CN107188133B - Device and method for separating sucralose tail gas - Google Patents
Device and method for separating sucralose tail gas Download PDFInfo
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- CN107188133B CN107188133B CN201710476029.0A CN201710476029A CN107188133B CN 107188133 B CN107188133 B CN 107188133B CN 201710476029 A CN201710476029 A CN 201710476029A CN 107188133 B CN107188133 B CN 107188133B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
- C01B17/56—Separation; Purification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0009—Physical processing
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Abstract
The invention relates to a device and a method for separating sucralose tail gas. The invention is compressed to 0.1MPa by a liquid ring pump, enters a solvent tower T101, and the trichloroethane and DMF are enriched at the bottom of the tower and enter a recovery processing procedure; the top of the column is enriched in SO2, HCl and air. The concentrated SO2 at the bottom of the tower is filled into the gas cylinder through a filling port after being compressed to 2.0MPa by the compressor and entering the refining tower T102 for material exchange in the tower, the HCl and air are enriched at the top of the tower, and the concentrated SO2 at the bottom of the tower is compressed to 5.0MPa by the compressor and enters the filling gas cylinder. The beneficial effects are that: the invention mostly utilizes equipment which runs under a higher pressure form, and no reaction kettle participates; the product of the invention is hydrogen chloride and sulfur dioxide which are separated and respectively canned in containers, and the solvents can be specially enriched and recovered considering the mixing of trace amounts of trichloroethane and DMF solvents in the production process of sucralose.
Description
Technical field
The present invention relates to a kind of Sucralose exhaust gas processing device and method, in particular to a kind of separation Sucralose tail gas
Device and method.
Background technique
Its chloridization process generates a large amount of hydrogen chloride and SO 2 tail gas in sucrose trichloride production process, and sweeps along micro-
The DMF and Separator of amount, the traditional absorption technique of these gases are that buck absorbs, and liquid alkaline consumption and operating cost are all
Very big, absorption process is easier pollution environment, and product hydrochloric acid and sodium sulfite purity is not high.
What Chinese patent literature Publication No. CN103113197A and our company applied before, patent name is " a kind of
The method that Sucralose produces exhaust gas comprehensive utilization ", it comprises the following production steps that firstly, what Sucralose chlorinating step generated
Hydrogen chloride and sulfur dioxide are sent into low-temperature condenser (E-1) and carry out sub-cooled, and cooling temperature realizes chlorination at -100 ~ -10 DEG C
The initial gross separation of hydrogen and sulfur dioxide, sulfur dioxide enter low-temperature storage tank (E-2)；Secondly, the chlorination containing trace sulfur dioxide
Hydrogen is after concentrated sulfuric acid kettle (E-3) is dry, into reaction kettle (E-4) and alcohol and acetonitrile reaction；Pass through hydrogen chloride and alcohol, acetonitrile
Salt-forming reaction carry out absorbing hydrogen chloride tail gas, then resulting salt reacted with ammonia can obtain Sucralose esterification step needed for original
Three ester of acetic acid.Beneficial effect is: the method realizes the comprehensive utilization of waste inside production system, is reducing waste discharge
Product cost is reduced simultaneously.Raw material needed for Sucralose produces is prepared using tail gas hydrogen chloride, realization is turned waste into wealth.
The patent of invention is using atmospheric low-temperature " -100 to -10 DEG C " by the leading liquefaction separation of sulfur dioxide, and hydrogen chloride is still
It is that reaction kettle catalyzing alcohols substance and acetonitrile reaction generation trimethyl orthoacetate are sent into after gaseous state is dried.Whole process is divided into low
Two parts of temperature liquefaction and chemical reaction had both used physical means and have also used chemical means.
In addition, there exists a further problem in that: foregoing invention patent realizes the low-temperature liquefaction separation of sulfur dioxide, and hydrogen chloride is made
It goes Acetonitrile and alcohols to react for a kind of catalyst and generates trimethyl orthoacetate, and hydrogen chloride itself is there are still reaction system,
Chlorination ammonium salt is finally formd by ammonia neutralization, and does not account for micro DMF, Separator problem.
