CN117510410A - Prochloraz purification method - Google Patents
Prochloraz purification method Download PDFInfo
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- CN117510410A CN117510410A CN202311496096.0A CN202311496096A CN117510410A CN 117510410 A CN117510410 A CN 117510410A CN 202311496096 A CN202311496096 A CN 202311496096A CN 117510410 A CN117510410 A CN 117510410A
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- prochloraz
- purification method
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- 239000005820 Prochloraz Substances 0.000 title claims abstract description 104
- TVLSRXXIMLFWEO-UHFFFAOYSA-N prochloraz Chemical compound C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl TVLSRXXIMLFWEO-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 238000000746 purification Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 43
- 238000002425 crystallisation Methods 0.000 claims abstract description 40
- 230000008025 crystallization Effects 0.000 claims abstract description 40
- 239000012043 crude product Substances 0.000 claims abstract description 13
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 68
- 239000000047 product Substances 0.000 claims description 34
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 24
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 15
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 2
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims description 2
- 125000003944 tolyl group Chemical group 0.000 claims description 2
- 239000012452 mother liquor Substances 0.000 abstract description 25
- 239000002351 wastewater Substances 0.000 abstract description 8
- 238000004064 recycling Methods 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000001953 recrystallisation Methods 0.000 abstract description 3
- 239000000575 pesticide Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000012065 filter cake Substances 0.000 description 17
- 239000010413 mother solution Substances 0.000 description 15
- 238000010812 external standard method Methods 0.000 description 14
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 6
- 230000000844 anti-bacterial effect Effects 0.000 description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000003899 bactericide agent Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000005923 long-lasting effect Effects 0.000 description 2
- 235000002867 manganese chloride Nutrition 0.000 description 2
- 239000011565 manganese chloride Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 208000031888 Mycoses Diseases 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008029 eradication Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- OXOKTPUZOHPXSA-UHFFFAOYSA-L manganese(2+);n-propyl-n-[2-(2,4,6-trichlorophenoxy)ethyl]imidazole-1-carboxamide;dichloride Chemical compound Cl[Mn]Cl.C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl.C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl.C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl.C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl OXOKTPUZOHPXSA-UHFFFAOYSA-L 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000003408 phase transfer catalysis Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D233/56—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Nitrogen And Oxygen As The Only Ring Hetero Atoms (AREA)
Abstract
The invention belongs to the field of pesticide chemical industry, and particularly relates to a purification method of prochloraz. The purification method provided by the invention realizes the characteristics of environmental friendliness, higher purity, simplicity in purification method, suitability for industrialization and the like through recrystallization of benign solvents and poor solvents, so that the purity of crude prochloraz can reach 99.9% from 96% through the purification method; according to the purification method provided by the invention, the crystallization mother liquor can be recycled, the problems of large wastewater use and difficult treatment are solved by the way of recycling the crystallization mother liquor and rectifying and recycling the mother liquor, and the purity of the prochloraz crude product purified by the mother liquor reaches more than 99.5%.
Description
Technical Field
The invention belongs to the field of pesticide chemical industry, and particularly relates to a purification method of prochloraz.
Background
Prochloraz belongs to imidazole efficient and systemic bactericides and has the functions of protection, treatment and eradication. The bactericide has the characteristics of long lasting period, belongs to a bactericide with the functions of protecting, treating and radically curing, has wide bactericidal spectrum and long lasting period, has the nutrition effect on crops, is safe to the crops when being used at recommended dosage, and has the control effect on various fungal diseases.
The crude product prepared by the existing prochloraz production process has lower purity, and the purity can reach 97% after a series of purification. Along with the increasing market share of prochloraz and the increasing requirements on prochloraz purity, the method for searching the prochloraz has the advantages of simplicity, energy saving, suitability for industrialization and obvious purification effect, and has greater significance. Chinese patent CN115850181 a discloses a synthesis method of prochloraz, and the purity of prochloraz obtained by washing reaction solution with water and desolventizing under reduced pressure is 97.5%. The method uses a large amount of water to wash out phase transfer catalysis, alkali and a small amount of organic matters, and has the defects of large wastewater quantity, large wastewater alkalinity, large amount of salt in wastewater, difficult wastewater treatment and the like. Chinese patent CN 109438356A discloses a method for purifying prochloraz technical, which comprises dissolving prochloraz crude product with organic solvent, and adding manganese dichloride solution to obtain prochloraz and manganese dichloride complex, which is precipitate. And filtering and separating. The obtained filter cake is subjected to liquid alkaline hydrolysis in toluene, then extraction is carried out, and the extract is subjected to water washing and reduced pressure concentration to prepare prochloraz with 99% purity, so that the characteristics of treatment of heavy metal manganese salt-containing wastewater and low prochloraz yield are present.
