CN105061133B - The recovery method of acetylene and retracting device during a kind of vinyl acetate production - Google Patents
The recovery method of acetylene and retracting device during a kind of vinyl acetate production Download PDFInfo
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- CN105061133B CN105061133B CN201510456301.XA CN201510456301A CN105061133B CN 105061133 B CN105061133 B CN 105061133B CN 201510456301 A CN201510456301 A CN 201510456301A CN 105061133 B CN105061133 B CN 105061133B
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- absorbing liquid
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- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 title claims abstract description 66
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000011084 recovery Methods 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000007872 degassing Methods 0.000 claims abstract description 117
- 238000010521 absorption reaction Methods 0.000 claims abstract description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052756 noble gas Inorganic materials 0.000 claims abstract description 13
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000007599 discharging Methods 0.000 claims abstract description 5
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims abstract description 4
- 238000004148 unit process Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 83
- 239000007789 gas Substances 0.000 claims description 63
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 239000006096 absorbing agent Substances 0.000 claims description 15
- 239000012267 brine Substances 0.000 claims description 11
- 238000006396 nitration reaction Methods 0.000 claims description 11
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 4
- 150000001299 aldehydes Chemical class 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229920002689 polyvinyl acetate Polymers 0.000 description 2
- 239000011118 polyvinyl acetate Substances 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 1
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 230000035508 accumulation Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000011354 acetal resin Substances 0.000 description 1
- 150000001345 alkine derivatives Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- -1 remove noble gas (N2 Natural products 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229920006163 vinyl copolymer Polymers 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention discloses recovery method and the retracting device of acetylene during a kind of vinyl acetate production, its feature is: by arranging absorption tower, degassing tower and water scrubber, the reacting gas discharging gas separation column from vinyl acetate synthesis operation carries out acetylene absorption, acetylene release and acetylene three unit processes of washing successively, remove the noble gas in reacting gas and acetaldehyde, it is thus achieved that the acetylene of concentration ＞ 98%.The present invention passes through synthetical recovery and the utilization of acetylene in Dichlorodiphenyl Acetate ethylene production, improves raw-material utilization rate, reduces the unit consumption of raw material and the energy, can greatly reduce cost.
Description
Technical field
The present invention relates to recovery method and the retracting device thereof of acetylene during vinyl acetate production.
Technical background
Vinyl acetate is one of Organic Chemicals that yield is bigger in the world, is widely used in production polyvinyl acetate (PVAc), gathers
A series of chemical industry and the changes such as vinyl alcohol, coating, slurry, binding agent, polyvinyl, thin film, vinyl copolymer resin, acetal resin
Fine product, its application relates to all trades and professions.
China's vinyl acetate production starts from the sixties in 20th century.Nineteen sixty-five, Beijing Organic Chemical Plant introduced acetylene method stream from Japan
Change bed technique, build up the most at home and overlap same device more.Recently as the development of polyvinyl alcohol, China's acetic acid Market for Ethylene
Constantly expand.According to statistics, China's vinyl acetate total productive capacity 2,200,000 tons/year at present, and in continuing growth trend.
Vinyl acetate production process route has ethylene process and acetylene method two kinds, and China is based on acetylene method.Acetic acid is produced at acetylene method
In the production process of ethylene, the conversion per pass of acetylene is only about 12%, and a large amount of unconverted acetylene recycle.For preventing
Reduce being smoothed out of concentration of acetylene impact reaction after the noble gas accumulations such as nitrogen, a part must be released from gas separation column
Gas, thus causes the loss of acetylene raw material.Develop suitable recovery method and retracting device, it is achieved the selection of acetylene gas
Property reclaim, reduce acetylene gas discharge, it is possible to reduce vinyl acetate production cost, improve the competitiveness of product in market.
Summary of the invention
It is an object of the invention to provide a kind of can during vinyl acetate production the method and apparatus of selective recovery acetylene,
Mainly remove noble gas (N2、CO2Deng), improve the purity of system, next to that the acetaldehyde in removing system, reduce system
In objectionable impurities.The method can reduce carbide acetylene method and produce the discharge of acetylene during vinyl acetate, lowers consumption of raw materials,
Save production cost.
