CN214570733U - Recovery unit of carbon oxysulfide in integrated chlorination technology tail gas - Google Patents
Recovery unit of carbon oxysulfide in integrated chlorination technology tail gas Download PDFInfo
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- CN214570733U CN214570733U CN202023053760.9U CN202023053760U CN214570733U CN 214570733 U CN214570733 U CN 214570733U CN 202023053760 U CN202023053760 U CN 202023053760U CN 214570733 U CN214570733 U CN 214570733U
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Abstract
The utility model discloses a recovery unit of carbonyl sulfide in integrated chlorination technology tail gas belongs to tail gas recycle technical field. The device comprises an organic solvent recovery module, a low-temperature rectification module and a byproduct cache module, wherein the organic solvent recovery module comprises a tail gas compressor, a first-stage condenser, a first-stage gas-liquid separator, a second-stage condenser and a second-stage gas-liquid separator; byproduct buffer module includes carbon oxysulfide product buffer tank and carbon oxysulfide filling pump, and carbon oxysulfide product buffer tank passes through the pipe connection with low temperature rectifying column. The utility model discloses reduced the raw materials use amount, reduced the three wastes and discharged, improved the utilization ratio of raw materials, economic nature is good.
Description
Technical Field
The utility model belongs to the technical field of tail gas recycle, concretely relates to recovery unit of carbonyl sulfide in integrated chlorination technology tail gas.
Background
Chlorination is a reaction of introducing chlorine atoms into molecules of compounds, is an important unit reaction in pharmaceutical and chemical industries, and has application in various fields such as bulk drugs, agriculture, light industry, rubber and the like. The tail gas of the chlorination process often contains byproduct hydrogen chloride, organic solvent and other byproducts, and has complex components and difficult recovery.
Solid phosgene is an important intermediate for medicine synthesis and pesticide manufacture. It can be used for synthesizing fine chemicals such as chloroformate and acyl chloride, medicines such as azlocillin and antihypertensive, and carbamate-type agricultural chemicals, herbicide, and pesticide. Compared with chlorinating agents such as phosphorus oxychloride and phosgene, the stability of the chlorinated polyether is relatively strong, and the chlorinated polyether is more favorable for chemical production. In the chlorination with solid phosgene, when the substance to be chlorinated contains a mercapto group, hydrogen chloride and carbonyl sulfide are by-produced in some cases. The carbonyl sulfide is an important raw material of pesticides, medicines and other chemical products, and particularly occupies an important position in the production process of thiocarbamate pesticides; in recent years, it has been discovered that high purity carbonyl sulfide can be used as an etching gas in integrated circuit manufacturing to replace fluoride etching gases that are difficult to degrade and have a greenhouse effect.
The common treatment mode of the existing solid phosgene chlorination tail gas is as follows: firstly, hydrogen chloride in tail gas is recovered through water absorption, then the residual tail gas is treated by liquid alkali to enable carbonyl sulfide in the tail gas to react to form sodium carbonate and sodium hydrosulfide, the sodium hydrosulfide is oxidized to sodium thiosulfate by hydrogen peroxide, and solid waste obtained after wastewater is concentrated is additionally treated. This treatment not only wastes valuable carbonyl sulfide by-products, but also produces a large amount of solid waste and waste water, increasing waste treatment costs.
With the gradual development of the application of the carbon oxysulfide, the use value of the carbon oxysulfide is further improved, and the recovery of the carbonyl sulfide as a byproduct of the chlorination of the solid phosgene and the sulfydryl has objective economic return, and can also reduce the generation of waste water and waste residue, reduce consumption and reduce emission.
SUMMERY OF THE UTILITY MODEL
In order to solve the problem, the utility model aims to provide a recovery unit of carbonyl sulfide in integrated chlorination technology tail gas.
An integrated recovery device for carbonyl sulfide in chlorination process tail gas comprises an organic solvent recovery module, a cryogenic rectification module and a byproduct cache module, and is characterized in that the organic solvent recovery module comprises a tail gas compressor, a first-stage condenser, a first-stage gas-liquid separator, a second-stage condenser and a second-stage gas-liquid separator, wherein the tail gas compressor is sequentially connected with the first-stage condenser, the first-stage gas-liquid separator, the second-stage condenser and the second-stage gas-liquid separator; the low-temperature rectification module comprises a feeding condenser, a low-temperature rectification tower, a tower top condenser and a tower bottom reboiler, the feeding condenser is connected with the low-temperature rectification tower, the tower top condenser is arranged above the low-temperature rectification tower, the tower bottom reboiler is arranged below the low-temperature rectification tower, and the feeding condenser is connected with the secondary gas-liquid separator through a pipeline; byproduct buffer module include carbon oxysulfide product buffer tank and carbon oxysulfide filling pump, carbon oxysulfide product buffer tank passes through the pipe connection with the low temperature rectifying column.
