-reduction.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
With reference to accompanying drawing, the production technology of carbendazim, it is characterized in particular in following steps:
1) amination: water 120kg, concentration is 50.8% cyanamide 39.9kg, concentration is 99% methylchloroformate 52.6kg, concentration is the sodium chloride solution 57kg of 50%, these raw materials put into amination still and carry out aminating reaction, have cyanogen amidocarbonic acid first sodium salt 58.8kg, water 182.5kg and sodium chloride 28.2kg after reaction in solution.
2) condensation: solution amination still generated by mother solution pump is transported in condensation kettle, toward condensation kettle in, add concentration be simultaneously 50.8% neck phenylenediamine 43.2kg and concentration is that 31% hydrochloric acid 75kg carries out condensation reaction, solution has after reaction water 252.53kg, carbendazim 72kg, sodium chloride 44.1kg, leads phenylenediamine 0.9kg, carbendazim hydrochloride 0.05kg, hydrogen chloride 0.12kg, ammonium chloride 18kg.
3) solid-liquid separation: the 2nd) reacted solution is transported in centrifuge and carries out solid-liquid separation in step, mainly carbendazim 71.56kg and a small amount of water 4.297kg, sodium chloride 0.6kg, neck phenylenediamine 0.04kg, carbendazim hydrochloride 0.001kg, hydrogen chloride 0.002kg and ammonium chloride 0.1kg in isolated solid；Isolated liquid mainly contains water 248.233kg, sodium chloride 43.5kg, ammonium chloride 17.9kg and a small amount of carbendazim 0.44kg, neck phenylenediamine 0.86kg, carbendazim hydrochloride 0.049kg and hydrogen chloride 0.118kg.
4) dry finished product: the 3rd) isolated solid is dried in step, and 4kg moisture drying is gone out, obtains carbendazim finished product 72.6kg.
5) two-stage precipitation: the 3rd) isolated liquid carries out secondary precipitation separation in step, isolates a small amount of solid carbendazim 0.4kg, a small amount of carbendazim is transported to the 4th) step dries together.
6) evaporation: the 5th) secondary separation goes out in step liquid is evaporated, and evaporates moisture 220kg, and after evaporation, liquid residual volume is the 1/3 of original volume, and the gas evaporated carries out cooling down recycling.
7) centrifuge washing: the 6th) remaining liquid is transported in centrifuge and carries out solid-liquid separation in step, (clear water needs 300kg to separate conveying clear water in backward centrifuge, clear water can use the evaporation condensed water in the 6th step, recycle, save the energy) centrifuge is carried out, containing a small amount of water 1.8kg in isolated solid, ammonium chloride 0.4 and substantial amounts of sodium chloride 7.5kg, containing substantial amounts of water 326.433kg in isolated liquid, the ammonium chloride 17.5kg and sodium chloride 36kg of middle amount, the carbendazim 0.04kg of trace, o-phenylenediamine 0.86kg, carbendazim hydrochloride 0.049kg and hydrogen chloride 0.118kg；The aqueous solution herein produced is transported to sewage disposal system.
8) dry: the 7th) isolated solid is dried in step, and make water 1.0kg and ammonium chloride 0.4kg volatilize away, obtain sodium chloride salt byproduct finished product 7.5kg.
The carbendazim quality index produced:
| Project | Index |
| Outward appearance | Colorless crystalline powder |
| Mass fraction/% | ≥98 |
| Solid insoluble/% | ≤0.2 |
| Moisture/% | ≤0.5 |
Claims (7)
1. the production technology of carbendazim, it is characterised in that following steps:
Amination: these raw materials of water, cyanamide, methylchloroformate and sodium hydroxide solution are put into amination still and carries out aminating reaction, have cyanogen amidocarbonic acid first sodium salt, water and sodium chloride after reaction in solution；
Condensation: solution amination still generated by mother solution pump is transported in condensation kettle, in condensation kettle, add neck phenylenediamine simultaneously and hydrochloric acid carries out condensation reaction, solution has after reaction water, carbendazim, sodium chloride, neck phenylenediamine, carbendazim hydrochloride, hydrogen chloride, ammonium chloride；
Solid-liquid separation: the 2nd) reacted solution is transported in centrifuge and carries out solid-liquid separation in step, mainly carbendazim and a small amount of water, sodium chloride, neck phenylenediamine, carbendazim hydrochloride, hydrogen chloride and ammonium chloride in isolated solid；Isolated liquid mainly contains water, sodium chloride, ammonium chloride and a small amount of carbendazim, neck phenylenediamine, carbendazim hydrochloride and hydrogen chloride；
Dry finished product: the 3rd) isolated solid is dried in step, and moisture drying is gone out, obtains carbendazim finished product；
Two-stage precipitation: the 3rd) isolated liquid carries out secondary precipitation separation in step, isolates a small amount of solid carbendazim, a small amount of carbendazim is transported to the 4th) step dries together；
Evaporation: the 5th) secondary separation goes out in step liquid is evaporated, and after evaporation, liquid residual volume is the 1/3 of original volume, and the gas evaporated carries out cooling down recycling；
Centrifuge washing: the 6th) remaining liquid is transported in centrifuge and carries out solid-liquid separation in step, separate and backward centrifuge is carried clear water centrifuge is carried out, containing a small amount of water, ammonium chloride and substantial amounts of sodium chloride in isolated solid, containing substantial amounts of water, the ammonium chloride of middle amount and sodium chloride, the carbendazim of trace, o-phenylenediamine, carbendazim hydrochloride and hydrogen chloride in isolated liquid；
Dry: the 7th) isolated solid is dried in step, and make water and ammonium chloride volatilize away, obtain sodium chloride salt byproduct finished product.
