CN110028147B - Deep catalytic oxidation treatment method and device for acesulfame potassium production sewage - Google Patents
Deep catalytic oxidation treatment method and device for acesulfame potassium production sewage Download PDFInfo
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- CN110028147B CN110028147B CN201910368050.8A CN201910368050A CN110028147B CN 110028147 B CN110028147 B CN 110028147B CN 201910368050 A CN201910368050 A CN 201910368050A CN 110028147 B CN110028147 B CN 110028147B
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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
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
Abstract
The invention relates to a deep catalytic oxidation treatment method and a deep catalytic oxidation treatment device for acesulfame potassium production sewage, wherein the deep catalytic oxidation treatment device comprises the following components: the device comprises a sewage preheater, a high-pressure plunger pump, a spraying gas-liquid mixer, a catalytic oxidation reactor, a heat exchanger, a flash evaporator, an oxidizing liquid storage tank and an oxidizing liquid delivery pump. The deep catalytic oxidation treatment device for the acesulfame potassium production sewage effectively oxidizes even toxic high molecular organic matters with high content and difficult treatment into non-toxic small molecular organic matters, thereby being more beneficial to biochemical treatment; the organic phosphorus which is difficult to treat can be converted into the organic phosphorus which can be treated; the sulfur-containing compound is converted into sulfate ions, so that salt formation is facilitated, and the treatment is easy; the organic chlorine is oxidized into chloride ions, so that salt formation is facilitated, and the treatment is easy; the method has the characteristics of high polymer organic matter removal efficiency, short flow, automation realization and the like.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a deep catalytic oxidation treatment method and device for acesulfame potassium production sewage.
Background
Acesulfame potassium is a sugar-free sweetener, and is prepared at home and abroad by firstly synthesizing triethylamine sulfamate, then acylating the triethylamine sulfamate into a diacetyl-aminosulfonate intermediate by diketene, and further performing dehydration cyclization by sulfur trioxide and neutralization by potassium hydroxide. The production process has long route, more reaction byproducts, product yield of below 70 percent and most byproducts which are organic matters and enter wastewater after extraction, so that the process wastewater has high COD and deep color, and is difficult to reach the discharge standard by a single method or a biochemical method combined with Fenton and other process methods, and is always a restriction factor for the production of acesulfame.
Disclosure of Invention
The invention aims to provide a deep catalytic oxidation treatment device for sewage generated in acesulfame potassium production.
The invention relates to a deep catalytic oxidation treatment device for acesulfame potassium production sewage, which comprises: the device comprises a sewage preheater, a high-pressure plunger pump, a spraying gas-liquid mixer, a catalytic oxidation reactor, a heat exchanger, a flash evaporator, an oxidation liquid storage tank and an oxidation liquid delivery pump; the sewage preheater is communicated with the high-pressure plunger pump, the spraying gas-liquid mixer is communicated with the sewage preheater, the catalytic oxidation reactor is communicated with the spraying gas-liquid mixer, the heat exchanger is respectively communicated with the catalytic oxidation reactor, the spraying gas-liquid mixer and the oxidizing liquid storage tank, and the oxidizing liquid storage tank is respectively communicated with the flash evaporator and the oxidizing liquid delivery pump.
The deep catalytic oxidation treatment device for the acesulfame potassium production sewage effectively oxidizes even toxic high molecular organic matters with high content and difficult treatment into non-toxic small molecular organic matters, thereby being more beneficial to biochemical treatment; the organic phosphorus which is difficult to treat can be converted into the organic phosphorus which can be treated; the sulfur-containing compound is converted into sulfate ions, so that salt formation is facilitated, and the treatment is easy; the organic chlorine is oxidized into chloride ions, so that salt formation is facilitated, and the treatment is easy; the method has the characteristics of high polymer organic matter removal efficiency, short flow, automation realization and the like.
In addition, the deep catalytic oxidation treatment device for the acesulfame potassium production sewage can also have the following additional technical characteristics:
furthermore, a feeding distributor is arranged in the spraying gas-liquid mixer.
Further, a feeding distributor and a catalyst bed layer structure are arranged in the catalytic oxidation reactor.