The present invention solves technical problem and adopts the following technical scheme that
The recovery method of acetylene during vinyl acetate production of the present invention, its feature is: include acetylene absorption, acetylene release and
Acetylene three unit processes of washing, concretely comprise the following steps:
Step 1, acetylene absorption
The reacting gas discharged by gas separation column in vinyl acetate synthesis operation is collected to discharging gas-collection vessel；Described instead
Acetylene, noble gas and acetaldehyde, described noble gas include nitrogen and carbon dioxide to answer gas to include；
Arranging absorption tower, the reacting gas in discharge gas-collection vessel is after the first pressurized equipment pressurization, from absorption tower lower entrances
Being passed through absorption tower, absorbing liquid is passed through absorption tower, reacting gas and absorbing liquid counter current contacting from absorption tower upper entrance, makes reaction gas
Acetylene and acetaldehyde in body are absorbed, and discharge from absorption tower outlet at bottom with absorbing liquid；Unabsorbed noble gas is from absorption
Top of tower outlet is discharged；
Described absorbing liquid is at least one in acetic acid and vinyl acetate；
Step 2, acetylene discharge
Degassing tower is set, after the tower bottoms of absorption tower outlet at bottom discharge pumps into heat exchanger heat exchange by the first pump, then from degassing
Tower centre entrance enters degassing tower stripping stage, makes absorbed gas parse from absorbing liquid under high-temperature low-pressure, inhales after desorbing
Receiving liquid to discharge from degassing tower outlet at bottom, the major part desorbed includes that the gas of acetylene, acetaldehyde and vinyl acetate is from degassing tower
Upper outlet extraction, remainder continues upwardly into degassing tower absorber portion；From the gas of degassing tower middle and upper part outlet extraction through salt
Water condenser condenses, and returns in degassing tower after being condensed by vinyl acetate therein, and uncooled acetylene and aldehydes gas are sent into and reclaimed
Gas-collection vessel；
Absorbing liquid enters degassing tower absorber portion from degassing tower upper entrance, not from gas and the absorption of the outlet extraction of degassing tower middle and upper part
Liquid counter current contacting, major part is absorbed, and remainder is discharged from degassing tower top exit, and sends into discharge gas-collection vessel, continues
Continue and process；Complete the absorbing liquid after absorbing to discharge from degassing tower outlet at bottom equally；
Step 3, acetylene are washed
Water scrubber is set, the gas in gas recovery collecting tank is sent into water scrubber bottom inlet, washing by the second pressurized equipment
Tower is two sections of settings, sequentially consists of water scrubber one section and water scrubber two-stage nitration；
Gas at water scrubber one section and water scrubber two-stage nitration and water counter current contacting, removes the acetaldehyde in gas successively, and residue acetylene is from water
Wash top of tower outlet to discharge, send into reuse in acetylene method vinyl acetate synthesis operation.
The operation pressure on absorption tower described in step 1 is 35～45KPa, and absorbing liquid temperature is 0～3 DEG C；
The tower pressure of degassing tower described in step 2 is 1～3Kpa, and wherein the temperature of degassing tower stripping stage is 60～90 DEG C, and degassing tower is inhaled
Receiving absorbing liquid temperature in section is 0～3 DEG C；From degassing tower middle and upper part, outlet expellant gas is cooled to 0～5 DEG C through brine condenser；
In water scrubber described in step 3 water temperature of water scrubber one section control 4～7 DEG C, the voltage-controlled system of tower 18～22KPa, water scrubber
The water temperature of two-stage nitration controls at 0～3 DEG C, and the voltage-controlled system of tower is 18～22Kpa.
The absorbing liquid warp discharged from degassing tower outlet at bottom pumps into heat exchanger heat exchange by the second pump, then lowers the temperature through absorbing liquid condenser
After, introducing absorption tower upper entrance and degassing tower upper entrance, absorbing liquid recycles on absorption tower and degassing tower.
The lower end of described degassing tower stripping stage is absorbing liquid canned paragraphs, and the degassing tower outlet at bottom bottom described absorbing liquid canned paragraphs is even
Being connected to the absorbing liquid entrance of reboiler, the steam (vapor) outlet of described reboiler is communicated in more than the liquid level of described absorbing liquid canned paragraphs；Institute
The absorbing liquid outlet stating reboiler is connected to the second pump；
The temperature of described degassing tower stripping stage is to heat absorbing liquid by reboiler, and the absorbing liquid steam of generation enters Analytic Tower and realizes.