The integrated device for recovering carbonyl sulfide in chlorination process tail gas is characterized in that an upper outlet of the top of the low-temperature rectifying tower is connected with an upper inlet of a tower top condenser, and a lower outlet of the tower top condenser is divided into two branches which are respectively connected with a lower inlet of the top of the low-temperature rectifying tower and an outlet for recovering hydrogen chloride.
The integrated device for recovering the carbonyl sulfide in the chlorination process tail gas is characterized in that an emptying valve is arranged on the carbonyl sulfide product buffer tank.
The integrated recovery device for carbonyl sulfide in chlorination process tail gas is characterized in that an upper inlet at the bottom of the low-temperature rectifying tower is connected with an upper outlet of a reboiler at the bottom of the tower, and a lower outlet at the bottom of the tower is connected with a lower inlet of the reboiler at the bottom of the tower.
The integrated recovery device for carbonyl sulfide in chlorination process tail gas is characterized in that a bottom lower outlet of the low-temperature rectifying tower is divided into two branches which are respectively connected with a lower inlet of a tower bottom reboiler and an upper inlet of a carbonyl sulfide product buffer tank.
The integrated recovery device for the carbonyl sulfide in the chlorination process tail gas is characterized in that a liquid level detection device is arranged on a carbonyl sulfide product buffer tank, and when the liquid level reaches a certain amount, a carbonyl sulfide filling pump is started to fill.
The integrated recovery device for carbonyl sulfide in chlorination process tail gas is characterized in that the primary gas-liquid separator and the secondary gas-liquid separator are provided with outlets for recovering organic solvents.
The recovery device for carbonyl sulfide in integrated chlorination process tail gas comprises the following process steps:
1) after the chlorinated tail gas to be recovered enters an organic solvent recovery module, after the chlorinated tail gas is pressurized by a tail gas compressor, the chlorinated tail gas is condensed by a primary condensation and gas-liquid separator, and condensed by a secondary condensation and gas-liquid separator and then is combined with the gas-liquid separator, the liquid-phase organic solvent is effectively condensed and recovered; and the gas-phase hydrogen chloride and the carbonyl sulfide enter the low-temperature rectification module.
2) And the gas-phase mixture is condensed by a feeding condenser and then enters a low-temperature rectifying tower for rectification separation, a byproduct hydrogen chloride is separated from the tower top and is dehydrated and absorbed, and a carbon oxysulfide byproduct carbon oxysulfide product buffer tank is obtained at the tower bottom.
3) And (3) allowing the high-purity carbonyl sulfide to enter a carbonyl sulfide product buffer tank for temporary storage, and periodically filling and discharging the product through a carbonyl sulfide filling pump.
In the recycle of present chlorination technology tail gas, adopt the utility model discloses following beneficial effect can be reached:
1) a large amount of byproduct carbonyl sulfide which needs to be treated by the consumed cleaning agent is recycled, so that the consumption of raw materials is reduced, the discharge of three wastes is reduced, and the utilization rate of the raw materials is improved;
2) the efficient high-purity recovery of the carbonyl sulfide in the chlorinated tail gas is realized, and the economic value of a tail gas recovery process and a tail gas recovery device is further increased;
3) the device for recycling the carbonyl sulfide in the chlorination process tail gas is high in integration degree and can be modularized, and the fixed cost of recycling and treating the chlorinated tail gas is reduced.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
In the figure: 1-an organic solvent recovery module; 2-a cryogenic rectification module; 3-byproduct cache module; 4-a tail gas compressor; 5-a first-stage condenser; 6-first-stage gas-liquid separator; 7-a secondary condenser; 8-a secondary gas-liquid separator; 9-feed condenser; 10-a low temperature rectification column; 11-overhead condenser; 12-overhead condenser; 13-a bottoms reboiler; a 14-carbonyl sulfide product buffer tank; 15-carbonyl sulfide filling pump.
Detailed Description
The invention will be further described with reference to the following examples and the accompanying drawings, but the scope of the invention is not limited thereto.