2. the production technology of carbendazim according to claim 1, it is characterised in that the 1st) chemical equation of aminating reaction is in step:。
3. the production technology of carbendazim according to claim 1, it is characterised in that the 2nd) chemical equation of condensation reaction is in step:。
4. the production technology of carbendazim according to claim 1, it is characterised in that the 1st) step Raw part by weight is water 120kg, concentration is 50.8% cyanamide 39.9kg, and concentration is 99% methylchloroformate 52.6kg, and concentration is the sodium chloride solution 57kg of 50%.
5. the production technology of carbendazim according to claim 1, it is characterised in that the 2nd) concentration added in step condensation reaction is 50.8% neck phenylenediamine 43.2kg, concentration is 31% hydrochloric acid 75kg.
6. the production technology of carbendazim according to claim 1, it is characterised in that the 4th) the carbendazim finished product concentration that obtains in step is more than 98%.
7. the production technology of carbendazim according to claim 1, it is characterised in that the 8th) the sodium chloride salt finished product concentration that obtains in step is more than 98%.
Priority Applications (1)
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|---|---|---|---|
| CN201610219619.0A CN105732512A (en) | 2016-04-11 | 2016-04-11 | Carbendazim production technology |
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| CN201610219619.0A CN105732512A (en) | 2016-04-11 | 2016-04-11 | Carbendazim production technology |
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| CN105732512A true CN105732512A (en) | 2016-07-06 |
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| CN201610219619.0A Pending CN105732512A (en) | 2016-04-11 | 2016-04-11 | Carbendazim production technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041267A (en) * | 2019-05-29 | 2019-07-23 | 宁夏蓝丰精细化工有限公司 | Carbendazim clean-production system |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3997553A (en) * | 1969-06-25 | 1976-12-14 | E. I. Du Pont De Nemours And Company | 2-Benzimidazolecarbamic acid esters by the cyanamide process |
| CN102070535A (en) * | 2011-02-23 | 2011-05-25 | 江苏蓝丰生物化工股份有限公司 | Preparing method for synthesizing sanmate from calcium cyanamide |
| CN102850278A (en) * | 2012-10-09 | 2013-01-02 | 江苏宝众宝达药业有限公司 | Method for decoloring imidazole anthelmintics |
| CN103242237A (en) * | 2013-05-10 | 2013-08-14 | 常州亚邦齐晖医药化工有限公司 | New preparation method for anthelmintic fenbendazole |
-
2016
- 2016-04-11 CN CN201610219619.0A patent/CN105732512A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3997553A (en) * | 1969-06-25 | 1976-12-14 | E. I. Du Pont De Nemours And Company | 2-Benzimidazolecarbamic acid esters by the cyanamide process |
| CN102070535A (en) * | 2011-02-23 | 2011-05-25 | 江苏蓝丰生物化工股份有限公司 | Preparing method for synthesizing sanmate from calcium cyanamide |
| CN102850278A (en) * | 2012-10-09 | 2013-01-02 | 江苏宝众宝达药业有限公司 | Method for decoloring imidazole anthelmintics |
| CN103242237A (en) * | 2013-05-10 | 2013-08-14 | 常州亚邦齐晖医药化工有限公司 | New preparation method for anthelmintic fenbendazole |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041267A (en) * | 2019-05-29 | 2019-07-23 | 宁夏蓝丰精细化工有限公司 | Carbendazim clean-production system |
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Application publication date: 20160706 |
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