CN113562912B - Method for treating spironolactone intermediate production wastewater - Google Patents
Method for treating spironolactone intermediate production wastewater Download PDFInfo
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- CN113562912B CN113562912B CN202110717346.3A CN202110717346A CN113562912B CN 113562912 B CN113562912 B CN 113562912B CN 202110717346 A CN202110717346 A CN 202110717346A CN 113562912 B CN113562912 B CN 113562912B
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- 239000002351 wastewater Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 22
- LXMSZDCAJNLERA-ZHYRCANASA-N spironolactone Chemical compound C([C@@H]1[C@]2(C)CC[C@@H]3[C@@]4(C)CCC(=O)C=C4C[C@H]([C@@H]13)SC(=O)C)C[C@@]21CCC(=O)O1 LXMSZDCAJNLERA-ZHYRCANASA-N 0.000 title claims abstract description 17
- 229960002256 spironolactone Drugs 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 238000005406 washing Methods 0.000 claims abstract description 27
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 239000000706 filtrate Substances 0.000 claims abstract description 14
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 13
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims 1
- 238000004065 wastewater treatment Methods 0.000 abstract description 6
- 230000006837 decompression Effects 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000543 intermediate Substances 0.000 abstract description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 8
- 230000002194 synthesizing effect Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- HHVIBTZHLRERCL-UHFFFAOYSA-N sulfonyldimethane Chemical compound CS(C)(=O)=O HHVIBTZHLRERCL-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 229940122522 Mineralocorticoid antagonist Drugs 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- -1 acetylthio Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000002934 diuretic Substances 0.000 description 1
- 230000001882 diuretic effect Effects 0.000 description 1
- 238000006735 epoxidation reaction Methods 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 239000002394 mineralocorticoid antagonist Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- KKVTYAVXTDIPAP-UHFFFAOYSA-M sodium;methanesulfonate Chemical compound [Na+].CS([O-])(=O)=O KKVTYAVXTDIPAP-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- GKASDNZWUGIAMG-UHFFFAOYSA-N triethyl orthoformate Chemical compound CCOC(OCC)OCC GKASDNZWUGIAMG-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Peptides Or Proteins (AREA)
- Steroid Compounds (AREA)
Abstract
The invention discloses a method for treating spironolactone intermediate production wastewater, which is characterized by comprising the following four steps: 1) Performing neutralization reaction; 2) Separating filtrate, solid and washing liquid by decompression, cooling, solvent adding, cooling, filter pressing and washing; 3) Vacuum drying the solid to obtain sodium bromide; 4) The filtrate and the washing liquid are combined and the solvent is recovered for direct use, and the dimethyl sulfoxide is evaporated from the residual liquid. According to the invention, HBr aqueous solution is adopted to carry out neutralization reaction on wastewater generated by spironolactone intermediate, filtrate, solid and washing liquid are separated out by decompression, cooling, solvent adding, cooling, filter pressing and washing, and the solvent is recovered by utilizing pressure, so that the solvent can be changed into valuables, the difficulty and time of wastewater treatment are reduced, the efficiency of wastewater treatment is improved, environmental pollution is avoided, and the pressure of environmental protection treatment is reduced.
Description
Technical Field
The invention belongs to the technical field of wastewater recovery treatment, and relates to a method for treating spironolactone intermediate production wastewater.
Background
Spironolactone (1), chemically known as (7 c, 170 c) -7. (acetylthio) 17. Hydroxy-3. Oxopregna.4-ene-21. Carboxylic acid 1L lactone, is a mineralocorticoid antagonist developed by seires corporation, has been marketed in many countries and is clinically used as a diuretic. However, 17b, 20b-epoxy-3-ethoxy-17 a-pregna-3,5-diene is an important intermediate for synthesizing spironolactone, the main preparation method is to take 4-AD as a raw material, after protecting a 3-carbonyl group by triethyl orthoformate, take dimethyl sulfoxide as a solvent, perform epoxidation reaction with trimethyl bromide under the catalysis of sodium ethoxide, decompress and evaporate ethanol after the reaction is finished, then add water to separate out a product, about 15 tons of wastewater is generated for each 1 ton of product, and at the present stage, the wastewater directly enters a wastewater treatment system for treatment, so that the wastewater treatment difficulty is increased, the treatment time is longer, and even the environmental pollution is directly caused.
Through retrieval, chinese patent document publication No. CN104311460A, publication No. 2015, 01.28.2015, discloses a method for recovering and treating dimethyl sulfoxide waste salt, and proposes that nitric acid is added into a dimethyl sulfoxide waste salt solution to perform a neutralization reaction and an oxidation reaction, and then dimethyl sulfone, sodium nitrate and sodium methanesulfonate crystals are separated.
The invention discloses a method for preparing a low-residue flocculant in waste water and a method for recycling the waste water, wherein the method is disclosed in Chinese patent document publication No. CN110372805A, publication date 2019, 10 months and 25 days, and the method for preparing the flocculant comprises the following steps: step a: synthesizing an environment-responsive flocculant intermediate; step b: synthesizing temperature stimulus responsive starch; step c: synthesizing temperature/pH stimuli-responsive starch ", which is still in the laboratory stage, and requires a long time for industrial application.
