CN208776607U - Acetic acid refining and entrainer regenerating unit in polyvinyl alcohol disposing mother liquor unit - Google Patents
Acetic acid refining and entrainer regenerating unit in polyvinyl alcohol disposing mother liquor unit Download PDFInfo
- Publication number
- CN208776607U CN208776607U CN201821267309.7U CN201821267309U CN208776607U CN 208776607 U CN208776607 U CN 208776607U CN 201821267309 U CN201821267309 U CN 201821267309U CN 208776607 U CN208776607 U CN 208776607U
- Authority
- CN
- China
- Prior art keywords
- acetic acid
- tower
- entrainer
- acid refining
- unit
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application belongs to chemical production technical field, and in particular to acetic acid refining and entrainer regenerating unit in a kind of polyvinyl alcohol disposing mother liquor unit.Described device includes: acetic acid refining unit, entrainer recovery unit and entrainer regeneration unit；The acetic acid refining unit, entrainer recovery unit and entrainer regeneration unit are sequentially connected composition circulation；The acetic acid refining unit further includes two branches, and a branch is connected with entrainer regeneration unit, and one is connected with finished product acetic acid cooler, recovery of acetic acid.The entrainer regenerating unit of the application improves product quality stability to the operational stability of enhancing acetic acid refining process, and reducing process material consumption has important practical significance, and can bring significant economic benefit for manufacturing enterprise.
Description
Technical field
The utility model belongs to chemical production technical field, and in particular to acetic acid in a kind of polyvinyl alcohol disposing mother liquor unit
Purification and entrainer regenerating unit.
Background technique
Polyvinyl alcohol (abbreviation PVA) appearance is white powder, is a kind of water soluble polymer, performance is between plastics
Between rubber, in terms of textile industry, building decoration industry, chemical industry, agricultural, daily cosmetics and high-frequency quenching
It is widely used.PVA be uniquely can polyvinyl by bacterium as carbon source and using energy source, belonging to a kind of biology can drop
Solve high molecular material.PVA can be mass produced by Non oil-based route, cheap, oil resistant, solvent resistant and gas barrier property
It is outstanding, food, in terms of have unique advantage.
Generate a large amount of alcohol hydrolysis mother liquor during polyvinyl acetate alcoholysis production polyvinyl alcohol, main group become methanol,
Methyl acetate and sodium acetate etc..These are all important industrial chemicals and should be recycled.Methyl acetate is actually by raw material vinegar
What acid and methanol generated, 1 ton of polyvinyl alcohol of every production just generates about 1.5 tons of methyl acetates.Although methyl acetate is also a kind ofization
Work raw material, but demand is small is generally sold not as by-product, need to methyl acetate hydrolysis at acetic acid and methanol, through separation and
Vinyl acetate synthesis and polymerization are back to after purification.In industrial processes, methyl acetate is in storng-acid cation exchange resin
Under the action of, be shown below hydrolysis, generate acetic acid and methanol:
CH3COOCH3+H2O===CH3OH+CH3COOH
Because acetic acid is extremely low in the relative volatility of low concentration region and water, the spirit of vinegar that methyl acetate hydrolysis generates is in concentration essence
It is separated during system frequently with heterogeneous azeotropic rectification method.Entrainer multiselect acetates, such as acetic acid is just
Butyl ester, n-propyl acetate, isopropyl acetate and ethyl acetate etc..In the actual production process, with entrainer service life
Increase, entrainer quality reduces, and band outlet capacity declines, and acetic acid refining tower energy consumption increases.For example, inventor has found that acetates exist
In azeotropic distillation dehydration and water, acetic acid are constantly in fluidized state together, and it is anti-to issue unboiled water solution in acetic acid autocatalysis
It answers, generates acetic acid and corresponding alcohol.These generate alcohol and raw material spirit of vinegar bring methanol and methyl acetate has together constituted with vinegar
The impurity source of entrainer in acid concentration subtractive process.Since entrainer is recycled, these impurity are gradually concentrated into originally
Several times, even tens times, on the one hand can destroy the azeotropism of acetate and water, in addition also will affect azeotropic mixture split-phase effect
Fruit.In order to solve the problems, such as that entrainer band outlet capacity declines, at present using discharge portion at regular intervals in industrial processes
Divide useless entrainer, and the method for supplementing the new entrainer of equivalent maintains device normally to produce.Although this measure is to a certain extent
The problem of entrainer quality reduces can be alleviated, but interval is mended, row's entrainer can cause entrainer water separation capability to fluctuate, and causes to operate
Stability is poor, and operation energy consumption is high；And in the useless entrainer discharged still based on acetate entrainer, entrainer consumption is higher.
Utility model content
To solve the above problems, the utility model provides the following technical solutions:
Acetic acid refining and entrainer regenerating unit in a kind of polyvinyl alcohol disposing mother liquor unit, comprising: acetic acid refining unit,
Entrainer recovery unit and entrainer regeneration unit；
The acetic acid refining unit, entrainer recovery unit and entrainer regeneration unit are sequentially connected composition circulation；
The acetic acid refining unit includes two branches, and a branch is connected with entrainer regeneration unit, one and finished product
Acetic acid cooler is connected, and sends out purification acetic acid.
