CN1931848B - Process of recovering epoxy chloropropane from effluent - Google Patents
Process of recovering epoxy chloropropane from effluent Download PDFInfo
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- CN1931848B CN1931848B CN200610096477A CN200610096477A CN1931848B CN 1931848 B CN1931848 B CN 1931848B CN 200610096477 A CN200610096477 A CN 200610096477A CN 200610096477 A CN200610096477 A CN 200610096477A CN 1931848 B CN1931848 B CN 1931848B
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Abstract
The process of recovering epoxy chloropropane from effluent features that effluent containing epoxy chloropropane is pumped with material pump from the storage tank through the heat exchanger to the rectifying tower for rectifying at the tower temperature controlled at 95-102 deg.c and tower top temperature controlled at 87-95 deg.c, and the azeotrope of epoxy chloropropane and water flowing out through the tower top is condensed in the condenser and delaminated in the phase separator, with the upper layer of liquid being reflowed into the tower and the lower layer of liquid being collected in the epoxy chloropropane storing tank. The said process has epoxy chloropropane recovering rate of 70-90 % and epoxy chloropropane content in the recovered product up to 95-98 %, lowers the epoxy chloropropane consumption in epoxy resin production and facilitates effluent treatment.
Description
One, technical field
The present invention relates to a kind of treatment process of waste water, especially be particularly related to the technology that reclaims epoxy chloropropane in a kind of waste water that from the Resins, epoxy production technique, contains epoxy chloropropane.
Two, background technology
In the Resins, epoxy production process, have the processing wastewater that contains epoxy chloropropane and produce, in the saturated at normal temperatures epoxy chloropropane waste water, its content is 6.58%.And concentration be the C0D of 6.58% epoxy chloropropane waste water up to 110,000, if directly send sewage works to handle, processing cost and difficulty are all very high.The method that reclaims epoxy chloropropane at present from this processing wastewater is to add water earlier in waste liquid, by rectification under vacuum, lower floor's overhead product by simple distillation, is gone out epoxy chloropropane 117 ℃ of rectifying separation, such recovery complex process, not easy to operate, equipment is huge, and product purity is not high.
Three, summary of the invention
Technical problem to be solved by this invention is: overcome the existing technical process complexity that reclaims, not easy to operate, equipment is huge, reclaim the not high shortcoming of epoxy chloropropane purity, a kind of new method that reclaims epoxy chloropropane from contain epoxy chloropropane waste water is provided, reclaim raw material epoxy chloropropane contained in the waste water effectively, reduce the cost and the difficulty of wastewater treatment.
Technical solution of the present invention is:
A kind of technology that from the waste water that contains epoxy chloropropane, reclaims epoxy chloropropane, the waste water that will contain epoxy chloropropane passes through discharging pump by basin, squeezes into rectifying tower through interchanger and carries out rectifying; Charging in the tower, temperature is controlled at 95～102 ℃ at the bottom of the still, and tower top temperature is controlled at 87～95 ℃; The azeotrope of epoxy chloropropane and water flows out from cat head, and through layering in phase splitter after the condenser condenses, supernatant liquid is by being back in the tower in the tower, and lower floor's liquid is collected in the epoxy chloropropane basin.
Epoxy chloropropane is slightly soluble in water, and at normal temperatures, its content in water reaches capacity when being about 6.58% (wt%).Epoxy chloropropane and water azeotropic, epoxy chloropropane content is 72% (wt%) in the azeotrope.The waste water that will contain epoxy chloropropane carries out rectifying, can collect the azeotrope of epoxy chloropropane and water, because of epoxy chloropropane content in the azeotrope is higher than its solubleness far away, most epoxy chloropropane and water stratification after the condensation, thereby can reclaim the epoxy chloropropane in the waste water effectively, and obtain the epoxy chloropropane that can reclaim again usefulness of high density.
Among the present invention, the mass percent concentration of epoxy chloropropane is 1.5% to its saturation concentration in water in the described waste water.
According to the present invention to containing the waste water reclamation epoxy chloropropane of epoxy chloropropane, the rate of recovery of epoxy chloropropane reaches 70～90%, the content that reclaims the product epoxy chloropropane can reach 95～98%, reduce the consumption of raw material epoxy chloropropane in the Resins, epoxy production process, reduced the cost and the difficulty of wastewater treatment.
Four, description of drawings
Fig. 1 is a process flow diagram of the present invention.
Among the figure: (1) epoxy chloropropane waste water basin, (2) discharging pump, (3) interchanger, (4) rectifying tower, (5) condenser, (6) phase splitter, (7) epoxy chloropropane basin
The partial enlarged drawing of Fig. 2 interchanger (3).
Tube side is walked for the water outlet of tower still in the left side among the figure, and shell side is walked for water inlet in the right side
Five, embodiment
Below in conjunction with specific embodiment the present invention is illustrated.
