CN109987770B - Triethyl phosphite wastewater treatment process - Google Patents
Triethyl phosphite wastewater treatment process Download PDFInfo
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- CN109987770B CN109987770B CN201910383966.0A CN201910383966A CN109987770B CN 109987770 B CN109987770 B CN 109987770B CN 201910383966 A CN201910383966 A CN 201910383966A CN 109987770 B CN109987770 B CN 109987770B
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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
- 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
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5281—Installations for water purification using chemical agents
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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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
- C02F2001/007—Processes including a sedimentation step
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/14—NH3-N
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Abstract
The invention relates to a triethyl phosphite wastewater treatment process, and belongs to the technical field of chemical synthesis. The invention takes lime milk and polymeric ferric sulfate as precipitant, oxidizes phosphorous acid into orthophosphoric acid under the action of ozone oxidation, and precipitates phosphorus ions in wastewater by adjusting PH value. The invention utilizes a high-temperature heating method to volatilize organic matters (benzene and triethylamine) and ammonia ions in the wastewater to reduce ammonia nitrogen and COD in the wastewater, and then most phosphorus ions are settled by lime cream to reduce the dosage of a secondary settlement medicament, thereby reducing the wastewater treatment cost. The dosage of the traditional Chinese medicine is small, and the precipitate generated by the first-level sedimentation has certain economic benefit. The wastewater treatment process is green and environment-friendly, reduces the production cost, and is suitable for industrial expanded production.
Description
Technical Field
The invention relates to a triethyl phosphite wastewater treatment process, and belongs to the technical field of chemical synthesis.
Background
Triethyl phosphite is an important intermediate for producing medicaments such as phosphoryl triethyl acetate, AE-active ester and the like. The pesticide is used for preparing the pesticides such as glufosinate, fenobucarb and the like, is widely applied to agriculture and forestry in China, and has good pesticide effect and great demand. The dye industry is used for manufacturing styrene biphenyl fluorescent whitening agents, and is also used for manufacturing plasticizers and stabilizers in the plastic industry, and additives of lubricating oil and lubricating grease, and the development and application prospects are good. The main technological route of triethyl phosphite is that phosphorus trichloride and ethanol are used as main raw materials, benzene is used as solvent, triethyl phosphite is generated through synthetic reaction, hydrogen chloride gas is generated in the process, triethylamine is used as acid-binding agent, sodium hydroxide is added to resolve triethylamine out, and sodium chloride salt is generated at the same time. The waste water contains a large amount of by-product sodium chloride and a small amount of oily solvent benzene and triethylamine. The waste water has the characteristics of high salt content and high chemical oxygen consumption, so that the waste water is extremely difficult to treat by a common sewage treatment method. Because the treatment cost is very high, the production cost is greatly increased, enterprises are generally difficult to bear, and most triethyl phosphite production enterprises directly discharge the wastewater, thereby causing great environmental pollution and resource waste. Therefore, the wastewater treatment in the production process of triethyl phosphite is a major bottleneck for the survival and development of enterprises.
A triethyl phosphite wastewater treatment process is that at present, phosphorous acid is oxidized into orthophosphoric acid by direct oxidation and then phosphorus is removed, the phosphorous acid is oxidized into the orthophosphoric acid under the action of oxidant ozone, then limestone is added and stirred and then directly discharged, or the limestone is directly added into wastewater and stirred and then discharged. The difference between the two methods is whether to oxidize or not, and the phosphorus content of the total phosphorus in the external drainage in the two schemes is more than 100mg/L and more than 2000 COD (chemical oxygen demand) 2000mg/L, which can not reach the national discharge standard completely.
Disclosure of Invention
The invention aims to provide the method which has the advantages of less equipment investment, low production cost, good wastewater treatment effect and green and environment-friendly preparation process; can effectively avoid the treatment process of triethyl phosphite wastewater with overhigh total phosphorus, ammonia nitrogen and COD in the discharged wastewater.