According to the utility model, the acetic acid refining unit further with the hydrolysis vinegar in polyvinyl alcohol disposing mother liquor unit
The preamble unit of sour methyl esters is connected.
According to the utility model, it includes but is not limited to acetic acid refining tower that the acetic acid refining unit, which is selected from,；The entrainer
It includes but is not limited to entrainer recovery tower that recovery unit, which is selected from,；It includes but is not limited to be esterified instead that the entrainer regeneration unit, which is selected from,
Answer device.
According to the utility model, the acetic acid refining tower, entrainer recovery tower and esterifier are sequentially connected composition and follow
Ring.
According to the utility model, the acetic acid refining unit further includes acetic acid refining tower condenser, acetic acid refining tower split-phase
Device, entrainer water phase pans and entrainer recovery tower feed pump；
The acetic acid refining tower condenser, acetic acid refining tower phase-splitter, entrainer water phase pans and entrainer recovery tower
Feed pump is sequentially connected according to flow direction of material；The outlet phase of the entrance of the acetic acid refining tower condenser and acetic acid refining tower top
Even；The outlet of the entrainer recovery tower feed pump is connected with the entrance on entrainer recovery tower top.
According to the utility model, the acetic acid refining unit further includes acetic acid refining tower reflux pump；
The arrival end of the acetic acid refining tower reflux pump is connected with acetic acid refining tower phase-splitter, outlet end and acetic acid refining
The tower top of tower is connected.
According to the utility model, the acetic acid refining tower phase-splitter is also connect with the device that can supplement fresh entrainer.
According to the utility model, the entrainer is selected from acetic acid C2-6Arrcostab, wherein the C2-6Alkyl, which is selected from, contains 2 to 6
The linear or branched alkyl group of a carbon atom.
Preferably, the entrainer be selected from include but is not limited to: n-butyl acetate, n-propyl acetate, isopropyl acetate or
One of ethyl acetate, two or more.
According to the utility model, the acetic acid refining unit further includes the acetic acid refining tower for being set to acetic acid refining tower tower reactor
Reboiler.
According to the utility model, the acetic acid refining unit further includes the acetic acid refining tower for being set to acetic acid refining tower tower reactor
Kettle goes out to pump.
According to the utility model, the acetic acid refining unit further includes the acetic acid refining tower being connected with acetic acid refining tower tower reactor
Adopt pump in side；It adopts pump while being connected with entrainer regeneration unit and finished product acetic acid cooler in acetic acid refining tower side.
According to the utility model, the entrainer recovery unit further includes being total to what entrainer recycling column overhead was sequentially connected
Boiling agent recovery tower condenser, entrainer recovery tower phase-splitter and entrainer recovery tower distillate pump；The entrainer recovery tower distillates
The outlet of pump is connected with entrainer regeneration unit.
According to the utility model, the entrainer recovery tower phase-splitter further with entrainer water phase in acetic acid refining unit
Pans are connected.
According to the utility model, the entrainer recovery unit further includes the entrainer for being set to entrainer recovery tower tower reactor
Recycle tower reboiler.
According to the utility model, the entrainer recovery unit further includes the entrainer for being set to entrainer recovery tower tower reactor
Tower reactor is recycled to go out to pump.
According to the utility model, the entrainer regeneration unit further includes esterification reaction solution cooler；The esterification
Liquid cooler distillates pump with entrainer recovery tower and is connected.
According to the utility model, when the entrainer regeneration unit further includes esterification reaction solution cooler, the acetic acid
It adopts pump and is connected with the esterification reaction solution cooler in entrainer regeneration unit in treating column side.
According to the utility model, the entrainer regeneration unit further include be set to esterifier and acetic acid refining tower it
Between accurate filter.
According to the utility model, the number of the accurate filter is one, two or more；When the secondary filter
When device is two or more, the accurate filter first connect and/or parallel connection after the entrance phase with acetic acid refining tower top again
Even.
According to the utility model, the accurate filter use Nomex as filter medium or other with pore
Diameter is small, and porosity is big, the filter medium of the big feature of filtering medium layer thickness.
