CN106349190B - The method of rectification residue and liquid extraction ketene dimer after pump - Google Patents
The method of rectification residue and liquid extraction ketene dimer after pump Download PDFInfo
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- CN106349190B CN106349190B CN201610750191.2A CN201610750191A CN106349190B CN 106349190 B CN106349190 B CN 106349190B CN 201610750191 A CN201610750191 A CN 201610750191A CN 106349190 B CN106349190 B CN 106349190B
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- C07—ORGANIC CHEMISTRY
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- C07D305/00—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms
- C07D305/02—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms not condensed with other rings
- C07D305/10—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms not condensed with other rings having one or more double bonds between ring members or between ring members and non-ring members
- C07D305/12—Beta-lactones
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Abstract
The present invention relates to the methods of rectification residue and liquid extraction ketene dimer after pump, comprise the following steps：A, in hydrolysing step, level-one residue is with liquid after pump with 2:1 ratio mixing, 65-75.C is heated to by kestner long-tube evaporator, ketene dimer is evaporated, the crude product ketene dimer to be cooled down by level-one, secondary condenser enters high-level storage groove and enters rectification section together after the crude product ketene dimer mixing that polymerization workshop section generates；B, the two level residue and the aceticanhydride of condenser that kestner long-tube evaporator is formed, which are entered in hydrolysis workshop section, to be hydrolyzed, and obtains acetone, spirit of vinegar and solid waste residue；C, the tail gas of workshop section is hydrolyzed, send to water scrubber and absorbs.It is an advantage of the invention that the ketene dimer by kestner long-tube evaporator heating recovery, improves the yield of ketene dimer in internal system, reduce the consumption of glacial acetic acid, the exhaust gas and residue of production process generation, the zero-emission largely reduced with sewage of solid waste are digested and assimilated.
Description
Technical field
The invention belongs to the production method that the acetic acid cracking method in chemical production field prepares ketene dimer, more particularly to one
The method of kind rectification residue and liquid extraction ketene dimer after pump.
Background technology
Acetic acid cracking method is to prepare the main method of ketene dimer at present.Because of ketene dimer category heat-sensitive substance, synthesizing
The high polymer and autopolymer of indissoluble are easily formed in the process, and the primary solids that these polymers are constituted in ketene dimer technique are residual
Slag.Mainly comprising aceticanhydride, ketene dimer, ketenes high polymer etc. in residue, and with penetrating odor.At present to residue
Processing method mainly hydrolyzes, and after being recycled after hydrolysis to acetone and acetic acid, residual residue is directly discharged in environment, meeting
Very big pollution is caused, and wastes fuel and active principle valuable in residue.In addition, ketene dimer produced
Cheng Zhonghui generates a large amount of gases, is typically chosen direct discharge, will also result in very big loss of material and environmental pollution.How to realize
After pump the extraction of 40-50% contents ketene dimer and the residue that generates and exhaust gas in ketene dimer production process are realized in liquid
Recycling comprehensive utilization becomes ketene dimer industry problem urgently to be resolved hurrily.
The content of the invention
Present invention aim to solve the reluctant defect of corresponding ketene dimer, a kind of rectification residue provided
With the method for liquid extraction ketene dimer after pump.
The technical solution adopted by the present invention is as follows：
A kind of method of rectification residue and liquid extraction ketene dimer after pump, including following basic process steps：Cracking, step by step condensation,
Separator and oily piece-rate system, absorption, polymerization, rectifying, Slag recovering processing, hydrolysis, dilute acid recycle, concentrate, it is characterised in that：
A, in hydrolysing step, the level-one residue generated after rectification section is with liquid after pump with 2:It is residual that 1 ratio is mixed into level-one
Slag dilution, level-one residue dilution are heated to 65-75.C by kestner long-tube evaporator, ketene dimer are evaporated, passes through one
Grade condensation is cooled to 18-22 C °, is cooled to 5-10 C ° into secondary condenser, the crude product ketene dimer of condensation enters high-order storage
Slot and from absorb, polymerization workshop section generation crude product ketene dimer mixing after together enter rectification section；
B, kestner long-tube evaporator is formed two level residue and 4#-6# condensers and the aceticanhydride that separator generates enter two level residue
Thinning tank carries out being mixed into two level residue dilution, is sent in hydrolysis workshop section and is hydrolyzed after two level residue dilution；
Heating diluted acid is first passed through in the hydrolysis kettle of hydrolysis workshop section, forms reflux, then two level residue dilution is added dropwise
Enter, reaction, wherein ketene dimer and acetic acid reaction generation aceticanhydride, acetone and carbon dioxide is hydrolyzed；Aceticanhydride and water reaction
Acetic acid is generated, final products obtained therefrom is acetone, spirit of vinegar and solid waste residue, and workshop section separates back the acetone of gained in hydrolysis
It receives, the acetone of recycling becomes product by purification 99%.Reaction equation is：
Ketene dimer acetic acid aceticanhydride acetone carbon dioxide
（CH3CO）2O+H2O — 2CH3COOH
Aceticanhydride water acetic acid
In hydrolysis, workshop section separates and recovers the acetone of gained, and the acetone of recycling becomes product by purification 99%,
C, the tail gas during the solid waste residue blowing of workshop section is hydrolyzed, being evacuated to water scrubber by air-introduced machine absorbs, and works as concentration
Reach 15% or so and turn to the recycling use of concentrate dilute acid bath.