Below among each embodiment, used rectifying tower can be used various customary filler, theoretical plate number embodiment 3,5,7 is 5, embodiment 9,11 is 6, embodiment 2,4,6,8 is 8, embodiment 10,12 is 10.Epoxy chloropropane yield (mass percent) is meant the kilogram number of per hundred kilograms of epoxy chloropropane waste water reclamation epoxy chloropropane (100%); The epoxy chloropropane rate of recovery is meant epoxy chloropropane yield/epoxy chloropropane waste strength * 100%.
Embodiment 1:
The saturated epoxy chloropropane waste water that content is about 6.58% (wt%) passes through discharging pump 2 from epoxy chloropropane waste water basin 1, squeezes into rectifying tower 4 rectifying through interchanger 3, charging in the tower, and flow is 100kg/h; Temperature is controlled at 95～99 ℃ at the bottom of the still, and tower top temperature is controlled at 87～90 ℃; The tower bottom flow amount is 94kg/h, azeotrope passes through condenser 5 condensations with the flow of 8.3kg/h from the cat head discharging, be collected in the phase splitter 6 and leave standstill, upper strata liquid is back to from tower in the tower after the layering, and flow is 2.3kg/h, lower floor's liquid flow rate is 6kg/h, be collected in the epoxy chloropropane basin 7, per hundred kilograms of recyclable epoxy chloropropane of epoxy chloropropane waste water are 5.2 kilograms, and promptly the epoxy chloropropane yield is 5.6% (mass percent), reclaim the content 96.8% of epoxy chloropropane, the rate of recovery is 85.1%.Theoretical number of plates of rectifying tower can be 5～10.
Embodiment 2:
Content is about 6.58% saturated epoxy chloropropane waste water by discharging pump 2, squeezes into rectifying tower 4 rectifying, charging in the tower through interchanger 3; Temperature is controlled at 100～102 ℃ at the bottom of the still, and tower top temperature is controlled at 91～95 ℃; Azeotrope passes through condenser 5 from the cat head discharging, be collected in the phase splitter 6 and leave standstill, after the layering reflux in the upper strata, feed supplement in the tower, lower floor's liquid is collected in the epoxy chloropropane basin 7, the epoxy chloropropane yield is 5.9% (mass percent), reclaims the content 97.2% of epoxy chloropropane, and the rate of recovery is 89.7%.
Embodiment 3:
5.5% epoxy chloropropane waste water is squeezed into rectifying tower 4 rectifying, charging in the tower by discharging pump 2 through interchanger 3; Temperature is controlled at 95～99 ℃ at the bottom of the still, and tower top temperature is controlled at 87～90 ℃; Azeotrope, is collected in the phase splitter 6 and leaves standstill by condenser 5 from the cat head discharging, and after the layering reflux in the upper strata, feed supplement in the tower, and lower floor's liquid is collected in the epoxy chloropropane basin 7, and the epoxy chloropropane yield is 4.7% (mass percent).
Embodiment 4:
5.5% epoxy chloropropane waste water is squeezed into rectifying tower 4 rectifying, charging in the tower by discharging pump 2 through interchanger 3; Temperature is controlled at 100～102 ℃ at the bottom of the still, and tower top temperature is controlled at 91～95 ℃; Azeotrope passes through condenser 5 from the cat head discharging, be collected in the phase splitter 6 and leave standstill, after the layering reflux in the upper strata, feed supplement in the tower, lower floor's liquid is collected in the epoxy chloropropane basin 7, the epoxy chloropropane yield is 5.0% (mass percent), reclaims the content 97.8% of epoxy chloropropane, and the rate of recovery is 91%.
Embodiment 5:
4.5% epoxy chloropropane waste water is squeezed into rectifying tower 4 rectifying, charging in the tower by discharging pump 2 through interchanger 3; Temperature is controlled at 95～99 ℃ at the bottom of the still, and tower top temperature is controlled at 87～90 ℃; Azeotrope, is collected in the phase splitter 6 and leaves standstill by condenser 5 from the cat head discharging, and after the layering reflux in the upper strata, feed supplement in the tower, and lower floor's liquid is collected in the epoxy chloropropane basin 7, and the epoxy chloropropane yield is 3.8% (mass percent), and the rate of recovery is 84.4%.