At present, few reports are given to the prochloraz purification method, and various problems of low purity after purification, production of a large amount of heavy metal salt-containing wastewater, complicated purification method and the like exist.
Disclosure of Invention
According to the defects of the existing purification method, the purification method of prochloraz is provided, and the method has the characteristics of environmental friendliness, higher purity, simplicity in purification method, suitability for industrialization and the like through recrystallization of benign solvents and poor solvents, so that the purity of crude prochloraz can reach 99.9% from 96% through the purification method. The problems of large waste water use and difficult treatment are solved by the way of recycling crystallization mother liquor and rectifying and recovering the mother liquor, and the crude prochloraz product purified by the mother liquor has the purity of more than 99.5 percent.
The technical scheme adopted by the invention for achieving the purpose is as follows:
the invention provides a purification method of prochloraz, which comprises the following steps:
(1) Adding the prochloraz crude product into benign solvent, stirring and dissolving;
(2) After the crude prochloraz is completely dissolved, adding a certain amount of poor solvent, and cooling and crystallizing after the poor solvent is added; filtering the separated crystals, washing with poor solvent, and drying to obtain prochloraz pure product.
In the purification method provided by the invention, the benign solvent is selected from one or more of toluene, xylene and chlorobenzene; most preferably, the benign solvent is toluene.
Further, in the step (1), the mass ratio of the prochloraz crude product to the benign solvent is 1:2 to 5.
In the purification method provided by the invention, the poor solvent is cyclohexane, n-hexane or n-heptane; most preferably, the poor solvent is n-hexane.
Further, in the step (2), the mass ratio of the prochloraz crude product to the poor solvent is 1:0.5 to 1.5.
Further, in the step (2), the cooling crystallization is performed for 2 hours at the temperature of-10 to-5 ℃.
Further, in the step (2), the drying temperature is lower than 35 ℃ and the drying time is 2 hours.
In the purification method provided by the invention, after crystallization is finished, low-temperature filtration is carried out, and a filter cake is washed by using a poor solvent. The purified prochloraz wet product is dried for 2 hours at 35 ℃. The crystallization mother liquor is recycled for 3 to 5 times, and the recycling is stopped when the purity of the mother liquor for purifying the crude product is less than 99 percent. And separating and recovering the benign solvent and the poor solvent from the mother solution which is stopped by the application by using a rectification mode.
The beneficial effects of the invention are as follows:
(1) The purification method provided by the invention realizes the characteristics of environmental friendliness, higher purity, simplicity in purification method, suitability for industrialization and the like through recrystallization of benign solvents and poor solvents, so that the purity of crude prochloraz can reach 99.9% from 96% through the purification method;
(2) According to the purification method provided by the invention, the crystallization mother liquor can be recycled, the problems of large wastewater use and difficult treatment are solved by the way of recycling the crystallization mother liquor and rectifying and recycling the mother liquor, and the purity of the prochloraz crude product purified by the mother liquor reaches more than 99.5%.
Description of the preferred embodiments
The technical advancement of the invention, the energy saving and emission reduction aspects and the advantage of improving the prochloraz purity are specifically described by specific implementation cases. The following examples merely aid in understanding the invention and are not intended to limit the scope of the invention.
Example 1
100g of 96% prochloraz was put into a 1L three-necked flask at normal temperature, and then 300g of toluene solvent was added thereto to dissolve prochloraz with stirring. After prochloraz is completely dissolved, 50g of normal hexane solvent is added, and the temperature is reduced, and the crystallization temperature is-5 ℃. At this temperature, crystallization was carried out with stirring for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-hexane. The obtained prochloraz wet product is dried for 2 hours at 35 ℃. 83.4g of purified prochloraz pure product, the color is pure white, and the content is 99.9 percent by an external standard method. Mass of mother solution: 336g, and washed with n-hexane.
Example 2
100g of 96% prochloraz was put into a 1L three-necked flask at normal temperature, and then 300g of toluene solvent was added thereto to dissolve prochloraz with stirring. After prochloraz is completely dissolved, 80g of normal hexane solvent is added, and the temperature is reduced, and the crystallization temperature is-5 ℃. At this temperature, crystallization was carried out with stirring for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-hexane. The obtained prochloraz wet product is dried for 2 hours at 35 ℃. 84.3g of purified prochloraz pure product with pure white color and the content of which is 99.9 percent measured by an external standard method. Mass of mother solution: 325g of washed n-hexane was collected separately.
