CN104193071A - Treating method of high-ammonia-nitrogen mother liquor wastewater in MCP (methyl cyclopentenolone) production - Google Patents
Treating method of high-ammonia-nitrogen mother liquor wastewater in MCP (methyl cyclopentenolone) production Download PDFInfo
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- CN104193071A CN104193071A CN201410501487.1A CN201410501487A CN104193071A CN 104193071 A CN104193071 A CN 104193071A CN 201410501487 A CN201410501487 A CN 201410501487A CN 104193071 A CN104193071 A CN 104193071A
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Abstract
The invention provides a treating method of high-ammonia-nitrogen mother liquor wastewater in MCP (methyl cyclopentenolone) production. A water phase and an organic phase are separated from high-ammonia-nitrogen mother liquor through an extraction agent; the extraction agent can be recycled and MCP can be recovered through distillation and condensation of the organic phase; dimethylamine hydrochloride can be recovered and continuously put into production for use through decolorization and distillation crystallization treatment of the water phase, and steam used for distillation is waste heat tail gas. With the adoption of the method, MCP crude products can be effectively recovered, meanwhile, the waste heat tail gas is used for evaporating the wastewater, and the dimethylamine hydrochloride is recovered, so that multiple effects of cleanness, environmental pollution and recycling of resources are realized.
Description
Technical field
The present invention relates to the treatment process of high ammonia nitrogen mother liquor waste water in a kind of methyl cyclopentenyl ketone production.
Background technology
Methyl cyclopentenyl ketone is a kind of flavouring agent, but can produce a large amount of high salt high ammonia-nitrogen wastewaters in producing.A global difficult problem for the processing of high salt high ammonia-nitrogen wastewater at present, present sewage work adopts dilution artifact facture mostly, and this method cost is little, and can not cause secondary pollution, but limitation is that processing power is poor, can not reach the demand of Production in Chemical Plant far away.Another kind method is evaporation process, can meet the Chemical Manufacture needs of certain scale, but too high for energy consumption requirement in process, cost is too large, and also very difficult processing of the waste residue producing, and causes secondary pollution.
Summary of the invention
The object of the invention is to solve methyl cyclopentenyl ketone in prior art produce in the problem of high ammonia nitrogen mother liquor waste water processing, provide a kind of methyl cyclopentenyl ketone produce in the treatment process of high ammonia nitrogen mother liquor waste water.
Concrete technical scheme
The treatment process of high ammonia nitrogen mother liquor waste water in a kind of methyl cyclopentenyl ketone (MCP) production, is characterized in that comprising the following steps:
A. high ammonia nitrogen mother liquor production station being produced is sent into after mother liquor tank metering, with mother liquor pump suction extraction kettle, adds mother liquor volume 0.2-0.3 extraction agent (chloroform) doubly, stirs 25-35 minute, leaves standstill layering after 2.5-3.5 hour, separates water and organic phase;
B. organic phase is carried out to underpressure distillation by pump suction still kettle, temperature remains on 40～45 DEG C and reclaims extraction agent, and the extraction agent distillating (chloroform) enters accumulator tank and can be recycled after condensation, and residuum is further extraction and application;
C. after the mother liquor that the residuum of distillation is added to 100-200L stirs, send into freezing and crystallizing still salt solution and be cooled to 10～13 DEG C, put into whizzer after being incubated after 25-35 minute to get rid of material, obtain MCP crude product, waste water enters geosyncline, send sewage plant processing.
On technique scheme basis, there is following further improvement project:
A step is extracted to the water pump suction decolouring still separating, add 18-22kg gac and be warming up to 80～85 DEG C, be incubated press filtration after 25-35 minute, filtrate delivered to still kettle, underpressure distillation, steam water and enter tank, steam 75% left and right of liquid, stop steaming, send into the cooling of freezing and crystallizing still, crystallization kettle is cooled to 5～7 DEG C, is incubated centrifuge dripping after 30 minutes and obtains dimethylamine hydrochloride.
In above-mentioned d step, it is the waste heat tail gas in producing that filtrate is distilled required steam.
The invention has the advantages that and can reclaim MCP crude product, use waste heat tail gas evaporating waste water, reclaim dimethylamine hydrochloride, reach clean environment firendly, the multi-efficiency of resource recycling.