During the vinyl acetate production of above-mentioned recovery method, the structure of the retracting device of acetylene is:
Including discharge gas-collection vessel, the first pressurized equipment, absorption tower, the first pump, degassing tower, gas recovery collecting tank, the
Two pressurized equipments, water scrubber, absorbing liquid condenser, brine condenser, the second pump, reboiler and heat exchanger；
Absorption tower outlet at bottom, absorption tower lower entrances, absorption tower upper entrance and suction it is provided with from bottom to up on described absorption tower
Receipts top of tower exports；
Described degassing tower is that syllogic is arranged, and sequentially consists of absorbing liquid canned paragraphs, degassing tower stripping stage and degassing tower and absorbs
Section；It is degassing tower outlet at bottom bottom described absorbing liquid canned paragraphs；Described degassing tower stripping stage is provided with degassing tower centre entrance,
Between described degassing tower stripping stage and degassing tower absorber portion, it is provided with the outlet of degassing tower middle and upper part, sets at described degassing tower absorber portion
It is equipped with degassing tower upper entrance, described degassing tower absorber portion top is provided with degassing tower top exit；
Described water scrubber is that two-part is arranged, and sequentially consists of water scrubber one section and water scrubber two-stage nitration, at the bottom of described water scrubber
Portion is provided with water scrubber bottom inlet, and top is provided with water scrubber top exit；
The outlet of described discharge gas-collection vessel is communicated in absorption tower lower entrances by the first pressurized equipment；
Between absorption tower outlet at bottom and the degassing tower centre entrance of described degassing tower on described absorption tower, the first pump and heat exchange are set
Device, after the tower bottoms of absorption tower outlet at bottom discharge pumps into heat exchanger heat exchange by the first pump, then enters from degassing tower centre entrance
Enter degassing tower stripping stage；
The outlet of described degassing tower middle and upper part is communicated in gas recovery collecting tank by brine condenser；Described gas recovery collecting tank leads to
Cross the second pressurized equipment and be connected to the water scrubber bottom inlet of water scrubber；It is provided with on described brine condenser and is connected into described degassing tower
Backflow；
Described degassing tower top exit is connected to described discharge gas-collection vessel；
Described degassing tower outlet at bottom is connected to the absorbing liquid entrance of reboiler, and the steam (vapor) outlet of described reboiler is communicated in described suction
Receive more than the liquid level of liquid canned paragraphs；The absorbing liquid of described reboiler exports successively through the second pump, heat exchanger and absorbing liquid condenser,
It is connected to absorption tower upper entrance and degassing tower upper entrance.
Compared with the prior art, the present invention has the beneficial effect that:
1, the present invention is by the synthetical recovery of acetylene in Dichlorodiphenyl Acetate ethylene production and utilization, improves raw-material utilization rate,
Reduce the unit consumption of raw material and the energy, cost can be greatly reduced；The acetylene gas concentration reclaimed by the inventive method is more than
98%.
2, retracting device of the present invention is simple, easy to implement.
Accompanying drawing explanation
Fig. 1 is the retracting device of acetylene during the vinyl acetate production being applied to the inventive method.
Label in figure: 1 discharges gas-collection vessel；2 first pressurized equipments；3 absorption towers；3a absorption tower lower entrances；3b inhales
Receive tower upper entrance；3c absorption tower outlet at bottom；3d absorption tower top exit；4 first pumps；5 degassing towers；51 degassing tower solutions
Inhale section；52 degassing tower absorber portions；53 absorbing liquid canned paragraphs；5a degassing tower centre entrance；5b degassing tower middle and upper part exports；5c
Degassing tower upper entrance；5d degassing tower top exit；5e degassing tower outlet at bottom；6 gas recovery collecting tanks；7 second pressurizations
Equipment；8 water scrubbers；81 water scrubbers one section；82 water scrubber two-stage nitration；8a water scrubber bottom inlet；8b water scrubber top exit；
9 absorbing liquid condensers；10 brine condensers；11 second pumps；12 reboilers；13 heat exchangers.