Summary of the invention
The purpose of the present invention is to drawbacks described above of the existing technology, a kind of separation Sucralose tail gas is provided
Hydrogen chloride and sulfur dioxide liquefaction are carried out the essence of mass-and heat-transfer using the method for compression rectification by device and method in rectifying column
Process is evaporated, tower top isolates chlorination hydrogen production, and tower bottom isolates sulfur dioxide product, and whole process is all physical process, does not relate to
And chemical reaction.
A kind of method for separation Sucralose tail gas that the present invention mentions, technical solution are to include the following steps to be made:
1) mixed tail gas after Sucralose production chlorination, by pipeline to liquid rotary pump YP101 and liquid rotary pump YP102,
Liquid rotary pump absorbs micro-moisture using the concentrated sulfuric acid, while entering demisting tank V101 after mixed airflow is pressurizeed, and removes concentrated sulfuric acid mist
Enter surge tank V102 afterwards；
2) air-flow comes out from surge tank V102 enters low pressure compressor P101, low pressure compressor P102 and low pressure compressor
P103, pressure increase to 5bar, subsequently into solvent column T101；
3) solvent trichloroethanes and DMF are enriched at the tower bottom of solvent column T101, are expelled to flash tank from tower bottom
The a small amount of HCl and SO2 dissolved in V103, solvent trichloroethanes and DMF is entered pendular ring from flash tank V103 tank deck by thermal evaporation
Pump the import of YP101 and liquid rotary pump YP102；Simultaneously flash tank V103 tank bottom be discharged pure trichloroethanes and DMF mixing it is molten
Agent goes to be recycled；
4) gas that the tower top of solvent column T101 comes out, which enters after solvent column gas-gas heat exchanger H101 shell side is heated, enters
Intermediate pressure compressor P201, intermediate pressure compressor P202 and intermediate pressure compressor P203, pressure are pressurized to 20bar by 5bar, then into
Enter and enter solvent column condenser H102 after solvent column gas-gas heat exchanger H101 tube side is cooled, after hydrogen chloride and sulfur dioxide liquefaction
Into return tank V104, the discharging of the bottom return tank V104 is divided into two parts: a part returns to solvent column T101, and another part enters essence
Tower T102 processed；Material into treating column T102 is the mixture of pure hydrogen chloride sulfur dioxide and air；
5) rectifying separation is carried out after entering treating column T102, tower bottom has reboiler H105 heating and thermal insulation, in tower bottom titanium dioxide
Sulphur exists in liquid form, and the sulfur dioxide liquid of tower bottom, which enters after sulfur dioxide cooler H107, fills face into sulfur dioxide
Plate F102 carries out filling steel cylinder operation；
6) the tower top discharge hydrogen chloride and air mixture material for the treatment of column T102, into treating column gas gas exchanger H103 shell
Journey, which enters high pressure compressor P301 and high pressure compressor P302, pressure after being heated, increases to 55bar by 20bar, into purification
Enter treating column condenser H104 after the tube side cooling of tower gas gas exchanger H103, enters treating column return tank after chlorination liquefaction of hydrogen
V105；The discharging of return tank bottom is divided into two parts: a part returns to treating column T102, and another part enters hydrogen chloride reactor product cooler
H106 fills panel F101 subsequently into chlorination hydrogen production, and then chlorination hydrogen production is filled enters steel cylinder.
Preferably, the mixed tail gas after above-mentioned Sucralose production chlorination contains SO2 60.52%, HCl 36.31%, three chloroethenes
Alkane 0.99%, DMF 0.25%, air 1.93%, 12 DEG C of temperature.
Preferably, the bottom the return tank V104 discharging in step 4 is divided into two parts: a part returns to solvent column T101, reflux
On the one hand it ensure that the material into treating column T102 does not have organic solvent, another aspect throttling expansion makes the tower of solvent column T101
Top obtains low temperature.