The invention also aims to provide a deep catalytic oxidation treatment method for sewage generated in the production of acesulfame potassium by using the device.
The deep catalytic oxidation treatment method for the sewage generated in the production of acesulfame potassium by using the device comprises the following steps: s101: pumping the pretreated sewage into the upper part of the sewage preheater through the high-pressure plunger pump, exchanging heat with air entering from the lower part of the high-pressure plunger pump, and then entering the spraying gas-liquid mixer; s102: the sewage and the air are mixed in the jet gas-liquid mixer and then enter the catalytic oxidation reactor from the bottom of the catalytic oxidation reactor, the catalytic oxidation reaction is carried out under the catalytic action of a catalyst in the catalytic oxidation reactor, the obtained gas-phase product is output from the top of the catalytic oxidation reactor and then enters the heat exchanger, and the gas-liquid separation is realized after the gas-liquid separation is carried out on the gas-phase product and the sewage in the heat exchanger and the air in the flash evaporator; s103: the gas phase separated in the step S102 escapes from the top of the flash evaporator, the liquid phase separated in the step S102 flows into the oxidizing liquid storage tank, is pumped out by the oxidizing liquid delivery pump, and is classified according to the properties of the oxidizing liquid.
Further, the temperature of the top of the catalytic oxidation reactor is 160-320 ℃, and the pressure of the top of the catalytic oxidation reactor is 2.0-8.5 MPa.
Further, the temperature of the middle part of the catalytic oxidation reactor is 180-300 ℃.
Further, the air inlet pressure of the injection gas-liquid mixer is 2.0 MPa-6.5 MPa.
Further, the preparation method of the catalyst in the catalytic oxidation reactor comprises the following steps: mixing activated carbon and pseudo-boehmite according to the weight ratio of 1 (0.8-1.2), heating to 300-700 ℃, sintering and forming, then soaking in a solution containing rare metal ions, and sintering at 800-1100 ℃ to obtain a catalyst; wherein the rare metal at least comprises one of Ti, Ce, Cs, Ni, Ru, Rb and Nd.
Further, the gas-liquid ratio in the catalytic oxidation reactor is (300-500): 1.
additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a schematic structural view of a deep catalytic oxidation treatment device for acesulfame potassium production wastewater.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In a first aspect, the invention provides a deep catalytic oxidation treatment device for sewage generated in acesulfame potassium production.
As shown in figure 1, the invention provides a deep catalytic oxidation treatment device for acesulfame potassium production sewage, which comprises: the system comprises a sewage preheater 110, a high-pressure plunger pump 120, a jet gas-liquid mixer 130, a catalytic oxidation reactor 140, a heat exchanger 150, a flash evaporator 160, an oxidation liquid storage tank 170 and an oxidation liquid delivery pump 180.
The sewage preheater 110 is communicated with the high-pressure plunger pump 120, the jet gas-liquid mixer 130 is communicated with the sewage preheater 110, the catalytic oxidation reactor 140 is communicated with the jet gas-liquid mixer 130, the heat exchanger 150 is respectively communicated with the catalytic oxidation reactor 140, the jet gas-liquid mixer 130 and the oxidizing liquid storage tank 170, and the oxidizing liquid storage tank 170 is respectively communicated with the flash evaporator 160 and the oxidizing liquid delivery pump 180. A feeding distributor is arranged in the spraying gas-liquid mixer; and a feeding distributor and a catalyst bed layer structure are arranged in the catalytic oxidation reactor.
In a second aspect, the invention provides a deep catalytic oxidation treatment method for sewage generated in acesulfame potassium production by using the device, which comprises the following steps:
(1) pumping the pretreated sewage into the upper part of the sewage preheater through the high-pressure plunger pump, exchanging heat with air entering from the lower part of the high-pressure plunger pump, and then entering the spraying gas-liquid mixer; the air inlet pressure of the injection gas-liquid mixer is 2.5MPa to 6.5 MPa.
