CN108997323A - A kind of difenoconazole new cleanproduction process - Google Patents
A kind of difenoconazole new cleanproduction process Download PDFInfo
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- CN108997323A CN108997323A CN201810594954.8A CN201810594954A CN108997323A CN 108997323 A CN108997323 A CN 108997323A CN 201810594954 A CN201810594954 A CN 201810594954A CN 108997323 A CN108997323 A CN 108997323A
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- difenoconazole
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- triazole
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D405/00—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom
- C07D405/02—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom containing two hetero rings
- C07D405/06—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom containing two hetero rings linked by a carbon chain containing only aliphatic carbon atoms
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- Organic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to a kind of difenoconazole new cleanproduction process, the dosage of triazole and potassium hydroxide is strict controlled in micro- excessive state by the optimization of process conditions, greatly reduce the ratio of impurity in potassium bromide, pass through the processing such as centrifugation elution and drying again, the not only fixed product of the difenoconazole of available high-purity, and the bromination potassium content after being reacted is up to 95%, the standard of industrial products is reached, it can be used as international sale, dangerous waste amount and dangerous waste expense are greatly reduced, product profit is improved.
Description
Technical field
The invention belongs to difenoconazole production technical field more particularly to a kind of new works of difenoconazole clean manufacturing
Skill.
Background technique
Difenoconazole is a kind of fungicide of broad-spectrum high efficacy, the main biosynthesis for inhibiting germ cell ergosterol,
To destroy membrane structure and function, it is mainly used for the crops such as fruit tree, vegetables, wheat, potato, beans, melon, to vegetables
There is protection and therapeutic effect well with a variety of fungal diseases such as melon and fruit.Difenoconazole is safety in triazole bactericidal agent
Property is relatively high, is widely used in the crops such as fruit tree, vegetables, effectively prevents scab, anthrachose of grape, white rot, spot defoliation,
Powdery mildew, brown spot, rust, stripe rust, head blight etc..Simultaneously to beet cercospora leaf spot, wheat glume blotch, leaf blight, rust and
The mildew as caused by several pathogenic bacteria, scab of apple, powdery mildew, uncinula necator, target, leaf spot of peanut,
Net blotch etc. has preferable therapeutic effect.
But in existing difenoconazole production, bromine ketal and triazole, potassium hydroxide react in a solvent, are condensed
To difenoconazole.Water and potassium bromide can be generated simultaneously.In original process, the potassium bromide of generation is due to aqueous and solvent and excess
Other raw materials, and become dangerous waste.
Summary of the invention
The present invention is to solve well-known technique and provide a kind of difenoconazole new cleanproduction process.
The present invention is adopted the technical scheme that solve well-known technique: a kind of difenoconazole is clear
Clean production new technique, the following steps are included:
1) condensation reaction: choosing bromine ketal solution, 160-200 parts of solubility that 80-100 parts of concentration is 95% is 50%
80-100 parts of bromine ketal solvent is heated reaction first by triazole solution and 160-200 parts of 50% potassium hydroxide solution
In kettle, while 80-100 parts of triazole liquid and potassium hydroxide solution is added, and stir evenly by blender, and by anti-
The heater in kettle is answered to control the temperature of reaction solution at 45-60 DEG C；By remaining triazole liquid and potassium hydroxide solution according to
Volume fraction ratio 1:1 is gradually added in reaction kettle, and progress condensation reaction between bromine ketal and triazole, hydroxide is made to obtain phenylate
Methyl cyclic-azole, water and potassium bromide.
2) centrifugal treating: 1) reaction of reaction kettle internal condensation generates in difenoconazole, water and potassium bromide are mixed molten
Liquid is added in centrifuge and carries out centrifugal treating, since difenoconazole is that white solid can be by benzene under the action of centrifuge
Ether methyl cyclic-azole is separated with potassium bromide solution realization；
3) elution is handled: 2) the difenoconazole solid that middle centrifugation obtains being put into strainer or filter cloth, passes through simultaneously top
Spray equipment carry out spray process, spray time 20-40min, convenient for a small amount of impurity for containing on removal difenoconazole
Potassium bromide solution；
4) drying and processing: 3) the difenoconazole solid after spray process in is put into drying oven and carries out at drying by a.
Reason, drying time 2-5h, and temperature are controlled at 40-70 DEG C, while no more than 75 DEG C of in-furnace temperature, to obtain high-purity
Difenoconazole solid.
In the present invention, the triazole is 1,2,4- triazoles.
The present invention has the advantage that as follows with good effect:
1. a kind of difenoconazole new cleanproduction process proposed by the present invention, by the optimization of process conditions by triazole
It is strict controlled in micro- excessive state with the dosage of potassium hydroxide, greatly reduces the ratio of impurity in potassium bromide, then pass through centrifugation
The processing such as elution and drying, the not only fixed product of the difenoconazole of available high-purity, and the potassium bromide after being reacted
Content is up to 95%, has reached the standard of industrial products, can be used as international sale, greatly reduces dangerous waste amount and dangerous waste
Expense improves product profit.
Specific embodiment
In order to further understand the content, features and effects of the present invention, hereby enumerating following embodiment, and cooperate detailed
It is described as follows.
