CN117582682A - Mixed salt treatment device and method - Google Patents
Mixed salt treatment device and method Download PDFInfo
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- CN117582682A CN117582682A CN202311543353.1A CN202311543353A CN117582682A CN 117582682 A CN117582682 A CN 117582682A CN 202311543353 A CN202311543353 A CN 202311543353A CN 117582682 A CN117582682 A CN 117582682A
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- 150000003839 salts Chemical class 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 142
- 238000000605 extraction Methods 0.000 claims abstract description 58
- 238000010306 acid treatment Methods 0.000 claims abstract description 23
- 238000011084 recovery Methods 0.000 claims description 62
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 48
- 239000000203 mixture Substances 0.000 claims description 44
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 40
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 39
- 239000002253 acid Substances 0.000 claims description 38
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 238000004891 communication Methods 0.000 claims description 27
- 239000000126 substance Substances 0.000 claims description 25
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 14
- 239000012266 salt solution Substances 0.000 claims description 14
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 14
- 235000011152 sodium sulphate Nutrition 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 13
- 230000003068 static effect Effects 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000012546 transfer Methods 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 238000000855 fermentation Methods 0.000 claims description 9
- 230000004151 fermentation Effects 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 6
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- UHOPWFKONJYLCF-UHFFFAOYSA-N 2-(2-sulfanylethyl)isoindole-1,3-dione Chemical compound C1=CC=C2C(=O)N(CCS)C(=O)C2=C1 UHOPWFKONJYLCF-UHFFFAOYSA-N 0.000 claims description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 2
- 229940090181 propyl acetate Drugs 0.000 claims description 2
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 239000012071 phase Substances 0.000 description 53
- 239000008346 aqueous phase Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 4
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 3
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 3
- 229940035437 1,3-propanediol Drugs 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
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- 238000005260 corrosion Methods 0.000 description 2
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- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 1
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- 239000000835 fiber Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a mixed salt treatment device and a method, wherein the mixed salt treatment device comprises an acid treatment unit, a stripping unit, a centrifugal extraction unit and a rectifying unit; the stripping unit comprises a stripping tower and a stripping tower reboiler, the stripping tower reboiler comprises a first channel and a second channel, the first channel is respectively communicated with the acid treatment unit and the centrifugal extraction unit, and the stripping tower is respectively communicated with the second channel and the centrifugal extraction unit; the rectification unit comprises a heat exchanger, a first gas-liquid separator, a vapor compressor and a first reboiler; the heat exchanger comprises a third channel and a fourth channel, the first reboiler comprises a fifth channel and a sixth channel, the third channel is respectively communicated with the centrifugal extraction unit and the first gas-liquid separator, the top of the first gas-liquid separator is communicated with the vapor compressor, the bottom of the first gas-liquid separator is communicated with the fifth channel, and the sixth channel is respectively communicated with the vapor compressor and the fourth channel. The mixed salt treatment apparatus of the present invention has low external energy consumption and continuously treats mixed salt.
Description
Technical Field
The invention belongs to the technical field of chemical separation, and particularly relates to a mixed salt treatment device and method.
Background
1, 3-propanediol is abbreviated as PDO, is a colorless transparent odorless liquid, is miscible with water, alcohol and various organic solvents, is slightly soluble in benzene and chloroform, and has typical properties of alcohol and glycol. The 1, 3-propanediol is used as an important chemical raw material, and is mainly used for synthesizing plasticizers, detergents, preservatives and emulsifying agents, and also can be used in industries of foods, cosmetics, pharmacy and the like, but is mainly used as a high polymer material with excellent polymer monomer synthesizing performance to replace ethylene glycol and butanediol to produce polyol polyester, is used for manufacturing novel polyester fiber PTT with excellent performance, and is further applied to markets of clothing, carpets, electronics, automobiles and the like.
In recent years, a method for producing 1, 3-propanediol by anaerobic fermentation using industrial glycerin as a raw material has been developed, but this method produces a large amount of by-product organic mixed salts, which contain acetate, butyrate, lactate and the like. At present, an evaporation crystallization process is often adopted to treat the organic mixed salt, but a large amount of steam is consumed in the treatment process, so that the cost is high, the market popularization is difficult, meanwhile, the mixed salt sometimes contains organic matters, and the national dangerous waste emission standard is difficult to reach by adopting the evaporation crystallization process. For this reason, a great deal of effort is devoted to research and treatment of organic mixed salts, for example, chinese patent document CN112479868A discloses a method and apparatus for extracting organic acid from mixed salts obtained by separation of fermentation broth, by which organic acid can be efficiently extracted from mixed salts obtained by separation of fermentation broth, specifically, the recovery rate of acetic acid can reach 68.7%, and the recovery rate of butyric acid can reach 81.6%, however, the heat sources of the two apparatuses, i.e., the rectifying tower and the phase separation tank, are high in energy consumption due to the complete dependence of external steam supply, which greatly affects the economic benefits of the process.
Accordingly, there is a need for a mixed salt treatment apparatus and method for reducing external energy consumption and continuously treating mixed salt.
Disclosure of Invention
The purpose of the present invention is to provide a mixed salt treatment apparatus with which the external energy consumption can be reduced and the mixed salt can be continuously treated.
