CN114230071A - Treatment method of DMF (dimethyl formamide) -containing wastewater - Google Patents
Treatment method of DMF (dimethyl formamide) -containing wastewater Download PDFInfo
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0003—Condensation of vapours; Recovering volatile solvents by condensation by using heat-exchange surfaces for indirect contact between gases or vapours and the cooling medium
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/0075—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with heat exchanging
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0078—Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
- B01D5/0093—Removing and treatment of non condensable gases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1406—Multiple stage absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/10—Inorganic absorbents
- B01D2252/103—Water
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/406—Ammonia
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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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
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- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
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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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/586—Treatment of water, waste water, or sewage by removing specified dissolved compounds by removing ammoniacal nitrogen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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Abstract
A treatment method of DMF-containing wastewater comprises the following steps of introducing the DMF-containing wastewater into an alkaline hydrolysis tower, adding a proper amount of liquid alkali into a water inlet pipeline for mixing, mixing with the wastewater, heating by a heat exchanger, then entering the alkaline hydrolysis tower, feeding the alkaline hydrolysis wastewater into a deamination tower, carrying out negative pumping by a negative pressure system, pumping out ammonia and dimethylamine obtained by alkaline hydrolysis, absorbing the ammonia and the dimethylamine by an ammonia recovery device, absorbing tail gas by a tail gas absorption tower, and feeding ammonia-absorbing water into an ammonia trough by the ammonia recovery device, thereby achieving the purposes of alkaline hydrolysis deamination of the DMF-containing wastewater and reducing total nitrogen. The method can reduce the total nitrogen in the wastewater, thereby reducing the wastewater treatment difficulty of a biochemical system and achieving the purpose of standard discharge of the wastewater treatment.
Description
Technical Field
The invention relates to a method for treating waste water containing DMF.
Background
The wastewater containing organic nitrogen such as ammonia nitrogen and DMF generated in the production process of sucralose, the denitrification in the traditional biochemistry reduces the total nitrogen and has higher requirement on water quality, the wastewater containing high-concentration total nitrogen is difficult to solve, and especially the wastewater containing DMF is difficult to completely treat only by using a biochemical system.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for treating DMF-containing wastewater, which can reduce the total nitrogen in the wastewater, thereby reducing the wastewater treatment difficulty of a biochemical system and achieving the purpose of standard-reaching discharge of wastewater treatment.
In order to solve the technical problem, the invention provides a treatment method of DMF-containing wastewater, which comprises the following steps:
(1) leading out waste water containing DMF and organic nitrogen from a waste water pool, adding liquid caustic soda to adjust the pH of the waste water to 10-12, wherein the liquid caustic soda is 32% sodium hydroxide solution;
(2) the wastewater after pH adjustment sequentially passes through a No. 1 plate heat exchanger, a No. 2 plate heat exchanger and a No. 3 plate heat exchanger which are connected in series through a lift pump and is sent into an alkaline hydrolysis tower for alkaline hydrolysis reaction, wherein the No. 1 plate heat exchanger heats the wastewater to 60 ℃, the No. 2 plate heat exchanger heats the wastewater to 90 ℃, the No. 3 plate heat exchanger heats the wastewater to 120 ℃, and DMF in the wastewater reacts with sodium hydroxide in the alkaline hydrolysis tower to generate dimethylamine;
(3) the wastewater after the alkaline hydrolysis passes through the No. 2 plate heat exchanger in the form of a heat exchange medium, and the temperature of materials in the No. 2 plate heat exchanger is increased while the wastewater is cooled;
(4) waste water passing through the No. 2 plate heat exchanger enters the deamination tower from the top of the deamination tower, is sprayed from top to bottom in the deamination tower in a spraying mode, steam is introduced upwards from the bottom of the deamination tower, the sprayed waste water and the upward steam form convection, dimethylamine and part of free ammonia in the waste water volatilize from the waste water under the action of the steam and leave the deamination tower upwards along with the steam, the residual waste water in the deamination tower passes through the No. 1 plate heat exchanger in a heat exchange medium mode, the temperature of materials in the No. 1 plate heat exchanger is increased while the waste water is cooled, and finally the waste water enters a biochemical treatment section for treatment;
(5) the gas phase leaving the deamination tower enters an evaporative cooler for cooling, wherein water vapor is changed into liquid water, and then the liquid water is sent into a gas-liquid separation tank together for gas-liquid separation, wherein the gas phase part is dimethylamine and ammonia gas, the liquid phase part is water in which part of the dimethylamine and the ammonia gas are dissolved, the liquid phase reflows to the deamination tower and is sprayed for deamination again, and the gas phase enters an ammonia recovery device under the action of a vacuum pump;
(6) soft water for absorbing gas phase is stored in the ammonia recovery device, and a circulating cooler is connected with the ammonia recovery device, a gas phase pipeline in the ammonia recovery device is submerged in water, a part of gas phase enters the ammonia recovery device and is absorbed by water, residual tail gas enters a tail gas absorption tower from the bottom of the tail gas absorption tower, and the top of the tail gas absorption tower sprays the soft water downwards to carry out secondary absorption on the residual tail gas;
(7) the water after spraying and absorbing the residual tail gas is refluxed to the ammonia recovery device from the bottom of the tail gas absorption tower and is mixed with the water in the ammonia recovery device, when the ammonia nitrogen content in the water in the ammonia recovery device is greater than 12 percent or the dimethylamine content is greater than 30 percent, the water in the ammonia recovery device is introduced into the ammonia water tank, and soft water is replenished into the ammonia recovery device through the soft water replenishing device.