The technical scheme of the invention is
The triethyl phosphite wastewater treatment process is characterized by comprising the following steps
1) Placing triethyl phosphite wastewater in a stirring kettle, installing a condenser communicated with the stirring kettle above the stirring kettle, wherein the condenser is used for refluxing water vapor generated by heating, starting stirring, the stirring speed is 150-200 revolutions per minute, the temperature is slowly increased to 70-80 ℃, and the stirring and heating time is 2-2.5 hours;
2) after the triethyl phosphite wastewater in the stirring kettle is stirred and heated, the material is put into an oxidation tower for cooling, and when the temperature is reduced to room temperature, ozone is introduced and stirred to aerate the material; the ozone is introduced for 7 to 8 hours; after aeration is finished, measuring the PH value to be about 6-7;
3) after aeration is finished, transferring the materials into a primary sedimentation tank, adding lime milk, stirring for half an hour, and settling and overflowing; the feeding amount of the lime milk is 1 percent of the weight of the triethyl phosphite wastewater, and the settling time is 7-9 hours;
4) after the sedimentation is finished, the overflow water enters a dephosphorization pool (a secondary sedimentation pool), hydrochloric acid is added to adjust the pH value to be less than 7, and then polymeric ferric sulfate is added to be stirred for half an hour, wherein the adding amount of the polymeric ferric sulfate is one thousandth of the weight of the triethyl phosphite wastewater; then adding lime milk to adjust the pH value to be more than 11.5, slowly and slowly stirring for settling for 7-9 hours, wherein the total phosphorus content of the wastewater is less than 5PPM, the COD (chemical oxygen demand) is less than 500PPM, and the ammonia nitrogen content is less than 50 PPM; and then the wastewater can be discharged outside.
Compared with the prior art, the invention has the beneficial effects of
In the triethyl diphosphite wastewater treatment process, phosphorous acid is oxidized into orthophosphoric acid by ozone, and the orthophosphoric acid and polymeric ferric sulfate are settled after limestone is primarily settled, so that the total phosphorus content finally meets the process requirements. The process flow is simple and easy to operate, the solid precipitate generated in the primary sedimentation process is calcium hydroxy phosphate, the phosphate fertilizer has economic benefit, and the problem of solid waste generated in the sewage treatment process is well solved. Secondly, the ozone oxidation does not bring other pollution sources, and the phosphorous acid which is not easy to generate precipitation is converted into the precipitable orthophosphoric acid. Limestone is added for the first precipitation, so that the consumption of polymeric ferric sulfate is reduced, and the treatment cost is reduced. In the first step, ammonia in the wastewater is volatilized by high-temperature stirring, so that the content of ammonia nitrogen is effectively reduced. The triethyl phosphite wastewater treatment process can complete the whole production process by only one set of stirring kettle, one set of oxidation tower and two settling ponds, saves production equipment and reduces production cost.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention, but may be embodied in any form described in the summary of the invention.
Example 1
Putting triethyl phosphite wastewater into a stirring kettle, and starting stirring at a stirring speed of more than 200 revolutions per minute. Slowly raising the temperature to 80 ℃, and keeping the temperature for two hours to fully separate out organic matters and ammonia gas in the wastewater. After the triethyl phosphite wastewater in the stirring kettle is stirred and heated for 2 hours, the material is put into an oxidation tower for cooling, and when the temperature is reduced to room temperature, the ozone is continuously introduced for stirring; the ozone is led in for 8 hours, and three-stage oxidation can be carried out in the process. After the oxidation is finished, the phosphorous acid in the wastewater is completely oxidized into orthophosphoric acid. The pH was measured at about 6-7. Then transferring the materials into a primary sedimentation tank, adding lime milk and PAM, stirring for half an hour, and settling and overflowing. The feeding amount of the lime milk is 1 percent of the weight of the triethyl phosphite wastewater, the feeding amount of the PAM is two millionths, and the settling time is 8 hours. The triethyl phosphite wastewater is firstly heated at high temperature to reduce the content of ammonia nitrogen and COD, then is oxidized by ozone without introducing other pollution sources, and then is pre-settled by limestone to reduce the subsequent dosage.
