CN115260102A - Method for recovering imidazole from anecortave acetate silicon ether production wastewater - Google Patents
Method for recovering imidazole from anecortave acetate silicon ether production wastewater Download PDFInfo
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- CN115260102A CN115260102A CN202211107797.6A CN202211107797A CN115260102A CN 115260102 A CN115260102 A CN 115260102A CN 202211107797 A CN202211107797 A CN 202211107797A CN 115260102 A CN115260102 A CN 115260102A
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- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 title claims abstract description 228
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229960001232 anecortave Drugs 0.000 title claims abstract description 37
- YUWPMEXLKGOSBF-GACAOOTBSA-N Anecortave acetate Chemical compound O=C1CC[C@]2(C)C3=CC[C@]4(C)[C@](C(=O)COC(=O)C)(O)CC[C@H]4[C@@H]3CCC2=C1 YUWPMEXLKGOSBF-GACAOOTBSA-N 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 239000002351 wastewater Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 22
- 239000010703 silicon Substances 0.000 title claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 238000000926 separation method Methods 0.000 claims abstract description 23
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000004090 dissolution Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 60
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 57
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 40
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 32
- JDIIGWSSTNUWGK-UHFFFAOYSA-N 1h-imidazol-3-ium;chloride Chemical compound [Cl-].[NH2+]1C=CN=C1 JDIIGWSSTNUWGK-UHFFFAOYSA-N 0.000 claims description 23
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000011780 sodium chloride Substances 0.000 claims description 16
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 239000007791 liquid phase Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 239000012071 phase Substances 0.000 claims description 10
- 239000007790 solid phase Substances 0.000 claims description 10
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000012452 mother liquor Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- 238000011084 recovery Methods 0.000 abstract description 10
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 230000006837 decompression Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 23
- 239000007789 gas Substances 0.000 description 8
- -1 ether compound Chemical class 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000006266 etherification reaction Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- ITKVLPYNJQOCPW-UHFFFAOYSA-N chloro-(chloromethyl)-dimethylsilane Chemical compound C[Si](C)(Cl)CCl ITKVLPYNJQOCPW-UHFFFAOYSA-N 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical compound [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- JXJTWJYTKGINRZ-UHFFFAOYSA-J silicon(4+);tetraacetate Chemical compound [Si+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O JXJTWJYTKGINRZ-UHFFFAOYSA-J 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000007039 two-step reaction Methods 0.000 description 1
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- 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
- C07D233/58—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 with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring nitrogen atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a method for recovering imidazole from anecortave acetate silicon ether production wastewater, which comprises the following steps: pH value adjustment, concentration, azeotropic water carrying, dissolution, solid-liquid separation, decompression concentration, cooling crystallization, solid-liquid separation and drying. The recovery rate of the imidazole in the wastewater recovered by the process method reaches over 90 percent, and the recovered imidazole can meet the production requirement of anecortave acetate silicon ether. The process provided by the invention is reasonable, the product quality is good, and the recovery rate of imidazole is high.
Description
Technical Field
The invention belongs to the field of medical environment chemical industry, and particularly relates to a method for recovering imidazole from anecortave acetate production wastewater.
Background
The anecortave acetate silicon ether compound is obtained by taking anecortave acetate hydroxyl compound as an initial raw material and carrying out two-step reaction of elimination of 9-position hydroxyl and etherification of 17-position hydroxyl silicon, and the specific synthetic route is as follows:
the synthesis method of the anecortave acetate silicon ether comprises the following steps: (1) elimination reaction; (2) quenching reaction; (3) adjusting the pH value; (4) dehydrating; (5) carrying out a silyl ether reaction; (6) washing and layering; (7) concentrating and crystallizing; (8) carrying out solid-liquid separation; and (9) drying. In the 17-position hydroxysilyl etherification reaction, imidazole is added to provide a weak alkaline environment, the anecortave acetate cyano reacts with chloromethyl dimethylchlorosilane, and the byproduct hydrogen chloride reacts with imidazole to generate imidazole hydrochloride. After water washing the layers separated, the aqueous imidazole hydrochloride solution was separated from the organic phase. In layered water, the mass fraction of imidazole hydrochloride is 30-40%.