On the basis of above-mentioned technical proposal, there can be following further improvement project：
The acetic acid of gained enters spirit of vinegar concentrate workshop section in hydrolysis workshop section, and film is carried out after the Sewage treatment butyl acetate of generation
Separation, isolated recovery of acetic acid and dense acetic acid are configured to the raw material cracking acid of cracking workshop section, and separating obtained water is suction
It receives used in tower and water scrubber.
For the exhaust gas that rectifying, hydrolysis workshop section generate using water is concentrated to absorb, exhaust gas is mainly uncooled ketenes and acetic acid
Gas also cracks the gas that workshop section's side reaction generates, and the main component after water absorbs is methane, carbon monoxide, titanium dioxide
Carbon, ethylene.Into the special burner combustion of pyrolysis furnace after Safety water seal, as a part of heat of acetic acid cracking, reaction
Equation is as follows：
Cracking side-reaction generates gas：
2CH3COOH ——CH2= CO + CH4 + H2O + CO2
Vinyl acetate ketone methane water carbon dioxide
2CH2=CO —C2H4 + 2CO
Ketenes ethylene carbon monoxide
2CH2=CO — CH4+CO2 +2C
Ketenes methane carbon
Water absorbs chemical equation：
CH2=CO+H2O —CH3COOH
Ketenes water acetic acid
CH2=CO+CH3COOH —（CH3CO）2O
Ketenes acetic acid aceticanhydride
（CH3CO）2O+H2O —2CH3COOH
Aceticanhydride water acetic acid
It is an advantage of the invention that by Optimizing Flow, recycled in advance in dilution by the heating of level-one kestner long-tube evaporator
Ketene dimer, while the circulation route recycled by tail gas and draining improves the yield of ketene dimer inside the system,
Reduce the consumption of glacial acetic acid, digest and assimilate production process generation exhaust gas and residue, largely reduce with sewage the zero of solid waste
Discharge.
The yield of ketene dimer is further improved on the basis of inventory is constant, reduces the consumption of raw material glacial acetic acid, simultaneously
The residue emission reduction generated in ketene dimer production process and exhaust gas, the problem of complex utilization of waste water are solved, a kind of rectifying is provided
The method of residue and liquid extraction ketene dimer after pump.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Specific implementation method：
Embodiment 1
As shown in Figure 1, the present invention provides the production method of a kind of rectification residue and liquid mixed liquor extraction ketene dimer after pump,
Comprise the following steps：
A. 85% spirit of vinegar recycled 99.8% dense acetic acid and system is configured to cracking acid in proportion, is thrown in pyrolysis furnace
1.8 T 96% cracking acid, pyrolysis furnace control of export temperature be 710-730 degree, 75-80 KPa of pressure.By No. 1-6 condensation
The ketene gas of device condensation, is sent into polymerization workshop section, obtains the thick ketene dimers of 0.846 T, and then rectification and purification obtains 0.765 T pairs
Ketenes finished product generates level-one residue 0.085T.
B. liquid after the pump level-one residue generated after rectification section generated with oily piece-rate system（Wherein crude product ketene dimer
Content 40%, acid anhydride content 40-50%, rest part are acetic acid）, with 2:1 ratio is mixed into level-one residue dilution, actual amount
Liquid and 0.8-1.0T level-one residues after being pumped for 0.4-0.5T are heated to 65-75.C double second by film-type evaporation heater
Ketenes is evaporated, and two level residue is expelled to two level residue thinning tank and 4#-6# condensers and separator generation aceticanhydride mixing shape
It is diluted into two level residue, is sent in hydrolysis workshop section and is hydrolyzed.It hydrolyzes and 0.9T spirit of vinegars is put into the hydrolysis kettle of workshop section（Concentration
40%）, in 5-10a of pressure, temperature is maintained at dropwise addition two level residue dilution at 150-155 DEG C, and time for adding is 2-3h, instead
For for 24 hours between seasonable.To the end of reaction, acetone 150-200 Kg, 80% spirit of vinegar, 1200 Kg of 40-50% are recycled.In addition hydrolyze
Solid waste 50KG（Former technique 500kg）.
C. the tail gas during two dropwise addition residue blowings and the tail gas during slagging are evacuated to water scrubber by air-introduced machine and inhale
It receives, the recycling use of concentrate dilute acid bath is turned to when acetate concentration reaches 15%.
D. 15% spirit of vinegar recycled enters spirit of vinegar concentrate workshop section, puts into 1800 Kg spirit of vinegars per hour, obtains 1200 Kg
85% acetic acid generates 600 Kg waste water.A small amount of butyl acetate acetone recycling in waste water, returns to diluted acid concentrate workshop section.Then
Waste water enters seperation film, and isolated recovery of acetic acid is configured to the raw material cracking acid of cracking workshop section with dense acetic acid, and separates institute
The water obtained is used in absorption tower and water scrubber.
