CN106064864B - Process method for recovering propylene glycol from propylene oxide wastewater - Google Patents
Process method for recovering propylene glycol from propylene oxide wastewater Download PDFInfo
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- CN106064864B CN106064864B CN201610605951.0A CN201610605951A CN106064864B CN 106064864 B CN106064864 B CN 106064864B CN 201610605951 A CN201610605951 A CN 201610605951A CN 106064864 B CN106064864 B CN 106064864B
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- 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
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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Abstract
The invention provides a method for recovering propylene glycol from propylene oxide wastewater, which comprises the steps of firstly adjusting the pH value of the wastewater to 5-8, and then carrying out atmospheric distillation to obtain a fraction and a still residue; after the residual liquid in the kettle is subjected to suction filtration and salt removal, filtrate and salt are obtained; and carrying out reduced pressure distillation on the filtrate, and collecting a fraction with the gas phase temperature of 100-120 ℃, namely the propylene glycol. The treatment method can remove toxic pollutants in the wastewater and recover the propylene glycol, and the COD removal rate of the recovered fraction after biochemical treatment is more than 70 percent, thereby ensuring that the wastewater can be stably discharged up to the standard.
Description
Technical Field
The invention relates to the field of chemical production wastewater treatment, in particular to a process method for recovering propylene glycol from propylene oxide wastewater.
Background
Propylene oxide is an important basic organic chemical synthesis raw material and is mainly used for producing polyether, propylene glycol and the like. It is also the main raw material for producing non-ionic surfactant, demulsifier for oil field, emulsifier for agricultural chemicals, etc. The derivative of the epoxypropane is widely applied to industries such as automobiles, buildings, foods, tobaccos, medicines, cosmetics and the like. The produced downstream products are hundreds of types and are important raw materials of fine chemical products.
In the production process of propylene oxide, a large amount of organic wastewater is generated, and the organic matters in the wastewater are mainly propylene glycol as a propylene oxide byproduct. The conventional propylene oxide wastewater treatment method mostly destroys organic matters in the wastewater, discharges the wastewater after the wastewater reaches the standard, has high treatment cost and wastes resources.
Therefore, a new method for treating propylene oxide wastewater is needed, so that propylene glycol can be recovered from the wastewater, the treated wastewater has biodegradability, and the wastewater can reach the discharge standard stably through conventional biochemical treatment.
Disclosure of Invention
The invention aims to provide a process method for recovering propylene glycol from propylene oxide wastewater, which aims to remove organic pollutants in the wastewater and recover the propylene glycol so as to ensure that the wastewater stably reaches the standard and is discharged.
In order to achieve the above object, the present invention firstly provides a process for recovering propylene glycol from propylene oxide wastewater, the process comprising: s10, adjusting the pH value of the wastewater to 5-8, and then carrying out atmospheric distillation to obtain a fraction and a still residue; s20, performing suction filtration on the kettle residual liquid obtained in the step S10 to remove salt, and obtaining filtrate and salt; and S30, carrying out reduced pressure distillation on the filtrate obtained in the step S20, and collecting fractions with the gas phase temperature of 100-120 ℃, namely the propylene glycol.
In an embodiment of the present invention, the mass ratio of water to propylene oxide in the still residue obtained in the step S10 is controlled to be 8 to 20.
In one embodiment of the present invention, in the step S30, the reduced pressure distillation is performed on the filtrate under a pressure of-0.095 mpa and an external heating temperature of 200 ℃.
In an embodiment of the present invention, step S21 is further included after step S20. the salt obtained in step S20 is subjected to high temperature calcination.
In a preferred embodiment of the present invention, there is provided a process for recovering propylene glycol from propylene oxide wastewater, the process comprising: s10, adjusting the pH value of the wastewater to 5-8, and then carrying out atmospheric distillation to obtain a fraction and kettle residual liquid, wherein the mass ratio of water to epoxypropane in the kettle residual liquid is controlled to be 8-20; s20, performing suction filtration on the kettle residual liquid obtained in the step S10 to remove salt, and obtaining filtrate and salt; s21, calcining the salt obtained in the step S20 at a high temperature to obtain industrial dry salt; and S30, carrying out reduced pressure distillation on the filtrate obtained in the step S20, and collecting fractions with the gas phase temperature of 100-120 ℃, namely the propylene glycol.