Example 3 purification of mother liquor
1) In example 1, the mother liquor after crystallization was used as a mother liquor. 336g of the mother liquor were admixed with toluene: n-hexane=6: 1 to 350g, and is applied for the first time.
100g of 96% prochloraz crude product is added into crystallization mother liquor to be stirred, the crystallization temperature is reduced to minus 5 ℃ and the mixture is stirred for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-hexane. The obtained prochloraz wet product is dried at 35 ℃ for 2 hours. 95.8g of purified prochloraz pure product with pure white color and 99.7 percent of external standard method content. Mass of mother solution: 339g, and washed with n-hexane.
2) Mother liquor is used for the second time, and the mother liquor is prepared by toluene: n-hexane=6: 1 to 350g.
100g of 96% prochloraz crude product is added into secondary crystallization mother liquor to be stirred, the crystallization temperature is reduced to minus 5 ℃ and the mixture is stirred for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-hexane. The obtained prochloraz wet product is dried at 35 ℃ for 2 hours. 97.5g of purified prochloraz pure product, the color is pure white, and the content of the prochloraz pure product by an external standard method is 99.8 percent. Mass of mother solution: 340g of washed n-hexane was collected separately.
3) The mother liquor is reused for the third time, and the mother liquor is pressed into toluene: n-hexane=6: 1 to 350g.
100g of 96% prochloraz crude product is added into the three-time crystallization mother liquor to be stirred, the crystallization temperature is reduced to minus 5 ℃ and the mixture is stirred for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-hexane. The obtained prochloraz wet product is dried at 35 ℃ for 2 hours. 97.2g of purified prochloraz pure product, the color is pure white, and the content of the prochloraz pure product by an external standard method is 99.6 percent. Mass of mother solution: 345g, n-hexane was washed and collected separately. And collecting the washing liquid, uniformly treating, rectifying, separating and collecting normal hexane, and reusing the normal hexane for washing filter cakes. After repeated application of the crystallization mother liquor, the solvent is recovered under reduced pressure, and prochloraz manganese is prepared from kettle residues, so that 100% recovery is realized.
Example 4
100g of 96% prochloraz was put into a 1L three-necked flask at normal temperature, and then 300g of xylene solvent was added thereto to dissolve prochloraz with stirring. After prochloraz is completely dissolved, 50g of normal hexane solvent is added, and the temperature is reduced, and the crystallization temperature is-5 ℃. At this temperature, crystallization was carried out with stirring for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-hexane. The obtained prochloraz wet product is dried for 2 hours at 35 ℃. 82.1g of purified prochloraz pure product has pure white color and the content is 99.8 percent measured by an external standard method. Mass of mother solution: 335g, and the washed n-hexane was collected separately.
Example 5
100g of 96% prochloraz was put into a 1L three-necked flask at normal temperature, and then 300g of chlorobenzene solvent was added thereto to dissolve prochloraz with stirring. After prochloraz is completely dissolved, 50g of normal hexane solvent is added, and the temperature is reduced, and the crystallization temperature is-5 ℃. At this temperature, crystallization was carried out with stirring for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-hexane. The obtained prochloraz wet product is dried for 2 hours at 35 ℃. 81.7g of purified prochloraz pure product with pure white color and the content of which is 99.9 percent measured by an external standard method. Mass of mother solution: 335g, and the washed n-hexane was collected separately.
Example 6
100g of 96% prochloraz was put into a 1L three-necked flask at normal temperature, and then 300g of toluene solvent was added thereto to dissolve prochloraz with stirring. After prochloraz is completely dissolved, 50g of cyclohexane solvent is added, and the temperature is reduced, and the crystallization temperature is-5 ℃. At this temperature, crystallization was carried out with stirring for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g cyclohexane. The obtained prochloraz wet product is dried for 2 hours at 35 ℃. 79.8g of purified prochloraz pure product, the color is pure white, and the content is 99.8 percent by an external standard method. Mass of mother solution: 341g, cyclohexane was washed and collected separately.
Example 7
100g of 96% prochloraz was put into a 1L three-necked flask at normal temperature, and then 300g of toluene solvent was added thereto to dissolve prochloraz with stirring. After prochloraz is completely dissolved, 50g of n-heptane solvent is added, and the temperature is reduced, and the crystallization temperature is-5 ℃. At this temperature, crystallization was carried out with stirring for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-heptane. The obtained prochloraz wet product is dried for 2 hours at 35 ℃. 81.3g of purified prochloraz pure product with pure white color and the content of which is 99.8 percent measured by an external standard method. Mass of mother solution: 342g, n-heptane was washed and collected separately.