Embodiment 6:
4.5% epoxy chloropropane waste water is squeezed into rectifying tower 4 rectifying, charging in the tower by discharging pump 2 through interchanger 3; Temperature is controlled at 100～102 ℃ at the bottom of the still, and tower top temperature is controlled at 91～95 ℃; Azeotrope, is collected in the phase splitter 6 and leaves standstill by condenser 5 from the cat head discharging, and after the layering reflux in the upper strata, feed supplement in the tower, lower floor's liquid is collected in the epoxy chloropropane basin 7, and the epoxy chloropropane yield is 4.0% (mass percent), reclaims the content 97.1%. of epoxy chloropropane
Embodiment 7:
3.5% epoxy chloropropane waste water is squeezed into rectifying tower 4 rectifying, charging in the tower by discharging pump 2 through interchanger 3; Temperature is controlled at 95～99 ℃ at the bottom of the still, and tower top temperature is controlled at 87～90 ℃; Azeotrope, is collected in the phase splitter 6 and leaves standstill by condenser 5 from the cat head discharging, and after the layering reflux in the upper strata, feed supplement in the tower, lower floor's liquid is collected in the epoxy chloropropane basin 7, and the epoxy chloropropane yield is 2.8% (mass percent), reclaims the content 98.1% of epoxy chloropropane.
Embodiment 8:
3.5% epoxy chloropropane waste water is squeezed into rectifying tower 4 rectifying, charging in the tower by discharging pump 2 through interchanger 3; Temperature is controlled at 100～102 ℃ at the bottom of the still, and tower top temperature is controlled at 91～95 ℃; Azeotrope, is collected in the phase splitter 6 and leaves standstill by condenser 5 from the cat head discharging, and after the layering reflux in the upper strata, feed supplement in the tower, and lower floor's liquid is collected in the epoxy chloropropane basin 7, and the epoxy chloropropane yield is 3.0% (mass percent).
Embodiment 9:
2.5% epoxy chloropropane waste water is squeezed into rectifying tower 4 rectifying, charging in the tower by discharging pump 2 through interchanger 3; Temperature is controlled at 95～99 ℃ at the bottom of the still, and tower top temperature is controlled at 87～90 ℃; Azeotrope, is collected in the phase splitter 6 and leaves standstill by condenser 5 from the cat head discharging, and after the layering reflux in the upper strata, feed supplement in the tower, and lower floor's liquid is collected in the epoxy chloropropane basin 7, and the epoxy chloropropane yield is 1.9% (mass percent).
Embodiment 10:
2.5% epoxy chloropropane waste water is squeezed into rectifying tower 4 rectifying, charging in the tower by discharging pump 2 through interchanger 3; Temperature is controlled at 100～102 ℃ at the bottom of the still, and tower top temperature is controlled at 91～95 ℃; Azeotrope, is collected in the phase splitter 6 and leaves standstill by condenser 5 from the cat head discharging, and after the layering reflux in the upper strata, feed supplement in the tower, and lower floor's liquid is collected in the epoxy chloropropane basin 7, and the epoxy chloropropane yield is 2.1% (mass percent).
Embodiment 11:
1.5% epoxy chloropropane waste water is squeezed into rectifying tower 4 rectifying, charging in the tower by discharging pump 2 through interchanger 3; Temperature is controlled at 95～99 ℃ at the bottom of the still, and tower top temperature is controlled at 87～90 ℃; Azeotrope, is collected in the phase splitter 6 and leaves standstill by condenser 5 from the cat head discharging, and after the layering reflux in the upper strata, feed supplement in the tower, and lower floor's liquid is collected in the epoxy chloropropane basin 7, and the epoxy chloropropane yield is 1.1% (mass percent).
Embodiment 12:
1.5% epoxy chloropropane waste water is squeezed into rectifying tower 4 rectifying, charging in the tower by discharging pump 2 through interchanger 3; Temperature is controlled at 100～102 ℃ at the bottom of the still, and tower top temperature is controlled at 91～95 ℃; Azeotrope, is collected in the phase splitter 6 and leaves standstill by condenser 5 from the cat head discharging, and after the layering reflux in the upper strata, feed supplement in the tower, and lower floor's liquid is collected in the epoxy chloropropane basin 7, and the epoxy chloropropane yield is 1.2% (mass percent).
Claims (4)
1. a technology that reclaims epoxy chloropropane from the waste water that contains epoxy chloropropane is characterized in that the waste water that will contain epoxy chloropropane passes through discharging pump (2) by basin (1), squeezes into rectifying tower (4) through interchanger (3) and carries out rectifying; Charging in the tower, temperature is controlled at 95～102 ℃ at the bottom of the still, and tower top temperature is controlled at 87～95 ℃; The azeotrope of epoxy chloropropane and water flows out from cat head, and through layering in phase splitter (6) after condenser (5) condensation, supernatant liquid is by being back in the tower in the tower, and lower floor's liquid is collected in the epoxy chloropropane basin (7).
2. the technology that reclaims epoxy chloropropane from the waste water that contains epoxy chloropropane according to claim 1, the mass percent concentration that it is characterized in that epoxy chloropropane in the waste water are 1.5% to its saturation concentration in water.