By adopting the synthesis process, about 2 tons of imidazole-containing wastewater can be generated every 1 ton of anecortave acetate silicon ether. The imidazole-containing wastewater has high imidazole content, 4-5 ten thousand yuan/ton of imidazole and high recovery value. The imidazole is recycled, so that on one hand, the production cost of the anecortave acetate silicon ether compound can be greatly reduced; on the other hand, the energy can be saved, the emission can be reduced, and the environmental protection pressure can be reduced.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for recovering imidazole from anecortave acetate production wastewater so as to solve the technical problem.
In order to achieve the above object, the present invention provides a method for recovering imidazole from anecortave acetate production wastewater, wherein the wastewater contains: imidazole hydrochloride with the mass fraction of 30-40%, tetrahydrofuran with the mass fraction of about 5% and water with the mass fraction of 55-65%; the method for recovering imidazole from anecortave acetate silicon ether production wastewater comprises the following steps:
step (1), pH value adjustment: adding sodium hydroxide into the production wastewater of anecortave acetate to be treated, adjusting the pH value to 11-13, converting imidazole hydrochloride into imidazole and sodium chloride, and feeding the materials to the next step;
step (2), concentration: concentrating the material obtained in the step (1) to 50-60% of the weight of the waste liquid, condensing the gas phase to obtain tetrahydrofuran and water respectively, further treating the tetrahydrofuran and the water, and applying the tetrahydrofuran and the water to the production procedure of anecortave silicon acetate, wherein the rest material enters the next step;
step (3), carrying out azeotropic water carrying: adding an entrainer into the residual material concentrated in the step (2), continuing to concentrate and carry water, separating water by a water separator, and allowing the dehydrated material to enter the next step;
step (4), temperature-controlled dissolution: adding methanol into the dehydrated material obtained in the step (3), controlling the temperature to be 20-40 ℃ to fully dissolve imidazole, and enabling the material to enter the next step;
step (5), solid-liquid separation: performing solid-liquid separation on the material obtained in the step (4), wherein the solid phase is a crude sodium chloride product, performing further treatment to obtain a finished sodium chloride product, and the liquid phase is an imidazole solution, and performing the next step;
step (6), concentration: concentrating the imidazole solution in the step (5) to 1.0-2.0 times of the weight of the waste liquid, condensing the gas phase to obtain a mixed solution of an entrainer and methanol, further treating and separating, respectively sleeving the entrainer and the methanol in the step (3) and the step (4), and feeding the concentrated material to the next step;
step (7), cooling and crystallizing: cooling the material concentrated in the step (6) to-5 ℃, controlling the temperature for 1-5 h, and enabling the material to enter the next step;
step (8), solid-liquid separation: performing solid-liquid separation on the material obtained in the step (7), wherein a liquid phase is mother liquor, the liquid phase is concentrated after enrichment, and a solid phase is an imidazole wet product;
step (9), drying: and (3) placing the imidazole wet product obtained in the step (8) at 40-60 ℃ for vacuum drying to obtain an imidazole finished product, and applying the imidazole finished product in the production process of anecortave acetate silicon ether.
Optionally, in the step (3), the reaction entrainer is at least one of dichloromethane, toluene or chloroform;
the mass ratio of the entrainer to the wastewater is 1-3.
Optionally, in the step (4), the mass ratio of the methanol to the wastewater is 0.5 to 3.
The method for recovering imidazole from anecortave acetate siloxane production wastewater has the following advantages:
(1) The imidazole hydrochloride has higher added value than the imidazole hydrochloride, and the invention fully utilizes the characteristic of the reaction of the imidazole hydrochloride and sodium hydroxide and adopts the pH value adjusting technology to convert the imidazole hydrochloride into imidazole and sodium chloride, thereby realizing the recovery of imidazole from the production wastewater.
(2) Imidazole has a high solubility in water, and the solubility at 20 ℃ is 63.3g of imidazole per 100g of water. At present, the imidazole is mainly produced and prepared by adopting an evaporation concentration method. While the boiling point of imidazole is 256 ℃, and the energy consumption of the evaporation concentration technology is high.
The method fully utilizes the characteristic that imidazole has higher solubility in dichloromethane, toluene or a mixed solution of chloroform and methanol, adopts azeotropic dehydration and solvent displacement technologies, can realize energy conservation and emission reduction, and can recycle the entrainer and the methanol.