Detailed description of the invention
As it is shown in figure 1, first the present embodiment arranges following retracting device: include discharging gas-collection vessel the 1, first pressurized equipment 2,
Absorption tower the 3, first pump 4, degassing tower 5, gas recovery collecting tank the 6, second pressurized equipment 7, water scrubber 8, absorbing liquid condense
Device 9, brine condenser the 10, second pump 11, reboiler 12 and heat exchanger 13；
Absorption tower outlet at bottom 3c, absorption tower lower entrances 3a, absorption tower upper entrance it is disposed with from bottom to up on absorption tower
3b and absorption tower top exit 3d；
Degassing tower 5 is arranged for syllogic, sequentially consists of absorbing liquid canned paragraphs 53, degassing tower stripping stage 51 and degassing tower
Absorber portion 52；It is degassing tower outlet at bottom 5e bottom absorbing liquid canned paragraphs 53, is provided with in degassing tower at degassing tower stripping stage 51
Portion entrance 5a, is provided with degassing tower middle and upper part outlet 5b, in degassing between degassing tower stripping stage 51 and degassing tower absorber portion 52
Tower absorber portion 52 is provided with degassing tower upper entrance 5c, and degassing tower absorber portion 52 top is provided with degassing tower top exit 5d；
Water scrubber 8 is arranged for two-part, sequentially consists of water scrubber one section 81 and water scrubber two-stage nitration 82, at water scrubber 8
Bottom is provided with water scrubber bottom inlet 8a, and top is provided with water scrubber top exit 8b；
Discharge the outlet absorption tower lower entrances 3a by the first pressurized equipment 2 connection with absorption tower 3 of gas-collection vessel 1；
First pump 4 is set between the absorption tower outlet at bottom 3c and the degassing tower centre entrance 5a of degassing tower 5 on absorption tower 3 and changes
Hot device 13, after the tower bottoms of absorption tower outlet at bottom 3c discharge pumps into heat exchanger 13 heat exchange by the first pump 4, then from degassing
Tower centre entrance 5a enters degassing tower stripping stage 51；
Degassing tower middle and upper part outlet 5b is communicated in gas recovery collecting tank 6 by brine condenser 10；Gas recovery collecting tank 6
The water scrubber bottom inlet 8a of water scrubber 8 it is connected to by the second pressurized equipment 7；Be provided with on brine condenser 10 be connected into de-
The backflow of gas tower；
Degassing tower top exit 5d is connected to discharge gas-collection vessel 1；
Degassing tower outlet at bottom 5e is connected to the absorbing liquid entrance of reboiler 12, and the steam (vapor) outlet of reboiler 12 is communicated in absorbing liquid
More than the liquid level of canned paragraphs 53；The absorbing liquid outlet of reboiler 12 condenses through the second pump 11, heat exchanger 13 and absorbing liquid successively
Device 9, is connected to absorption tower upper entrance 3b and degassing tower upper entrance 5c.
Utilizing above-mentioned retracting device, in Dichlorodiphenyl Acetate ethylene production, acetylene carries out the method reclaimed, including acetylene absorption, acetylene
Three unit processes washed by release and acetylene, concretely comprise the following steps:
Step 1, acetylene absorption
The reacting gas discharged by gas separation column in vinyl acetate synthesis operation is collected to discharging gas-collection vessel 1；Reaction
Gas includes acetylene, noble gas, acetaldehyde, and wherein noble gas includes nitrogen and carbon dioxide；
By the reacting gas in discharge gas-collection vessel 1 after the first pressurized equipment 2 pressurizes, from absorption tower, lower entrances 3a is passed through
Absorption tower 3, absorbing liquid is passed through absorption tower 3, reacting gas and absorbing liquid counter current contacting from absorption tower upper entrance 3b, makes reaction
Acetylene and acetaldehyde in gas are absorbed, and discharge from absorption tower outlet at bottom 3c with absorbing liquid；Unabsorbed noble gas from
Absorption tower top exit 3d discharges；
Absorbing liquid is acetic acid and the mixed liquor of vinyl acetate 1:1 by volume composition, and absorbing liquid temperature is 0～3 DEG C；By absorbing
The discharge capacity control tower pressure of noble gas in top of tower outlet, the operation pressure making absorption tower is 40KPa；
Step 2, acetylene discharge
After the tower bottoms of absorption tower outlet at bottom 3c discharge pumps into heat exchanger 13 heat exchange by the first pump 4, then from degassing tower
Portion entrance 5a enters and makes absorbed gas parse from absorbing liquid at degassing tower stripping stage 51,80 DEG C, absorbs after desorbing
Liquid is discharged from degassing tower outlet at bottom 5e；The most of gas (including acetylene, acetaldehyde and vinyl acetate) desorbed is from degassing tower
Middle and upper part outlet 5b discharges and is cooled to 0 DEG C through brine condenser 10, returns in degassing tower after being condensed by vinyl acetate therein,
Uncooled acetylene and aldehydes gas send into gas recovery collecting tank 6；The residue small portion of gas desorbed continues upwardly into de-
Gas tower absorber portion 52；
The absorbing liquid of 2 DEG C enters degassing tower absorber portion 52 from degassing tower upper entrance 5c, not from degassing tower middle and upper part outlet 5b row
The gas gone out and absorbing liquid counter current contacting, major part is absorbed, and remainder is discharged from degassing tower top exit 5d, and the row of feeding
Go out gas-collection vessel 1, proceed to process；Complete the absorbing liquid after absorbing to discharge from degassing tower outlet at bottom 5e equally；
The tower pressure of degassing tower is 3Kpa；The lower end of degassing tower stripping stage 51 is absorbing liquid canned paragraphs 53, absorbing liquid canned paragraphs 53
The degassing tower outlet at bottom of bottom is connected to the absorbing liquid entrance of reboiler 12, and the steam (vapor) outlet of reboiler 12 is communicated in absorbing liquid
More than the liquid level of canned paragraphs 53；The absorbing liquid outlet of reboiler 12 is connected to the second pump 11；The temperature of degassing tower stripping stage is logical
Crossing reboiler 12 and heat absorbing liquid, the absorbing liquid steam of generation enters Analytic Tower 5 and realizes.