3. the technology that reclaims epoxy chloropropane from the waste water that contains epoxy chloropropane according to claim 1, the theoretical plate number that it is characterized in that rectifying tower (4) is 5～10.
4. the technology that reclaims epoxy chloropropane from the waste water that contains epoxy chloropropane according to claim 1 is characterized in that the content of lower floor's epoxy chloropropane of collecting is 95%～98%.
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| CN200610096477A CN1931848B (en) | 2006-09-28 | 2006-09-28 | Process of recovering epoxy chloropropane from effluent |
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| CN200610096477A CN1931848B (en) | 2006-09-28 | 2006-09-28 | Process of recovering epoxy chloropropane from effluent |
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| CN1931848B true CN1931848B (en) | 2010-05-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8729282B2 (en) | 2008-08-01 | 2014-05-20 | Momentive Specialty Chemicals Inc. | Process for the manufacture of a 1,2-epoxide |
| US8802873B2 (en) | 2008-08-01 | 2014-08-12 | Momentive Specialty Chemicals Inc. | Process for the manufacture of epichlorohydrin |
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| RU2593205C1 (en) * | 2015-06-10 | 2016-08-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Чувашский государственный университет имени И.Н. Ульянова" | Method for extracting concentrated epichlorohydrin from products of allyl chloride epoxidation with hydrogen peroxide on titanium-containing zeolite catalyst |
| CN109134405B (en) * | 2018-07-27 | 2022-05-17 | 深圳市瑞升华科技股份有限公司 | Waste heat recovery equipment and process utilizing MVR technology |
| CN113817137B (en) * | 2020-06-18 | 2023-10-10 | 南通星辰合成材料有限公司 | Recycling method of epichlorohydrin wastewater and preparation method of epoxy resin |
| CN114539187A (en) * | 2020-11-25 | 2022-05-27 | 伊斯拓通用设备江苏有限公司 | Method for treating biochemical wastewater in production of electronic-grade epoxy resin |
| CN113264905A (en) * | 2021-06-07 | 2021-08-17 | 张家港衡业特种树脂有限公司 | Method for removing biochemical toxicity of rectification wastewater in epoxy resin manufacturing |
| CN117551060B (en) * | 2024-01-11 | 2024-04-09 | 万华化学集团股份有限公司 | Method for purifying epichlorohydrin containing ether impurities |
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| CN1047668A (en) * | 1989-06-02 | 1990-12-12 | 岳阳石油化工总厂研究院 | A kind of method that reclaims epoxy chloropropane and toluene |
| US5169964A (en) * | 1988-04-06 | 1992-12-08 | Deutsche Solvay-Werke Gmbh | Process for preparing high purity epichlorohydrin |
| CN1096498A (en) * | 1992-09-06 | 1994-12-21 | 德国索尔瓦有限公司 | From wastewater treatment method and equipment the Epicholorohydrin biology, that contain organism, especially organochlorine compound |
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2006
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Patent Citations (4)
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| US5169964A (en) * | 1988-04-06 | 1992-12-08 | Deutsche Solvay-Werke Gmbh | Process for preparing high purity epichlorohydrin |
| CN1047668A (en) * | 1989-06-02 | 1990-12-12 | 岳阳石油化工总厂研究院 | A kind of method that reclaims epoxy chloropropane and toluene |
| CN1096498A (en) * | 1992-09-06 | 1994-12-21 | 德国索尔瓦有限公司 | From wastewater treatment method and equipment the Epicholorohydrin biology, that contain organism, especially organochlorine compound |
| US5393428A (en) * | 1992-09-06 | 1995-02-28 | Solvay Deutschland Gmbh | Process for treating waste water containing chlorinated organic compounds from production of epichlorohydrin |
Non-Patent Citations (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8729282B2 (en) | 2008-08-01 | 2014-05-20 | Momentive Specialty Chemicals Inc. | Process for the manufacture of a 1,2-epoxide |
| US8802873B2 (en) | 2008-08-01 | 2014-08-12 | Momentive Specialty Chemicals Inc. | Process for the manufacture of epichlorohydrin |
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| CN1931848A (en) | 2007-03-21 |
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Owner name: XINGCHEN SYNTHETIC MATRIALS CO., LTD., NANTONG Free format text: FORMER OWNER: WUXI RESIN FACTORY OF BLUE STAR NEW CHEMICAL MATERIAL CO., LTD. Effective date: 20141126 |
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Effective date of registration: 20141126 Address after: 226017 Nantong economic and Technological Development Zone, Jiangsu, Hong Kong Road, No. 118 Patentee after: Xingchen Synthetic Matrials Co., Ltd., Nantong Address before: 214011 No. 18 Zhuang Road, Wuxi New District, Jiangsu, Wuxi Patentee before: Wuxi Resin Factory of Blue Star New Chemical Material Co., Ltd. |