Brief description of the drawings
Fig. 1 is the process flow sketch of high ammonia nitrogen mother liquor waste water during methyl cyclopentenyl ketone of the present invention (MCP) is produced.
Embodiment
Embodiment 1
The treatment process of high ammonia nitrogen mother liquor waste water in a kind of methyl cyclopentenyl ketone (MCP) production, is characterized in that comprising the following steps:
A. high ammonia nitrogen mother liquor production station being produced is sent into mother liquor tank metering, and the volume of mother liquor is 1m
3, with mother liquor pump suction extraction kettle, add the extraction agent (chloroform) of 250L, stir 30 minutes, leave standstill layering after 3 hours, separate water and organic phase;
B. organic phase is carried out to underpressure distillation by pump suction still kettle, remain on-0.092-0.096MPa of pressure, temperature remains on 40～45 DEG C and reclaims extraction agent, and the extraction agent distillating (chloroform) enters accumulator tank and can be recycled after condensation, and residuum is further extraction and application;
C. after the mother liquor that the residuum of distillation is added to 150L stirs, send into freezing and crystallizing still salt solution and be cooled to 10～13 DEG C, be incubated and after 30 minutes, put into whizzer and get rid of material, obtain 10Kg MCP crude product, waste water enters geosyncline, send sewage plant processing;
D. a step is extracted to the water pump suction decolouring still separating, add 20kg gac and be warming up to 80～85 DEG C, be incubated press filtration after 30 minutes, filtrate is delivered to still kettle, use 120-125 degree, the waste heat tail gas intensification underpressure distillation of 2.5-3MPa, steams water and enters tank, steams 75% left and right of liquid, stop steaming, send into the cooling of freezing and crystallizing still, crystallization kettle is cooled to 6 DEG C, is incubated centrifuge dripping after 30 minutes and obtains 100Kg dimethylamine hydrochloride.
Claims (3)
1. a treatment process for high ammonia nitrogen mother liquor waste water in methyl cyclopentenyl ketone production, is characterized in that comprising the following steps:
A. high ammonia nitrogen mother liquor methyl cyclopentenyl ketone production station being produced is sent into after mother liquor tank metering, with mother liquor pump suction extraction kettle, add mother liquor volume 0.2-0.3 extraction agent doubly, stir 25-35 minute, leave standstill layering after 2.5-3.5 hour, separate water and organic phase;
B. organic phase is carried out to underpressure distillation by pump suction still kettle, pressure is that-0.092--0.096MPa temperature remains on 40～45 DEG C of recovery extraction agents, and the extraction agent distillating enters accumulator tank and recycles after condensation, the further extraction and application of residuum;
C. after the residuum of above-mentioned distillation being added the mother liquor of 100-200L to stir, send into freezing and crystallizing still salt solution and be cooled to 10～13 DEG C, be incubated and after 25-35 minute, put into whizzer and get rid of material, obtain MCP crude product, waste water enters geosyncline, send sewage plant processing.
2. the treatment process of high ammonia nitrogen mother liquor waste water in a kind of methyl cyclopentenyl ketone production according to claim 1, characterized by further comprising following steps:
By the water suction decolouring still described in a step in claim 1, add gac, be warming up to 80～85 DEG C, be incubated press filtration after 25-35 minute, filtrate is delivered to still kettle, underpressure distillation, steams water and enters tank, steams 75% of liquid, stop steaming, residuum is sent into the cooling of freezing and crystallizing still, and crystallization kettle is cooled to 5～7 DEG C, is incubated centrifuge dripping after 25-35 minute and obtains dimethylamine hydrochloride.
