CN114276336A - Propiconazole molecular distillation refining method - Google Patents
Propiconazole molecular distillation refining method Download PDFInfo
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- CN114276336A CN114276336A CN202111537565.XA CN202111537565A CN114276336A CN 114276336 A CN114276336 A CN 114276336A CN 202111537565 A CN202111537565 A CN 202111537565A CN 114276336 A CN114276336 A CN 114276336A
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Abstract
The invention discloses a molecular distillation refining method of propiconazole, which comprises the following steps: (1) the prepared propiconazole crude product is degassed through thin film evaporation; the degassing temperature is 205-; (2) adding the degassed crude propiconazole into a feeder of a molecular distillation device, setting a vacuum degree, setting a distillation temperature and a temperature of a built-in condenser after the pressure is stable, adjusting the rotating speed of a scraping film after the vacuum degree, the distillation temperature and the temperature of the built-in condenser reach set values, opening a feeding valve for feeding, controlling the feeding amount, starting molecular distillation, collecting a light component which is refined propiconazole; the distillation temperature is 205-250 ℃, the temperature of the built-in condenser is 90-110 ℃, and the vacuum degree is 130-160 pa. The method of the invention adopts molecular distillation (short path distillation) to directly separate and obtain the propiconazole, has short heating time, effectively avoids the pyrolysis of the propiconazole, does not use any solvent, effectively separates in a vacuum state, and has the advantages of safety, high efficiency, energy saving, environmental protection and the like.
Description
Technical Field
The invention relates to the technical field of pesticide raw material preparation, and particularly relates to a propiconazole molecular distillation refining method.
Background
The propiconazole, namely 1- [2- (2, 4-dichlorophenyl) -4-propyl-1, 3-dioxolane-2-ylmethyl ] -1, 2, 4-triazole is a triazole bactericide, is a sterol demethylation inhibitor, and has broad spectrum and systemic property. The propiconazole can prevent and treat diseases caused by pathogenic bacteria such as ascomycetes, basidiomycetes, imperfect fungi and the like. Propiconazole is not only a fruit preservative and preservative, but also a bactericide for cereal crops and vegetables.
The molecular structure of the propiconazole contains two chiral centers, namely 2-position and 4-position on dioxolane respectively have an asymmetric carbon atom, and both the 2-position and the 4-position have optical isomers; because of the existence of saturated five-membered ring, each optical isomer has 2 geometric isomers (cis, trans), and the unique structure ensures that the bactericidal activity is higher. Propiconazole is a sterol demethylation inhibitor that mainly interferes with fungal steroid biosynthesis, inhibiting the formation of ergosterol. In most fungi, the absence of ergosterol, which makes up the cell membrane, will result in irreparable damage to the cell membrane, thereby causing the fungus to die. Propiconazole can be absorbed by the roots, stems, leaves and will soon be conducted upwards in the plant. The propiconazole can prevent and treat diseases caused by pathogenic bacteria such as ascomycetes, basidiomycetes, adelomycetes and the like, has good prevention and treatment effects on wheat root rot, charcoal disease, rice bakanae disease, grape powdery mildew, leaf spot of peanuts and bananas, can prevent and treat various fungal diseases such as leaf blight, rust disease, fishy black disease and the like, has obvious effects on fruit crop storage preservation and preservation insurance, and particularly has obvious effects on the storage of main fruit varieties such as oranges, apples and the like.
Propiconazole is a systemic fungicide of the epoxiconazole type developed by Ciba-Geigy, Switzerland. Currently, there are dozens of enterprises in China, such as Anhui Fengle agricultural chemical company Limited, Changzhou Fengdong agricultural chemical plant, Changzhou City Fengdong agricultural chemical plant, Jiangsu Chang chemical company Limited, Jiangsu Huachang (group) corporation Limited, Jiangsu Qizhou Green chemical industry Co., Ltd, Jiangsu Dongzhong Yingyi chemical industry Co., Ltd, Jima chemical industry Co., Ltd, Nanjing Aisen Fine chemical industry Co., Ltd, Shanghai Sheng agricultural biochemical products Co., Ltd, Wenzhou Longwan agricultural chemical plant, Wujin Jiang Jiangnan chemical plant, Zhang City Ganghou Qizhou pesticide chemical industry Co., Ltd, Zhejiang Yanjiang Yangtze Jiangnan chemical plant, etc.
The world demand of propiconazole is more than 20 million tons at present, the domestic demand is more than 3 million tons, and the propiconazole has a trend of increasing year by year. At present, the production capacity of propiconazole in China is about 2 tons (folding hundred); the others depend on foreign import.
The existing production method of the propiconazole refined product generally has the defects of easy volatilization, insufficient environmental protection and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a molecular distillation refining method for propiconazole.