Example 8
100g of 96% prochloraz was put into a 1L three-necked flask at normal temperature, and then 500g of toluene solvent was added thereto to dissolve prochloraz with stirring. After prochloraz is completely dissolved, 50g of normal hexane solvent is added, and the temperature is reduced, and the crystallization temperature is-5 ℃. At this temperature, crystallization was carried out with stirring for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-hexane. The obtained prochloraz wet product is dried for 2 hours at 35 ℃. 76.7g of purified prochloraz pure product with pure white color and the content of which is 99.8 percent measured by an external standard method. Mass of mother solution: 349g of washed n-hexane was collected separately.
Example 9
100g of 96% prochloraz was put into a 1L three-necked flask at normal temperature, and then 300g of toluene solvent was added thereto to dissolve prochloraz with stirring. After prochloraz is completely dissolved, 150g of normal hexane solvent is added, and the temperature is reduced, and the crystallization temperature is-5 ℃. At this temperature, crystallization was carried out with stirring for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-hexane. The obtained prochloraz wet product is dried for 2 hours at 35 ℃. 81.7g of purified prochloraz pure product with pure white color and the content of which is 99.5 percent measured by an external standard method. Mass of mother solution: 332g, and the washed n-hexane was collected separately.
Comparative example 1
100g of 96% prochloraz was put into a 1L three-necked flask at normal temperature, and then 300g of ethyl acetate solution was added thereto to dissolve prochloraz with stirring. After prochloraz is completely dissolved, 50g of normal hexane solvent is added, and the temperature is reduced, and the crystallization temperature is-5 ℃. At this temperature, crystallization was carried out with stirring for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-hexane. The obtained prochloraz wet product is dried for 2 hours at 35 ℃. 68.5g of purified prochloraz pure product with pure white color and the content of which is 99.4 percent measured by an external standard method. Mass of mother solution: 356g, and washed with n-hexane.
Comparative example 2
100g of 96% prochloraz was put into a 1L three-necked flask at normal temperature, and then 300g of toluene solvent was added thereto to dissolve prochloraz with stirring. After prochloraz is completely dissolved, 50g of methylcyclohexane solvent is added, and the temperature is reduced, and the crystallization temperature is-5 ℃. At this temperature, crystallization was carried out with stirring for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g methylcyclohexane. The obtained prochloraz wet product is dried for 2 hours at 35 ℃. 82.1g of purified prochloraz pure product has pure white color and the content is 99.3 percent measured by an external standard method. Mass of mother solution: 328g, and the methylcyclohexane was washed and collected separately.
Comparative example 3
100g of 96% prochloraz was put into a 1L three-necked flask at normal temperature, and then 550g of toluene solvent was added thereto to dissolve prochloraz with stirring. After prochloraz is completely dissolved, 50g of normal hexane solvent is added, and the temperature is reduced, and the crystallization temperature is-5 ℃. At this temperature, crystallization was carried out with stirring for 2 hours. The filter cake was filtered under vacuum at low temperature and washed twice with 100g of n-hexane. The obtained prochloraz wet product is dried for 2 hours at 35 ℃. 76.8g of purified prochloraz pure product with pure white color and 99.8 percent of content measured by an external standard method. Mass of mother solution: 341g, n-hexane was washed and collected separately.
Claims (9)
1. The purification method of prochloraz is characterized by comprising the following steps:
(1) Adding the prochloraz crude product into benign solvent, stirring and dissolving;
(2) After the crude prochloraz is completely dissolved, adding a certain amount of poor solvent, and cooling and crystallizing after the poor solvent is added; filtering the separated crystals, washing with poor solvent, and drying to obtain prochloraz pure product.
2. The purification method according to claim 1, wherein in step (1), the benign solvent is selected from one or more of toluene, xylene and chlorobenzene.
3. The purification method of claim 2, wherein the benign solvent is toluene.
4. A purification process according to any one of claims 1 to 3, wherein the mass ratio of prochloraz crude to benign solvent is 1:2 to 5.
5. A purification process according to any one of claims 1 to 3, wherein in step (2) the poor solvent is cyclohexane, n-hexane, n-heptane.
6. The method according to claim 5, wherein the poor solvent is n-hexane.
7. The purification method according to claim 1, 5 or 6, wherein the mass ratio of prochloraz crude product to poor solvent is 1:0.5 to 1.5.
8. The purification method according to claim 1, wherein in the step (2), the temperature-lowering crystallization is crystallization for 2 hours at a temperature of-10 to-5 ℃.
9. The purification method according to claim 1 or 8, wherein in step (2), the drying temperature is lower than 35 ℃ and the drying time is 2 hours.
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| CN202311496096.0A CN117510410A (en) | 2023-11-10 | 2023-11-10 | Prochloraz purification method |
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