(3) The purity of the imidazole recovered by the method is more than 99 percent, the production requirement of anecortave acetate silicon ether can be met, and the recovery rate of the imidazole (the recovery rate =100 percent, the actual recovery rate of the imidazole/the theoretical content of the imidazole in the wastewater) reaches more than 90 percent.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, the present invention is described in detail with reference to the accompanying drawings and the detailed description thereof.
The following describes the implementation of the method of the present invention in detail by way of examples.
Example 1
The wastewater from anecortave acetate production contains: imidazole hydrochloride with the mass fraction of 40%, tetrahydrofuran with the mass fraction of about 5% and water with the mass fraction of 55%; the method for recovering imidazole from wastewater comprises the following steps:
step (1), pH value adjustment: adding sodium hydroxide into 100kg of production wastewater of anecortave acetate silicon ether to be treated, adjusting the pH value to 13, converting imidazole hydrochloride into imidazole and sodium chloride, and feeding the materials to the next step;
step (2), concentration: concentrating the material obtained in the step (1) to 60kg, condensing the gas phase to obtain 5kg of tetrahydrofuran and 35kg of water respectively, further treating the tetrahydrofuran and the water, and applying the tetrahydrofuran and the water to the production process of anecortave acetate silicon ether, wherein the rest material enters the next step;
step (3), azeotropic entrainment of water: adding 300kg of dichloromethane into the residual material concentrated in the step (2), continuing to concentrate and carry water, separating water by a water separator, and allowing the dehydrated material to enter the next step;
step (4), temperature-controlled dissolution: adding 50kg of methanol into the dehydrated material obtained in the step (3), controlling the temperature to be 20 ℃ to fully dissolve imidazole, and enabling the material to enter the next step;
step (5), solid-liquid separation: performing solid-liquid separation on the material obtained in the step (4), wherein the solid phase is a crude sodium chloride product, performing further treatment to obtain a finished sodium chloride product, and the liquid phase is an imidazole solution, and performing the next step;
step (6), concentration: concentrating the imidazole solution in the step (5) to 200kg, condensing a gas phase to obtain a mixed solution of an entrainer and methanol, further treating and separating, respectively sleeving the entrainer and the methanol in the step (3) and the step (4), and feeding the concentrated material to the next step;
step (7), cooling and crystallizing: cooling the material concentrated in the step (6) to-5 ℃, controlling the temperature for 5 hours, and enabling the material to enter the next step;
step (8), solid-liquid separation: performing solid-liquid separation on the material obtained in the step (7), wherein a liquid phase is mother liquor, and concentrated treatment is performed after enrichment, and a solid phase is an imidazole wet product;
step (9), drying: and (3) placing the imidazole wet product obtained in the step (8) at 40 ℃ for vacuum drying to obtain 24.0kg of imidazole finished product, and applying the imidazole finished product in the anecortave acetate silyl production process, wherein the purity of the imidazole is 99.2%, and the recovery rate is 92%.