In summary, the spironolactone intermediate wastewater at the present stage has the problems of high treatment difficulty, long time and difficult recovery. For this reason, a new technical solution is needed to solve the above-mentioned technology.
Disclosure of Invention
The invention aims to provide a method for treating wastewater from spironolactone intermediate production, which aims to solve the problems of great difficulty and long time for treating wastewater from spironolactone intermediate production at the present stage in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for treating spironolactone intermediate production wastewater is characterized by comprising the following specific steps:
1) Adding 17b, 20b-epoxy-3-ethoxy-17 a-pregna-3,5-diene generated wastewater into a reaction kettle, and dropwise adding 30-50% aqueous HBr solution into the reaction kettle to perform a neutralization reaction until the pH is =5-7;
2) Evaporating water from the wastewater after the neutralization reaction under the conditions that the pressure is-0.095 Mpa and the temperature is controlled below 90 ℃ until no water flows out, then cooling the feed liquid without water to 25-35 ℃, adding a solvent with the weight ratio of 1-2 times, continuously cooling to-15-5 ℃, carrying out filter pressing to form a filtrate, and washing with the solvent with the weight ratio of 0.4-0.6 time to form a washing liquid and a solid;
3) Vacuum drying the solid formed by washing in the step 2 at 35-45 ℃ for 3-5 hours to obtain sodium bromide;
4) And simultaneously combining the filtrate and the washing liquid in the step 2, recovering the solvent under normal pressure for direct application, and evaporating the dimethyl sulfoxide from the residual liquid under the conditions that the pressure is 0.098Mpa and the temperature is controlled below 90 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, HBr aqueous solution is adopted to carry out neutralization reaction on wastewater generated by spironolactone intermediate, filtrate, solid and washing liquid are separated out by decompression, cooling, solvent adding, cooling, filter pressing and washing, and the solvent is recovered by utilizing pressure, so that the solvent can be changed into valuables, the difficulty and time of wastewater treatment are reduced, the efficiency of wastewater treatment is improved, the environmental pollution is avoided, and the pressure of environmental protection treatment is reduced.
2. The invention utilizes the dimethyl sulfoxide, sodium bromide and sodium hydroxide in the wastewater as resources by controlling the pressure and the temperature, and eliminates the discharge of the wastewater.
3. The method has the characteristics of simple process, environment-friendly treatment process and high yield.
Detailed Description
The following examples are intended to further illustrate the invention and are not intended to limit its application.
Example 1:
2500kg of waste water generated in 17b, 20b-epoxy-3-ethoxy-17 a-pregna-3,5-diene synthesis is added into a reaction kettle, 40% of HBr aqueous solution is dropwise added into the reaction kettle to carry out neutralization reaction until the pH is =7, at this time, 126kg of HBr aqueous solution is consumed, 1326kg of water is distilled out under the condition that the pressure is-0.095 Mpa and the temperature is controlled at 70 ℃, 1326kg of water can be directly recycled as process water, then, the feed liquid without water outflow is cooled to 30 ℃, 1950kg of dichloromethane is added, the temperature is kept at-15 ℃, after 5 hours of heat preservation and crystallization, filter pressing is carried out to form filtrate, 130kg of dichloromethane is used for washing to generate washing liquid, 400kg of solid is generated after washing, the generated solid is subjected to vacuum drying at 40 ℃ for 4 hours to obtain 340kg of sodium bromide (the content is 98.5% by analysis and meets the requirements of industrial products), after the formed filtrate and the washing liquid are combined, the internal temperature is guaranteed to be 90 Mpa, the recovery is carried out under the condition that the temperature is reduced, the residual liquid is directly recovered under the temperature of 90 ℃ of 80.80 ℃ and the temperature is controlled to be 99 kg of dichloromethane (GC 5 kg, 99.5 kg) and the residual liquid is directly applied to be used as a residual liquid under the temperature, and the temperature of 99.80 kg of 99 kg of the temperature.
Example 2:
2500kg of wastewater generated by synthesizing 17b, 20b-epoxy-3-ethoxy-17 a-pregna-3,5-diene is added into a reaction kettle, 40% HBr aqueous solution is dropwise added into the reaction kettle to perform a neutralization reaction until the pH is =7, at this time, 126kg of HBr aqueous solution is consumed, 1350kg of water is evaporated under the condition that the pressure is-0.095 Mpa and the temperature is controlled at 50 ℃, at this time, 1350kg of water can be directly recycled as process water, the feed liquid without water outflow is cooled to 30 ℃, 2552kg of chloroform is added, the temperature is kept at-15 ℃, after 5 hours of heat preservation and crystallization, filter pressing is performed to form filtrate, 130kg of chloroform is used for washing to generate washing liquid, at the same time, 410kg of solid is generated after washing, the generated solid is subjected to vacuum drying at 40 ℃ for 4 hours to obtain 350kg of sodium bromide (the content is analyzed, 98.7% of which meets the requirement of industrial products), after the formed filtrate and the washing liquid are combined, the internal temperature is ensured to be below 90 Mpa, the temperature is 930 ℃, the residual liquid is directly subjected to recovery under the GC temperature of 0.098 kg (GC, the residual liquid is obtained by a method, and the method is directly applied to recover the temperature is controlled at the temperature of 99.098 kg of 0.098 kg).