In order to achieve the purpose, the invention adopts the following technical scheme:
a molecular distillation refining method of propiconazole comprises the following steps:
(1) the prepared propiconazole crude product is degassed through thin film evaporation; the degassing temperature is 205-;
(2) adding the degassed crude propiconazole into a feeder of a molecular distillation device, setting a vacuum degree, setting a distillation temperature and a temperature of a built-in condenser after the pressure is stable, adjusting the rotating speed of a scraping film after the vacuum degree, the distillation temperature and the temperature of the built-in condenser reach set values, opening a feeding valve for feeding, controlling the feeding amount, starting molecular distillation, collecting a light component which is refined propiconazole; the distillation temperature is 205-250 ℃, the temperature of the built-in condenser is 90-110 ℃, and the vacuum degree is 130-160 pa.
Further, in the step (1), the propiconazole mass content in the crude propiconazole product is 20% -98.5%.
Further, in the step (2), the feeding amount is 30-70kg/m2·h。
Further, in the step (2), the film scraping rotating speed is 85-110 r/min.
Further, the preparation process of the crude propiconazole in the step (1) is as follows: adding the brominated ketal, the triazole sodium, the xylene and the catalyst potassium iodide into a reaction kettle, reacting for 4h at the temperature of 120-150 ℃, filtering after the reaction is finished, and washing with water to be neutral after the filtration to obtain a desolventized propiconazole crude product.
The invention has the beneficial effects that: the method of the invention adopts molecular distillation (short path distillation) to directly separate and obtain the propiconazole, has short heating time, effectively avoids the pyrolysis of the propiconazole, does not use any solvent, effectively separates in a vacuum state, and has the advantages of safety, high efficiency, energy saving, environmental protection and the like.
Detailed Description
The present invention will be further described below, and it should be noted that the present embodiment is based on the technical solution, and a detailed implementation manner and a specific operation process are provided, but the protection scope of the present invention is not limited to the present embodiment.
Example 1
The embodiment provides a propiconazole molecular distillation refining method, which comprises the following specific processes:
adding 0.1mol of brominated ketal, 0.13mol of triazole sodium, 100ml of xylene and 1.0g of catalyst (potassium iodide) into a reaction kettle, reacting for 4 hours at 150 ℃, removing the sodium bromide after the reaction is finished, and washing to be neutral to remove solvent, thereby obtaining 40.6g of crude propiconazole. Degassing the crude product of the propiconazole by a film evaporator, wherein the degassing temperature is 230 ℃, and the degassing vacuum degree is 150 Pa. Degassing, adding into a feeder of a molecular distillation device, setting a vacuum degree of 150pa, setting a distillation temperature of 230 ℃ and a built-in condenser temperature of 90 ℃ after the pressure is stabilized, adjusting a film scraping rotation speed of 85r/min after the vacuum degree and the temperature reach the set values, opening a feeding valve, and controlling the feeding amount of a crude product of propiconazole to be 30kg/m2And h, starting molecular distillation, and collecting the light components which are separated out to obtain 33.3g of propiconazole product with the content of 98.2%.
Example 2
The embodiment provides a propiconazole molecular distillation refining method, which comprises the following specific processes:
reacting 0.15mol of brominated ketal, 0.19mol of sodium triazole, 150ml of dimethylbenzene and 1.5g of catalyst (potassium iodide) at 120 ℃ for 4 hours, removing the sodium bromide after the reaction is finished, washing to be neutral and desolventizing to obtain 60.9g of propisocyclic ringAnd (4) crude oxazole. The crude propiconazole is degassed by a film evaporator, the degassing vacuum degree is 150pa, and the degassing temperature is 225 ℃. Degassing, adding into a feeder of a molecular distillation device, setting a vacuum degree of 150pa, setting a distillation temperature of 225 ℃ and a built-in condenser temperature of 95 ℃ after the pressure is stabilized, adjusting a film scraping rotation speed of 85r/min after the vacuum degree and the temperature reach the set values, opening a feeding valve, and controlling the feeding amount of crude propiconazole of 70kg/m2And h, starting molecular distillation, and collecting the light components which are separated out to obtain 51.9g of propiconazole product with the content of 98.5%.
Example 3
The embodiment provides a propiconazole molecular distillation refining method, which comprises the following specific processes:
0.2mol of brominated ketal, 0.26mol of triazole sodium, 200ml of dimethylbenzene and 2.0g of catalyst ((potassium iodide), the reaction is carried out for 4 hours at 150 ℃, after the reaction is finished, the sodium bromide is removed, the reaction is washed to be neutral and desolventized to obtain 81g of crude propiconazole, the crude propiconazole is degassed by a thin film evaporator, the degassing vacuum degree is 160Pa, the degassing temperature is 205 ℃, the crude propiconazole is degassed and then is added into a feeder of a molecular distillation device, the vacuum degree is 160Pa, the distillation temperature is 205 ℃ and the temperature of a built-in condenser is 90 ℃ after the pressure is stabilized, the film scraping rotation speed is adjusted to 110r/min, a feeding valve is opened, and the feeding amount of the crude propiconazole is controlled to be 50kg/m2And h, starting molecular distillation, and collecting the light components which are separated out to obtain 77.1g of propiconazole product with the content of 98%.