Preferably, the treating column bottom the return tank V105 discharging in step 6 is divided into two parts: a part returns to treating column
On the one hand T102, reflux ensure that the material of extraction hydrogen chloride does not have sulfur dioxide, another aspect throttling expansion makes treating column
T102 tower top obtains low temperature.
A kind of device for separation Sucralose tail gas that the present invention mentions, technical solution be include demisting tank V101, it is slow
Rush tank V102, solvent column T101, flash tank V103, solvent column gas-gas heat exchanger H101, solvent column condenser H102, return tank
V104, treating column T102, reboiler H105, sulfur dioxide cooler H107, sulfur dioxide fill panel F102, treating column gas gas
Exchanger H103, treating column condenser H104, treating column return tank V105, hydrogen chloride reactor product cooler H106, chlorination hydrogen production
Panel F101 is filled, the import of the solvent column T101 is connected to Sucralose production by surge tank V102, demisting tank V101
The bottom of mixed tail gas efferent duct after chlorination, solvent column T101 connects flash tank V103, and solvent trichloroethanes and DMF obtain richness
Collection；Top connection solvent column gas-gas heat exchanger H101, solvent column condenser H102 and the return tank V104 of the solvent column T101,
The gas that tower top comes out is further conveyed to treating column T102 processing, and reboiler H105 is installed in the bottom of the treating column T102,
The sulfur dioxide liquid of tower bottom, which enters after sulfur dioxide cooler H107, fills panel F102 into sulfur dioxide, carries out filling steel
Bottle operation；Tower top connection treating column gas gas exchanger H103, treating column condenser H104 and the treating column of the solvent column T101
Hydrogen chloride and air mixture material is discharged after treatment in return tank V105, tower top, connects hydrogen chloride reactor product cooler H106, so
Enter hydrogen chloride product afterwards and fill panel F101, then chlorination hydrogen production is filled enters steel cylinder.
Preferably, low pressure compressor P101, low pressure compressor are installed between above-mentioned surge tank V102 and solvent column T101
P102 and low pressure compressor P103.
Preferably, it is installed between the output end of shell side and the input terminal of tube side of above-mentioned solvent column gas-gas heat exchanger H101
Intermediate pressure compressor P201, intermediate pressure compressor P202 and intermediate pressure compressor P203.
Preferably, it is installed between the output end of shell side and the input terminal of tube side of above-mentioned treating column gas gas exchanger H103
High pressure compressor P301 and high pressure compressor P302.
Preferably, liquid rotary pump YP101 and liquid rotary pump YP102 are installed in the front end of above-mentioned demisting tank V101.
The beneficial effects of the present invention are: the present invention uses the method for compression rectification by hydrogen chloride and sulfur dioxide liquefaction in essence
The distillation process that mass-and heat-transfer is carried out in tower is evaporated, tower top isolates chlorination hydrogen production, and tower bottom isolates sulfur dioxide product；Separately
Outside, the present invention is the equipment using running under elevated pressures form, 20 bar of intermediate pressure compressor, high pressure compressor 55 mostly
20 bar of bar, treating column T102 pressure is participated in without reaction kettle；
Product of the invention is to be separated the hydrogen chloride come, sulfur dioxide, and used container canned respectively, and examine
Considered trichloroethanes micro in sucrose trichloride production process, DMF solvent is mixed into, these solvents can be specially enriched with back
It receives.