In an embodiment of the present invention, the fraction obtained in step S10 and the fraction at the gas phase temperature of 20 to 100 ℃ in step S30 are collected, diluted by 5 to 10 times, and then subjected to subsequent biochemical treatment.
The treatment method can remove organic pollutants in the wastewater and recover the propylene glycol, and the COD removal rate of the recovered fraction after biochemical treatment is more than 70 percent, thereby ensuring that the wastewater can be stably discharged after reaching the standard.
Therefore, the process method for recovering the propylene glycol from the propylene oxide wastewater provided by the invention has the advantages of simple steps, mild reaction conditions and the like, and has obvious environmental, economic and social benefits.
Detailed Description
Hereinafter, the technique of the present invention will be described in detail with reference to specific embodiments. It should be understood that the following detailed description is only for the purpose of assisting those skilled in the art in understanding the present invention, and is not intended to limit the present invention.
Example 1
In this example, a process for recovering propylene glycol from propylene oxide wastewater is provided. The treated object is taken from wastewater of a certain propylene oxide production company in Jiangxi province, and the water quality of raw water is as follows: COD 300000mg/L, salt content of 16%, pH value of 14 and propylene glycol content of 5%. The treatment process is specifically as follows.
And S10, taking 800ml of the wastewater, adding 74ml of hydrochloric acid to adjust the pH value of the wastewater to 7, distilling under normal pressure, receiving 400ml of fraction and kettle residual liquid, and detecting that the COD value of the fraction is 8489 mg/L.
And S20, carrying out suction filtration on the kettle residual liquid obtained in the step S10 to remove salt, and obtaining filtrate and 114g of salt.
And S30, carrying out reduced pressure distillation on the filtrate obtained in the step S20 under the conditions that the pressure is-0.095 mpa and the external heating temperature is 200 ℃ to obtain 325ml of fraction (the COD value is 15346mg/L) with the gas phase temperature of 20-100 ℃ and 38ml of fraction with the gas phase temperature of 100-120 ℃. Through detection, the content of the 1, 2-propylene glycol in the fraction with the gas phase temperature of 100-120 ℃ is 95.3 percent, and the recovery rate is 90.5 percent.
And diluting the fraction obtained in the step S10 and the fraction with the gas phase temperature of 20-100 ℃ in the step S30 by 5-10 times, and then performing subsequent biochemical treatment. 98.4g of salt is obtained after the salt obtained in the step S20 is calcined, and the first-grade industrial dry salt product meets the national standard GB/T5462-2015.
Example 2
In this example, a process for recovering propylene glycol from propylene oxide wastewater is provided. The water quality to be treated was the same as in example 1. The treatment process is specifically as follows.
And S10, taking 800ml of the wastewater, adding 34ml of hydrochloric acid to adjust the pH value of the wastewater to 12, distilling under normal pressure, receiving 400ml of fraction and kettle residual liquid, and detecting that the COD value of the fraction is 8489 mg/L.
S20, carrying out suction filtration on the kettle residual liquid obtained in the step S10 to remove salt, and obtaining filtrate and 74g of salt;
and S30, carrying out reduced pressure distillation on the filtrate obtained in the step S20 under the conditions that the pressure is-0.095 mpa and the external heating temperature is 200 ℃ to obtain 350ml of fraction (COD value is 32346mg/L) with the gas phase temperature of 20-100 ℃ and 30ml of fraction with the gas phase temperature of 100-120 ℃. Through detection, the content of the 1, 2-propylene glycol in the fraction with the gas phase temperature of 100-120 ℃ is 89.7%.
And diluting the fraction obtained in the step S10 and the fraction with the gas phase temperature of 20-100 ℃ in the step S30 by 5-10 times, and then performing subsequent biochemical treatment. The salt obtained in the step S20 is calcined to obtain 56.2g of salt, which meets the national standard GB/T5462-2015 industrial dry salt first-grade product.
Example 3
In this example, a process for recovering propylene glycol from propylene oxide wastewater is provided. The water quality to be treated was the same as in example 1. The treatment process is specifically as follows.
And S10, taking 800ml of the wastewater, adding 75ml of hydrochloric acid to adjust the pH value of the wastewater to 7, distilling under normal pressure, receiving 500ml of fraction and kettle residual liquid, and detecting that the COD value of the fraction is 10559 mg/L.