3. the treatment process of high ammonia nitrogen mother liquor waste water in a kind of methyl cyclopentenyl ketone production according to claim 2, is characterized in that the steam using in steam intensification underpressure distillation is the waste heat tail gas in producing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410501487.1A CN104193071A (en) | 2014-09-27 | 2014-09-27 | Treating method of high-ammonia-nitrogen mother liquor wastewater in MCP (methyl cyclopentenolone) production |
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| CN201410501487.1A CN104193071A (en) | 2014-09-27 | 2014-09-27 | Treating method of high-ammonia-nitrogen mother liquor wastewater in MCP (methyl cyclopentenolone) production |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106366003A (en) * | 2016-08-30 | 2017-02-01 | 安徽金禾实业股份有限公司 | Method for recycling dimethylamine in MCP hydrolysis mother liquor |
| CN106675081A (en) * | 2017-01-16 | 2017-05-17 | 铜陵清华科技有限公司 | Environment-friendly preparation method of solvent blue 104 dye |
| CN108083535A (en) * | 2017-12-21 | 2018-05-29 | 临泉县烜槿餐饮管理有限公司 | A kind of food and drink waste water processing and the method recycled |
| CN110127919A (en) * | 2019-04-01 | 2019-08-16 | 南京简迪环境工程有限公司 | A kind of agricultural chemicals waste water recycling treatment process |
| CN112174411A (en) * | 2020-08-03 | 2021-01-05 | 宜兴市阳洋塑料助剂有限公司 | Recovery and utilization of neutralization water in production process of plasticizer DOTP |
| CN114735872A (en) * | 2022-03-17 | 2022-07-12 | 佛山市南海北沙制药有限公司 | Method for recycling and reusing sulfanilamide quinoxaline process wastewater |
| CN115872847A (en) * | 2022-11-17 | 2023-03-31 | 安徽金禾实业股份有限公司 | Purification device and purification method for rinsing crude product of methyl cyclopentenolone |
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| CN101125839A (en) * | 2007-09-18 | 2008-02-20 | 安徽金禾实业股份有限公司 | Processing method for mother liquid in maltol production and device thereof |
| CN101555053A (en) * | 2008-04-11 | 2009-10-14 | 中国科学院广州地球化学研究所 | Compound coagulant used for treating rare-earth highly concentrated ammonian wastewater to recover industry ammonium chloride and treatment method |
| CN102910757A (en) * | 2012-09-27 | 2013-02-06 | 新泰昊原化工有限责任公司 | Treatment technique of waste water generated in production of o-nitrophenol |
| US20140114103A1 (en) * | 2012-10-18 | 2014-04-24 | Basf Se | Process for preparing cyclohexane comprising a prior removal of dimethylpentanes |
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| CN101125839A (en) * | 2007-09-18 | 2008-02-20 | 安徽金禾实业股份有限公司 | Processing method for mother liquid in maltol production and device thereof |
| CN101555053A (en) * | 2008-04-11 | 2009-10-14 | 中国科学院广州地球化学研究所 | Compound coagulant used for treating rare-earth highly concentrated ammonian wastewater to recover industry ammonium chloride and treatment method |
| CN102910757A (en) * | 2012-09-27 | 2013-02-06 | 新泰昊原化工有限责任公司 | Treatment technique of waste water generated in production of o-nitrophenol |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106366003A (en) * | 2016-08-30 | 2017-02-01 | 安徽金禾实业股份有限公司 | Method for recycling dimethylamine in MCP hydrolysis mother liquor |
| CN106675081A (en) * | 2017-01-16 | 2017-05-17 | 铜陵清华科技有限公司 | Environment-friendly preparation method of solvent blue 104 dye |
| CN106675081B (en) * | 2017-01-16 | 2019-04-02 | 安徽清科瑞洁新材料有限公司 | A kind of environment-friendly preparation method of 04 dyestuff of solvent blue 19 |
| CN108083535A (en) * | 2017-12-21 | 2018-05-29 | 临泉县烜槿餐饮管理有限公司 | A kind of food and drink waste water processing and the method recycled |
| CN110127919A (en) * | 2019-04-01 | 2019-08-16 | 南京简迪环境工程有限公司 | A kind of agricultural chemicals waste water recycling treatment process |
| CN112174411A (en) * | 2020-08-03 | 2021-01-05 | 宜兴市阳洋塑料助剂有限公司 | Recovery and utilization of neutralization water in production process of plasticizer DOTP |
| CN114735872A (en) * | 2022-03-17 | 2022-07-12 | 佛山市南海北沙制药有限公司 | Method for recycling and reusing sulfanilamide quinoxaline process wastewater |
| CN115872847A (en) * | 2022-11-17 | 2023-03-31 | 安徽金禾实业股份有限公司 | Purification device and purification method for rinsing crude product of methyl cyclopentenolone |
| CN115872847B (en) * | 2022-11-17 | 2024-03-29 | 安徽金禾实业股份有限公司 | Purification device and purification method for rinsing methyl cyclopentenolone crude product |
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Application publication date: 20141210 |