Detailed description of the invention
Attached drawing 1 is structural schematic diagram of the invention；
Attached drawing 2 is the temperature composition phasor of hydrogen chloride and sulfur dioxide under 20bar pressure；
In upper figure: demisting tank V101, surge tank V102, solvent column T101, flash tank V103, solvent column gas-gas heat exchanger
H101, solvent column condenser H102, return tank V104, treating column T102, reboiler H105, sulfur dioxide cooler H107, two
Sulfur oxide fills panel F102, treating column gas gas exchanger H103, treating column condenser H104, treating column return tank V105, chlorine
Change hydrogen production cooler H106, chlorination hydrogen production fills panel F101, low pressure compressor P101, low pressure compressor P102 and low pressure
Compressor P103, intermediate pressure compressor P201, intermediate pressure compressor P202 and intermediate pressure compressor P203, high pressure compressor P301 and high pressure
Compressor P302, liquid rotary pump YP101 and liquid rotary pump YP102.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
A kind of method for separation Sucralose tail gas that the present invention mentions, includes the following steps and is made:
1) mixed tail gas after Sucralose production chlorination (contains SO2 60.52%, HCl 36.31%, trichloroethanes
0.99%, DMF 0.25%, air 1.93%, 12 DEG C of temperature), flow about 2000kg/h, by pipeline to liquid rotary pump P101 and liquid
Ring pumps P102, and liquid rotary pump uses 98% concentrated sulfuric acid medium, absorbs micro-moisture and mixed airflow is forced into 1bar(gauge pressure simultaneously,
1bar=100kPa) enter demisting tank V101 afterwards, enter surge tank V102 after removing concentrated sulfuric acid mist；
2) air-flow comes out from surge tank V102 enters low pressure compressor P101, low pressure compressor P102 and low pressure compressor
P103, pressure increase to 5bar, subsequently into solvent column T101；
3) solvent trichloroethanes and DMF are enriched at tower bottom, are expelled to flash tank V103, solvent trichlorine from tower bottom
The a small amount of HCl and SO2 that dissolve in ethane and DMF are entered the import of liquid rotary pump by thermal evaporation from flash tank V103 tank deck；Simultaneously
The mixed solvent of pure trichloroethanes and DMF is discharged in flash tank V103 tank bottom, goes to be recycled；
4) during the gas that solvent column T101 tower top comes out enters after solvent column H101 gas-gas heat exchanger shell side is heated and enters
Pressure compressor P201, intermediate pressure compressor P202 and intermediate pressure compressor P203, pressure are pressurized to 20bar by 5bar, subsequently into
Enter solvent column condenser H102 after solvent column H101 tube side is cooled, enters return tank after hydrogen chloride and sulfur dioxide liquefaction
V104, the discharging of the bottom return tank V104 are divided into two parts: a part returns to solvent column T101(reflux and on the one hand ensure that into solvent
For the material of tower T102 without organic solvent, another aspect throttling expansion makes the tower top of solvent column T101 obtain low temperature), another portion
Divide and enters treating column T102.It is pure into material absolutely not organic solvent trichloroethanes and the DMF for the treatment of column T102
The mixture of hydrogen chloride sulfur dioxide and air；
5) progress rectifying knockout tower bottom has reboiler heating to maintain the temperature at 80 DEG C or so after entering treating column T102,
Tower bottom sulfur dioxide exists in liquid form and content reaches 99.9%, tower bottom control certain flow constantly produce it is pure
Sulfur dioxide liquid, into sulfur dioxide cooler H107 after enter sulfur dioxide and fill panel F102, fill steel cylinder behaviour
Make.
6) the tower top discharge hydrogen chloride and air mixture material for the treatment of column T102, into treating column gas gas exchanger H103's
Shell side, which enters high pressure compressor P301 and high pressure compressor P302, pressure after being heated, increases to 55bar by 20bar, into essence
Enter treating column condenser H104 after the tube side cooling of tower gas gas exchanger H103 processed, enters treating column after chlorination liquefaction of hydrogen and flow back
Tank V105.The discharging of return tank bottom is divided into two parts: on the one hand a part, which returns to treating column T102(reflux, ensure that extraction hydrogen chloride
Material without sulfur dioxide, another aspect throttling expansion make treating column T102 tower top obtain low temperature), another part enters chlorine
Change hydrogen production cooler H106, fill panel F101 subsequently into chlorination hydrogen production, then chlorination hydrogen production is filled enters steel
Bottle.