S20, absorbing and filtering the still residual liquid obtained in the step S10 to remove salt, and obtaining filtrate and 110g of salt;
and S30, carrying out reduced pressure distillation on the filtrate obtained in the step S20 under the conditions that the pressure is-0.095 mpa and the external heating temperature is 200 ℃ to obtain 325ml of fraction (the COD value is 15346mg/L) with the gas phase temperature of 20-100 ℃ and 35ml of fraction with the gas phase temperature of 100-120 ℃. Through detection, the content of the 1, 2-propylene glycol in the fraction with the gas phase temperature of 100-120 ℃ is 90.3%.
And diluting the fraction obtained in the step S10 and the fraction with the gas phase temperature of 20-100 ℃ in the step S30 by 5-10 times, and then performing subsequent biochemical treatment. And (4) calcining the salt obtained in the step S20 to obtain 95.8g of salt, wherein the salt meets the national standard GB/T5462-2015 industrial dry salt first-grade product.
The treatment method can remove toxic pollutants in the wastewater and recover the propylene glycol, and the COD removal rate of the recovered fraction after biochemical treatment is more than 70 percent, thereby ensuring that the wastewater can be stably discharged up to the standard.
The present invention has been described in relation to the above embodiments, which are only exemplary of the implementation of the present invention. It must be noted that the disclosed embodiments do not limit the scope of the invention. Rather, modifications and equivalent arrangements included within the spirit and scope of the claims are included within the scope of the invention.
Claims (5)
1. A method for recovering propylene glycol from propylene oxide wastewater, which is characterized by comprising the following steps:
s10, adjusting the pH value of the wastewater to 5-8, and then carrying out atmospheric distillation to obtain a fraction and a still residue;
s20, performing suction filtration on the kettle residual liquid obtained in the step S10 to remove salt, and obtaining filtrate and salt;
and S30, carrying out reduced pressure distillation on the filtrate obtained in the step S20, and collecting fractions with the gas phase temperature of 100-120 ℃, namely the propylene glycol.
2. The method of claim 1, wherein the mass ratio of water to propylene oxide in the still residue obtained in the step S10 is controlled to be in the range of 8 to 20.
3. The method of claim 1, wherein in the step S30, the reduced pressure distillation of the filtrate is performed under a pressure of-0.095 mpa and an external heating temperature of 200 ℃.
4. The method of claim 1, further comprising a step S21 after the step S20. the salt obtained in the step S20 is subjected to high temperature calcination.
5. The method according to claim 1, wherein the fraction obtained in the step S10 and the fraction having the gas phase temperature of 20 ℃ to 100 ℃ in the step S30 are collected, diluted 5 to 10 times, and then subjected to the subsequent biochemical treatment.
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| CN201610605951.0A CN106064864B (en) | 2016-07-28 | 2016-07-28 | Process method for recovering propylene glycol from propylene oxide wastewater |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108298618A (en) * | 2018-02-28 | 2018-07-20 | 中国天辰工程有限公司 | A kind of method and separator of epoxy propane waste water pretreatment and separation |
| CN110104862A (en) * | 2019-05-21 | 2019-08-09 | 中国天辰工程有限公司 | The salt-containing organic wastewater generated in a kind of HPPO production is saltoutd method for concentration |
| KR102481854B1 (en) | 2019-12-19 | 2022-12-27 | 완후아 케미컬 그룹 코., 엘티디 | Treatment method of production wastewater according to the production of propylene oxide through the co-oxidation method |
| CN113003847B (en) * | 2019-12-19 | 2023-03-03 | 万华化学集团股份有限公司 | Treatment method for wastewater generated in production of preparing epoxypropane by co-oxidation method |
| CN111559819B (en) * | 2020-04-30 | 2022-07-12 | 常州瑞华化工工程技术股份有限公司 | Method for recovering propylene glycol and other organic matters from propylene epoxidation alkaline washing wastewater |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103788026A (en) * | 2012-10-29 | 2014-05-14 | 中国石油化工股份有限公司 | Method of purifying propylene epoxide |
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| JP2013082680A (en) * | 2012-07-26 | 2013-05-09 | Sumitomo Chemical Co Ltd | Method for recovering propylene glycol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103788026A (en) * | 2012-10-29 | 2014-05-14 | 中国石油化工股份有限公司 | Method of purifying propylene epoxide |
Non-Patent Citations (1)
| Title |
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| 环氧丙烷水合制丙二醇的新工艺;成力军;《精细化工中间体》;20010630;第31卷(第3期);1部分第1段、3部分第1-2段 * |
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