Preferably, the 3# plate heat exchanger takes steam as a heat exchange medium to heat the material, and the steam enters the condensate tank to be collected after passing through the 3# plate heat exchanger.
Preferably, steam is introduced into the alkaline hydrolysis tower to maintain the reaction temperature.
The invention has the advantages that: the invention leads the waste water containing DMF into an alkaline hydrolysis tower, adds proper liquid alkali into a water inlet pipeline for mixing, mixes the waste water with the waste water, heats the waste water by a heat exchanger and then enters the alkaline hydrolysis tower, the waste water after alkaline hydrolysis enters a deamination tower, negative pumping is carried out by a negative pressure system, and ammonia gas obtained by alkaline hydrolysis is pumped out, thereby achieving the purposes of alkaline hydrolysis deamination of the waste water containing DMF and reducing total nitrogen. The method can reduce the total nitrogen in the wastewater, thereby reducing the wastewater treatment difficulty of a biochemical system and achieving the purpose of wastewater treatment discharge up to standard, and has the advantages of simple steps, convenient operation and higher efficiency, wherein the liquid-phase materials discharged by the alkaline hydrolysis tower and the deamination tower utilize self heat as the heat exchange medium of the plate heat exchanger, thereby not only reducing the temperature of the materials, but also heating the materials and playing the role of saving energy and killing two birds with one stone.
Drawings
FIG. 1 is a schematic flow diagram of the present invention.
Detailed Description
Referring to fig. 1, a method for treating DMF-containing wastewater comprises the following steps:
(1) leading out waste water containing DMF and organic nitrogen from a waste water pool, adding liquid caustic soda to adjust the pH of the waste water to 10-12, wherein the liquid caustic soda is 32% sodium hydroxide solution;
(2) the wastewater after pH adjustment sequentially passes through a No. 1 plate heat exchanger, a No. 2 plate heat exchanger and a No. 3 plate heat exchanger which are connected in series through a lift pump and is sent into an alkaline hydrolysis tower for alkaline hydrolysis reaction, wherein the No. 1 plate heat exchanger heats the wastewater to 60 ℃, the No. 2 plate heat exchanger heats the wastewater to 90 ℃, the No. 3 plate heat exchanger heats the wastewater to 120 ℃, and DMF in the wastewater reacts with sodium hydroxide in the alkaline hydrolysis tower to generate dimethylamine;
(3) the wastewater after the alkaline hydrolysis passes through the No. 2 plate heat exchanger in the form of a heat exchange medium, and the temperature of materials in the No. 2 plate heat exchanger is increased while the wastewater is cooled;
(4) waste water passing through the No. 2 plate heat exchanger enters the deamination tower from the top of the deamination tower, is sprayed from top to bottom in the deamination tower in a spraying mode, steam is introduced upwards from the bottom of the deamination tower, the sprayed waste water and the upward steam form convection, dimethylamine and part of free ammonia in the waste water volatilize from the waste water under the action of the steam and leave the deamination tower upwards along with the steam, the residual waste water in the deamination tower passes through the No. 1 plate heat exchanger in a heat exchange medium mode, the temperature of materials in the No. 1 plate heat exchanger is increased while the waste water is cooled, and finally the waste water enters a biochemical treatment section for treatment;
(5) the gas phase leaving the deamination tower enters an evaporative cooler for cooling, wherein water vapor is changed into liquid water, and then the liquid water is sent into a gas-liquid separation tank together for gas-liquid separation, wherein the gas phase part is dimethylamine and ammonia gas, the liquid phase part is water in which part of the dimethylamine and the ammonia gas are dissolved, the liquid phase reflows to the deamination tower and is sprayed for deamination again, and the gas phase enters an ammonia recovery device under the action of a vacuum pump;
(6) soft water for absorbing gas phase is stored in the ammonia recovery device, and a circulating cooler is connected with the ammonia recovery device, a gas phase pipeline in the ammonia recovery device is submerged in water, a part of gas phase enters the ammonia recovery device and is absorbed by water, residual tail gas enters a tail gas absorption tower from the bottom of the tail gas absorption tower, and the top of the tail gas absorption tower sprays the soft water downwards to carry out secondary absorption on the residual tail gas;
(7) the water after spraying and absorbing the residual tail gas is refluxed to the ammonia recovery device from the bottom of the tail gas absorption tower and is mixed with the water in the ammonia recovery device, when the ammonia nitrogen content in the water in the ammonia recovery device is greater than 12 percent or the dimethylamine content is greater than 30 percent, the water in the ammonia recovery device is introduced into the ammonia water tank, and soft water is replenished into the ammonia recovery device through the soft water replenishing device.