As shown in fig. 1, a recovery device for carbonyl sulfide in integrated chlorination process tail gas is divided into an organic solvent recovery module 1, a cryogenic rectification module 2 and a byproduct buffer module 3, and comprises a tail gas compressor 4, a first-stage condenser 5, a first-stage gas-liquid separation 6, a second-stage condenser 7, a second-stage gas-liquid separator 8, a feeding condenser 9, a cryogenic rectification tower 10, a tower top condenser 11, a tower bottom reboiler 12, a carbonyl sulfide product buffer 13 and a carbonyl sulfide filling pump 14.
An outlet of the tail gas compressor 4 is connected with an outlet of a first-stage condenser 5, the first-stage condenser 5 is connected with a first-stage gas-liquid separator 6, an upper outlet of the first-stage gas-liquid separator 6 is connected with an inlet of a second-stage condenser 7, and the second-stage condenser 7 is connected with a second-stage gas-liquid separator 8; the inlet of the feeding condenser 9 is connected with the outlet of the secondary gas-liquid separator 8, the outlet of the feeding condenser 9 is connected with the low-temperature rectifying tower 10, the upper outlet of the tower top of the low-temperature rectifying tower 10 is connected with the upper inlet of the tower top condenser 11, the lower outlet of the tower top condenser 11 is divided into two branches, and the two branches are respectively connected with the lower inlet of the tower top of the low-temperature rectifying tower 10 and the outlet of the recovered HCL. The upper inlet of the tower bottom of the low-temperature rectifying tower 11 is connected with the upper outlet of the tower bottom reboiler 12, and the lower outlet of the tower bottom is connected with the lower inlet of the tower bottom reboiler 12. The lower outlet of the tower bottom of the low-temperature rectifying tower 11 is divided into two branches which are respectively connected with the lower inlet of a tower bottom reboiler 12 and the upper inlet of a carbon oxysulfide product buffer tank 13. The carbon oxysulfide filling pump 14 is connected with the carbon oxysulfide product buffer tank 13, and the carbon oxysulfide product buffer tank 13 is provided with an emptying valve.
After the recycled chlorinated tail gas is pressurized by a tail gas compressor 4, the chlorinated tail gas is condensed by a first-stage condenser 5, then is subjected to gas-liquid separation by a first-stage gas-liquid separator 6, and then is condensed by a second-stage condenser 7 and a second-stage gas-liquid separator 8 and is subjected to gas-liquid separation, so that the liquid-phase organic solvent is effectively condensed and recycled; the gaseous hydrogen chloride and carbonyl sulphide enter the feed condenser 9. The gas phase mixture is condensed by a feeding condenser 9 and then enters a low-temperature rectifying tower 10 for rectification separation, a byproduct hydrogen chloride is separated from the top of the tower for dehydration absorption, and a carbon oxysulfide byproduct buffer tank 13 for removing carbon sulfide products is obtained at the bottom of the tower. The high-purity carbonyl sulfide enters a carbonyl sulfide product buffer tank 13 for temporary storage, and is filled and discharged by a carbonyl sulfide filling pump 14 at regular intervals.
Example 1
Adopt the utility model discloses carbon oxysulfide among the chlorination tail gas containing toluene retrieves. The total flow rate of the tail gas to be recovered is 100kg/h, wherein the mass fraction of the carbonyl sulfide is 60%, the mass fraction of the hydrogen chloride is 38%, and the mass fraction of the toluene is 2%. The outlet pressure of the tail gas compressor 4 is 2MPa, the refrigerant of the first-stage condenser 5 is circulating water, the refrigerant of the second-stage condenser 7 is low-temperature water, the refrigerant of the feed condenser 9 is-30 ℃ deep-cooling calcium chloride, the heating medium of the reboiler 12 at the bottom of the tower is 75 ℃ hot water, and the cooling medium of the condenser 11 at the top of the tower is-30 ℃ deep-cooling calcium chloride. The flow rate of the recovered carbonyl sulfide is 48.87kg/h, the mass fraction is 99.2 percent, and the recovery rate is 80.8 percent.
Example 2
Adopt the utility model discloses carbon oxysulfide in to containing ethanol chlorination tail gas retrieves. The total flow rate of the tail gas to be recovered is 100kg/h, wherein the mass fraction of the carbonyl sulfide is 55%, the mass fraction of the hydrogen chloride is 40%, and the mass fraction of the ethanol is 5%. The outlet pressure of the tail gas compressor 4 is 2MPa, the refrigerant of the primary condenser 5 is circulating water, the refrigerant of the secondary condenser 7 is frozen ethylene glycol at the temperature of minus 15 ℃, the refrigerant of the feeding condenser 9 is cryogenic calcium chloride at the temperature of minus 30 ℃, the heating medium of the reboiler 12 at the bottom of the tower is hot water at the temperature of 75 ℃, and the cooling medium of the condenser 11 at the top of the tower is cryogenic calcium chloride at the temperature of minus 30 ℃. The flow rate of the recovered carbonyl sulfide is 45.58kg/h, the mass fraction is 99.3 percent, and the recovery rate is 82.3 percent.