For improving efficiency, the absorbing liquid warp discharged from degassing tower outlet at bottom 5e pumps into heat exchanger 13 heat exchange by the second pump 11,
Again after absorbing liquid condenser 9 is lowered the temperature, introducing absorption tower upper entrance 3b and degassing tower upper entrance 5c, absorbing liquid is absorbing
Tower 3 and degassing tower 5 recycle.
Step 3, acetylene are washed
Gas in gas recovery collecting tank 6 is sent into water scrubber bottom inlet 8a by the second pressurized equipment 7；
Gas in water scrubber one section 81 and water scrubber two-stage nitration 82 and water counter current contacting, is removed the acetaldehyde in gas, is remained second successively
Alkynes is discharged from water scrubber top exit 8b, sends into the sodium chlorate scrubbing tower reuse of acetylene method vinyl acetate synthesis operation.
In water scrubber the water temperature of water scrubber one section control 5 DEG C, the voltage-controlled system of tower at 20KPa, the water temperature of water scrubber two-stage nitration control 0～
1 DEG C, the voltage-controlled system of tower is at 19Kpa.
Repeated mensuration, in the reacting gas that gas separation column is discharged, concentration of acetylene is not higher than 92%, and through side of the present invention
The process of method, goes out the concentration of acetylene ＞ 98% collected at water scrubber top exit.
Claims (4)
1. the recovery method of acetylene during a vinyl acetate production, it is characterised in that: include the release of acetylene absorption, acetylene and acetylene three unit processes of washing, concretely comprise the following steps:
Step 1, acetylene absorption
The reacting gas discharged by gas separation column in vinyl acetate synthesis operation is collected to discharging gas-collection vessel (1)；Described reacting gas includes that acetylene, noble gas and acetaldehyde, described noble gas include nitrogen and carbon dioxide；
Absorption tower (3) is set, discharge the reacting gas in gas-collection vessel (1) after the first pressurized equipment (2) pressurizes, it is passed through absorption tower (3) from absorption tower lower entrances (3a), absorbing liquid is passed through absorption tower (3) from absorption tower upper entrance (3b), reacting gas and absorbing liquid counter current contacting, make the acetylene in reacting gas and acetaldehyde be absorbed, and discharge from absorption tower outlet at bottom (3c) with absorbing liquid；Unabsorbed noble gas is discharged from absorption tower top exit (3d)；
Described absorbing liquid is at least one in acetic acid and vinyl acetate；
Step 2, acetylene discharge
Degassing tower (5) is set, after the tower bottoms discharged from absorption tower outlet at bottom (3c) pumps into heat exchanger (13) heat exchange by the first pump (4), degassing tower stripping stage (51) is entered again from degassing tower centre entrance (5a), absorbed gas is made to desorb from absorbing liquid under high-temperature low-pressure, after desorbing, absorbing liquid is discharged from degassing tower outlet at bottom (5e), the major part desorbed includes acetylene, the gas of acetaldehyde and vinyl acetate exports (5b) extraction from degassing tower middle and upper part, remainder continues upwardly into degassing tower absorber portion (52)；Condensing through brine condenser (10) from the gas of degassing tower middle and upper part outlet (5b) extraction, return in degassing tower after being condensed by vinyl acetate therein, uncooled acetylene and aldehydes gas send into gas recovery collecting tank (6)；
Absorbing liquid enters degassing tower absorber portion (52) from degassing tower upper entrance (5c), not from gas and the absorbing liquid counter current contacting of outlet (5b) extraction of degassing tower middle and upper part, major part is absorbed, remainder is discharged from degassing tower top exit (5d), and send into discharge gas-collection vessel (1), proceed to process；Complete the absorbing liquid after absorbing to discharge from degassing tower outlet at bottom (5e) equally；
Step 3, acetylene are washed
Water scrubber (8) is set, gas in gas recovery collecting tank (6) is sent into water scrubber bottom inlet (8a) by the second pressurized equipment (7), water scrubber (8) is two sections of settings, sequentially consist of water scrubber one section (81) and water scrubber two-stage nitration (82)
Gas is successively in water scrubber one section (81) and water scrubber two-stage nitration (82) and water counter current contacting, remove the acetaldehyde in gas, residue acetylene is discharged from water scrubber top exit (8b), sends into reuse in acetylene method vinyl acetate synthesis operation.