As example, the acetic acid refining unit includes: acetic acid refining tower, acetic acid refining tower reactor pump, acetic acid refining tower out
Reboiler, acetic acid refining tower condenser, acetic acid refining tower phase-splitter, entrainer water phase pans, entrainer recovery tower feed pump,
Pump and finished product acetic acid cooler are adopted in acetic acid refining tower reflux pump, acetic acid refining tower side；
The acetic acid refining tower reactor goes out to pump and acetic acid refining tower reboiler is arranged in acetic acid refining tower tower reactor；
The acetic acid refining tower condenser, acetic acid refining tower phase-splitter, entrainer water phase pans and entrainer recovery tower
Feed pump is sequentially connected, and the acetic acid refining tower condenser inlet is connected with acetic acid refining column overhead, the entrainer recycling
Tower charging pump discharge boils agent recovery unit together and is connected；The acetic acid refining tower condenser, acetic acid refining tower phase-splitter and acetic acid
Treating column reflux pump is sequentially connected, and the acetic acid refining tower condenser inlet is connected with acetic acid refining column overhead, the acetic acid
Treating column reflux pump is connected with acetic acid refining column overhead；
The acetic acid refining tower phase-splitter is also connected with the device of acetic acid refining column overhead and the fresh entrainer of offer；
It adopts pump and is connected with acetic acid refining tower lower part in acetic acid refining tower side；Acetic acid refining tower side adopt pump further with
Finished product acetic acid cooler is connected；
The entrainer recovery unit includes: entrainer recovery tower, entrainer recovery tower condenser, entrainer recovery tower point
Phase device, entrainer recovery tower distillate pump, entrainer recycling tower reboiler and entrainer recycling tower reactor and go out to pump；
The entrainer recovery tower, entrainer recovery tower condenser, entrainer recovery tower phase-splitter, entrainer recovery tower evaporate
Pump is sequentially connected out, and the entrance of the entrainer recovery tower condenser is connected with entrainer recycling column overhead；The entrainer
The tower top of recovery tower is further connected with the entrainer recovery tower feed pump in acetic acid refining unit；
Entrainer recycling tower reboiler and entrainer recycling tower reactor go out to pump respectively with the tower reactor phase of entrainer recovery tower
Even；
The entrainer regeneration unit includes: esterification reaction solution cooler, esterifier and accurate filter；
The esterification reaction solution cooler is connected with esterifier tower top, and further and in entrainer recovery unit
Entrainer recovery tower distillates pump and is connected；The accurate filter is connected with the tower reactor of the esterifier, and further with vinegar
The tower reactor of acetic acid refining tower is connected in acid treating unit；
Acetic acid refining tower side adopts pump and is further also connected with esterification reaction solution cooler in the acetic acid refining unit.
The application also provides acetic acid refining and entrainer regeneration technology in a kind of polyvinyl alcohol disposing mother liquor unit, comprising:
(1) entrainer is added into acetic acid refining unit；
(2) spirit of vinegar of the preamble unit from hydrolysis methyl acetate is sent into acetic acid refining unit, to through acetic acid refining
Acetic acid a part of unit separation is collected, and another part enters entrainer regeneration unit；
(3) by the liquid of the alcohols generated comprising water phase, entrainer and entrainer hydrolysis distilled out through acetic acid refining unit
Body introduces entrainer recovery unit；The entrainer that entrainer recovery unit is recycled introduces acetic acid refining unit, remaining a small amount of total
It boils agent and alcohols introduces entrainer regeneration unit, and entrainer recovery unit is discharged in isolated water；
(4) alcohols that the part acetic acid and step (3) that step (2) is collected into obtain is esterified instead in entrainer regeneration unit
It answers and is reacted in the presence of catalyst, generate entrainer；
(5) entrainer that the entrainer collected in entrainer recovery unit and esterification generate is concomitantly introduced into acetic acid essence
Unit processed recycles；
Wherein, the technique carries out on device as described above.
According to the technique of the application, in step (1), the entrainer is selected from acetic acid C2-6Arrcostab；The acetic acid C2-6Alkane
Base ester, which is selected from, includes but is not limited to: one of n-butyl acetate, n-propyl acetate, isopropyl acetate or ethyl acetate, two kinds
Or more.
According to the technique of the application, in step (4), the catalyst of esterification is preferably cation exchange resin, such as
Sulfonic group Purolite C100H/6101 gel-type ion-exchange resin.
According to the technique of the application, in step (4), the temperature of esterification material is 60~80 DEG C, preferably 75 DEG C.
According to the technique of the application, in step (4), the time of esterification is 60~150 minutes, preferably 100 minutes.