(2) The sewage and the air are mixed in the jet gas-liquid mixer and then enter the catalytic oxidation reactor from the bottom of the catalytic oxidation reactor, the catalytic oxidation reaction is carried out under the catalytic action of a catalyst in the catalytic oxidation reactor, the obtained gas-phase product is output from the top of the catalytic oxidation reactor and then enters the heat exchanger, and the gas-liquid separation is realized after the gas-liquid separation is carried out on the gas-phase product and the sewage in the heat exchanger and the air in the flash evaporator; the temperature of the top of the catalytic oxidation reactor is 160-320 ℃, and the pressure of the top of the catalytic oxidation reactor is 2.0-8.5 MPa. The middle temperature of the catalytic oxidation reactor is 180-300 ℃. The preparation method of the catalyst in the catalytic oxidation reactor comprises the following steps: mixing activated carbon and pseudo-boehmite according to the weight ratio of 1 (0.8-1.2), heating to 300-700 ℃, sintering and forming, then soaking in a solution containing rare metal ions, and sintering at 800-1100 ℃ to obtain a catalyst; wherein the rare metal at least comprises one of Ti, Ce, Cs, Ni, Ru, Rb and Nd. The gas-liquid ratio in the catalytic oxidation reactor is (300-500): 1.
(3) and (3) allowing the gas phase separated in the step (2) to escape from the top of the flash evaporator, allowing the liquid phase separated in the step (2) to flow into the oxidizing liquid storage tank, pumping out the liquid phase by the oxidizing liquid delivery pump, and performing classification treatment according to the properties of the liquid phase.
The present invention is described in detail below by way of specific examples.
Example 1 treatment of wastewater from acesulfame K production
The acesulfame potassium production process has long route, more reaction byproducts, mostly organic substances, the COD of mother liquor wastewater is 230000 mg/L, the COD of rectification raffinate is 340000 mg/L, the rectification raffinate contains a small amount of acetone, organic impurities, less than 1% of dichloromethane and the like, the color is dark, and the discharge standard is difficult to reach by a single treatment method or a biochemical method combined with Fenton and other processes.
(1) Opening a heat transfer oil heating medium for circulation to keep the temperature of the heat transfer oil in a normal state; and simultaneously opening the air and the sewage entering the catalytic oxidation reactor, controlling the sewage inlet pressure to be basically consistent with the air inlet pressure, controlling the gas-liquid ratio to be 400:1, and gradually raising the sewage temperature.
(2) The sewage and air are in a gas-liquid state at high temperature, and are subjected to catalytic oxidation reaction under the action of a catalyst in a catalytic oxidation reactor to produce small molecules or other corresponding substances, and simultaneously generate partial heat, the temperature of the top of the tower is controlled to be 230 ℃, a temperature control field and a remote transmission control system are arranged on the top of the tower, the opening of a heat conduction oil inlet valve is controlled to exceed 10% of the set temperature.
(3) The pressure at the top of the catalytic oxidation reactor is controlled to be 4.0MPa and exceeds 30 percent of the set pressure, and the pressure controller at the top of the catalytic oxidation reactor is controlled to adjust the opening of the air inlet valve so as to keep the normal operation state.
(4) And the gas phase removed from the top of the catalytic oxidation reactor enters a heat exchanger, exchanges heat with sewage and air entering the catalytic oxidation reactor, and then enters a flash evaporator to realize gas-liquid separation.
(5) The gas escapes from the top of the flash evaporator and comprises the main components of nitrogen, carbon dioxide, ammonia, water and air. And storing the cooled oxidizing liquid in an oxidizing liquid storage tank, and pumping out the oxidizing liquid by a pump to perform classification treatment according to the properties of the oxidizing liquid.
(6) Under the action of a self-made catalyst, introducing air or oxygen into the sewage, and oxidizing sulfur into sulfate radicals under the conditions of high temperature and high pressure; oxidizing nitrogen into ammonia or ammonium radicals; the methylene dichloride organic chloride is oxidized into chloride ions, so that high molecular compounds in the sewage are effectively removed, COD (chemical oxygen demand) and ammonia nitrogen are reduced, and meanwhile, the high molecular compounds are converted into processable substances, and the purpose of treatment is further achieved.