A kind of device for separation Sucralose tail gas that the present invention mentions, technical solution be include demisting tank V101, it is slow
Rush tank V102, solvent column T101, flash tank V103, solvent column gas-gas heat exchanger H101, solvent column condenser H102, return tank
V104, treating column T102, reboiler H105, sulfur dioxide cooler H107, sulfur dioxide fill panel F102, treating column gas gas
Exchanger H103, treating column condenser H104, treating column return tank V105, hydrogen chloride reactor product cooler H106, chlorination hydrogen production
Panel F101 is filled, the import of the solvent column T101 is connected to Sucralose production by surge tank V102, demisting tank V101
The bottom of mixed tail gas efferent duct after chlorination, solvent column T101 connects flash tank V103, and solvent trichloroethanes and DMF obtain richness
Collection；Top connection solvent column gas-gas heat exchanger H101, solvent column condenser H102 and the return tank V104 of the solvent column T101,
The gas that tower top comes out is further conveyed to treating column T102 processing, and reboiler H105 is installed in the bottom of the treating column T102,
The sulfur dioxide liquid of tower bottom, which enters after sulfur dioxide cooler H107, fills panel F102 into sulfur dioxide, carries out filling steel
Bottle operation；Tower top connection treating column gas gas exchanger H103, treating column condenser H104 and the treating column of the solvent column T101
Hydrogen chloride and air mixture material is discharged after treatment in return tank V105, tower top, connects hydrogen chloride reactor product cooler H106, so
Enter hydrogen chloride product afterwards and fill panel F101, then chlorination hydrogen production is filled enters steel cylinder.
Wherein, low pressure compressor P101, low pressure compressor P102 are installed between above-mentioned surge tank V102 and solvent column T101
With low pressure compressor P103；Preferably, the input terminal of the output end of the shell side of above-mentioned solvent column gas-gas heat exchanger H101 and tube side
Between be installed on intermediate pressure compressor P201, intermediate pressure compressor P202 and intermediate pressure compressor P203；Preferably, above-mentioned treating column gas gas
High pressure compressor P301 and high pressure compressor are installed between the output end of the shell side of exchanger H103 and the input terminal of tube side
P302；Install liquid rotary pump YP101 and liquid rotary pump YP102 in the front end of above-mentioned demisting tank V101.
Chlorination reaction mixed gas flow 2000kg/h is compressed to 0.1MPa(gauge pressure by liquid rotary pump) enter solvent column
T101, tower bottom are enriched with trichloroethanes and DMF, into recovery processing program；Tower top is enriched with SO2, HCl, air.By compressor plus
It is depressed into 2.0MPa(gauge pressure) enter treating column T102, mass exchange is carried out in tower, tower top is enriched with HCl and air, through overcompression
Machine is compressed to 5.0MPa(gauge pressure) into gas cylinder is filled, tower bottom enrichment SO2 is filled by filling mouth into gas cylinder.
In addition, it is necessary to further illustrate: the present invention and the prior art, the especially immediate prior art are compared
(hereinafter referred to as existing patent), difference and advantage are as follows:
1, there is essential distinction in the not identical i.e. processing means of principle
This is applied for a patent, and is passed hydrogen chloride and sulfur dioxide liquefaction in rectifying column using the method for compression rectification
The distillation process of matter heat transfer, tower top isolate chlorination hydrogen production, and tower bottom isolates sulfur dioxide product.Whole process is all physics
Process is not related to chemically reacting.
And existing patent, using atmospheric low-temperature " -100 to -10 DEG C " by the leading liquefaction separation of sulfur dioxide, hydrogen chloride is still
It is that reaction kettle catalyzing alcohols substance and acetonitrile reaction generation trimethyl orthoacetate are sent into after gaseous state is dried.Whole process is divided into low
Two parts of temperature liquefaction and chemical reaction.Both physical means had been used and have also used chemical means.