Example 3
Adopt the utility model discloses carbon oxysulfide to containing among the dichloromethane chlorination tail gas retrieves. The total flow rate of the tail gas to be recovered is 100kg/h, wherein the mass fraction of the carbonyl sulfide is 58%, the mass fraction of the hydrogen chloride is 39%, and the mass fraction of the dichloromethane is 3%. The outlet pressure of the tail gas compressor 4 is 2MPa, the refrigerant of the primary condenser 5 is low-temperature water, the refrigerant of the secondary condenser 7 is frozen ethylene glycol at the temperature of minus 15 ℃, the refrigerant of the feeding condenser 9 is cryogenic calcium chloride at the temperature of minus 30 ℃, the heating medium of the reboiler 12 at the bottom of the tower is hot water at the temperature of 75 ℃, and the cooling medium of the condenser 11 at the top of the tower is cryogenic calcium chloride at the temperature of minus 30 ℃. The flow rate of the recovered carbonyl sulfide is 50.11kg/h, the mass fraction is 99.1 percent, and the recovery rate is 85.6 percent.
Claims (7)
1. An integrated recovery device for carbonyl sulfide in chlorination process tail gas, which comprises an organic solvent recovery module (1), a cryogenic rectification module (2) and a byproduct buffer module (3),
the organic solvent recovery module (1) comprises a tail gas compressor (4), a primary condenser (5), a primary gas-liquid separator (6), a secondary condenser (7) and a secondary gas-liquid separator (8), wherein the tail gas compressor (4) is sequentially connected with the primary condenser (5), the primary gas-liquid separator (6), the secondary condenser (7) and the secondary gas-liquid separator (8);
the low-temperature rectification module (2) comprises a feeding condenser (9), a low-temperature rectification tower (10), an overhead condenser (11) and a tower bottom reboiler (12), the feeding condenser (9) is connected with the low-temperature rectification tower (10), the overhead condenser (11) is arranged above the low-temperature rectification tower (10), the tower bottom reboiler (12) is arranged below the low-temperature rectification tower (10), and the feeding condenser (9) is connected with the secondary gas-liquid separator (8) through a pipeline;
byproduct buffer module (3) including carbonyl sulfide product buffer tank (13) and carbonyl sulfide filling pump (14), carbonyl sulfide product buffer tank (13) pass through the pipe connection with low temperature rectifying column (10).
2. The integrated recovery device for carbonyl sulfide in chlorination process tail gas according to claim 1, wherein the upper outlet of the top of the low temperature rectification tower (10) is connected with the upper inlet of the top condenser (11), the lower outlet of the top condenser (11) is divided into two branches, which are respectively connected with the lower inlet of the top of the low temperature rectification tower (10) and the outlet for recovering hydrogen chloride.
3. An integrated recovery unit for carbonyl sulphide in chlorination process tail gas as claimed in claim 1, characterized in that the buffer tank (13) for carbonyl sulphide products is provided with an emptying valve.
4. An integrated recovery apparatus for carbonyl sulfide in chlorination process tail gas according to claim 1, characterized in that the upper inlet of the bottom of the low temperature rectification column (10) is connected with the upper outlet of the reboiler (12) at the bottom of the column, and the lower outlet of the bottom of the column is connected with the lower inlet of the reboiler (12) at the bottom of the column.
5. The integrated recovery device for carbonyl sulfide in chlorination process tail gas according to claim 4, wherein the bottom outlet of the low temperature rectification tower (10) is divided into two branches, which are respectively connected with the lower inlet of the tower bottom reboiler (12) and the upper inlet of the carbonyl sulfide product buffer tank (13).
6. The integrated recovery device for carbonyl sulfide in chlorination process tail gas as claimed in claim 1, wherein the carbonyl sulfide product buffer tank (13) is equipped with a liquid level detection device, when the liquid level reaches a certain amount, the carbonyl sulfide filling pump (14) is started to fill.
7. An integrated recovery unit for carbonyl sulphide in chlorination process tail gas according to claim 1, characterized in that the first gas-liquid separator (6) and the second gas-liquid separator (8) are provided with an outlet for recovering organic solvent.
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| CN202023053760.9U CN214570733U (en) | 2020-12-17 | 2020-12-17 | Recovery unit of carbon oxysulfide in integrated chlorination technology tail gas |
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