CN106349190A - Method for extracting ketene dimer by rectifying residues and pumped liquid - Google Patents
Method for extracting ketene dimer by rectifying residues and pumped liquid Download PDFInfo
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- CN106349190A CN106349190A CN201610750191.2A CN201610750191A CN106349190A CN 106349190 A CN106349190 A CN 106349190A CN 201610750191 A CN201610750191 A CN 201610750191A CN 106349190 A CN106349190 A CN 106349190A
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- ketene dimer
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- 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 invention relates to a method for extracting ketene dimer by rectifying residues and pumped liquid. The method comprises the following steps that firstly, hydrolysis is carried out, wherein primary residues and the pumped liquid are mixed in the proportion of 2:1 and heated to 65-75 DEG C through a membrane type evaporator, ketene dimer is evaporated out, crude ketene dimer obtained through cooling of a primary condenser and a secondary condenser enters a high-order storage tank and is mixed with crude ketene dimer generated in a polymerization section, and then mixed crude ketene dimer enters a rectifying section; secondly, secondary residues formed in the membrane type evaporator and acetic anhydride in the condensers enter a hydrolysis section for hydrolysis, and acetone, dilute acetic acid and solid waste residues are obtained; thirdly, tail gas at the hydrolysis section is fed to a water scrubber to be absorbed. The method has the advantages that crude ketene dimer is recycled through heating of the membrane evaporator, the yield of crude ketene dimer is increased inside the system, consumption of glacial acetic acid is reduced, waste gas and residues generated in the production process are digested and absorbed, solid waste is greatly reduced, and zero waste water emission is achieved.
Description
Technical field
The invention belongs to the acetic acid cracking method in chemical production field prepares the production method of ketene dimer, particularly to one
The method that after planting rectification residue and pump, liquid extracts ketene dimer.
Background technology
Acetic acid cracking method is to prepare the main method of ketene dimer at present.Because ketene dimer belongs to heat-sensitive substance, in synthesis
During easily form high polymer and the autopolymer of indissoluble, the primary solids that these polymers constitute in ketene dimer technique are residual
Slag.Mainly comprise acetic anhydride, ketene dimer, ketenes high polymer etc. in residue, and there is penetrating odor.At present to residue
Processing method is mainly hydrolysis, and after acetone and acetic acid being reclaimed after hydrolysis, residual residue is directly discharged in environment, meeting
Cause very big pollution, and waste valuable fuel in residue and active substance.In addition, ketene dimer produced
Cheng Zhonghui produces 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
The extraction of 40-50% content ketene dimer and realize residue and the waste gas producing in ketene dimer production process in liquid after pump
Reclaiming comprehensive utilization becomes a ketene dimer industry difficult problem urgently to be resolved hurrily.
Content of the invention
Present invention aim to solving the reluctant defect of corresponding ketene dimer, a kind of rectification residue providing
The method extracting ketene dimer with liquid after pump.
The technical solution used in the present invention is as follows:
A kind of method that after rectification residue and pump, liquid extracts ketene dimer, includings following basic process steps: crack, cold step by step
Solidifying, separator and separating of oil system, absorption, polymerization, rectification, Slag recovering process, hydrolysis, dilute acid recycle, concentration, its feature exists
In:
In a, hydrolysing step, after the one-level residue producing after rectification section and pump, to be mixed into one-level residue with the ratio of 2:1 dilute for liquid
Release liquid, one-level residue diluent is heated to 65 75.c by kestner long-tube evaporator, ketene dimer is evaporated, cold by one-level
Solidifying be cooled to c ° of 18-22, enter secondary condenser and be cooled to c ° of 5-10, the crude product ketene dimer of condensation enter high-level storage groove and
Enter rectification section together after the crude product ketene dimer absorbing, polymerization workshop section generates mixes；
Two grades of residues that b, kestner long-tube evaporator are formed and the acetic anhydride of 4#-6# condenser and separator generation enter two grades of residues dilutions
Tank carries out being mixed into two grades of residue diluents, delivers in hydrolysis workshop section and be hydrolyzed after two grades of residue diluents；
First pass through heating diluted acid in the hydrolysis kettle of hydrolysis workshop section, form backflow, then two grades of residue diluent Deca are entered,
Be hydrolyzed reaction, and wherein ketene dimer and acetic acid reaction generate acetic anhydride, acetone and carbon dioxide；Acetic anhydride and water reaction generate vinegar
Acid, final products obtained therefrom is acetone, spirit of vinegar and solid waste residue, and in hydrolysis, workshop section separates and recovers to the acetone of gained, returns
The acetone received passes through purification 99% and becomes product.Reaction equation is:
Ketene dimer acetic acid acetic anhydride acetone carbon dioxide
(ch3Co)2o+h2o — 2ch3cooh
Acetic anhydride water acetic acid
In hydrolysis, workshop section separates and recovers to the acetone of gained, and the acetone of recovery passes through purification 99% becomes product,
Tail gas during c, the solid waste residue blowing of hydrolysis workshop section, is evacuated to water scrubber by air-introduced machine and absorbs, when concentration reaches
15% about turns to concentration dilute acid bath reclaims use.