Example 2 treatment of wastewater from sucralose production
The sucralose takes natural sucrose as a raw material, sucrose-6-acetate is prepared by esterification, sucrose-4-acetate is used for generating sucrose-6-acetate under the action of a catalyst tert-butylamine, sucralose-6-acetate is prepared by chlorination, and byproducts such as monochloro sucrose-6-acetate, dichloro sucrose-6-acetate, monochloro sucrose-4-acetate, dichloro sucrose-4-acetate, tetrachlorosucrose and the like are generated by chlorination side reaction; then the sucralose is prepared by a series of processes such as neutralization, chloro-concentration, ethyl acetate extraction and the like. The process route is long, the conversion rate is low, the total yield is about 40%, a large amount of organic matters exist in sewage in the reaction process, the sewage is black, contains a large amount of chlorides, high-molecular organic matters, organic solvents and the like, the components are complex, and the treatment difficulty is high.
The sucralose produces nearly 30 tons of mother liquor per ton of finished product, the raw water COD is 15-20 PPM, the raw water contains 18% of ammonium chloride, and the main pollutants of the sucralose and derivatives thereof, DMF and other organic solvents.
(1) Opening a heat transfer oil heating medium for circulation to keep the temperature of the heat transfer oil in a normal state; and (3) simultaneously opening the air and the sewage entering the catalytic oxidation reactor, controlling the sewage inlet pressure to be basically consistent with the air inlet pressure, controlling the gas-liquid ratio to be 460:1, and gradually raising the sewage temperature.
(2) Under the action of catalyst in the catalytic oxidation reactor, the sewage and air are made into gas-liquid state at high temp. and made into catalytic oxidation reaction to produce small molecule or correspondent other substances, at the same time produce partial heat, and the temp. of tower top is controlled at 280 deg.C, and the temp. control field and remote transmission control system are set on the tower top, and the opening of heat-conducting oil inlet valve is controlled, and its temp. is above 10% of set temp.
(3) The top pressure of the catalytic oxidation reactor is controlled to be 6.5MPa and exceeds 20% of the set pressure, and the top pressure controller is controlled to adjust the opening of the air inlet valve so as to keep the normal operation state.
(4) And the gas phase removed from the top of the catalytic oxidation reactor enters a heat exchanger, exchanges heat with sewage and air entering the catalytic oxidation reactor, and then enters a flash evaporator to realize gas-liquid separation.
(5) The gas escapes from the top of the flash evaporator and comprises the main components of nitrogen, carbon dioxide, ammonia, water and air. And storing the cooled oxidation liquid in an oxidation liquid storage tank, wherein the oxidation liquid is light in color and dark red, pumping out the oxidation liquid by a pump to carry out MVR concentration to produce ammonium chloride, and carrying out biochemical treatment on the concentrated and separated sewage.
(6) Under the effect of this sulphur element in sewage, let in air or oxygen under high temperature, high pressure condition under this self-control catalyst, chlorine element oxidation is the chloride ion in the organic chloride, and the sucrose derivative oxidation becomes the micromolecule and is the material, removes the macromolecular compound in the sewage effectively, reduces COD, turns into the material that can handle simultaneously, and then reaches the purpose of handling, and the processing procedure does not produce solid useless.