Example 2
The wastewater from anecortave acetate production contains: imidazole hydrochloride with the mass fraction of 30%, tetrahydrofuran with the mass fraction of about 5% and water with the mass fraction of 65%; the method for recovering imidazole from wastewater comprises the following steps:
step (1), pH value adjustment: adding sodium hydroxide into 100kg of production wastewater of anecortave acetate to be treated, adjusting the pH value to 11, converting imidazole hydrochloride into imidazole and sodium chloride, and feeding the materials to the next step;
step (2), concentration: concentrating the material obtained in the step (1) to 50kg, condensing a gas phase to obtain 5kg of tetrahydrofuran and 45kg of water respectively, further treating the tetrahydrofuran and the water, and mechanically applying the tetrahydrofuran and the water to the production process of the anecortave acetate silicon ether substance, wherein the rest material enters the next step;
step (3), carrying out azeotropic water carrying: adding 100kg of toluene into the residual material concentrated in the step (2), continuously concentrating and carrying water, separating water by a water separator, and allowing the dehydrated material to enter the next step;
step (4), temperature-controlled dissolution: adding 300kg of methanol into the dehydrated material obtained in the step (3), controlling the temperature to be 40 ℃ to fully dissolve imidazole, and enabling the material to enter the next step;
step (5), solid-liquid separation: performing solid-liquid separation on the material obtained in the step (4), wherein the solid phase is a sodium chloride crude product, performing further treatment to obtain a sodium chloride finished product, and the liquid phase is an imidazole solution, and performing the next step;
step (6), concentration: concentrating the imidazole solution in the step (5) to 100kg, condensing a gas phase to obtain a mixed solution of an entrainer and methanol, further treating and separating, respectively sleeving the entrainer and the methanol in the step (3) and the step (4), and feeding the concentrated material to the next step;
step (7), cooling and crystallizing: cooling the material concentrated in the step (6) to 5 ℃, controlling the temperature for 1h, and enabling the material to enter the next step;
step (8), solid-liquid separation: performing solid-liquid separation on the material obtained in the step (7), wherein a liquid phase is mother liquor, and concentrated treatment is performed after enrichment, and a solid phase is an imidazole wet product;
step (9), drying: and (3) placing the imidazole wet product obtained in the step (8) at 60 ℃ for vacuum drying to obtain 23.5kg of an imidazole finished product, wherein the imidazole finished product is applied to the production process of anecortave acetate silicon ether substances, the purity of the imidazole is 99.3%, and the recovery rate is 90.3%.
Example 3
The wastewater from anecortave acetate production contains: imidazole hydrochloride with the mass fraction of 35%, tetrahydrofuran with the mass fraction of about 5% and water with the mass fraction of 60%; the method for recovering imidazole from wastewater comprises the following steps:
step (1), pH value adjustment: adding sodium hydroxide into 100kg of production wastewater of anecortave acetate silicon ether to be treated, adjusting the pH value to 12, converting imidazole hydrochloride into imidazole and sodium chloride, and feeding the materials to the next step;
step (2), concentration: concentrating the material obtained in the step (1) to 55kg, condensing the gas phase to obtain 5kg of tetrahydrofuran and 40kg of water respectively, further treating the tetrahydrofuran and the water, and applying the tetrahydrofuran and the water to the production process of anecortave acetate silicon ether, wherein the rest material enters the next step;
step (3), azeotropic entrainment of water: adding 200kg of chloroform into the residual material concentrated in the step (2), continuing to concentrate and carry water, separating water by a water separator, and feeding the dehydrated material to the next step;
step (4), temperature-controlled dissolution: adding 200kg of methanol into the dehydrated material obtained in the step (3), controlling the temperature to be 30 ℃ to fully dissolve imidazole, and enabling the material to enter the next step;
step (5), solid-liquid separation: performing solid-liquid separation on the material obtained in the step (4), wherein the solid phase is a crude sodium chloride product, performing further treatment to obtain a finished sodium chloride product, and the liquid phase is an imidazole solution, and performing the next step;
step (6), concentration: concentrating the imidazole solution in the step (5) to 150kg, condensing the gas phase to obtain a mixed solution of an entrainer and methanol, further treating and separating, respectively sleeving the entrainer and the methanol in the step (3) and the step (4), and feeding the concentrated material to the next step;
step (7), cooling and crystallizing: cooling the material concentrated in the step (6) to 0 ℃, controlling the temperature for 3 hours, and enabling the material to enter the next step;
step (8), solid-liquid separation: performing solid-liquid separation on the material obtained in the step (7), wherein a liquid phase is mother liquor, the liquid phase is concentrated after enrichment, and a solid phase is an imidazole wet product;
step (9), drying: and (3) placing the imidazole wet product obtained in the step (8) at 60 ℃ for vacuum drying to obtain 24.4kg of an imidazole finished product, wherein the imidazole finished product is applied to the production process of anecortave acetate silicon ether substances, the purity of the imidazole is 99.0 percent, and the recovery rate is 93.8 percent.