On the basis of technique scheme, can there is a further improvement project as follows:
In hydrolysis workshop section, the acetic acid of gained enters spirit of vinegar concentration workshop section, carries out film and divide after the waste water reclamation butyl acetate of generation
From it is sour with the raw material cracking that dense acetic acid is configured to crack workshop section to separate the recovery of acetic acid obtaining, and separating obtained water is to absorb
Used by tower and water scrubber.
Using concentrating water to absorb, waste gas is mainly uncooled ketenes and acetic acid to the waste gas that rectification, hydrolysis workshop section produce
Gas, the gas that also side reaction of cracking workshop section produces, the main component after absorbing through water is methane, carbon monoxide, titanium dioxide
Carbon, ethylene.Enter the special burner combustion of pyrolysis furnace after Safety water seal, as a part of heat of acetic acid cracking, react
Equation is as follows:
Cracking side-reaction generation 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 absorption chemical equation:
ch2= co + h2o — ch3cooh
Ketenes water acetic acid
ch2= co + ch3Cooh (ch3Co)2o
Ketenes acetic acid acetic anhydride
(ch3Co)2o+h2o —2ch3cooh
Acetic anhydride water acetic acid
It is an advantage of the invention that passing through Optimizing Flow, reclaimed double in diluent in advance by the heating of one-level kestner long-tube evaporator
Ketenes, pass through the circulation route that tail gas and draining are reclaimed simultaneously, improve the yield of ketene dimer, reduce inside the system
The consumption of glacial acetic acid, digests and assimilates waste gas and residue, a large amount of minimizings of solid waste and the zero-emission of sewage of production process generation.
Improve the yield of ketene dimer further on the basis of inventory is constant, reduces raw material glacial acetic acid and consume, simultaneously
Solve the problem of complex utilization of the residue reduction of discharging and waste gas, waste water producing in ketene dimer production process, a kind of rectification is provided
The method that after residue and pump, liquid extracts ketene dimer.
Brief description
Fig. 1 is the process chart of the present invention.
Specific implementation method:
Embodiment 1
As shown in figure 1, the present invention provides a kind of production method of liquid mixed liquor extraction ketene dimer after rectification residue and pump, including
Following steps:
A. 85% spirit of vinegar that 99.8% dense acetic acid and system reclaim is configured to cracking acid in proportion, throws 1.8 in pyrolysis furnace
The cracking acid of t 96%, pyrolysis furnace control of export temperature is 710-730 degree, pressure 75 80 kpa.Cold through 1-6 condenser
Solidifying ketene gas, send into polymerization workshop section, obtain the thick ketene dimer of 0.846 t, and then rectification and purification obtains the double ethylene of 0.765 t
Ketone finished product, produces one-level residue 0.085t.
B. liquid (wherein crude product ketene dimer after the pump one-level residue producing after rectification section being produced with separating of oil system
Content 40%, acid anhydride content 40 50%, remainder is acetic acid), one-level residue diluent, actual amount are mixed into the ratio of 2:1
For liquid after 0.4-0.5t pump and 0.8-1.0t one-level residue, 65 75.c are heated to double second by film-type evaporation heater
Ketenes is evaporated, and two grades of residues are expelled to two grades of residue thinning tanks and 4#-6# condenser and separator generation acetic anhydride mixing shape
Become two grades of residue dilutions, deliver in hydrolysis workshop section and be hydrolyzed.0.9t spirit of vinegar (concentration is put in the hydrolysis kettle of hydrolysis workshop section
40%), in pressure 5 10a, temperature be maintained at 150-155 DEG C at two grades of residue diluents of Deca, time for adding be 2 3h, instead
It is 24h between seasonable.Question response terminates, and reclaims acetone 150-200 kg, 80% spirit of vinegar 1200 kg of 40-50%.In addition hydrolyze
Former technique 500kg of solid waste 50kg().