Another object of the present invention is to provide a method for treating mixed salt using the above mixed salt treating apparatus, which has low external power consumption and continuously treats mixed salt.
In order to achieve the above object, the invention provides a mixed salt treatment device, which comprises an acid treatment unit, a stripping unit, a centrifugal extraction unit and a rectifying unit which are sequentially communicated;
the acid treatment unit is used for reacting concentrated sulfuric acid with the mixed salt;
the stripping unit comprises a stripping tower and a stripping tower reboiler, the stripping tower reboiler comprises a first channel and a second channel which are mutually isolated, the first channel is respectively communicated with the acid treatment unit and the centrifugal extraction unit, and the stripping tower is respectively communicated with the second channel and the centrifugal extraction unit;
the rectification unit comprises a first recovery system, wherein the first recovery system comprises a heat exchanger, a first gas-liquid separator, a vapor compressor and a first reboiler; the heat exchanger comprises a third channel and a fourth channel which are isolated from each other, the first reboiler comprises a fifth channel and a sixth channel which are isolated from each other, the third channel is respectively communicated with the centrifugal extraction unit and the first gas-liquid separator, the top of the first gas-liquid separator is communicated with the vapor compressor, the bottom of the first gas-liquid separator is communicated with the fifth channel, and the sixth channel is respectively communicated with the vapor compressor and the fourth channel.
Compared with the prior art, the invention has the advantages that the stripper reboiler is arranged between the acid treatment unit and the centrifugal extraction unit, the concentrated sulfuric acid and the mixed salt react to obtain the high-temperature acid-containing mixture, and when the acid-containing mixture flows out of the acid treatment unit and then flows through the first channel of the stripper reboiler, the heat of the acid-containing mixture can be transferred to the second channel to heat the stripper, so that the reaction heat of the concentrated sulfuric acid and the mixed salt is recycled by arranging the stripper reboiler, and the stripper does not completely depend on external heat supply, thereby reducing the external energy consumption of the stripper. Meanwhile, the heat exchanger, the vapor compressor and the first reboiler are further arranged, the vapor compressor is utilized to pressurize the extractant vapor separated from the top of the first gas-liquid separator to form high-temperature high-pressure gas, the high-temperature high-pressure gas enters a sixth channel of the first reboiler to be condensed to obtain high-temperature high-pressure liquid, and heat of the high-temperature high-pressure gas is transferred to a fifth channel of the first reboiler to recycle the condensation heat of the high-temperature high-pressure gas so as to heat the first gas-liquid separator, so that the first gas-liquid separator can separate oil phase matters without consuming external energy; in addition, the high-temperature high-pressure liquid flows into the fourth channel of the heat exchanger and transfers the heat of the high-temperature high-pressure liquid to the third channel, so that the oil phase matters flowing out of the centrifugal extraction unit can be preheated and the extractant can be partially gasified, and the energy consumed by the first gas-liquid separator for separating the oil phase matters can be further reduced. In addition, the cost of the vapor compressor is far lower than the cost of the first gas-liquid separator which relies entirely on external direct heat supply. The mixed salt treatment device of the invention can greatly reduce external energy consumption and continuously treat the mixed salt.
Preferably, the acid treatment unit comprises a static mixer, a concentrated sulfuric acid storage tank and a mixed salt solution storage tank, wherein a discharge port of the concentrated sulfuric acid storage tank and a discharge port of the mixed salt solution storage tank are respectively communicated with a feed port of the static mixer, and a discharge port of the static mixer is communicated with the first channel. The mixed salt solution in the mixed salt solution storage tank and the concentrated sulfuric acid in the concentrated sulfuric acid storage tank are subjected to exothermic reaction in the static mixer to generate a high-temperature acid-containing mixture, wherein the acid-containing mixture mainly comprises butyric acid, acetic acid, lactic acid and sodium sulfate.
Preferably, the centrifugal extraction unit comprises 1-x-stage centrifugal extractors, x is a positive integer greater than or equal to 3, the 2-x-stage centrifugal extractors are in countercurrent communication, the 1-stage centrifugal extractors are communicated with the first channel, the water phase outlets of the 1-stage centrifugal extractors are communicated with the 2-stage centrifugal extractors, the x-stage centrifugal extractors are communicated with the extractant tank, the water phase outlets of the x-stage centrifugal extractors are communicated with the stripping tower, and the oil phase outlets of the 1-stage centrifugal extractors and the oil phase outlets of the 2-stage centrifugal extractors are both communicated with the third channel. More specifically, the countercurrent communication is that the water phase outlet of the former-stage centrifugal extractor is communicated with the water phase inlet of the latter-stage centrifugal extractor, and the oil phase outlet of the latter-stage centrifugal extractor is communicated with the oil phase inlet of the former-stage centrifugal extractor. Centrifugal extractors are well known in the art and the construction of such centrifugal extractors is well known in the art.
Preferably, the fourth channel of the invention is also respectively communicated with the first extraction recovery tank and the first gas-liquid separator. After the high-temperature high-pressure liquid entering the fourth channel transfers heat to the third channel, one part of the high-temperature high-pressure liquid flows back to the first gas-liquid separator, and the other part of the high-temperature high-pressure liquid enters the first extraction recovery tank.
Preferably, a cooling device is further arranged between the centrifugal extraction unit and the first channel, and the cooling device is used for further cooling the acid-containing mixture flowing out of the first channel to normal temperature, so that the acid-containing mixture is subjected to normal temperature extraction in the centrifugal extraction unit, the extraction efficiency of normal temperature extraction is high, and the corrosion speed of the centrifugal extraction unit can be greatly reduced. Preferably, the rectification unit further comprises a second recovery system, a third recovery system and a fourth recovery system in sequence, wherein the second recovery system comprises a second gas-liquid separator and a second reboiler, the third recovery system comprises a third gas-liquid separator and a third reboiler, the fourth recovery system comprises a fourth gas-liquid separator and a fourth reboiler, the second gas-liquid separator is respectively communicated with the bottoms of the second reboiler and the first gas-liquid separator, the third gas-liquid separator is respectively communicated with the bottoms of the third reboiler and the second gas-liquid separator, and the fourth gas-liquid separator is respectively communicated with the bottoms of the fourth reboiler and the third gas-liquid separator. The mixture of the extracting agent, the butyric acid, the acetic acid and the like at the bottom of the first gas-liquid separator enters the second gas-liquid separator for separation so as to thoroughly recover the extracting agent, the mixture of the butyric acid, the acetic acid and the like at the bottom of the second gas-liquid separator enters the third gas-liquid separator for separation so as to recover the acetic acid, and the mixture of the butyric acid and the like at the bottom of the third gas-liquid separator enters the fourth gas-liquid separator for separation so as to recover the butyric acid.
Preferably, the second recovery system of the present invention further comprises a second extraction recovery tank and a first condenser, the third recovery system further comprises an acetic acid recovery tank and a second condenser, the fourth recovery system further comprises a butyric acid recovery tank and a third condenser, the second extraction recovery tank is communicated with the top of the second gas-liquid separator by the first condenser, the acetic acid recovery tank is communicated with the top of the third gas-liquid separator by the second condenser, and the butyric acid recovery tank is communicated with the top of the fourth gas-liquid separator by the third condenser.
Preferably, the bottom of the fourth gas-liquid separator is provided with a waste outlet, and residues at the bottom of the fourth gas-liquid separator are discharged to the incinerator from the waste outlet.
Preferably, the stripper bottoms of the present invention are in communication with an MVR evaporator. The aqueous phase flowing out of the centrifugal extraction unit comprises an extractant and sodium sulfate, the extractant is evaporated and separated from the top of the stripping tower, and sodium sulfate solution is discharged from the bottom of the stripping tower to an MVR evaporator for evaporation to recover sodium sulfate.
Preferably, the stripping column top of the invention comprises a third extraction recovery tank and a fourth condenser, and the third extraction recovery tank is communicated with the stripping column top by the fourth condenser. The aqueous phase flowing out of the centrifugal extraction unit comprises extractant and sodium sulfate, the aqueous phase is separated in a stripping tower, and the extractant is discharged from the top of the stripping tower to recover the extractant. In order to achieve the above object, the present invention further provides a method for treating mixed salt by the above mixed salt treatment apparatus, comprising the steps of:
(1) The mixed salt separated from the biological fermentation liquid enters an acid treatment unit to react with concentrated sulfuric acid to obtain a high-temperature acid-containing mixture;
(2) The acid-containing mixture after the step (1) enters a first channel for cooling, and the heat of the acid-containing mixture is transferred to a second channel;
(3) The extractant and the acid-containing mixture in the normal temperature state after the step (2) enter a centrifugal extraction unit for treatment to obtain a water phase substance and an oil phase substance;
(4) The water phase substance enters a stripping tower and flows into a second channel to be heated, and then the water phase substance is separated by the stripping tower to obtain an extractant and a sodium sulfate solution;
(5) The oil phase substance enters a third channel for preheating, then enters a first gas-liquid separator and flows into a fifth channel for heating, then the oil phase substance is separated by the first gas-liquid separator to obtain extractant steam, and the extractant steam enters a steam compressor from the top of the first gas-liquid separator for pressurizing to form high-temperature high-pressure gas;
(6) The high-temperature high-pressure gas enters a sixth channel to be condensed to obtain high-temperature high-pressure liquid, and the heat of the high-temperature high-pressure gas is transferred to a fifth channel;
(7) The high-temperature high-pressure liquid enters the fourth channel and transfers heat of the high-temperature liquid to the third channel.
Compared with the prior art, in the method for treating the mixed salt by the mixed salt treatment device, the reboiler of the stripping tower is adopted to recycle the reaction heat of the concentrated sulfuric acid and the mixed salt, so that the stripping tower does not completely depend on external heat supply, and the external energy consumption of the stripping tower can be reduced. Meanwhile, the steam compressor is adopted to pressurize the extractant steam separated from the top of the first gas-liquid separator to form high-temperature high-pressure gas, and the first reboiler is adopted to heat the first gas-liquid separator by using the condensation heat of the high-temperature high-pressure gas, so that the first gas-liquid separator can separate most of the extractant in the oil phase without depending on external energy; a heat exchanger is also employed to use the heat of the high temperature, high pressure liquid phase to preheat the oil phase effluent from the centrifugal extraction unit and partially gasify the extractant, which can further reduce the energy consumed by the first gas-liquid separator to separate the extractant. The method for treating mixed salt by the mixed salt treatment apparatus of the present invention has low external energy consumption and continuously treats the mixed salt.
Preferably, the temperature of the acid-containing mixture in step (1) of the present invention is >100 ℃; the pressure of the high-temperature high-pressure gas in the step (5) is 0.20-0.60 MPa, and the temperature is more than or equal to 100 ℃; the temperature of the high-temperature liquid in the step (6) is 100-160 ℃.
Preferably, the extractant of the present invention comprises at least one of ethyl acetate, propyl acetate, ethyl propionate, propyl propionate and butyl acetate. Preferably, the extractant of the present invention is ethyl acetate.
Drawings
Fig. 1 is a schematic structural view of a mixed salt treatment apparatus according to the present invention.
FIG. 2 is a schematic structural view of a mixed salt treatment apparatus used in comparative example 2.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to the appended drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The present invention may be embodied in many other forms than described herein and similarly modified by those skilled in the art without departing from the spirit of the invention, whereby the invention is not limited to the specific embodiments disclosed below.
In the description of the present invention, it should be understood that the terms "top" and "bottom" are used for convenience in describing the present invention and simplifying the description based on the orientation or positional relationship shown in the drawings, and do not indicate or imply that the apparatus or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," "fourth," "fifth," "sixth" are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or an implicit indication of the number of technical features indicated.
Referring to fig. 1, the mixed salt treatment apparatus 100 of the present invention includes an acid treatment unit 11, a stripping unit 12, a centrifugal extraction unit 13, and a rectification unit 14, which are sequentially connected; the acid treatment unit 11 is used for reacting concentrated sulfuric acid with mixed salt, the stripping unit 12 comprises a stripping tower 121 and a stripping tower reboiler 122, the stripping tower reboiler 122 comprises a first channel and a second channel which are isolated from each other, the first channel is respectively communicated with the acid treatment unit 11 and the centrifugal extraction unit 13, and the stripping tower 121 is respectively communicated with the second channel and the centrifugal extraction unit 13; the rectification unit 14 includes a first recovery system 141, the first recovery system 141 including a heat exchanger 1411, a first gas-liquid separator 1412, a vapor compressor 1413, a first reboiler 1414; the heat exchanger 1411 comprises a third channel and a fourth channel which are isolated from each other, the first reboiler 1414 comprises a fifth channel and a sixth channel which are isolated from each other, the third channel is respectively communicated with the centrifugal extraction unit 13 and the first gas-liquid separator 1412, the top of the first gas-liquid separator 1412 is communicated with the vapor compressor 1413, the bottom of the first gas-liquid separator 1412 is communicated with the fifth channel, and the sixth channel is respectively communicated with the vapor compressor 1413 and the fourth channel. According to the invention, the stripper reboiler 122 is arranged between the acid treatment unit 11 and the centrifugal extraction unit 13, the concentrated sulfuric acid and the mixed salt react to obtain a high-temperature acid-containing mixture, and when the acid-containing mixture flows out of the acid treatment unit 11 and flows through the first channel of the stripper reboiler 122, the heat of the acid-containing mixture can be transferred to the second channel to heat the stripper 121, so that the reaction heat of the concentrated sulfuric acid and the mixed salt is recycled by arranging the stripper reboiler 122, and the stripper 121 does not completely depend on external heat supply, so that the external energy consumption of the stripper 121 can be reduced. Meanwhile, the invention is also provided with a heat exchanger 1411, a vapor compressor 1413 and a first reboiler 1414, the vapor compressor 1413 is utilized to pressurize the extractant vapor separated from the top of the first gas-liquid separator 1412 to form high-temperature high-pressure gas, the high-temperature high-pressure gas enters a sixth channel of the first reboiler 1414 to be condensed to obtain high-temperature high-pressure liquid, and the heat of the high-temperature high-pressure gas is transferred to a fifth channel of the first reboiler 1414 to recycle part of the heat of the high-temperature high-pressure gas so as to heat the first gas-liquid separator 1412, so that the first gas-liquid separator 1412 can separate oil phase matters without consuming external energy; in addition, the high-temperature and high-pressure liquid flows into the fourth channel of the heat exchanger 1411 and transfers heat of the high-temperature and high-pressure liquid to the third channel, so that the oil phase matters flowing out of the centrifugal extraction unit 13 can be preheated and the extractant can be partially gasified, which can further reduce the energy consumed by the first gas-liquid separator 1412 for separating the oil phase matters. In addition, the cost of the vapor compressor 1413 is much lower than the cost of the first gas-liquid separator 1412 entirely relying on external direct heat supply. The mixed salt treatment apparatus 100 of the present invention can greatly reduce external power consumption and continuously treat mixed salt.
Specifically, stripper reboiler 122, heat exchanger 1411, and first reboiler 1414 configurations and heat transfer principles are well known in the art, such as a first or fourth or sixth channel being a flow-through for providing a heat exchange medium, and a second or third or fifth channel being a flow-through for providing a substance to be heat exchanged, e.g., the medium in the first channel is a high temperature acid-containing mixture, and the medium in the second channel is an aqueous phase exiting centrifugal extraction unit 13; therefore, the specific structures of the first channel, the second channel, the third channel, the fourth channel, the fifth channel and the sixth channel and the corresponding heat transfer principles are not described herein.
With continued reference to fig. 1, the acid treatment unit 11 of the present invention includes a static mixer 111, a concentrated sulfuric acid storage tank 112, and a mixed salt solution storage tank 113, wherein a discharge port of the concentrated sulfuric acid storage tank 112 and a discharge port of the mixed salt solution storage tank 113 are respectively communicated with a feed port of the static mixer 111, and a discharge port of the static mixer 111 is communicated with the first channel. The mixed salt solution in the mixed salt solution storage tank 113 and the concentrated sulfuric acid in the concentrated sulfuric acid storage tank 112 react exothermically in the static mixer 111 to produce a high temperature acid-containing mixture, which mainly includes butyric acid, acetic acid, lactic acid and sodium sulfate. More specifically, a cooling device 15 is further disposed between the centrifugal extraction unit 13 and the first channel, and the cooling device 15 is used for further cooling the acid-containing mixture flowing out of the first channel to normal temperature, so that the acid-containing mixture is extracted in the centrifugal extraction unit 13 at normal temperature, the extraction efficiency of normal temperature extraction is high, and the corrosion speed of the centrifugal extraction unit 13 can be greatly reduced.
With continued reference to fig. 1, the centrifugal extraction unit 13 of the present invention includes 1 to x stages of centrifugal extractors 131, x is a positive integer greater than or equal to 3, the specific structure of the centrifugal extractors 131 is known in the art, the 2 to x stages of centrifugal extractors 131 are in countercurrent communication, the 1 stage of centrifugal extractors 131 are in communication with the first channel, the aqueous phase outlet of the 1 stage of centrifugal extractors 131 is in communication with the 2 stage of centrifugal extractors 131, the x stage of centrifugal extractors 131 are in communication with the extractant tank 132, the aqueous phase outlet of the x stage of centrifugal extractors 131 is in communication with the stripper 121, and the oil phase outlet of the 1 stage of centrifugal extractors 131 and the oil phase outlet of the 2 stage of centrifugal extractors 131 are both in communication with the third channel. More specifically, the countercurrent communication is that the water phase outlet of the former-stage centrifugal extractor 131 is communicated with the water phase inlet of the latter-stage centrifugal extractor 131, and the oil phase outlet of the latter-stage centrifugal extractor 131 is communicated with the oil phase inlet of the former-stage centrifugal extractor 131. The acid-containing mixture flowing out of the first channel enters the 1-stage centrifugal extractor 131 to separate lighter oil phase matters and heavier water phase matters, the heavier water phase matters enter the 2-stage centrifugal extractor 131, the extractant enters the x-stage centrifugal extractor 131, and the water phase matters are in countercurrent contact with the extractant, so that butyric acid and acetic acid in the water phase flowing out of the 1-stage centrifugal extractor 131 are completely extracted.
With continued reference to FIG. 1, the fourth channel of the present invention is also in communication with the first extraction recovery tank 1414 and the first gas-liquid separator 1412, respectively. After the high temperature and high pressure liquid entering the fourth channel transfers heat to the third channel, a part of the liquid flows back to the first gas-liquid separator 1412, and the other part enters the first extraction recovery tank 1414.
With continued reference to fig. 1, the rectification unit 14 of the present invention further includes a second recovery system 142, a third recovery system 143, and a fourth recovery system 144 in sequence, where the second recovery system 142 includes a second gas-liquid separator 1421 and a second reboiler 1422, the third recovery system 143 includes a third gas-liquid separator 1431 and a third reboiler 1432, the fourth recovery system 144 includes a fourth gas-liquid separator 1441 and a fourth reboiler 1442, the second gas-liquid separator 1421 is respectively communicated with the bottoms of the second reboiler 1422 and the first gas-liquid separator 1412, the third gas-liquid separator 1431 is respectively communicated with the bottoms of the third reboiler 1432 and the second gas-liquid separator 1421, and the fourth gas-liquid separator 1441 is respectively communicated with the bottoms of the fourth reboiler 1442 and the third gas-liquid separator 1431. The mixture of the extractant, the butyric acid, the acetic acid, etc. at the bottom of the first gas-liquid separator 1412 enters the second gas-liquid separator 1421 to be separated to thoroughly recover the extractant, the mixture of the butyric acid, the acetic acid, etc. at the bottom of the second gas-liquid separator 1421 enters the third gas-liquid separator 1431 to be separated to recover the acetic acid, and the mixture of the butyric acid, etc. at the bottom of the third gas-liquid separator 1431 enters the fourth gas-liquid separator 1441 to be separated to recover the butyric acid. More specifically, the second recovery system 142 of the present invention further includes a second extraction recovery tank 1423 and a first condenser 1424, the third recovery system 143 further includes an acetic acid recovery tank 1433 and a second condenser 1434, the fourth recovery system 144 further includes a butyric acid recovery tank 1443 and a third condenser 1444, the second extraction recovery tank 1423 is in communication with the top of the second gas-liquid separator 1421 via the first condenser 1424, the acetic acid recovery tank 1433 is in communication with the top of the third gas-liquid separator 1431 via the second condenser 1434, and the butyric acid recovery tank 1443 is in communication with the top of the fourth gas-liquid separator 1441 via the third condenser 1444. The bottom of the fourth gas-liquid separator 1441 is provided with a waste outlet 1445, and the residue at the bottom of the fourth gas-liquid separator 1441 is discharged from the waste outlet 1445 to the incinerator. Specifically, the structures of the first gas-liquid separator 1412, the second gas-liquid separator 1421, the third gas-liquid separator 1431, and the fourth gas-liquid separator 1441 are well known in the art, and will not be described herein.
With continued reference to fig. 1, the bottom of the stripping column 121 of the present invention is in communication with an MVR evaporator 123. The aqueous phase flowing out of the centrifugal extraction unit 13 comprises an extractant and sodium sulfate, the extractant is evaporated and separated from the top of the stripping tower 121, and sodium sulfate solution is discharged from the bottom of the stripping tower 121 to the MVR evaporator 123 for evaporation to recover sodium sulfate. Preferably, the top of the stripping column 121 of the present invention comprises a third extraction recovery tank 124 and a fourth condenser 125, the third extraction recovery tank 124 being in communication with the top of the stripping column 121 via the fourth condenser 125.
In addition, the invention also provides a method for processing mixed salt by the mixed salt processing device 100, which comprises the following steps:
(1) The mixed salt separated from the biological fermentation liquid enters an acid treatment unit 11 to react with concentrated sulfuric acid to obtain a high-temperature acid-containing mixture;
(2) The acid-containing mixture after the step (1) enters a first channel for cooling, and the heat of the acid-containing mixture is transferred to a second channel;
(3) The extractant and the mixture containing acid in the normal temperature state after the step (2) enter a centrifugal extraction unit 13 for treatment to obtain a water phase substance and an oil phase substance;
(4) The water phase substance enters a stripping tower 121 and flows into a second channel to be heated, and then the water phase substance is separated by the stripping tower 121 to obtain an extractant and a sodium sulfate solution;
(5) The oil phase substance enters a third channel for preheating, then enters a first gas-liquid separator 1412 and flows into a fifth channel for heating, then is separated by the first gas-liquid separator 1412 to obtain extractant steam, and the extractant steam enters a steam compressor 1413 from the top of the first gas-liquid separator 1412 for pressurizing to form high-temperature high-pressure gas;
(6) The high-temperature high-pressure gas enters a sixth channel to be condensed to obtain high-temperature high-pressure liquid, and the heat of the high-temperature high-pressure gas is transferred to a fifth channel;
(7) The high-temperature high-pressure liquid enters the fourth channel and transfers heat of the high-temperature liquid to the third channel.
Specifically, the mixed salt separated from the biological fermentation liquid needs to be preheated to 100 ℃ or above, namely, the temperature of the mixed salt before the acidification reaction is 100 ℃ or above, so that the reaction heat of the concentrated sulfuric acid and the mixed salt can be more effectively recycled.
Specifically, the mass fractions of acetate and butyrate in the mixed salt are respectively 10-50%, 20-60% and 80-99% respectively.
Specifically, the flow rate of the mixed salt is 0.9-1.1 t/h, the flow rate of the concentrated sulfuric acid is 0.4-0.8 t/h, and the flow rate of the ethyl acetate is 3-6 t/h.
Specifically, the temperature of the acid-containing mixture in step (1) of the present invention is >100 ℃, more specifically, the temperature of the acid-containing mixture is >150 ℃.
Specifically, heat of the acid-containing mixture in the step (2) is transferred to the second channel so that the aqueous phase substance flowing into the second channel is maintained at 90-120 ℃. Specifically, the water phase in the step (4) enters the stripping tower 121 and flows into the second channel to be heated to 90-120 ℃ (steam with the steam flow rate of 0-1 t/h and the steam flow rate of 0-1 Mpa is also required to be externally supplied).
Specifically, the oil phase material in the step (5) enters a third channel for preheating to 65-95 ℃; the pressure of the high-temperature high-pressure gas is 0.20-0.60 MPa, and the temperature is more than or equal to 100 ℃.
Specifically, the heat of the high-temperature and high-pressure gas in the step (6) is transferred to the fifth channel so that the oil phase matters flowing into the fifth channel are heated to 90-120 ℃.
Specifically, the high-temperature high-pressure liquid in the step (7) enters the fourth channel and transfers the heat of the high-temperature liquid to the third channel so that the oil phase substance is preheated to 65-95 ℃.
In order to describe the mixed salt treatment apparatus 100 and method of the present invention in more detail, specific examples will be described below.
Example 1
The present embodiment provides a method for processing mixed salt by using the mixed salt processing apparatus 100 shown in fig. 1, including the steps of:
(1) Preheating a mixed salt solution obtained by separation from a biological fermentation liquid to 101 ℃, and then carrying out exothermic reaction on the mixed salt solution and concentrated sulfuric acid in a static mixer 111 to obtain an acid-containing mixture with the temperature of 160 ℃, wherein the flow rate of the mixed salt is 1t/h, the flow rate of the concentrated sulfuric acid is 0.55t/h, the mass fractions of acetate and butyrate in the mixed salt are respectively 20% and 30%, and the mass fraction of the concentrated sulfuric acid is 98%;
(2) The acid-containing mixture after the step (1) enters a first channel for cooling, and the heat of the acid-containing mixture is transferred to a second channel so that the water phase matters flowing into the second channel are kept at 100 ℃;
(3) Ethyl acetate and the acid-containing mixture in the normal temperature state after the step (2) enter a 1-3-stage centrifugal extractor 131 to obtain a water phase substance and an oil phase substance, wherein the flow rate of the ethyl acetate is 3.6t/h;
(4) The water phase enters a stripping tower 121 and flows into a second channel to be heated to 105 ℃ (0.1 t/h of 0.3Mpa steam is also required to be supplied externally), and then ethyl acetate and sodium sulfate solution are obtained through separation of the stripping tower 121;
(5) The oil phase substance enters a third channel to be preheated to 80 ℃, then enters a first gas-liquid separator 1412 and flows into a fifth channel to be heated to 100 ℃, then ethyl acetate steam is obtained through separation of the first gas-liquid separator 1412, and the ethyl acetate steam enters a steam compressor 1413 from the top of the first gas-liquid separator 1412 to be pressurized to form high-temperature and high-pressure gas with the pressure of 0.3MPa and 130 ℃;
(6) The high-temperature high-pressure gas enters a sixth channel to be condensed to obtain high-temperature high-pressure liquid, and the heat of the high-temperature high-pressure gas is transferred to a fifth channel to heat the oil phase matters flowing into the fifth channel to 100 ℃;
(7) The high-temperature high-pressure liquid enters a fourth channel and transfers heat of the high-temperature liquid to a third channel so that the oil phase is preheated to 80 ℃;
comparative example 1
The present comparative example provides a method of treating mixed salt using the mixed salt treating apparatus 100' shown in fig. 2, comprising the steps of:
(1) Preheating a mixed salt solution obtained by separation from a biological fermentation liquid to 101 ℃, and then reacting the mixed salt solution with concentrated sulfuric acid in a static mixer 111' to obtain an acid-containing mixture with the temperature of 160 ℃, wherein the flow rate of the mixed salt is 1t/h, the flow rate of the concentrated sulfuric acid is 0.55t/h, the mass fractions of acetate and butyrate in the mixed salt are respectively 20% and 30%, and the mass fraction of the concentrated sulfuric acid is 98%;
(2) Ethyl acetate and the acid-containing mixture in the normal temperature state after the step (1) enter a 1-3-stage centrifugal extractor 131' to obtain a water phase substance and an oil phase substance, wherein the flow rate of the ethyl acetate is 3.6t/h;
(4) The water phase enters a stripping tower 121 'and flows into a second channel to be heated to 105 ℃ (0.6 t/h of 0.3Mpa steam is required to be supplied externally), and then ethyl acetate and sodium sulfate solution are obtained through separation of the stripping tower 121';
(5) The oil phase enters the first gas-liquid separator 1412 'and flows into the fifth channel to be heated to 100 ℃ (0.3 Mpa steam is required to be supplied for 1.5 t/h), and then ethyl acetate steam is obtained through separation of the first gas-liquid separator 1412'.
The mixed salt treatment apparatus 100' of the present comparative example is shown in fig. 2, which is substantially the same as the mixed salt treatment apparatus 100 in fig. 1, except that the heat exchanger 1411 and the vapor compressor 1413 in fig. 1 are removed, and the acid treatment unit 11 is directly communicated with the cooling apparatus 15, i.e., the centrifugal extraction unit 13' in fig. 2 is directly communicated with the first gas-liquid separator 1412', and the acid treatment unit 11' is directly communicated with the cooling apparatus 15 '.
Comparing example 1 with comparative example 1, it can be seen that the first gas-liquid separator 1412 'of comparative example 1 requires 0.3MPa saturated steam 1.5t/h, the stripping column 121' requires 0.3MPa saturated steam 0.6t/h, and the first gas-liquid separator 1412 of example 1 requires 0.3MPa saturated steam 0t/h, the stripping column requires 0.3MPa saturated steam 0.1t/h, and the vapor compression shaft power is about 100KW, whereby it can be seen that 2 tons of steam per hour can be saved with the mixed salt treatment apparatus 100 of the present invention.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. The mixed salt treatment device is characterized by comprising an acid treatment unit, a stripping unit, a centrifugal extraction unit and a rectification unit which are sequentially communicated;
the acid treatment unit is used for reacting concentrated sulfuric acid with mixed salt;
the stripping unit comprises a stripping tower and a stripping tower reboiler, the stripping tower reboiler comprises a first channel and a second channel which are isolated from each other, the first channel is respectively communicated with the acid treatment unit and the centrifugal extraction unit, and the stripping tower is respectively communicated with the second channel and the centrifugal extraction unit;
the rectification unit comprises a first recovery system, wherein the first recovery system comprises a heat exchanger, a first gas-liquid separator, a vapor compressor and a first reboiler; the heat exchanger comprises a third channel and a fourth channel which are isolated from each other, the first reboiler comprises a fifth channel and a sixth channel which are isolated from each other, the third channel is respectively communicated with the centrifugal extraction unit and the first gas-liquid separator, the top of the first gas-liquid separator is communicated with the vapor compressor, the bottom of the first gas-liquid separator is communicated with the fifth channel, and the sixth channel is respectively communicated with the vapor compressor and the fourth channel.
2. The mixed salt treatment apparatus of claim 1, wherein the acid treatment unit comprises a static mixer, a concentrated sulfuric acid storage tank, and a mixed salt solution storage tank, wherein a discharge port of the concentrated sulfuric acid storage tank and a discharge port of the mixed salt solution storage tank are respectively communicated with a feed port of the static mixer, and a discharge port of the static mixer is communicated with the first channel.
3. The mixed salt treatment apparatus of claim 1, wherein the centrifugal extraction unit comprises 1 to x stages of centrifugal extractors, x is a positive integer greater than or equal to 3, the 2 to x stages of centrifugal extractors are in countercurrent communication, the 1 stage of centrifugal extractors are in communication with the first channel, the 1 stage of centrifugal extractors water phase outlets are in communication with the 2 stage of centrifugal extractors, the x stage of centrifugal extractors are in communication with an extractant tank, the x stage of centrifugal extractors water phase outlets are in communication with the stripper, and the 1 stage of centrifugal extractors oil phase outlets and the 2 stage of centrifugal extractors oil phase outlets are both in communication with the third channel.
4. The mixed salt processing apparatus of claim 1, wherein the fourth passage is further in communication with a first extraction recovery tank and the first gas-liquid separator, respectively.
5. The mixed salt treatment apparatus according to claim 1, wherein the rectification unit further comprises a second recovery system, a third recovery system and a fourth recovery system in this order, the second recovery system comprises a second gas-liquid separator and a second reboiler, the third recovery system comprises a third gas-liquid separator and a third reboiler, the fourth recovery system comprises a fourth gas-liquid separator and a fourth reboiler, the second gas-liquid separator is respectively communicated with the second reboiler and the bottom of the first gas-liquid separator, the third gas-liquid separator is respectively communicated with the third reboiler and the bottom of the second gas-liquid separator, and the fourth gas-liquid separator is respectively communicated with the fourth reboiler and the bottom of the third gas-liquid separator.
6. The mixed salt processing apparatus according to claim 5, wherein the second recovery system further comprises a second extraction recovery tank and a first condenser, the third recovery system further comprises an acetic acid recovery tank and a second condenser, the fourth recovery system further comprises a butyric acid recovery tank and a third condenser, the second extraction recovery tank is in communication with the second vapor-liquid separator top via the first condenser, the acetic acid recovery tank is in communication with the third vapor-liquid separator top via the second condenser, and the butyric acid recovery tank is in communication with the fourth vapor-liquid separator top via the third condenser.
7. The mixed salt treatment apparatus of claim 1, wherein the stripper bottoms are in communication with an MVR evaporator.
8. A method of treating a mixed salt in a mixed salt treating apparatus as claimed in any one of claims 1 to 7, comprising the steps of:
(1) The mixed salt obtained by separation from the biological fermentation liquid enters the acid treatment unit to react with concentrated sulfuric acid to obtain a high-temperature acid-containing mixture;
(2) The acid-containing mixture after the step (1) enters the first channel for cooling and the heat of the acid-containing mixture is transferred to the second channel;
(3) The extractant and the acid-containing mixture in the normal temperature state after the step (2) enter the centrifugal extraction unit for treatment to obtain a water phase substance and an oil phase substance;
(4) The water phase substance enters the stripping tower and flows into the second channel to be heated, and then the water phase substance is separated by the stripping tower to obtain an extractant and a sodium sulfate solution;
(5) The oil phase substance enters the third channel for preheating, then enters the first gas-liquid separator and flows into the fifth channel for heating, and then is separated by the first gas-liquid separator to obtain extractant steam, and the extractant steam enters the steam compressor from the top of the first gas-liquid separator for pressurizing to form high-temperature high-pressure gas;
(6) The high-temperature high-pressure gas enters the sixth channel to be condensed to obtain high-temperature high-pressure liquid, and the heat of the high-temperature high-pressure gas is transferred to the fifth channel;
(7) The high-temperature high-pressure liquid enters the fourth channel and transfers heat of the high-temperature liquid to the third channel.
9. The method of treating mixed salt in a mixed salt treating apparatus according to claim 8, wherein the temperature of the acid-containing mixture in step (1) is >100 ℃; the pressure of the high-temperature high-pressure gas in the step (5) is 0.20-0.60 MPa, and the temperature is more than or equal to 100 ℃; the temperature of the high-temperature liquid in the step (6) is 100-160 ℃.
10. The method of treating a mixed salt with a mixed salt treating apparatus according to claim 8, wherein the extractant includes at least one of ethyl acetate, propyl acetate, ethyl propionate, propyl propionate, and butyl acetate.
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