And after the sedimentation is finished, the overflow water enters a dephosphorization pool (a secondary sedimentation pool), hydrochloric acid is added to adjust the pH value to be less than 7, then polymeric ferric sulfate is added to stir for half an hour, then lime cream is added to adjust the pH value to be more than 11.5, the slow stirring is carried out to settle and overflow, and the sedimentation time is 8 hours. The feeding amount of the polymeric ferric sulfate is one thousandth of the weight of the triethyl phosphite wastewater. Regulating the pH value to be more than 11.5, slowly and slowly stirring for settling for 8 hours, wherein the total phosphorus content of the wastewater is less than 5PPM, the COD is less than 500PPM, and the ammonia nitrogen is less than 50 PPM; and then the wastewater can be discharged outside.
Example 2
Putting triethyl phosphite wastewater into a stirring kettle, and starting stirring at the stirring speed of 180 revolutions per minute. Slowly raising the temperature to 70 ℃, and keeping the temperature for two hours to fully separate out organic matters and ammonia gas in the wastewater. After the triethyl phosphite wastewater in the stirring kettle is stirred and heated for 2.5 hours, the material is put into an oxidation tower for cooling, and when the temperature is reduced to room temperature, the ozone is continuously introduced for stirring; the ozone is led in for 9 hours, and three-stage oxidation can be carried out in the process. After the oxidation is finished, the phosphorous acid in the wastewater is completely oxidized into orthophosphoric acid. The pH was measured at about 6-7. Then transferring the materials into a primary sedimentation tank, adding lime milk and PAM, stirring for half an hour, and settling and overflowing. The feeding amount of the lime milk is 1 percent of the weight of the triethyl phosphite wastewater, the feeding amount of the PAM is two parts per million, and the settling time is 9 hours. The triethyl phosphite wastewater is firstly heated at high temperature to reduce the content of ammonia nitrogen and COD, then is oxidized by ozone without introducing other pollution sources, and then is pre-settled by limestone to reduce the subsequent dosage.
And after the sedimentation is finished, the overflow water enters a dephosphorization pool (a secondary sedimentation pool), hydrochloric acid is added to adjust the pH value to be less than 7, then polymeric ferric sulfate is added to stir for half an hour, then lime cream is added to adjust the pH value to be more than 11.5, and the mixture is stirred slowly to settle and overflow, wherein the sedimentation time is 9 hours. The feeding amount of the polymeric ferric sulfate is one thousandth of the weight of the triethyl phosphite wastewater. Regulating the pH value to be more than 11.5, slowly and slowly stirring for settling for 8 hours, wherein the total phosphorus content of the wastewater is less than 5PPM, the COD is less than 500PPM, and the ammonia nitrogen is less than 50 PPM; and then the wastewater can be discharged outside.
Example 3
Putting triethyl phosphite wastewater into a stirring kettle, and starting stirring at the stirring speed of 150 revolutions per minute. Slowly raising the temperature to 75 ℃, and keeping the temperature for two hours to fully separate out organic matters and ammonia gas in the wastewater. After the triethyl phosphite wastewater in the stirring kettle is stirred and heated for 2.5 hours, the material is put into an oxidation tower for cooling, and when the temperature is reduced to room temperature, the ozone is continuously introduced for stirring; the ozone is led in for 7 hours, and three-stage oxidation can be carried out in the process. After the oxidation is finished, the phosphorous acid in the wastewater is completely oxidized into orthophosphoric acid. The pH was measured at about 6-7. Then transferring the materials into a primary sedimentation tank, adding lime milk and PAM, stirring for half an hour, and settling and overflowing. The feeding amount of the lime milk is 1 percent of the weight of the triethyl phosphite wastewater, the feeding amount of the PAM is two parts per million, and the settling time is 7 hours. The triethyl phosphite wastewater is firstly heated at high temperature to reduce the content of ammonia nitrogen and COD, then is oxidized by ozone without introducing other pollution sources, and then is pre-settled by limestone to reduce the subsequent dosage.