E. the gas sampling generated rectifying, hydrolysis workshop section, puts into 1.5m3Water Xun Huan is absorbed, when concentration reaches 15%
Left and right turns to the recycling of concentrate dilute acid bath and uses.
Claims (3)
1. the method for rectification residue and liquid extraction ketene dimer after pump, including following basic process steps：Cracking, step by step condensation,
Separator and oily piece-rate system are separated, absorbed, polymerize, rectifying, Slag recovering processing, hydrolysis, dilute acid recycle, concentrate,
It is characterized in that：
A, in hydrolysing step, the level-one residue generated after rectification section is with liquid after pump with 2:It is dilute that 1 ratio is mixed into level-one residue
Liquid is released, level-one residue dilution is heated to 75 DEG C of 65- by kestner long-tube evaporator, ketene dimer is evaporated, cold by level-one
It is solidifying to be cooled to 18-22 DEG C, be cooled to 5-10 DEG C into secondary condenser, the crude product ketene dimer of condensation enter high-level storage groove and from
It absorbs, enter rectification section together after the crude product ketene dimer mixing of polymerization workshop section generation；
B, kestner long-tube evaporator is formed two level residue and 4#-6# condensers and the aceticanhydride that separator generates enter the dilution of two level residue
Tank carries out being mixed into two level residue dilution, is sent in hydrolysis workshop section and is hydrolyzed after two level residue dilution；
Heating diluted acid is first passed through in the hydrolysis kettle of hydrolysis workshop section, forms reflux, then the dropwise addition of two level residue dilution is entered,
Reaction, wherein ketene dimer and acetic acid reaction generation aceticanhydride, acetone and carbon dioxide is hydrolyzed；Aceticanhydride and water reaction generation vinegar
Acid, final products obtained therefrom are acetone, spirit of vinegar and solid waste residue；
C, the tail gas during the solid waste residue blowing of workshop section is hydrolyzed, being evacuated to water scrubber by air-introduced machine absorbs, when concentration reaches
15%, which turns to the recycling of concentrate dilute acid bath, uses.
2. the method for rectification residue according to claim 1 and liquid extraction ketene dimer after pump, it is characterised in that：
The spirit of vinegar of gained enters spirit of vinegar concentrate workshop section in hydrolysis workshop section, and film point is carried out after the Sewage treatment butyl acetate of generation
From isolated recovery of acetic acid is configured to the raw material cracking acid of cracking workshop section with dense acetic acid, and separating obtained water is to absorb
Used in tower and water scrubber.
3. the method for rectification residue according to claim 1 or 2 and liquid extraction ketene dimer after pump, it is characterised in that：
For the exhaust gas that rectifying, hydrolysis workshop section generate using water is concentrated to absorb, exhaust gas is mainly uncooled ketenes and acetic gas,
The gas that workshop section's side reaction generates also is cracked, the main component after water absorbs is methane, carbon monoxide, carbon dioxide, second
Alkene, into the special burner combustion of pyrolysis furnace after Safety water seal, a part of heat as acetic acid cracking.
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| PT3319949T (en) | 2016-09-21 | 2020-10-12 | Celanese Int Corp | Acesulfame potassium compositions and processes for producing same |
| DK3319948T3 (en) | 2016-09-21 | 2021-09-27 | Celanese Int Corp | Acesulfame-potassium compositions and methods for their preparation |
| PL3322695T3 (en) | 2016-09-21 | 2021-01-11 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| CN108358874B (en) * | 2018-01-13 | 2022-02-15 | 安徽金禾实业股份有限公司 | Multi-section production method and device for diketene |
| CN110075661A (en) * | 2019-05-30 | 2019-08-02 | 山东亚邦化工科技有限公司 | The processing method and device of ketene dimer technology waste gas |
| CN110787496B (en) * | 2019-09-30 | 2022-01-25 | 安徽金禾实业股份有限公司 | Diketene standing oil recovery device and method |
| CN113135837B (en) * | 2020-01-18 | 2024-07-05 | 济宁康德瑞化工科技有限公司 | Triethylamine oxide cracking process tail gas treatment system |
| CN111333485B (en) * | 2020-03-16 | 2022-05-13 | 宁波王龙科技股份有限公司 | Treatment method of diketene production wastewater |
| CN115521198A (en) * | 2022-09-16 | 2022-12-27 | 宁波王龙科技股份有限公司 | Diluted acid hydrolysis process |
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| CN202128933U (en) * | 2011-06-09 | 2012-02-01 | 江苏天成生化制品有限公司 | Ketene dimer rectifying apparatus capable of discharging under normal pressure continuously |
| CN103113186A (en) * | 2012-11-11 | 2013-05-22 | 安徽金禾实业股份有限公司 | Treating method and treating device for ketene dimer production residues |
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| CN202128933U (en) * | 2011-06-09 | 2012-02-01 | 江苏天成生化制品有限公司 | Ketene dimer rectifying apparatus capable of discharging under normal pressure continuously |
| CN103113186A (en) * | 2012-11-11 | 2013-05-22 | 安徽金禾实业股份有限公司 | Treating method and treating device for ketene dimer production residues |
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