, appliance arrangement and process it is not identical
Principle is different, then the device designed is not also identical, the present invention is using under elevated pressures form mostly
The equipment of operation, 20 bar of intermediate pressure compressor, 20 bar of high pressure compressor 55 bar, treating column T102 pressure.There is no reaction kettle
It participates in.
Existing patent, using the equipment of atmospheric low-temperature, by sulfur dioxide liquefaction, it is difficult to the subsequent quilt of liquefied hydrogen chloride
The concentrated sulfuric acid is dry, is finally passed through reaction kettle catalyzing alcohols and acetonitrile reaction generates trimethyl orthoacetate.
, the effect of separation it is different
This is applied for a patent, and product is to be separated the hydrogen chloride come, sulfur dioxide, and used container canned respectively.
And consider trichloroethanes micro in sucrose trichloride production process, DMF solvent is mixed into, can be molten by these
The special enriching and recovering of agent.
Existing patent, realizes the low-temperature liquefaction separation of sulfur dioxide, and hydrogen chloride removes Acetonitrile as a kind of catalyst
It is reacted with alcohols and generates trimethyl orthoacetate.And there are still reaction systems for hydrogen chloride itself, finally form chlorine by ammonia neutralization
Change ammonium salt.And micro DMF, Separator problem are not accounted for.
, this patent be related to many thermodynamics contents
(1) macroscopic property of the determination of the pressure and temp parameter for the treatment of column T102 and hydrogen chloride, sulfur dioxide ceases manner of breathing
It closes.The temperature of hydrogen chloride and sulfur dioxide under 20bar pressure forms phasor, can be with computer drawing.
Chlorine line represents dew point line, and deep line is for bubble point line (downside single line).It is determined by phasor, column bottom temperature is about determined 80
DEG C, tower top temperature is about determined at -10 DEG C.Referring in particular to attached drawing 2.
(2) intermediate pressure compressor and high pressure compressor can also play the role of refrigeration in a device.The gas of working media,
Refrigerant is acted also as, is cleverly arranged, refrigerant throttling expansion is allowed to freeze.It is very big to do so energy-saving significance, so that we overcome
Dependence to cryogenic refrigeration machine.0 DEG C of chilled water is just sufficient for production needs.And it is first had in " existing patent " mixing
Tail gas is cooled to -100 to -10 DEG C.Cryogenic refrigeration machine is so just needed, energy consumption can be very high.
The above, is only part preferred embodiment of the invention, and anyone skilled in the art may benefit
Equivalent technical solution is modified or is revised as with the technical solution of above-mentioned elaboration.Therefore, technology according to the present invention
Any simple modification or substitute equivalents that scheme is carried out, belong to the greatest extent the scope of protection of present invention.
Claims (4)
1. a kind of method for separating Sucralose tail gas, is made it is characterized in that: including the following steps:
Sucralose produces the mixed tail gas after chlorination, by pipeline to liquid rotary pump YP101 and liquid rotary pump YP102, liquid rotary pump
Micro-moisture is absorbed using the concentrated sulfuric acid, while entering demisting tank V101 after mixed airflow is pressurizeed, is entered after removing concentrated sulfuric acid mist
Surge tank V102；
Air-flow comes out from surge tank V102 enters low pressure compressor P101, low pressure compressor P102 and low pressure compressor P103, presses
Power increases to 5bar, subsequently into solvent column T101；
Solvent trichloroethanes and DMF are enriched at the tower bottom of solvent column T101, are expelled to flash tank V103, solvent from tower bottom