A kind of difenoconazole new cleanproduction process of the invention, the following steps are included:
1) condensation reaction: choosing bromine ketal solution, 160-200 parts of solubility that 80-100 parts of concentration is 95% is 50%
80-100 parts of bromine ketal solvent is heated reaction first by triazole solution and 160-200 parts of 50% potassium hydroxide solution
In kettle, while 80-100 parts of triazole liquid and potassium hydroxide solution is added, and stir evenly by blender, and by anti-
The heater in kettle is answered to control the temperature of reaction solution at 45-60 DEG C；By remaining triazole liquid and potassium hydroxide solution according to
Volume fraction ratio 1:1 is gradually added in reaction kettle, and progress condensation reaction between bromine ketal and triazole, hydroxide is made to obtain phenylate
Methyl cyclic-azole, water and potassium bromide, wherein the triazole is 1,2,4- triazoles.
2) centrifugal treating: 1) reaction of reaction kettle internal condensation generates in difenoconazole, water and potassium bromide are mixed molten
Liquid is added in centrifuge and carries out centrifugal treating, since difenoconazole is that white solid can be by benzene under the action of centrifuge
Ether methyl cyclic-azole is separated with potassium bromide solution realization；
3) elution is handled: 2) the difenoconazole solid that middle centrifugation obtains being put into strainer or filter cloth, passes through simultaneously top
Spray equipment carry out spray process, spray time 20-40min, convenient for a small amount of impurity for containing on removal difenoconazole
Potassium bromide solution；
4) drying and processing: 3) the difenoconazole solid after spray process in is put into drying oven and carries out at drying by a.
Reason, drying time 2-5h, and temperature are controlled at 40-70 DEG C, while no more than 75 DEG C of in-furnace temperature, to obtain high-purity
Difenoconazole solid.
Wherein: key reaction equation is as follows:
The above is only the preferred embodiments of the present invention, and is not intended to limit the present invention in any form,
Any simple modification made to the above embodiment according to the technical essence of the invention, equivalent variations and modification, belong to
In the range of technical solution of the present invention.
Claims (2)
1. a kind of difenoconazole new cleanproduction process, it is characterised in that: the following steps are included:
1) three nitrogen that bromine ketal solution, 160-200 parts of solubility that 80-100 parts of concentration is 95% are 50% condensation reaction: are chosen
Azoles solution and 160-200 parts of 50% potassium hydroxide solution first heat 80-100 parts of bromine ketal solvent in reaction kettle,
80-100 parts of triazole liquid and potassium hydroxide solution is added simultaneously, and is stirred evenly by blender, and pass through reaction kettle
Interior heater controls the temperature of reaction solution at 45-60 DEG C；By remaining triazole liquid and potassium hydroxide solution according to volume
Component ratio 1:1 is gradually added in reaction kettle, and progress condensation reaction between bromine ketal and triazole, hydroxide is made to obtain phenyl ether methyl cyclic
Azoles, water and potassium bromide.
2) centrifugal treating: 1) reaction of reaction kettle internal condensation generates in difenoconazole, water and potassium bromide mixed solution are added
Enter and carry out centrifugal treating in centrifuge, since difenoconazole is that white solid can be by phenylate first under the action of centrifuge
Ring azoles is separated with potassium bromide solution realization；
3) elution is handled: 2) the difenoconazole solid that middle centrifugation obtains being put into strainer or filter cloth, passes through the spray at simultaneously top
Shower device carries out spray process, spray time 20-40min, convenient for a small amount of impurity bromination contained on removal difenoconazole
Potassium solution；
4) drying and processing: 3) the difenoconazole solid after spray process in is put into drying oven and carries out drying and processing by a., dries
The dry time is 2-5h, and temperature is controlled at 40-70 DEG C, while no more than 75 DEG C of in-furnace temperature, to obtain the benzene of high-purity
Ether methyl cyclic-azole solid.
2. a kind of difenoconazole new cleanproduction process according to claim 1, which is characterized in that the triazole is
1,2,4- triazole.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810594954.8A CN108997323A (en) | 2018-06-11 | 2018-06-11 | A kind of difenoconazole new cleanproduction process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810594954.8A CN108997323A (en) | 2018-06-11 | 2018-06-11 | A kind of difenoconazole new cleanproduction process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108997323A true CN108997323A (en) | 2018-12-14 |
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ID=64601283
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810594954.8A Pending CN108997323A (en) | 2018-06-11 | 2018-06-11 | A kind of difenoconazole new cleanproduction process |
Country Status (1)
| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593083A (en) * | 2018-12-28 | 2019-04-09 | 利民化工股份有限公司 | A kind of preparation method of difenoconazole nitrate |
-
2018
- 2018-06-11 CN CN201810594954.8A patent/CN108997323A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593083A (en) * | 2018-12-28 | 2019-04-09 | 利民化工股份有限公司 | A kind of preparation method of difenoconazole nitrate |
| CN109593083B (en) * | 2018-12-28 | 2022-03-01 | 利民化学有限责任公司 | Preparation method of difenoconazole nitrate |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181214 |
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| WD01 | Invention patent application deemed withdrawn after publication |