The 3# plate heat exchanger uses steam as a heat exchange medium to heat the material, and the steam enters the condensate tank to be collected after passing through the 3# plate heat exchanger.
And introducing steam into the alkaline hydrolysis tower to keep the reaction temperature.
The invention has the advantages that: the invention leads the waste water containing DMF into an alkaline hydrolysis tower, adds proper liquid alkali into a water inlet pipeline for mixing, mixes the waste water with the waste water, heats the waste water by a heat exchanger and then enters the alkaline hydrolysis tower, the waste water after alkaline hydrolysis enters a deamination tower, negative pumping is carried out by a negative pressure system, and ammonia gas obtained by alkaline hydrolysis is pumped out, thereby achieving the purposes of alkaline hydrolysis deamination of the waste water containing DMF and reducing total nitrogen. The method can reduce the total nitrogen in the wastewater, thereby reducing the wastewater treatment difficulty of a biochemical system and achieving the purpose of wastewater treatment discharge up to standard, and has the advantages of simple steps, convenient operation and higher efficiency, wherein the liquid-phase materials discharged by the alkaline hydrolysis tower and the deamination tower utilize self heat as the heat exchange medium of the plate heat exchanger, thereby not only reducing the temperature of the materials, but also heating the materials and playing the role of saving energy and killing two birds with one stone.
Claims (3)
1. A treatment method of DMF-containing wastewater is characterized by comprising the following steps:
(1) leading out waste water containing DMF and organic nitrogen from a waste water pool, adding liquid caustic soda to adjust the pH of the waste water to 10-12, wherein the liquid caustic soda is 32% sodium hydroxide solution;
(2) the wastewater after pH adjustment sequentially passes through a No. 1 plate heat exchanger, a No. 2 plate heat exchanger and a No. 3 plate heat exchanger which are connected in series through a lift pump and is sent into an alkaline hydrolysis tower for alkaline hydrolysis reaction, wherein the No. 1 plate heat exchanger heats the wastewater to 60 ℃, the No. 2 plate heat exchanger heats the wastewater to 90 ℃, the No. 3 plate heat exchanger heats the wastewater to 120 ℃, and DMF in the wastewater reacts with sodium hydroxide in the alkaline hydrolysis tower to generate dimethylamine;
(3) the wastewater after the alkaline hydrolysis passes through the No. 2 plate heat exchanger in the form of a heat exchange medium, and the temperature of materials in the No. 2 plate heat exchanger is increased while the wastewater is cooled;
(4) waste water passing through the No. 2 plate heat exchanger enters the deamination tower from the top of the deamination tower, is sprayed from top to bottom in the deamination tower in a spraying mode, steam is introduced upwards from the bottom of the deamination tower, the sprayed waste water and the upward steam form convection, dimethylamine and part of free ammonia in the waste water volatilize from the waste water under the action of the steam and leave the deamination tower upwards along with the steam, the residual waste water in the deamination tower passes through the No. 1 plate heat exchanger in a heat exchange medium mode, the temperature of materials in the No. 1 plate heat exchanger is increased while the waste water is cooled, and finally the waste water enters a biochemical treatment section for treatment;
(5) the gas phase leaving the deamination tower enters an evaporative cooler for cooling, wherein water vapor is changed into liquid water, and then the liquid water is sent into a gas-liquid separation tank together for gas-liquid separation, wherein the gas phase part is dimethylamine and ammonia gas, the liquid phase part is water in which part of the dimethylamine and the ammonia gas are dissolved, the liquid phase reflows to the deamination tower and is sprayed for deamination again, and the gas phase enters an ammonia recovery device under the action of a vacuum pump;