In conclusion, the deep catalytic oxidation treatment device for the acesulfame potassium production sewage effectively oxidizes even toxic high molecular organic matters with high content and difficult treatment into non-toxic small molecular organic matters, and is more beneficial to biochemical treatment; the organic phosphorus which is difficult to treat can be converted into the organic phosphorus which can be treated; the sulfur-containing compound is converted into sulfate ions, so that salt formation is facilitated, and the treatment is easy; the organic chlorine is oxidized into chloride ions, so that salt formation is facilitated, and the treatment is easy; the method has the characteristics of high polymer organic matter removal efficiency, short flow, automation realization and the like.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (4)
1. A deep catalytic oxidation treatment device of acesulfame potassium production sewage, which is characterized by comprising: the device comprises a sewage preheater, a high-pressure plunger pump, a spraying gas-liquid mixer, a catalytic oxidation reactor, a heat exchanger, a flash evaporator, an oxidation liquid storage tank and an oxidation liquid delivery pump;
the sewage preheater is communicated with the high-pressure plunger pump, the spraying gas-liquid mixer is communicated with the sewage preheater, the catalytic oxidation reactor is communicated with the spraying gas-liquid mixer, the heat exchanger is respectively communicated with the catalytic oxidation reactor, the spraying gas-liquid mixer and the flash evaporator, and the oxidizing liquid storage tank is respectively communicated with the flash evaporator and the oxidizing liquid delivery pump;
a feeding distributor and a catalyst bed layer structure are arranged in the catalytic oxidation reactor;
the temperature of the top of the catalytic oxidation reactor is 160-320 ℃, and the pressure of the top of the catalytic oxidation reactor is 2.0-8.5 MPa; the middle temperature of the catalytic oxidation reactor is 180-300 ℃;
the air inlet pressure of the injection gas-liquid mixer is 2.0MPa to 6.5 MPa;
the preparation method of the catalyst in the catalytic oxidation reactor comprises the following steps: mixing activated carbon and pseudo-boehmite according to the weight ratio of 1 (0.8-1.2), heating to 300-700 ℃, sintering and forming, then dipping in a solution containing rare metal ions, and sintering at 800-1100 ℃ to obtain a catalyst; wherein the rare metal at least comprises one of Ti, Cs, Ru, Rb and Nd;
the acesulfame potassium production sewage comprises mother liquor wastewater with COD of 230000 mg/L and rectification residual liquid with COD of 340000 mg/L.
2. The deep catalytic oxidation treatment device for acesulfame potassium production sewage according to claim 1, wherein a feed distributor is provided in the jet gas-liquid mixer.
3. The deep catalytic oxidation treatment method of acesulfame potassium production sewage by the device according to any one of claims 1 to 2, characterized by comprising the following steps:
s101: pumping pretreated sewage into the upper part of the sewage preheater through the high-pressure plunger pump, exchanging heat with air entering from the lower part of the sewage preheater, and then entering the spraying gas-liquid mixer;
s102: the sewage and the air are mixed in the spraying gas-liquid mixer and then enter the catalytic oxidation reactor from the bottom of the catalytic oxidation reactor, the catalytic oxidation reaction is carried out under the catalytic action of a catalyst in the catalytic oxidation reactor, the obtained gas-phase product is output from the top of the catalytic oxidation reactor and then enters the heat exchanger, and the gas-phase product exchanges heat with the air entering the spraying gas-liquid mixer in the heat exchanger and then enters the flash evaporator to realize gas-liquid separation;
s103: the gas phase separated in the step S102 escapes from the top of the flash evaporator, the liquid phase separated in the step S102 flows into the oxidizing liquid storage tank, is pumped out by the oxidizing liquid delivery pump, and is classified according to the properties of the oxidizing liquid.
4. The deep catalytic oxidation treatment method of acesulfame potassium production sewage according to claim 3, wherein the gas-liquid ratio in the catalytic oxidation reactor is (300-500): 1.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050006347A (en) * | 2003-07-08 | 2005-01-17 | 한국건설기술연구원 | BNR(Biological Nutrient Removal) system and method by organic acids generated from sewage sludge |
| CN106348421A (en) * | 2016-10-11 | 2017-01-25 | 羿太环保科技（上海）有限公司 | Continuous wet oxidation process for degrading high concentration organic waste water and equipment thereof |
| CN109621941A (en) * | 2019-01-17 | 2019-04-16 | 中国石油大学(北京) | A kind of spent bleaching clay prepares catalytic ozonation catalyst and its preparation and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050006347A (en) * | 2003-07-08 | 2005-01-17 | 한국건설기술연구원 | BNR(Biological Nutrient Removal) system and method by organic acids generated from sewage sludge |
| CN106348421A (en) * | 2016-10-11 | 2017-01-25 | 羿太环保科技（上海）有限公司 | Continuous wet oxidation process for degrading high concentration organic waste water and equipment thereof |
| CN109621941A (en) * | 2019-01-17 | 2019-04-16 | 中国石油大学(北京) | A kind of spent bleaching clay prepares catalytic ozonation catalyst and its preparation and application |
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