C. the tail gas during two Deca residue blowings and the tail gas during slagging are evacuated to water scrubber by air-introduced machine and inhale
Receive, turn to the recovery use of concentration dilute acid bath when acetate concentration reaches 15%.
D. 15% spirit of vinegar reclaiming enters spirit of vinegar concentration workshop section, puts into 1800 kg spirit of vinegars per hour, obtains 1200 kg
85% acetic acid, produces 600 kg waste water.A small amount of butyl acetate acetone in waste water reclaims, and returns to diluted acid concentration workshop section.Then
Waste water enters seperation film, separates the recovery of acetic acid obtaining and dense acetic acid is configured to crack the raw material cracking acid of workshop section, and separate institute
The water obtaining is used by absorption tower and water scrubber.
E. the gas sampling producing rectification, hydrolysis workshop section, puts into 1.5m3Water circulation is absorbed, when concentration reaches 15%
Left and right turns to concentration dilute acid bath and reclaims use.
Claims (3)
1. the method that after rectification residue and pump, liquid extracts ketene dimer, includings following basic process steps: cracking, condense step by step,
Separator and separating of oil system, absorption, polymerization, rectification, Slag recovering process, hydrolysis, dilute acid recycle, concentration it is characterised in that:
In a, hydrolysing step, after the one-level residue producing after rectification section and pump, to be mixed into one-level residue with the ratio of 2:1 dilute for liquid
Release liquid, one-level residue diluent is heated to 65 75.c by kestner long-tube evaporator, ketene dimer is evaporated, cold by one-level
Solidifying be cooled to c ° of 18-22, enter secondary condenser and be cooled to c ° of 5-10, the crude product ketene dimer of condensation enter high-level storage groove and
Enter rectification section together after the crude product ketene dimer absorbing, polymerization workshop section generates mixes；
Two grades of residues that b, kestner long-tube evaporator are formed and the acetic anhydride of 4#-6# condenser and separator generation enter two grades of residues dilutions
Tank carries out being mixed into two grades of residue diluents, delivers in hydrolysis workshop section and be hydrolyzed after two grades of residue diluents；
First pass through heating diluted acid in the hydrolysis kettle of hydrolysis workshop section, form backflow, then two grades of residue diluent Deca are entered,
Be hydrolyzed reaction, and wherein ketene dimer and acetic acid reaction generate acetic anhydride, acetone and carbon dioxide；Acetic anhydride and water reaction generate vinegar
Acid, final products obtained therefrom is acetone, spirit of vinegar and solid waste residue；
Tail gas during c, the solid waste residue blowing of hydrolysis workshop section, is evacuated to water scrubber by air-introduced machine and absorbs, when concentration reaches
15% about turns to concentration dilute acid bath reclaims use.
2. after rectification residue according to claim 1 and pump liquid extract ketene dimer method it is characterised in that:
In hydrolysis workshop section, the spirit of vinegar of gained enters spirit of vinegar concentration workshop section, carries out film and divide after the waste water reclamation butyl acetate of generation
From it is sour with the raw material cracking that dense acetic acid is configured to crack workshop section to separate the recovery of acetic acid obtaining, and separating obtained water is to absorb
Used by tower and water scrubber.
3. after rectification residue according to claim 1 and 2 and pump liquid extract ketene dimer method it is characterised in that:
Using concentrating water to absorb, waste gas is mainly uncooled ketenes and acetic gas to the waste gas that rectification, hydrolysis workshop section produce,
Also has the gas that the side reaction of cracking workshop section produces, the main component after absorbing through water is methane, carbon monoxide, carbon dioxide, second
Alkene, enters the special burner combustion of pyrolysis furnace, as a part of heat of acetic acid cracking after Safety water seal.
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| US10023546B2 (en) | 2016-09-21 | 2018-07-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10030000B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10029999B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
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| CN108358874A (en) * | 2018-01-13 | 2018-08-03 | 安徽金禾实业股份有限公司 | A kind of ketene dimer multiplexing section production method and device |
| 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 |
| CN110787496A (en) * | 2019-09-30 | 2020-02-14 | 安徽金禾实业股份有限公司 | Diketene standing oil recovery device and method |
| CN111333485A (en) * | 2020-03-16 | 2020-06-26 | 宁波王龙科技股份有限公司 | Treatment method of diketene production wastewater |
| CN113135837A (en) * | 2020-01-18 | 2021-07-20 | 济宁康德瑞化工科技有限公司 | Treatment system of triethylamine oxide cracking process tail gas |
| 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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