The a small amount of HCl and SO2 dissolved in trichloroethanes and DMF by thermal evaporation from flash tank V103 tank deck enter liquid rotary pump YP101 and
The import of liquid rotary pump YP102；The mixed solvent of pure trichloroethanes and DMF is discharged in flash tank V103 tank bottom simultaneously, goes to recycle
Processing；
The tower top of solvent column T101 come out gas enter after solvent column gas-gas heat exchanger H101 shell side is heated enter in press pressure
Contracting machine P201, intermediate pressure compressor P202 and intermediate pressure compressor P203, pressure are pressurized to 20bar by 5bar, subsequently into solvent
Enter solvent column condenser H102 after tower gas-gas heat exchanger H101 tube side is cooled, enters back after hydrogen chloride and sulfur dioxide liquefaction
Tank V104 is flowed, the discharging of the bottom return tank V104 is divided into two parts: a part returns to solvent column T101, and another part enters treating column
T102；Material into treating column T102 is the mixture of pure hydrogen chloride, sulfur dioxide and air；
Rectifying separation is carried out after into treating column T102, tower bottom has reboiler H105 heating and thermal insulation, in tower bottom sulfur dioxide with liquid
State form exists, and the sulfur dioxide liquid of tower bottom, which enters after sulfur dioxide cooler H107, fills panel into sulfur dioxide
F102 carries out filling steel cylinder operation；
The tower top discharge hydrogen chloride and air mixture material for the treatment of column T102, is added into treating column gas gas exchanger H103 shell side
Entering high pressure compressor P301 and high pressure compressor P302, pressure after heat increases to 55bar by 20bar, into treating column gas gas
Enter treating column condenser H104 after the tube side cooling of exchanger H103, enters treating column return tank V105 after chlorination liquefaction of hydrogen；
The discharging of return tank bottom is divided into two parts: a part returns to treating column T102, and another part enters hydrogen chloride reactor product cooler H106,
Panel F101 is filled subsequently into chlorination hydrogen production, then chlorination hydrogen production is filled enters steel cylinder.
2. the method for separation Sucralose tail gas according to claim 1, it is characterized in that: the Sucralose produces chlorination
Mixed tail gas afterwards contains SO260.52%, HCl 36.31%, trichloroethanes 0.99%, DMF 0.25%, air 1.93%, temperature 12
℃。
3. the method for separation Sucralose tail gas according to claim 1, it is characterized in that: the discharging of the bottom return tank V104 is divided into
Two parts: a part returns to solvent column T101, on the one hand reflux ensure that the material into treating column T102 does not have organic solvent,
Another aspect throttling expansion makes the tower top of solvent column T101 obtain low temperature.
4. the method for separation Sucralose tail gas according to claim 1, it is characterized in that: the bottom treating column return tank V105 goes out
Material is divided into two parts: a part returns to treating column T102, on the one hand reflux ensure that the material of extraction hydrogen chloride does not have titanium dioxide
Sulphur, another aspect throttling expansion make treating column T102 tower top obtain low temperature.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710476029.0A CN107188133B (en) | 2017-06-21 | 2017-06-21 | Device and method for separating sucralose tail gas |
| CN201811524680.1A CN109553075B (en) | 2017-06-21 | 2017-06-21 | Sucralose tail gas treatment device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710476029.0A CN107188133B (en) | 2017-06-21 | 2017-06-21 | Device and method for separating sucralose tail gas |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811524680.1A Division CN109553075B (en) | 2017-06-21 | 2017-06-21 | Sucralose tail gas treatment device |
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| Publication Number | Publication Date |