Recovery method the most according to claim 1, it is characterised in that:
The operation pressure on absorption tower described in step 1 is 35～45KPa, and absorbing liquid temperature is 0～3 DEG C；
The tower pressure of degassing tower described in step 2 is 1～3Kpa, and wherein the temperature of degassing tower stripping stage (51) is 60～90 DEG C, and in degassing tower absorber portion (52), absorbing liquid temperature is 0～3 DEG C；From degassing tower middle and upper part, outlet (5b) expellant gas is cooled to 0～5 DEG C through brine condenser (10)；
In water scrubber described in step 3 water temperature of water scrubber one section control 4～7 DEG C, the voltage-controlled system of tower 18～22KPa, the water temperature of water scrubber two-stage nitration controls at 0～3 DEG C, and the voltage-controlled system of tower is 18～22Kpa.
Recovery method the most according to claim 1 and 2, it is characterized in that: the absorbing liquid warp discharged from degassing tower outlet at bottom (5e) pumps into heat exchanger (13) heat exchange by the second pump (11), again after absorbing liquid condenser (9) is lowered the temperature, introducing absorption tower upper entrance (3b) and degassing tower upper entrance (5c), absorbing liquid recycles in absorption tower (3) and degassing tower (5).
Recovery method the most according to claim 3, it is characterized in that: the lower end of described degassing tower stripping stage (51) is absorbing liquid canned paragraphs (53), the degassing tower outlet at bottom of described absorbing liquid canned paragraphs (53) bottom is connected to the absorbing liquid entrance of reboiler (12), and the steam (vapor) outlet of described reboiler (12) is communicated in more than the liquid level of described absorbing liquid canned paragraphs (53)；The absorbing liquid outlet of described reboiler (12) is connected to the second pump (11)；
The temperature of described degassing tower stripping stage is to heat absorbing liquid by reboiler (12), and the absorbing liquid steam of generation enters Analytic Tower (5) and realizes.
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| CN108144648A (en) * | 2018-01-29 | 2018-06-12 | 安徽皖维高新材料股份有限公司 | A kind of preparation method of acetylene in gas phase method synthesizing vinyl acetate catalyst |
| CN111437784A (en) * | 2020-05-20 | 2020-07-24 | 内蒙古蒙维科技有限公司 | Device and method for accelerating shutdown replacement of vinyl acetate production system |
| CN113398721B (en) * | 2021-05-24 | 2022-10-04 | 太原科技大学 | Acetylene, chloroethylene and overflow water recycling system and method |
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| CN102701896B (en) * | 2012-06-06 | 2014-06-25 | 西南石油大学 | Composite solvent for purifying acetylene and purification method thereof |
| CN204752561U (en) * | 2015-07-27 | 2015-11-11 | 安徽皖维高新材料股份有限公司 | Recovery unit of acetylene in vinyl acetate production process |
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Denomination of invention: A method and device for recovering acetylene in the production process of vinyl acetate Granted publication date: 20160928 Pledgee: China Construction Bank Corporation Chaohu Tuanjie Road Branch Pledgor: ANHUI WANWEI UPDATED HIGH-TECH MATERIAL INDUSTRY Co.,Ltd. Registration number: Y2024980005092 |
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