As example, the technique includes the following steps:
S1. entrainer is added into acetic acid refining tower by acetic acid refining tower phase-splitter and acetic acid refining tower reflux pump；
S2. the spirit of vinegar of the preamble unit from hydrolysis methyl acetate enters acetic acid refining tower and carries out thickening purification；
Acetic acid refining tower steams the azeotropic mixture of water and entrainer from tower top；The gas phase mixture steamed from acetic acid refining column overhead is through vinegar
Enter acetic acid refining tower phase-splitter split-phase after the condensation of acid treating tower condenser, cooling；
Acetic acid refining tower adopts pump extraction finished product acetic acid through acetic acid refining tower side by lower part side line, and a part is cold through finished product acetic acid
But tank field is carried out after device is cooling, a part enters esterifier after esterification cooler is cooling；
S3. acetic acid refining tower phase-splitter split-phase upper oil phase is pumped into acetic acid refining top of tower through the reflux of acetic acid refining tower and returns
Stream；The alcohols and separation water that are generated comprising a small amount of entrainer, entrainer hydrolysis of acetic acid refining tower phase-splitter bottom, through entrainer
Water phase pans and entrainer recovery tower charging pumping entrainer recovery tower top-feed, to the entrainer that dissolves in separation water and
Alcohols recycling, the tower only set stripping section, and after overhead vapours condensation, lime set enters entrainer recovery tower phase-splitter split-phase, and water phase is returned
Return entrainer water phase pans；Oil comprising entrainer and alcohols mutually distillates pump through entrainer recovery tower and esterification reaction solution is cooling
Device enters esterifier；
S4. alcohols and acetic acid generate entrainer under the catalysis of cation exchange resin in esterifier, and generation is total to
It boils agent and original a small amount of entrainer and enters acetic acid refining tower together after accurate filter filters；
According to the technique of the application, the tower top temperature of acetic acid refining tower described in step S2 is 65-85 DEG C, for example, 70-
80℃；Bottom temperature is 110-140 DEG C, for example, 120-130 DEG C；Lower part side take-off temperature is 110-140 DEG C, for example,
120-130℃；Pressure is 0.005~1MPa, for example, 0.085~0.15MPa.
According to the technique of the application, entrainer recovery tower phase-splitter upper layer in side take-off acetic acid and step S3 in step S2
The mass ratio of oily phase is 2~6:1, preferably 3:1.
According to the technique of the application, in step S3, the tower top temperature of entrainer recovery tower is 80-110 DEG C, for example, 90-
100℃；Bottom temperature is 80-120 DEG C, for example, 90-110 DEG C；Pressure be 0.005~1MPa, for example, 0.085~
0.15MPa。
According to the technique of the application, in step S4, the tower top temperature of esterifier is 60-100 DEG C, for example, 70-90
℃；Bottom temperature is 80-120 DEG C, for example, 90-110 DEG C.
According to the technique of the application, in step S4, the tower top temperature of accurate filter is 55-75 DEG C, for example, 60-70
℃；Bottom temperature is 90-130 DEG C, for example, 100-120 DEG C.
Beneficial effect
Technique of the invention realizes that entrainer is continuous with acetic acid esterified by the alcohol for generating the hydrolysis of acetates entrainer
The stability of device operation and product quality can be improved instead of entrainer benefit, the drainage journey of the prior art in regeneration.It realizes altogether
After the cyclic regeneration of boiling agent for the polyvinyl alcohol process units of 100,000 tons/year of common scales, such as it can reduce per hour
Isopropyl acetate discharge amount is about 110~280 kgs/hr, operates 8000 hours and counts per year, can reduce 880~2240 every year
Ton isopropyl acetate consumption, can save expense 1144~29,120,000 yuan/year when isopropyl acetate price is 13000 yuan/ton.By
The high water separation capability of entrainer can be kept in the device of the application, to reduce operation energy consumption.The two can reduce polyethylene
The production cost of alcohol improves industry technology level, enhances the competitiveness of product in market.
In addition, the mass ratio of technological design side take-off acetic acid of the invention and entrainer recovery tower phase-splitter upper oil phase
For 2~6:1, which can be such that the water separation capability of entrainer greatly improves, to reduce operation energy consumption.
Further, present inventor is it was unexpectedly observed that the residence time for being esterified material in anti-device is 60~150 minutes
When, the alcohol and acetic acid esterified reaction conversion ratio that entrainer hydrolysis can be made to generate are higher, thus can reduce unreacted alcohol again
It is recycled into acetic acid refining tower, the service efficiency of entrainer is influenced, further increases energy consumption.
It is steady to improve product quality to entrainer regeneration technology of the invention to the operational stability of enhancing acetic acid refining process
Qualitative, reducing process material consumption has important practical significance, and can bring significant economic benefit for manufacturing enterprise.
Detailed description of the invention
Acetic acid refining and entrainer regenerating unit show in a kind of polyvinyl alcohol disposing mother liquor unit of Fig. 1 the embodiment of the present application 1
It is intended to；Wherein each appended drawing reference meaning is as follows: 01A --- the preamble unit of hydrolysis methyl acetate；01 --- acetic acid refining tower；
02 --- entrainer recovery tower；03 --- esterifier；04A --- accurate filter A, 04B --- accurate filter B；
05 --- acetic acid refining tower condenser；06 --- acetic acid refining tower phase-splitter；07 --- acetic acid refining tower reflux pump；09 --- vinegar
Acid treating tower reboiler；10 --- adopt pump in acetic acid refining tower side；11 --- finished product acetic acid cooler；12 --- acetic acid refining tower reactor
It pumps out；13 --- entrainer water phase pans；14 --- entrainer recovery tower feed pump；15 --- the condensation of entrainer recovery tower
Device；16 --- entrainer recovery tower phase-splitter；18 --- entrainer recovery tower distillates pump；19 --- entrainer recovery tower boils again
Device；20 --- entrainer recycles tower reactor and goes out to pump；21 --- esterification reaction solution cooler.
