CN107522640B - Method and device for recycling organic matters in dimethyl sulfoxide waste salt - Google Patents
Method and device for recycling organic matters in dimethyl sulfoxide waste salt Download PDFInfo
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- CN107522640B CN107522640B CN201710885771.7A CN201710885771A CN107522640B CN 107522640 B CN107522640 B CN 107522640B CN 201710885771 A CN201710885771 A CN 201710885771A CN 107522640 B CN107522640 B CN 107522640B
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- dimethyl sulfoxide
- waste salt
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- drying device
- bed drying
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/06—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/02—Preparation of sulfones; Preparation of sulfoxides by formation of sulfone or sulfoxide groups by oxidation of sulfides, or by formation of sulfone groups by oxidation of sulfoxides
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Abstract
The invention relates to a method for recycling organic matters in dimethyl sulfoxide waste salt, which specifically uses the physicochemical properties of the organic matters, directly heats and boils the waste salt by hot air at 80-120 ℃, and after the hot air is subjected to cyclone separation, the hot air is used for recycling dimethyl sulfone and dimethyl sulfoxide in gas by a water washing device, and after an absorption liquid reaches a certain concentration, the dimethyl sulfone is separated by cooling crystallization, and mother liquid can be absorbed in a two-cycle way. Meanwhile, a small amount of sodium nitrite in the waste salt can be oxidized into sodium nitrate under the action of hot air, so that the sodium sulfonate can be further recycled. The invention has the advantages of short process flow, no other chemical reactions, low energy consumption, no wastewater discharge, environmental protection and the like. The method recovers organic matters in the waste salt: dimethyl sulfoxide and dimethyl sulfone. The proportion of the sulfoxide in the salt waste is 25-35%, so that the production cost of the sulfoxide is reduced by 1-3%, and the economic benefit is quite considerable. And is favorable for recycling inorganic matters (sodium nitrate and sodium mesylate) of waste salt, so as to ensure that solid waste produced by dimethyl sulfoxide can be effectively treated.
Description
Technical Field
The dimethyl sulfoxide waste salt is solid waste generated by neutralizing nitrogen dioxide and nitric acid in dimethyl sulfoxide with sodium hydroxide in the process of producing dimethyl sulfoxide, and comprises the following components: sodium nitrate: 40-45%, sodium methylsulfonate: 20-25%, dimethyl sulfone: 12-16%, dimethyl sulfoxide: 1.5-5%, sodium sub-sales: 0.8-1.5%, moisture: 8-12%. The invention is used for recycling the dimethyl sulfone and the dimethyl sulfoxide in the dimethyl sulfoxide waste salt, and removing sodium nitrite and water in the dimethyl sulfoxide waste salt.
Background
In the existing technology for recovering dimethyl sulfoxide waste salt, as in the two patent application numbers 201220355966.3 and 201410467409.4 of China, methods such as evaporation, concentration, centrifugal separation, recrystallization and the like are adopted, so that the technology is complex and the energy consumption is high. The recrystallization method cannot completely separate the organic matters.
Disclosure of Invention
According to the components and material characteristics of the dimethyl sulfoxide waste salt, heating air to 80-120 ℃ by a hot blast stove, sending into a fluidized bed drying device or a boiling drying device, crushing into particles after the temperature in the drying device reaches more than 80 ℃, and sending the dimethyl sulfoxide waste salt into drying equipment, so as to keep the dimethyl sulfoxide waste salt in a boiling state in the drying process. Hot air enters a water absorption device after passing through a cyclone separator with the temperature of more than 80 ℃ and is washed by water to recover dimethyl sulfone and dimethyl sulfoxide. The concentration of the dimethyl sulfone in the absorption liquid is continuously increased, the dimethyl sulfone product can be obtained through extraction, cooling, crystallization and centrifugal separation, and the mother liquid returns to the water absorption device for recycling. When the dimethyl sulfoxide content in the absorption liquid reaches 30%, the mother liquid is dehydrated and concentrated to more than 95% in a negative pressure state, and then the dimethyl sulfone can be obtained by oxidizing with hydrogen peroxide. The treated waste salt is light white or white yellowish dry small particles, and the main components are sodium nitrate and sodium methylsulfonate, which are favorable for further separation and utilization.
The invention also provides a device for recycling the organic matters in the dimethyl sulfoxide waste salt, which is characterized in that a dimethyl sulfoxide waste salt conveyer belt is connected with a heater through spiral discharging, and a conveying pipe of the heater is connected with the lower part of a fluidized bed drying device;
the refrigerating fluid is connected with the lower part of the fluidized bed drying device through a delivery pipe and is opposite to the delivery pipe of the heater I;
the top of the fluidized bed drying device is connected with the cyclone separator through a material conveying pipe;
the cyclone top is connected to a water absorbing device.
The air filter is connected with the bottom of the fluidized bed drying device through the heater II; the second air filter is connected with the bottom of the fluidized bed drying device through an air cooler.
The conveying pipe of the first heater is connected to the inside of the fluidized bed drying device and is arranged above the fluidized bed drying device by 0.5-0.8m after the air filter enters the fluidized bed drying device through the second heater.