Example 4
The embodiment provides a propiconazole molecular distillation refining method, which comprises the following specific processes:
100g of crude propiconazole is prepared, and the crude propiconazole is degassed by a film evaporator at the degassing temperature of 250 ℃ and the degassing vacuum degree of 130 pa. And (3) degassing, adding the degassed solution into a feeder of a molecular distillation device, setting the vacuum degree to be 130pa, setting the distillation temperature to be 250 ℃ and the temperature of a built-in condenser to be 110 ℃ after the pressure is stabilized, adjusting the rotating speed of a film scraper to be 110r/min after the vacuum degree and the temperature reach the set values, opening a feeding valve, controlling the feeding amount of a crude product of propiconazole, starting molecular distillation, collecting and discharging light components to obtain a propiconazole product with the content of 92.5g and 98.6%.
Various corresponding changes and modifications can be made by those skilled in the art based on the above technical solutions and concepts, and all such changes and modifications should be included in the protection scope of the present invention.
Claims (5)
1. The molecular distillation refining method of propiconazole is characterized by comprising the following steps:
(1) the prepared propiconazole crude product is degassed through thin film evaporation; the degassing temperature is 205-;
(2) adding the degassed crude propiconazole into a feeder of a molecular distillation device, setting a vacuum degree, setting a distillation temperature and a temperature of a built-in condenser after the pressure is stable, adjusting the rotating speed of a scraping film after the vacuum degree, the distillation temperature and the temperature of the built-in condenser reach set values, opening a feeding valve for feeding, controlling the feeding amount, starting molecular distillation, collecting a light component which is refined propiconazole; the distillation temperature is 205-250 ℃, the temperature of the built-in condenser is 90-110 ℃, and the vacuum degree is 130-160 pa.
2. The method of claim 1, wherein: in the step (1), the propiconazole mass content in the crude propiconazole product is 20-98.5%.
3. The method of claim 1, wherein: in the step (2), the feeding amount is 30-70kg/m2·h。
4. The method of claim 1, wherein: in the step (2), the film scraping rotating speed is 85-110 r/min.
5. The method according to claim 1, wherein the crude propiconazole in step (1) is prepared by the following steps: adding the brominated ketal, the triazole sodium, the xylene and the catalyst potassium iodide into a reaction kettle, reacting for 4h at the temperature of 120-150 ℃, filtering after the reaction is finished, and washing with water to be neutral after the filtration to obtain a desolventized propiconazole crude product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114751895A (en) * | 2022-04-09 | 2022-07-15 | 山东东泰农化有限公司 | Difenoconazole molecular distillation decoloring method |
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| CN101323612A (en) * | 2008-07-14 | 2008-12-17 | 江苏七洲绿色化工股份有限公司 | Preparation of bactericide propiconazole |
| CN104402871A (en) * | 2014-12-01 | 2015-03-11 | 江苏耕耘化学有限公司 | Method for specifically preparing derivative of 2-(1H-1, 2, 4-triazole-1-methyl)-1, 3-dioxolane |
| CN107382979A (en) * | 2017-06-13 | 2017-11-24 | 周保东 | A kind of Difenoconazole molecular distillation process for purification |
| WO2019061593A1 (en) * | 2017-09-27 | 2019-04-04 | 泰兴瑞泰化工有限公司 | Method for extracting high-purity ethoxyquinoline by using multistage molecular distillation technology |
| CN109879862A (en) * | 2019-03-30 | 2019-06-14 | 长沙鑫本药业有限公司 | A kind of synthesis technology of propiconazole |
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- 2021-12-15 CN CN202111537565.XA patent/CN114276336A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323612A (en) * | 2008-07-14 | 2008-12-17 | 江苏七洲绿色化工股份有限公司 | Preparation of bactericide propiconazole |
| CN104402871A (en) * | 2014-12-01 | 2015-03-11 | 江苏耕耘化学有限公司 | Method for specifically preparing derivative of 2-(1H-1, 2, 4-triazole-1-methyl)-1, 3-dioxolane |
| CN107382979A (en) * | 2017-06-13 | 2017-11-24 | 周保东 | A kind of Difenoconazole molecular distillation process for purification |
| WO2019061593A1 (en) * | 2017-09-27 | 2019-04-04 | 泰兴瑞泰化工有限公司 | Method for extracting high-purity ethoxyquinoline by using multistage molecular distillation technology |
| CN109879862A (en) * | 2019-03-30 | 2019-06-14 | 长沙鑫本药业有限公司 | A kind of synthesis technology of propiconazole |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114751895A (en) * | 2022-04-09 | 2022-07-15 | 山东东泰农化有限公司 | Difenoconazole molecular distillation decoloring method |
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