Specific embodiment
Further detailed description is done below in conjunction with technical solution of the specific embodiment to the application.The following example
It is merely illustrative ground description and interpretation the application, and is not necessarily to be construed as the limitation to the application protection scope.It is all to be based on this Shen
Please the technology realized of above content be encompassed by the application and be intended in the range of protection.
Embodiment 1
Acetic acid refining and entrainer regenerating unit in a kind of polyvinyl alcohol disposing mother liquor unit, comprising: acetic acid refining tower 01
And the acetic acid refining tower reactor being connected with 01 bottom of acetic acid refining tower goes out the acetic acid essence for pumping 12 and being connected with 01 lower part of acetic acid refining tower
Tower reboiler 09 processed；
Acetic acid refining tower condenser 05, acetic acid refining tower phase-splitter 06, entrainer water phase pans 13 and entrainer recycling
Tower feed pump 14；The acetic acid refining tower condenser 05, acetic acid refining tower phase-splitter 06, entrainer water phase pans 13 and azeotropic
Agent recovery tower feed pump 14 is sequentially connected；And the acetic acid refining tower condenser 05 further with 01 top of acetic acid refining tower go out
Mouth is connected；
The acetic acid refining tower phase-splitter 06 further includes a branch；The branch by acetic acid refining tower reflux pump 07 with
The entrance on 01 top of acetic acid refining tower is connected；
The acetic acid refining tower phase-splitter 06 further includes another entrance, can be along acetic acid refining tower phase-splitter 06 by the entrance
Zhi Luxiang acetic acid refining tower 01 in inject entrainer；
Entrainer recovery tower 02 and the entrainer being connected with 02 bottom of entrainer recovery tower recycling tower reactor go out to pump 19 and together
It boils the connected entrainer in agent recovery tower lower part and recycles tower reboiler 20；
The entrainer recovery tower feed pump 14 is connected with the entrance on 02 top of entrainer recovery tower；
Entrainer recovery tower condenser 15, entrainer recovery tower phase-splitter 16 and entrainer recovery tower distillate pump 18；It is described
Entrainer recovery tower condenser 15, entrainer recovery tower phase-splitter 16 and entrainer recovery tower distillate pump 18 and are sequentially connected, and institute
Entrainer recovery tower condenser 15 is stated to be connected with the outlet on 02 top of entrainer recovery tower；
Esterifier 03 and the esterification reaction solution cooler 21 being connected with end entrance on esterifier 03 and with esterification
The outlet of 03 lower end of reactor connected two accurate filters 04A, 04B；Described accurate filter 04A, 04B are connected in parallel, and
Described accurate filter 04A, 04B are further connected with another entrance on 01 top of acetic acid refining tower；
01 lower part of acetic acid refining tower further includes two branches, the entrance of a branch and esterification reaction solution cooler 21
It is connected, one is connected by finished product acetic acid cooler 11 with tank field；
Described device further includes that the acetic acid refining tower side being arranged between two branches of acetic acid refining tower and acetic acid refining tower is adopted
Pump 10；
Further, the acetic acid refining tower is connected with the preamble unit 01A of hydrolysis methyl acetate；
The device of the application is 100,000 tons/year of scales.
Embodiment 2
Acetic acid refining is carried out using above-mentioned apparatus and the regenerated technique of entrainer includes passing through entrainer isopropyl acetate
Acetic acid refining tower phase-splitter 06 and acetic acid refining tower reflux pump 07 are injected into acetic acid refining tower 01.
Spirit of vinegar from preamble unit 01A enters acetic acid refining tower 01 and carries out thickening purification.Acetic acid refining tower 01
Using the azeotropism of entrainer isopropyl acetate and water, the azeotropic mixture of water and isopropyl acetate is steamed from tower top.From acetic acid
The gas phase mixture that 01 tower top for the treatment of column steams condenses through acetic acid refining tower condenser 05, enters acetic acid refining tower split-phase after cooling
06 split-phase of device.Upper layer isopropyl acetate is mutually sent into 01 overhead reflux of acetic acid refining tower through acetic acid refining tower reflux pump 07.Reflux stream
Adopt acetic acid amount=5.5 in amount/side.The water phase of 06 bottom of acetic acid refining tower phase-splitter contains a small amount of entrainer isopropyl acetate and hydrolysis
The isopropanol of generation send entrainer recovery tower 02 to feed, it is different to recycle acetic acid therein after the collection of entrainer water phase pans 13
Propyl ester and isopropanol.Acetic acid refining tower 01 adopts 10 extraction finished product acetic acid of pump through acetic acid refining tower side by lower part side line, and tower bottoms is
Residue and tar.The tower reactor heat source of acetic acid refining tower 01 is provided by acetic acid refining tower reboiler 09.