The method for recovering imidazole from anecortave acetate production wastewater provided by the invention is described in detail above, a specific example is applied in the method for explaining the principle and the implementation mode of the invention, and the description of the example is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (3)
1. A method for recovering imidazole from anecortave acetate silicon ether production wastewater is characterized in that the wastewater contains: imidazole hydrochloride with the mass fraction of 30-40%, tetrahydrofuran with the mass fraction of 5% and water with the mass fraction of 55-65%; the method for recovering imidazole from anecortave acetate silicon ether production wastewater comprises the following steps:
step (1), pH value adjustment: adding sodium hydroxide into the anecortave acetate production wastewater to be treated, adjusting the pH value to 11-13, converting imidazole hydrochloride into imidazole and sodium chloride, and feeding the materials to the next step;
step (2), concentration: concentrating the material obtained in the step (1) to 50-60% of the weight of the waste liquid, condensing the gas phase to obtain tetrahydrofuran and water respectively, further treating the tetrahydrofuran and the water, and applying the tetrahydrofuran and the water to the production process of anecortave acetate silicon ether, wherein the rest material enters the next step;
step (3), azeotropic entrainment of water: adding an entrainer into the residual material concentrated in the step (2), continuing to concentrate and carry water, separating water by a water separator, and allowing the dehydrated material to enter the next step;
step (4), temperature-controlled dissolution: adding methanol into the dehydrated material obtained in the step (3), controlling the temperature to be 20-40 ℃ to fully dissolve imidazole, and enabling the material to enter the next step;
step (5), solid-liquid separation: performing solid-liquid separation on the material obtained in the step (4), wherein the solid phase is a crude sodium chloride product, performing further treatment to obtain a finished sodium chloride product, and the liquid phase is an imidazole solution, and performing the next step;
step (6), concentration: concentrating the imidazole solution obtained in the step (5) to 1.0-2.0 times of the weight of the waste liquid, condensing a gas phase to obtain a mixed solution of an entrainer and methanol, further treating and separating the mixed solution, respectively sleeving the entrainer and the methanol in the step (3) and the step (4), and feeding the concentrated material to the next step;
step (7), cooling and crystallizing: cooling the material concentrated in the step (6) to-5 ℃, controlling the temperature for 1-5 h, and enabling the material to enter the next step;
step (8), solid-liquid separation: performing solid-liquid separation on the material obtained in the step (7), wherein a liquid phase is mother liquor, and concentrated treatment is performed after enrichment, and a solid phase is an imidazole wet product;
step (9), drying: and (3) placing the imidazole wet product obtained in the step (8) at 40-60 ℃ for vacuum drying to obtain an imidazole finished product, and applying the imidazole finished product in the production process of anecortave acetate silicon ether.
2. The method according to claim 1, wherein in the step (3), the entrainer is one or more of dichloromethane, toluene or chloroform;
the mass ratio of the entrainer to the wastewater is 1-3.
3. The method according to claim 1, wherein in the step (4), the mass ratio of the methanol to the wastewater is 0.5-3.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4921638A (en) * | 1986-11-05 | 1990-05-01 | The Upjohn Company | 17β-cyano-9α,17α-dihydroxyandrost-4-en-3-one |
| CN102603842A (en) * | 2012-02-20 | 2012-07-25 | 湖南诺凯生物医药有限公司 | Preparation method of hydrocortisone acetate or analogue thereof |
| CN105017364A (en) * | 2015-07-06 | 2015-11-04 | 湖南新合新生物医药有限公司 | Methylprednisolone intermediate, preparation method therefor and application thereof |
| CN113307774A (en) * | 2021-05-17 | 2021-08-27 | 山东汇海医药化工有限公司 | Method for recovering imidazole from imidazole hydrochloride wastewater |
-
2022
- 2022-09-13 CN CN202211107797.6A patent/CN115260102A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4921638A (en) * | 1986-11-05 | 1990-05-01 | The Upjohn Company | 17β-cyano-9α,17α-dihydroxyandrost-4-en-3-one |
| CN102603842A (en) * | 2012-02-20 | 2012-07-25 | 湖南诺凯生物医药有限公司 | Preparation method of hydrocortisone acetate or analogue thereof |
| CN105017364A (en) * | 2015-07-06 | 2015-11-04 | 湖南新合新生物医药有限公司 | Methylprednisolone intermediate, preparation method therefor and application thereof |
| CN113307774A (en) * | 2021-05-17 | 2021-08-27 | 山东汇海医药化工有限公司 | Method for recovering imidazole from imidazole hydrochloride wastewater |
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