(6) soft water for absorbing gas phase is stored in the ammonia recovery device, and a circulating cooler is connected with the ammonia recovery device, a gas phase pipeline in the ammonia recovery device is submerged in water, a part of gas phase enters the ammonia recovery device and is absorbed by water, residual tail gas enters a tail gas absorption tower from the bottom of the tail gas absorption tower, and the top of the tail gas absorption tower sprays the soft water downwards to carry out secondary absorption on the residual tail gas;
(7) the water after spraying and absorbing the residual tail gas is refluxed to the ammonia recovery device from the bottom of the tail gas absorption tower and is mixed with the water in the ammonia recovery device, when the ammonia nitrogen content in the water in the ammonia recovery device is greater than 12 percent or the dimethylamine content is greater than 30 percent, the water in the ammonia recovery device is introduced into the ammonia water tank, and soft water is replenished into the ammonia recovery device through the soft water replenishing device.
2. The method for treating DMF-containing wastewater according to claim 1, which comprises the following steps: the 3# plate heat exchanger uses steam as a heat exchange medium to heat the material, and the steam enters the condensate tank to be collected after passing through the 3# plate heat exchanger.
3. The method for treating DMF-containing wastewater according to claim 1, which comprises the following steps: and introducing steam into the alkaline hydrolysis tower to keep the reaction temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111419981.XA CN114230071A (en) | 2021-11-26 | 2021-11-26 | Treatment method of DMF (dimethyl formamide) -containing wastewater |
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| CN202111419981.XA CN114230071A (en) | 2021-11-26 | 2021-11-26 | Treatment method of DMF (dimethyl formamide) -containing wastewater |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114931829A (en) * | 2022-06-27 | 2022-08-23 | 山东戴瑞克新材料有限公司 | Phthalimide wastewater and waste gas treatment system and treatment process |
| CN115784899A (en) * | 2022-11-17 | 2023-03-14 | 安徽金禾实业股份有限公司 | Method for recovering dimethylamine in sucralose production |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910020A (en) * | 2015-05-20 | 2015-09-16 | 盐城捷康三氯蔗糖制造有限公司 | Method for recovering dimethylamine from sucralose production wastewater |
| CN108658095A (en) * | 2018-08-01 | 2018-10-16 | 杭州鹊帆环保科技有限公司 | The energy-saving reclaiming process and system that a kind of ammonium hydroxide recycling concentration is easily adjusted |
| CN109956605A (en) * | 2017-12-25 | 2019-07-02 | 盐城捷康三氯蔗糖制造有限公司 | The processing method of extraction wastewater in Sucralose production |
| CN111662203A (en) * | 2020-05-25 | 2020-09-15 | 安徽金禾实业股份有限公司 | Method and device for recycling heat energy of DMF (dimethyl formamide) rectification recovery device |
-
2021
- 2021-11-26 CN CN202111419981.XA patent/CN114230071A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910020A (en) * | 2015-05-20 | 2015-09-16 | 盐城捷康三氯蔗糖制造有限公司 | Method for recovering dimethylamine from sucralose production wastewater |
| CN109956605A (en) * | 2017-12-25 | 2019-07-02 | 盐城捷康三氯蔗糖制造有限公司 | The processing method of extraction wastewater in Sucralose production |
| CN108658095A (en) * | 2018-08-01 | 2018-10-16 | 杭州鹊帆环保科技有限公司 | The energy-saving reclaiming process and system that a kind of ammonium hydroxide recycling concentration is easily adjusted |
| CN111662203A (en) * | 2020-05-25 | 2020-09-15 | 安徽金禾实业股份有限公司 | Method and device for recycling heat energy of DMF (dimethyl formamide) rectification recovery device |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114931829A (en) * | 2022-06-27 | 2022-08-23 | 山东戴瑞克新材料有限公司 | Phthalimide wastewater and waste gas treatment system and treatment process |
| CN115784899A (en) * | 2022-11-17 | 2023-03-14 | 安徽金禾实业股份有限公司 | Method for recovering dimethylamine in sucralose production |
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