Acetic acid refining tower 01 is adopted the finished product acetic acid of 10 extraction of pump by lower part side line through acetic acid refining tower side, extracts 1200kg/h out
It adopts after acetic acid is mixed with the 400kg/h material of the oily phase side extraction of entrainer recovery tower phase-splitter 16 through esterification reaction solution cooler side
21 be cooled to 80 DEG C after enter esterifier 03, participate in the esterification regenerative response of entrainer；Rest part is cold through finished product acetic acid
But device 11 is cooled to the storage of 35 DEG CHou tank sending areas.
Separation water from acetic acid refining tower phase-splitter 06 is fed through entrainer water phase pans 13 and entrainer recovery tower
Pump 14 send entrainer recovery tower 02 top-feed, recycles to the isopropyl acetate and isopropanol agent that dissolve in separation water, the tower is only
If stripping section, after overhead vapours condensation, lime set enters 16 split-phase of entrainer recovery tower phase-splitter, and water phase returns to entrainer water phase and connects
By tank 13, oily phase side material, which is sent into esterifier 03, carries out regeneration treatment.The tower reactor heat source of entrainer recovery tower 02 is by altogether
Agent recycling tower reboiler 19 is boiled to provide.
Side from acetic acid refining tower 01 enters after adopting acetic acid and the oil of entrainer recovery tower the phase-splitter 16 mutually mixing of stream stock
Esterification reaction solution cooler 21 is cooled to 80 DEG C, enters back into esterifier 03 in catalyst sulfonic group Purolite C100H/
Esterification generates acetate entrainer, the filling of cation exchange resin again under 6101 gel-type ion-exchange resin catalytic action
Amount is 2.9m3, which makes residence time 60 minutes of material.It, should to prevent shredded resin Dichlorodiphenyl Acetate treating column at corrosion
Esterification reaction solution is filtered through accurate filter 04A and 04B, and the accurate filter uses Nomex as filter medium.Filtering
The charging of 01 top of acetic acid refining tower, the entrainer isopropyl acetate return system after regeneration are returned afterwards.
Wherein, the technique ginseng of acetic acid refining tower in above-mentioned technique, entrainer recovery tower, esterifier and accurate filter
Number is as follows:
The device of embodiment 1 can realize the polyvinyl alcohol after the cyclic regeneration of entrainer to 100,000 tons/year of common scales
For process units, can reduce isopropyl acetate discharge amount per hour is about 169 kgs/hr, operates 8000 hours and counts per year,
It can reduce by 1350 tons of isopropyl acetate consumption every year, expense 17,550,000 can be saved when isopropyl acetate price is 13000 yuan/ton
Member/year.
Comparative example 1
Polyvinyl alcohol mother liquor is returned using identical equipment in embodiment 1 and the identical technique of embodiment 2 in this comparative example
Receive unit in acetic acid refined, as different from Example 2, acetic acid refining tower 01 by lower part side take-off acetic acid together
The mass ratio for boiling oily phase in agent recovery tower phase-splitter 16 is respectively 12:1 and 10:1, and the energy consumption of the system is relative to embodiment 2
2.3% and 1.9% has been respectively increased.
Comparative example 2
Polyvinyl alcohol mother liquor is returned using identical equipment in embodiment 1 and the identical technique of embodiment 2 in this comparative example
Receive unit in acetic acid refined, as different from Example 2, in esterifier the residence time of material be 40 minutes and
45 minutes, acetic acid refining tower 01 was needed by the acetic acid of lower part side take-off and the mass ratio of phase oily in entrainer recovery tower phase-splitter 16
9:1 and 8:1 is respectively increased, 1.7% and 1.5% has been respectively increased relative to embodiment 2 in the energy consumption of the system.
More than, presently filed embodiment is illustrated.But the application is not limited to above embodiment.It is all
Within spirit herein and principle, any modification, equivalent substitution, improvement and etc. done should be included in the guarantor of the application
Within the scope of shield.
Claims (10)
1. acetic acid refining and entrainer regenerating unit in a kind of polyvinyl alcohol disposing mother liquor unit characterized by comprising acetic acid
Refined unit, entrainer recovery unit and entrainer regeneration unit；
The acetic acid refining unit, entrainer recovery unit and entrainer regeneration unit are sequentially connected composition circulation；
The acetic acid refining unit includes two branches, and a branch is connected with entrainer regeneration unit, one and finished product acetic acid
Cooler is connected, and sends out purification acetic acid.
2. regenerating unit according to claim 1, which is characterized in that the acetic acid refining unit further with polyvinyl alcohol
The preamble unit of hydrolysis methyl acetate in disposing mother liquor unit is connected；
It includes but is not limited to acetic acid refining tower that the acetic acid refining unit, which is selected from,；The entrainer recovery unit is selected from
It is limited to entrainer recovery tower；It includes but is not limited to esterifier that the entrainer regeneration unit, which is selected from,；
The acetic acid refining tower, entrainer recovery tower and esterifier are sequentially connected composition circulation.