And after the sedimentation is finished, the overflow water enters a dephosphorization pool (a secondary sedimentation pool), hydrochloric acid is added to adjust the pH value to be less than 7, then polymeric ferric sulfate is added to stir for half an hour, then lime cream is added to adjust the pH value to be more than 11.5, and the mixture is stirred slowly to settle and overflow, wherein the sedimentation time is 7 hours. The feeding amount of the polymeric ferric sulfate is one thousandth of the weight of the triethyl phosphite wastewater. Regulating the pH value to be more than 11.5, slowly and slowly stirring for settling for 7 hours, wherein the total phosphorus content of the wastewater is less than 5PPM, the COD is less than 500PPM, and the ammonia nitrogen is less than 50 PPM; and then the wastewater can be discharged outside.
While the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (1)
1. The triethyl phosphite wastewater treatment process is characterized by comprising the following steps
1) Placing triethyl phosphite wastewater in a stirring kettle, installing a condenser communicated with the stirring kettle above the stirring kettle, wherein the condenser is used for refluxing water vapor generated by heating, starting stirring, the stirring speed is 150-200 revolutions per minute, the temperature is slowly increased to 70-80 ℃, and the stirring and heating time is 2-2.5 hours;
2) after the triethyl phosphite wastewater in the stirring kettle is stirred and heated, the material is put into an oxidation tower for cooling, and when the temperature is reduced to room temperature, ozone is introduced and stirred to aerate the material; the ozone is introduced for 7 to 8 hours; after aeration is finished, measuring the pH value to be about 6-7;
3) after aeration is finished, transferring the materials into a primary sedimentation tank, adding lime milk, stirring for half an hour, and settling and overflowing; the feeding amount of the lime milk is 1 percent of the weight of the triethyl phosphite wastewater, and the settling time is 7-9 hours; triethyl phosphite wastewater is firstly heated at high temperature to reduce the content of ammonia nitrogen and COD, then is oxidized by ozone without introducing other pollution sources, and then is pre-settled by lime milk to reduce the dosage of subsequent agents;
4) after the sedimentation is finished, the overflow water enters a dephosphorization pool, hydrochloric acid is added to adjust the pH value to be less than 7, and then polymeric ferric sulfate is added to be stirred for half an hour, wherein the adding amount of the polymeric ferric sulfate is one thousandth of the weight of the triethyl phosphite wastewater; then adding lime milk to adjust the pH value to be more than 11.5, slowly and slowly stirring for settling for 7-9 hours, wherein the total phosphorus and phosphorus content of the wastewater is less than 5ppm, the COD (chemical oxygen demand) is less than 500ppm, and the ammonia nitrogen content is less than 50 ppm; and then the wastewater can be discharged outside.
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Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4689154A (en) * | 1985-11-15 | 1987-08-25 | Occidental Chemical Corporation | Process for removing phosphorus from industrial waste water |
| CN1234373A (en) * | 1999-04-21 | 1999-11-10 | 邯郸滏阳化工集团有限公司 | Method for treatment of waste liquid from production process of trimethyl phosphite, dimethyl phosphite and phosphates and other waste liquids containing nitrogen |
| TWI301474B (en) * | 2003-01-03 | 2008-10-01 | Huei Tarng Liou | Method for reducing cod (chemical oxygen demand) in waste water by using o3 with divalention |
| CN101624400B (en) * | 2009-08-07 | 2011-06-22 | 湖北三才堂化工科技有限公司 | Production method of triethyl phosphite |
| CN103964622B (en) * | 2013-02-05 | 2016-02-24 | 江苏优士化学有限公司 | A kind of comprehensive treating process of industrial organophosphorus waste liquid and resource utilization method |
| CN105130822B (en) * | 2015-09-21 | 2017-04-12 | 四川乐创科技有限公司 | Method for recovering triethylamine, removing phosphorus pollutants and recovering phosphorus resources in glyphosate mother liquor |
| CN105906026A (en) * | 2016-06-08 | 2016-08-31 | 浙江奇彩环境科技股份有限公司 | Treatment method for wastewater containing small-molecular organic matter |
| CN208008608U (en) * | 2017-08-17 | 2018-10-26 | 佛山市顺德区澄至环境工程有限公司 | A kind of device of processing triethyl phosphite phosphorus-containing wastewater |
| CN207986908U (en) * | 2018-02-26 | 2018-10-19 | 武夷学院 | A kind of pesticide waste water treatment device |
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