The refrigerating fluid conveying pipe is connected to the inside of the fluidized bed drying device and is arranged above the fluidized bed drying device by 1.0-1.5m through the air cooler.
According to the technical scheme, by utilizing the characteristic of dimethyl sulfone thermal sublimation, the dimethyl sulfoxide waste salt is heated by hot air, so that the dimethyl sulfone is heated and rises to be in a gaseous state, and the dimethyl sulfone enters a water absorption device along with the hot air to be recycled.
According to the technical scheme, the dimethyl sulfoxide is heated by hot air by utilizing the principle of thermal diffusion of dimethyl sulfoxide in gas, and dimethyl sulfoxide is heated and diffused into hot air and then enters a water absorption device for recycling.
The technical scheme of the invention utilizes the instability of sodium nitrite in air, and hot air is used for accelerating the oxidation of sodium nitrite into sodium nitrate.
Drawings
Fig. 1 is a flow chart of the apparatus of the present invention.
Wherein, 1 is a waste salt conveying belt; 2. the device comprises a heater, an air filter I, a heater, an air filter II, an air cooler 6, a fluidized bed drying device 7, refrigerating fluid 8, a cyclone separator 9, a recovery device I and a recovery device II.
Detailed Description
Example 1
A method for recycling organic matters in dimethyl sulfoxide waste salt comprises the steps of heating air to 80-120 ℃ by a hot blast stove, sending the air into a fluidized bed drying device or a boiling drying device, sending granular dimethyl sulfoxide waste salt crushed into 40 meshes into drying equipment after the temperature in the drying device reaches 90 ℃, and keeping the dimethyl sulfoxide waste salt in a boiling state in the drying process;
hot air enters a water absorption device after passing through a cyclone separator which is insulated at 90 ℃, dimethyl sulfone is heated to be gaseous, enters the water absorption device along with the hot air, is washed to recover dimethyl sulfone and dimethyl sulfoxide, the concentration of the dimethyl sulfone in absorption liquid is continuously increased, a dimethyl sulfone product can be obtained through extraction, cooling, crystallization and centrifugal separation, and mother liquor returns to the water absorption device for recycling;
the instability of sodium nitrite in air is utilized, and hot air is used for accelerating the oxidation of sodium nitrite into sodium nitrate.
When the dimethyl sulfoxide content in the absorption liquid reaches 30%, the mother liquid is dehydrated and concentrated to more than 95% in a negative pressure (-70 Kpa) state, and then the dimethyl sulfone is obtained by oxidizing with hydrogen peroxide, wherein the purity of the dimethyl sulfone is 99.5%.
The dimethyl sulfoxide waste salt is solid waste generated by neutralizing nitrogen dioxide and nitric acid in dimethyl sulfoxide with sodium hydroxide in the process of producing dimethyl sulfoxide, and comprises the following components: sodium nitrate: 45% sodium methylsulfonate: 23%, dimethyl sulfone: 14%, dimethyl sulfoxide: 2.2%, sodium nitrite: 1.8 percent of water: 10%.
Example 2
The device for recycling organic matters in dimethyl sulfoxide waste salt is characterized in that a dimethyl sulfoxide waste salt conveyer belt 1 is connected with a heater I2 through spiral discharging, and a conveying pipe of the heater I2 is connected with the lower part of a fluidized bed drying device 7;
the refrigerating fluid 8 is connected with the lower part of the fluidized bed drying device 7 through a delivery pipe and is opposite to the delivery pipe of the heater I2;
the top of the fluidized bed drying device 7 is connected with a cyclone separator 9 through a material conveying pipe;
the top of the cyclone 9 is connected to a water absorbing device.
The first air filter 3 is connected with the bottom of the fluidized bed drying device 7 through the second heater 4; the second air filter 5 is connected with the bottom of the fluidized bed drying device 7 through an air cooler 6.
The conveying pipe of the first heater 2 is connected to the inside of the fluidized bed drying device 7, and is arranged above the fluidized bed drying device 7 by 0.8m when the first air filter 3 enters the fluidized bed drying device 7 through the second heater 4.
The delivery pipe of the refrigerating fluid 8 is connected to the inside of the fluidized bed drying device 7 and is arranged above the fluidized bed drying device 7 by 1.5m through the air cooler 6 by the air filter II 5.
Claims (7)
1. A method for recycling organic matters in dimethyl sulfoxide waste salt is characterized in that,
heating air to 80-120deg.C with hot blast furnace, feeding into fluidized bed drying device, and feeding into drying equipment after the temperature in the drying device reaches above 80deg.C, to keep dimethyl sulfoxide salt in boiling state during drying;
hot air enters a water absorption device after passing through a cyclone separator with the temperature of more than 80 ℃, dimethyl sulfone and dimethyl sulfoxide are recovered by washing, the concentration of the dimethyl sulfone in absorption liquid is continuously increased, a dimethyl sulfone product can be obtained by extracting, cooling, crystallizing and centrifugally separating, and mother liquor returns to the water absorption device for recycling;
when the dimethyl sulfoxide content in the absorption liquid reaches 30%, the mother liquid is dehydrated and concentrated to more than 95% in a negative pressure-70 Kpa state, and then the dimethyl sulfone can be obtained by oxidizing with hydrogen peroxide.
2. The method for recycling organic matters in dimethyl sulfoxide waste salt according to claim 1, wherein the negative pressure state is-70 Kpa to-80 Kpa.
3. The method for recycling organic matters in dimethyl sulfoxide waste salt according to claim 1, wherein the dimethyl sulfoxide waste salt is solid waste generated by neutralizing nitrogen dioxide and nitric acid in dimethyl sulfoxide with sodium hydroxide in the process of producing dimethyl sulfoxide, and comprises the following steps: sodium nitrate: 40-48%, sodium methylsulfonate: 20-25%, dimethyl sulfone: 12-16%, dimethyl sulfoxide: 1.5-5%, sodium sub-sales: 0.8-2%, moisture: 8-12%.
4. A method for recycling organic matters in dimethyl sulfoxide waste salt according to any one of claims 1-3, characterized in that the device used in the method is that a dimethyl sulfoxide waste salt conveyer belt (1) is connected with a first heater (2) through spiral discharging, and a conveying pipe of the first heater (2) is connected with the lower part of a fluidized bed drying device (7);
the refrigerating fluid (8) is connected with the lower part of the fluidized bed drying device (7) through a delivery pipe and is opposite to the delivery pipe of the heater I (2);
the top of the fluidized bed drying device (7) is connected with a cyclone separator (9) through a material conveying pipe;
the top of the cyclone separator (9) is connected to the water absorbing device.
5. The method for recycling organic matters in dimethyl sulfoxide waste salt according to claim 4, wherein the first air filter (3) is connected with the bottom of the fluidized bed drying device (7) through the second heater (4); the second air filter (5) is connected with the bottom of the fluidized bed drying device (7) through an air cooler (6).
6. The method for recycling organic matters in dimethyl sulfoxide waste salt according to claim 5, wherein the conveying pipe of the first heater (2) is connected to the inside of the fluidized bed drying device (7) and is arranged above the fluidized bed drying device (7) by 0.5-0.8m after the first air filter (3) enters the fluidized bed drying device (7) through the second heater (4).
7. The method for recycling organic matters in dimethyl sulfoxide waste salt according to claim 5, wherein a conveying pipe of the refrigerating fluid (8) is connected to the inside of the fluidized bed drying device (7) and is arranged in the air filter II (5) and enters the upper part 1.0-1.5m of the fluidized bed drying device (7) through the air cooler (6).
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| CN201710885771.7A CN107522640B (en) | 2017-09-27 | 2017-09-27 | Method and device for recycling organic matters in dimethyl sulfoxide waste salt |
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| CN107522640B true CN107522640B (en) | 2023-05-02 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101195595A (en) * | 2007-12-12 | 2008-06-11 | 湖北兴发化工集团股份有限公司 | Method for recycling dimethyl sulfone and sodium nitrate from dimethyl sulfoxide waste slag |
| CN201209123Y (en) * | 2008-04-15 | 2009-03-18 | 河南未来铝业（集团）有限公司 | Dry method aluminun fluoride production apparatus |
| CN202116466U (en) * | 2011-02-23 | 2012-01-18 | 常熟振氟新材料有限公司 | Device for drying and recycling hexachloroethane |
| CN102600625A (en) * | 2012-03-23 | 2012-07-25 | 南京龙源环保有限公司 | Process for removing chloride ions by combing with ammonium sulfate drying system |
| CN103408331A (en) * | 2013-07-08 | 2013-11-27 | 河南晋开化工投资控股集团有限责任公司 | Dust-free urea cooling method |
| CN104592067A (en) * | 2015-01-30 | 2015-05-06 | 湖北大学 | Method for recycling dimethyl sulfoxide waste residue through multi-stage extraction |
-
2017
- 2017-09-27 CN CN201710885771.7A patent/CN107522640B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101195595A (en) * | 2007-12-12 | 2008-06-11 | 湖北兴发化工集团股份有限公司 | Method for recycling dimethyl sulfone and sodium nitrate from dimethyl sulfoxide waste slag |
| CN201209123Y (en) * | 2008-04-15 | 2009-03-18 | 河南未来铝业（集团）有限公司 | Dry method aluminun fluoride production apparatus |
| CN202116466U (en) * | 2011-02-23 | 2012-01-18 | 常熟振氟新材料有限公司 | Device for drying and recycling hexachloroethane |
| CN102600625A (en) * | 2012-03-23 | 2012-07-25 | 南京龙源环保有限公司 | Process for removing chloride ions by combing with ammonium sulfate drying system |
| CN103408331A (en) * | 2013-07-08 | 2013-11-27 | 河南晋开化工投资控股集团有限责任公司 | Dust-free urea cooling method |
| CN104592067A (en) * | 2015-01-30 | 2015-05-06 | 湖北大学 | Method for recycling dimethyl sulfoxide waste residue through multi-stage extraction |
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