3. regenerating unit according to claim 2, which is characterized in that the acetic acid refining unit further includes acetic acid refining tower
Condenser, acetic acid refining tower phase-splitter, entrainer water phase pans and entrainer recovery tower feed pump；
The acetic acid refining tower condenser, acetic acid refining tower phase-splitter, entrainer water phase pans and the charging of entrainer recovery tower
Pump is sequentially connected according to flow direction of material；The entrance of the acetic acid refining tower condenser is connected with the outlet on acetic acid refining tower top；
The outlet of the entrainer recovery tower feed pump is connected with the entrance on entrainer recovery tower top.
4. regenerating unit according to claim 3, which is characterized in that the acetic acid refining unit further includes acetic acid refining tower
Reflux pump；
The arrival end of the acetic acid refining tower reflux pump is connected with acetic acid refining tower phase-splitter, outlet end and acetic acid refining tower
Tower top is connected；
The acetic acid refining tower phase-splitter is also connect with the device that can supplement fresh entrainer.
5. regenerating unit according to claim 4, which is characterized in that the acetic acid refining unit further includes being set to acetic acid
The acetic acid refining tower reboiler for the treatment of column tower reactor；
The acetic acid refining unit further include be set to acetic acid refining tower tower reactor acetic acid refining tower reactor go out pump；
The acetic acid refining unit further includes that pump is adopted in the acetic acid refining tower side being connected with acetic acid refining tower tower reactor；The acetic acid refining
It adopts pump while being connected with entrainer regeneration unit and finished product acetic acid cooler in tower side.
6. regenerating unit according to claim 5, which is characterized in that the entrainer recovery unit further includes and entrainer
Entrainer recovery tower condenser, entrainer recovery tower phase-splitter and the entrainer recovery tower that recycling column overhead is sequentially connected distillate
Pump；The outlet that the entrainer recovery tower distillates pump is connected with entrainer regeneration unit；
The entrainer recovery tower phase-splitter is further connected with entrainer water phase pans in acetic acid refining unit.
7. regenerating unit according to claim 6, which is characterized in that the entrainer recovery unit further includes being set to altogether
The entrainer for boiling agent recovery tower tower reactor recycles tower reboiler；
The entrainer recovery unit further include be set to entrainer recovery tower tower reactor entrainer recycling tower reactor go out pump.
8. regenerating unit according to claim 6, which is characterized in that the entrainer regeneration unit further includes esterification
Liquid cooler；The esterification reaction solution cooler distillates pump with entrainer recovery tower and is connected.
9. regenerating unit according to claim 8, which is characterized in that the entrainer regeneration unit further includes being set to ester
Change the accurate filter between reactor and acetic acid refining tower；
The number of the accurate filter is one, two or more；When the accurate filter is two or more,
The accurate filter first connect and/or parallel connection after be connected again with the entrance on acetic acid refining tower top.
10. -9 described in any item regenerating units according to claim 1, which is characterized in that the acetic acid refining unit includes: vinegar
Acid treating tower, acetic acid refining tower reactor go out pump, acetic acid refining tower reboiler, acetic acid refining tower condenser, acetic acid refining tower phase-splitter,
Pump and finished product vinegar are adopted in entrainer water phase pans, entrainer recovery tower feed pump, acetic acid refining tower reflux pump, acetic acid refining tower side
Acid cooler；
The acetic acid refining tower reactor goes out to pump and acetic acid refining tower reboiler is arranged in acetic acid refining tower tower reactor；
The acetic acid refining tower condenser, acetic acid refining tower phase-splitter, entrainer water phase pans and the charging of entrainer recovery tower
Pump is sequentially connected, and the acetic acid refining tower condenser inlet is connected with acetic acid refining column overhead, the entrainer recovery tower into
Material pump discharge is connected with entrainer recovery unit；The acetic acid refining tower condenser, acetic acid refining tower phase-splitter and acetic acid refining
Tower reflux pump is sequentially connected, and the acetic acid refining tower condenser inlet is connected with acetic acid refining column overhead, the acetic acid refining
Tower reflux pump is connected with acetic acid refining column overhead；
The acetic acid refining tower phase-splitter is also connected with the device of acetic acid refining column overhead and the fresh entrainer of offer；
It adopts pump and is connected with acetic acid refining tower lower part in acetic acid refining tower side；Acetic acid refining tower side adopt pump further with finished product
Acetic acid cooler is connected；
The entrainer recovery unit includes: entrainer recovery tower, entrainer recovery tower condenser, entrainer recovery tower split-phase
Device, entrainer recovery tower distillate pump, entrainer recycling tower reboiler and entrainer recycling tower reactor and go out to pump；