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| CN107188133A CN107188133A (en) | 2017-09-22 |
| CN107188133B true CN107188133B (en) | 2019-03-29 |
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| CN201710476029.0A Active CN107188133B (en) | 2017-06-21 | 2017-06-21 | Device and method for separating sucralose tail gas |
| CN201811524680.1A Active CN109553075B (en) | 2017-06-21 | 2017-06-21 | Sucralose tail gas treatment device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108299225A (en) * | 2018-01-13 | 2018-07-20 | 安徽金禾实业股份有限公司 | A kind of method and device recycling trichloroethanes and DMF |
| CN108373139A (en) * | 2018-01-13 | 2018-08-07 | 安徽金禾实业股份有限公司 | The retracting device and recovery method of sulfur dioxide in a kind of Sucralose chlorination reaction |
| CN109724368A (en) * | 2018-12-10 | 2019-05-07 | 安徽金禾实业股份有限公司 | The recovery method of chlorinated exhaust in a kind of production of Sucralose |
| CN109503314B (en) * | 2018-12-10 | 2021-10-22 | 安徽金禾实业股份有限公司 | Method for recovering trichloroethane in tail gas in sucralose production |
| CN110368785B (en) * | 2019-01-30 | 2021-07-30 | 山东康宝生化科技有限公司 | Method for solving problems of carbon black generation and excessive air generation in sucralose tail gas separation process |
| CN110508105B (en) * | 2019-08-28 | 2021-08-10 | 山东康宝生化科技有限公司 | Device and method for separating carbon dioxide and hydrogen chloride from sucralose tail gas |
| CN110803978A (en) * | 2019-11-16 | 2020-02-18 | 安徽金禾实业股份有限公司 | Method for recovering trichloroethane from sucralose chlorination reaction tail gas |
| CN113634071A (en) * | 2020-04-27 | 2021-11-12 | 张吉瑞 | Method for recycling chemical tail gas and treatment device thereof |
| CN111662164A (en) * | 2020-05-22 | 2020-09-15 | 安徽金禾实业股份有限公司 | Method for producing chloromethyl ether by using sucralose chlorination tail gas |
| CN112221311A (en) * | 2020-09-26 | 2021-01-15 | 安徽金禾实业股份有限公司 | Method for treating sucralose chlorination tail gas |
| CN112010268A (en) * | 2020-09-26 | 2020-12-01 | 安徽金禾实业股份有限公司 | Medium-pressure rectification separation method for sucralose chlorination tail gas |
| CN112723630A (en) * | 2020-11-28 | 2021-04-30 | 安徽金禾实业股份有限公司 | Device and method for recovering trichloroethane in total discharge of sucralose chlorination section |
| CN113318469A (en) * | 2021-05-29 | 2021-08-31 | 安徽金禾实业股份有限公司 | Rectification treatment method for HCl (hydrochloric acid) in sucralose chlorination tail gas |
| WO2023279279A1 (en) * | 2021-07-07 | 2023-01-12 | 安徽金禾实业股份有限公司 | Method for treating tail gas |
| CN114291795B (en) * | 2022-01-18 | 2023-04-18 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for preparing high-purity sulfur dioxide |
| CN116409750B (en) * | 2023-03-30 | 2024-05-17 | 利津鸿蒙新业生物科技有限公司 | Device and method for separating high-purity hydrogen chloride from byproduct hydrogen chloride of sucralose |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101791487B (en) * | 2010-03-30 | 2012-01-25 | 中国天辰工程有限公司 | Method for recycling hydrogen chloride in tail gas of polysilicon production |
| RU2583024C2 (en) * | 2010-10-29 | 2016-04-27 | Мекс, Инк. | Regenerative extraction of sulphur dioxide from gaseous emissions |
| CN103113197B (en) * | 2013-02-06 | 2014-11-26 | 山东康宝生化科技有限公司 | Method for comprehensively utilizing trichlorosucrose production waste gas |
| CN103466550B (en) * | 2013-08-28 | 2015-07-15 | 张吉瑞 | Recovery system of D-acid esterification tail gas in amoxicillin production technology |
| CN103496670B (en) * | 2013-09-12 | 2015-05-13 | 聊城市鲁西化工工程设计有限责任公司 | HCl recovery technique |
| ZA201408684B (en) * | 2014-11-26 | 2018-12-19 | Lifezone Ltd | A treatment process for recovery and separation of elements from liquors |
| CN205412614U (en) * | 2015-12-18 | 2016-08-03 | 山东三和维信生物科技有限公司 | Tail gas recycling apparatus of sucralose chlorination workshop section |
| CN106466548A (en) * | 2016-08-30 | 2017-03-01 | 安徽金禾实业股份有限公司 | A kind of processing method of sucralose tail gas |
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| CN109553075A (en) | 2019-04-02 |
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