Example 3:
2500kg of waste water generated by synthesizing 17b, 20b-epoxy-3-ethoxy-17 a-pregna-3,5-diene is added into a reaction kettle, 40% of HBr aqueous solution is dropwise added into the reaction kettle to carry out neutralization reaction until the pH value is =7, 126kg of HBr aqueous solution is consumed at the moment, 1326kg of water is distilled out under the condition that the pressure is-0.095 MPa and the temperature is controlled to be 60 ℃, 1326kg of water can be directly recycled as process water at the moment, then, the feed liquid which does not flow out is cooled to 30 ℃, 1300kg of chloroform is added, the temperature is kept and crystallized for 5 hours, filter pressing is carried out to form filtrate, 130kg of chloroform is used for washing to generate washing liquid, 380kg of solid is generated after washing, vacuum drying is carried out at the temperature of 40 ℃ for 4 hours to obtain 330kg of sodium bromide (the content is analyzed, the content is 98.3% and meets the requirements of industrial products), the formed filtrate and the washing liquid are combined, the internal temperature is kept below 90 ℃ and is kept to be 1350 ℃, the residual liquid is directly dried under the temperature, the temperature is used for recovery of chloroform, and the residual liquid is used as 99.8 kg of dimethyl sulfoxide under the GC (GC, the temperature is controlled to be 99.8 kg) under the temperature is controlled to be 99.095 kg).
Claims (3)
1. A method for treating spironolactone intermediate production wastewater is characterized by comprising the following specific steps:
1) Adding wastewater generated by a spironolactone intermediate into a reaction kettle, and dropwise adding 30-50% HBr aqueous solution into the reaction kettle to perform neutralization reaction, wherein the spironolactone intermediate is 17b, 20b-epoxy-3-ethoxy-17 a-pregna-3,5-diene;
2) Evaporating water from the wastewater after the neutralization reaction under reduced pressure until no water flows out, then cooling the feed liquid without water flowing out to 25-35 ℃, adding a solvent with the weight ratio of 1-2 times, continuously cooling to-15-5 ℃, carrying out filter pressing to form filtrate, and washing with the solvent with the weight ratio of 0.4-0.6 time to form washing liquid and solid, wherein the pressure of reduced pressure is controlled to-0.095 Mpa, and the temperature is controlled to be below 90 ℃;
3) Vacuum drying the solid formed by washing in the step 2 at 35-45 ℃ for 3-5 hours to obtain sodium bromide;
4) And simultaneously combining the filtrate and the washing liquid in the step 2, recovering the solvent under normal pressure for direct application, and evaporating the residual liquid under reduced pressure to remove dimethyl sulfoxide, wherein the pressure of the reduced pressure is controlled to be-0.098 MPa, and the temperature is controlled to be below 90 ℃.
2. The method for treating wastewater from spironolactone intermediate production according to claim 1, wherein in step 1, the pH of the neutralization reaction is 5 to 7.
3. The method for treating wastewater from spironolactone intermediate production according to claim 1, wherein in step 2, the solvent is any one of methanol, ethanol, dichloromethane, tetrahydrofuran, acetonitrile and chloroform.
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| GB1544642A (en) * | 1976-06-04 | 1979-04-25 | Bristol Myers Co | 9,11-epoxy steroids and synthesis of corticosteroids therefrom |
| CN102249993A (en) * | 2011-05-10 | 2011-11-23 | 浙江爱迪亚营养科技开发有限公司 | Method for treating waste water generated from production of 3-cyanopyridine and recovering nicotinic acid |
| CN102417498B (en) * | 2011-08-24 | 2015-09-09 | 重庆紫光化工股份有限公司 | The synthetic method of 3-(α-methoxyl group) methene cumarone-2 (3H)-one |
| CN103508869B (en) * | 2013-10-24 | 2015-04-22 | 昆山力田医化科技有限公司 | Synthetic method for 2-benzyl cyclopentanone |
| CN103694296B (en) * | 2013-12-18 | 2015-12-02 | 湖南科瑞生物制药股份有限公司 | The preparation method of DHEA intermediate 3 β-acetoxy-androst-3,5-diene-17-ketone |
| CN108373492B (en) * | 2018-04-20 | 2021-12-21 | 江苏远大仙乐药业有限公司 | Preparation method of cortisone acetate |
| CN109134852A (en) * | 2018-09-06 | 2019-01-04 | 南京工业大学 | Method for realizing zero discharge of poly (p-phenylene terephthalamide) filtering and washing wastewater |
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Denomination of invention: A method for treating wastewater from the production of spironolactone intermediates Granted publication date: 20230407 Pledgee: Jiangsu Rudong Rural Commercial Bank Co.,Ltd. Yangkou Branch Pledgor: Jiaerke Biotechnology Nantong Co.,Ltd. Registration number: Y2024980022502 |