The entrainer recovery tower, entrainer recovery tower condenser, entrainer recovery tower phase-splitter, entrainer recovery tower distillate pump
It is sequentially connected, and the entrance of the entrainer recovery tower condenser is connected with entrainer recycling column overhead；The entrainer recycling
The tower top of tower is further connected with the entrainer recovery tower feed pump in acetic acid refining unit；
The entrainer recycling tower reboiler and entrainer recycling tower reactor go out to pump to be connected with the tower reactor of entrainer recovery tower respectively；
The entrainer regeneration unit includes: esterification reaction solution cooler, esterifier and accurate filter；The esterification is anti-
It answers liquid cooler to be connected with esterifier tower top, and further distillates pump with the entrainer recovery tower in entrainer recovery unit
It is connected；The accurate filter is connected with the tower reactor of the esterifier, and further smart with acetic acid in acetic acid refining unit
The tower reactor of tower processed is connected；
Acetic acid refining tower side adopts pump and is further also connected with esterification reaction solution cooler in the acetic acid refining unit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821267309.7U CN208776607U (en) | 2018-08-03 | 2018-08-03 | Acetic acid refining and entrainer regenerating unit in polyvinyl alcohol disposing mother liquor unit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821267309.7U CN208776607U (en) | 2018-08-03 | 2018-08-03 | Acetic acid refining and entrainer regenerating unit in polyvinyl alcohol disposing mother liquor unit |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN208776607U true CN208776607U (en) | 2019-04-23 |
Family
ID=66156013
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201821267309.7U Active CN208776607U (en) | 2018-08-03 | 2018-08-03 | Acetic acid refining and entrainer regenerating unit in polyvinyl alcohol disposing mother liquor unit |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN208776607U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116606204A (en) * | 2023-07-17 | 2023-08-18 | 成都普什医药塑料包装有限公司 | Recovered acetic acid for low-chroma acetic anhydride and cellulose acetate, and recovery method and application thereof |
-
2018
- 2018-08-03 CN CN201821267309.7U patent/CN208776607U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116606204A (en) * | 2023-07-17 | 2023-08-18 | 成都普什医药塑料包装有限公司 | Recovered acetic acid for low-chroma acetic anhydride and cellulose acetate, and recovery method and application thereof |
| CN116606204B (en) * | 2023-07-17 | 2023-10-20 | 成都普什医药塑料包装有限公司 | Recovered acetic acid for low-chroma acetic anhydride and cellulose acetate, and recovery method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101811965B (en) | Process for separating and recovering butyl acetate and butyl alcohol in wastewater by using azeotropic rectification | |
| CN101238091A (en) | Production of di-(2-ethylhexyl) terephthalate | |
| CN107739300A (en) | A kind of process for producing high-purity isobutene and ethylene glycol mono-tert-butyl ether | |
| CN111747828B (en) | Preparation method and system of ethylene glycol monopropyl ether | |
| CN105037094A (en) | Energy coupling distillation method for preparing ethyl alcohol by means of acetic acid ester hydrogenation | |
| CN108059597A (en) | A kind of reactive distillation integrates the method and its device of production ethyl acetate with infiltration evaporation | |
| CN102584544B (en) | Process for separating ethylene glycol monomethyl ether and water with intermittent azeotropic distillation method | |
| CN103827072A (en) | Method for recovering acetic acid | |
| CN105111079A (en) | Method and device for separating acetic acid sec-butyl ester and sec-butyl alcohol | |
| CN111574375A (en) | Separation method and separation equipment for methyl acrylate crude product gas | |
| CN102229523B (en) | Preparation method of 3-chloro-1,2-propanediol | |
| CN109721567A (en) | A kind of method of catalyst and catalysis preparation glycidyl methacrylate | |
| CN106946654A (en) | A kind of separation method of biomass ethylene glycol | |
| CN100364947C (en) | Method of continuous and high-yield separating and extracting 1,3-dihydroxypropane from fermentation liquid | |
| CN101186575B (en) | Methyl acetate catalysis rectification hydrolysis technique | |
| CN102134191B (en) | Process method for producing ethyl acetate by catalytic rectification | |
| CN208776607U (en) | Acetic acid refining and entrainer regenerating unit in polyvinyl alcohol disposing mother liquor unit | |
| CN101684065A (en) | Efficient energy-saving process for continuously processing dihydromyrcenol | |
| CN208776603U (en) | A kind of recyclable device of polyvinyl alcohol alcohol hydrolysis mother liquor | |
| CN109467497B (en) | Recovery process and device for polyvinyl alcohol alcoholysis mother liquor | |
| CN205528530U (en) | Apparatus for producing of two different butyl esters of 1, 2 - cyclohexane dioctyl phthalate | |
| CN110981721A (en) | Method for continuously producing n-propyl acetate | |
| CN204275534U (en) | A kind of dimethoxym ethane process for refining equipment of producing glyphosate by using glycine accessory substance | |
| CN109467501A (en) | Acetic acid refining and entrainer regeneration technology and device in polyvinyl alcohol disposing mother liquor unit | |
| CN203007176U (en) | Alcoholysis device system for preparing dioctyl terephthalate from Dacron wastes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |