CN107311856A - A kind of purification recovery system of acetic acid waste liquid - Google Patents
A kind of purification recovery system of acetic acid waste liquid Download PDFInfo
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- CN107311856A CN107311856A CN201710689124.9A CN201710689124A CN107311856A CN 107311856 A CN107311856 A CN 107311856A CN 201710689124 A CN201710689124 A CN 201710689124A CN 107311856 A CN107311856 A CN 107311856A
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- acetic acid
- adsorption tanks
- waste liquid
- acid
- acid waste
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
Abstract
The invention discloses a kind of purification recovery system of acetic acid waste liquid, it is arranged on before distillation system, including filter, upper inlet of the filter by material conveying pipe after filtering respectively with the first adsorption tanks and the second adsorption tanks is connected；First adsorption tanks and the second adsorption tanks bottom are provided with the 3rd spent acid material purging line W3；Acetic acid spent acid material discharge line connects distillation system.The present invention effectively reduction metal ion content, blocking of the follow-up distillation system of solution before rectifying is carried out, on the one hand makes distillation system even running, on the other hand greatly improves the rate of recovery of acetic acid and propionic acid；The environmental benefit of the present invention is notable：The scene that generation escape is caused during reducing spent acid storage/stock first is pungent, foul odour, and rainy weather is especially notable；Secondly, spent acid low price is outer after sale, and the metal ion being used for more by enterprise in the PH for adjusting chemical enterprise water system, spent acid enters water system therewith, is finally discharged with the sewerage of enterprise and causes secondary pollution.
Description
Technical field
The present invention relates to Production Technology of Acetic Acid field, and in particular to a kind of purification recovery system of acetic acid waste liquid.
Background technology
Low-pressure methanol liquid phase process is most common technique in current China production of acetic acid, and more than 80% acetic acid is used should
Technique.The technique uses the content sum of acetic acid and propionic acid in germanium/iodine catalyst system, the waste liquid of distillation system finishing column to exist
More than 95%, with very high recovery value.Manufacturing enterprise how supporting rectifier unit is reclaimed, but it was verified that due to
Contain substantial amounts of metal ion in the waste liquid（Mainly potassium ion）, heavy constituent is generated in distillation process, causes rectification and purification to fill
Put less efficient, rectifying byproduct acetic acid and the propionic acid rate of recovery are less than 50%, be unfavorable for the yield control and cost control of acetate products
System, causes very big waste.Remaining heavy constituent is difficult to disposal and forms dangerous waste, it is necessary to substantial amounts of disposal fund.Recombinated when serious
Divide blocking pipeline, frequently result in distillation system parking.The rectifier unit of majority acetic acid enterprise is in idle state at present, and spent acid is honest and clean
Valency is sold outside.
In order to improve rectification efficiency, reduce blocking of the metal ion to pipeline, people distillation system has been carried out research and
Transformation, it is proposed that a variety of rectification process, it is specific as follows：Zhang Wenfeng is in " recovery of propionic acid in acetic acid waste liquid "（Gas chemical industry
2013,38（2）:63-65）In propose a kind of device distillation system waste liquid from acetic acid synthesis from methanol carbonylation in propionic acid reclaim
Technical scheme, scheme is as follows：Technique uses two-tower process, and the first tower is by removed overhead acetic acid and a small amount of water, and tower bottoms enters
Two towers.Second tower top isolates the propionic acid for reaching target level of product quality, propionic acid solution of the tower reactor discharge containing acetate.
Publication number CN100546968C discloses a kind of useless acetic acid separated produced from low-pressure methanol carbonyl process and extracts acetic acid
With the method for propionic acid, comprise the following steps：First will be containing acetic acid, propionic acid, iodide, acetaldehyde, methyl acetate, organic and inorganic
The useless acetic acid input rectifying column of the impurity such as salt；Then, by multistep rectification process reclaim high-purity and high concentration acetic acid and
Propionic acid, described rectification process uses general rectification process.
Publication number CN104672078B discloses a kind of technique of useless acetic acid processing, is to give up by carbonyl synthesis acetic acid accessory substance
Acetic acid purifies propionic acid processed through a step distillation technique and a step rectification process, is specially：(1) distillation technique：Remove and boiled in useless acetic acid
Waste residue of the point higher than 150 DEG C simultaneously controls distillation tower reactor tower top temperature to be 120-138 DEG C, and nitration mixture is distilled out in tower top, cold through nitration mixture
To nitration mixture groove after condenser condensation；(2) rectification process：By in the nitration mixture feeding rectification process in nitration mixture groove, rectifying column tower top is controlled
Temperature is 100-109 DEG C of rectifying extraction acetic acid, is gas phase extraction propionic acid at 134-137 DEG C in rectifying column side stream temperature.
Publication number CN100551895C discloses a kind of method of the recovery of acetic acid from waste water, using multi-effect distillation
System recovery of acetic acid, using the overhead vapours of previous tower as latter tower reboiler thermal source, or by the tower top of latter tower
Steam as previous tower reboiler thermal source, it is possible to decrease the energy consumption of distillation process, improve recovery rate.
These above-mentioned methods, most transformation both for rectification process, be intended to by adjust operating condition reduce metal from
The amount of precipitation of son, mitigates the blocking of pipeline, improves the rate of recovery of acetic acid and propionic acid, but can not tackle the problem at its root.
Therefore, the purification recovery system of existing acetic acid waste liquid how is improved, is a good problem to study.
The content of the invention
In order to overcome above-mentioned deficiency of the prior art, it can effectively reduce golden in acetic acid waste liquid the invention provides one kind
Belong to ion concentration, reduction spent acid viscosity and colourity, so that distillation system high load capacity even running, and then improve acetic acid and propionic acid
The rate of recovery, and a kind of purification recovery system of acetic acid waste liquid of rectifying device pipeline will not be blocked.
The object of the present invention is achieved like this：
A kind of purification recovery system of acetic acid waste liquid, is arranged on before distillation system, including filter 1, and filter 1 passes through filtering
Upper inlets of the material conveying pipe W2 respectively with the first adsorption tanks 2 and the second adsorption tanks 3 is connected afterwards；The first described adsorption tanks
2 and the bottom of the second adsorption tanks 3 be provided with the 3rd spent acid material purging line W3；Described acetic acid spent acid material discharge line W3 connects
Connect distillation system；
Described the first adsorption tanks 2 and the second adsorption tanks 3 are arranged in parallel, and top is connected to acid solution conveyance conduit W4 and de-
Salt solution conveyance conduit W5；
Resin is provided with the first described adsorption tanks 2 and the second adsorption tanks 3, is entered while top is provided with polymeric adsorbent regenerated liquid
Mouthful, bottom is provided with the outlet of polymeric adsorbent regenerated liquid；
The described top of filter 1 is provided with acetic acid waste liquid import, connection acetic acid waste liquid material conveying pipe W1；
A kind of technological process of the purification recovery system of described acetic acid waste liquid is：Acetic acid waste liquid is conveyed by acetic acid waste liquid material
The top of pipeline W1 connections filter 1 enters filter, after less than 50 microns of granule foreign is removed by filtering, the vinegar after filtering
The bottom of acid waste liquid from filter 1 comes out, and is then delivered to the He of the first adsorption tanks 2 respectively by material conveying pipe W2 after filtering
The upper inlet of second adsorption tanks 3, more than 97% metal ion is by the resin adsorption in the first adsorption tanks 2 and the second adsorption tanks 3
After interception, concentration of metal ions is less than 1g/L waste liquids after the lower part outlet parallel connection of the first adsorption tanks 2 and the second adsorption tanks 3 converges
It is delivered to by the 3rd spent acid material purging line W3 to distillation system；First adsorption tanks 2 and the top and bottom of the second adsorption tanks 3
Provided with polymeric adsorbent regenerated liquid inlet and outlet, the water treatment system of regenerated liquid Entry Firm after polymeric adsorbent；
Described regenerated liquid is the acid and demineralized water that mass fraction is less than 10%；During resin regeneration, pass first into mass fraction and be less than
10% acid is regenerated, and mass fraction is less than the water treatment system of 10% acid Entry Firm after polymeric adsorbent；Work as outlet
The acidity of place's acid is stable to be stopped being passed through acid in certain value；Then, desalted water is passed through to be rinsed；When the acid of exit desalted water
Degree is stable to be stopped being passed through desalted water in certain value；The water treatment system of desalted water Entry Firm after polymeric adsorbent.
Positive beneficial effect：The present invention effectively reduces metal ion content before rectifying is carried out, after fundamentally solving
The blocking of continuous distillation system, on the one hand makes distillation system even running, on the other hand greatly improves the rate of recovery of acetic acid and propionic acid；
The environmental benefit of the present invention is notable：The scene that generation escape is caused during reducing spent acid storage/stock first is pungent, effluvium
Taste, rainy weather is especially notable；Secondly, spent acid is outer at a low price is used for the PH for adjusting chemical enterprise water system by enterprise more after sale, useless
Metal ion in acid enters water system therewith, is finally discharged with the sewerage of enterprise and causes secondary pollution.
Brief description of the drawings
Fig. 1 is system diagram of the invention；
It is in figure：Material after filter 1, the first adsorption tanks 2, the second adsorption tanks 3, acetic acid waste liquid material conveying pipe W1, filtering
Conveyance conduit W2, acetic acid spent acid material discharge line W3, acid solution conveyance conduit W4, desalted water conveyance conduit W5, waste water discharge
Pipeline W6.
Embodiment
Below in conjunction with the accompanying drawings, the present invention is described further：
As described in Figure 1, a kind of purification recovery system of acetic acid waste liquid, is arranged on before distillation system, including filter 1, filtering
Upper inlet of the device 1 by material conveying pipe W2 after filtering respectively with the first adsorption tanks 2 and the second adsorption tanks 3 is connected；It is described
The first adsorption tanks 2 and the bottom of the second adsorption tanks 3 be provided with the 3rd spent acid material purging line W3；Described acetic acid spent acid material
Discharge line W3 connection distillation systems；
Described the first adsorption tanks 2 and the second adsorption tanks 3 are arranged in parallel, and top is connected to acid solution conveyance conduit W4 and de-
Salt solution conveyance conduit W5；
Resin is provided with the first described adsorption tanks 2 and the second adsorption tanks 3, is entered while top is provided with polymeric adsorbent regenerated liquid
Mouthful, bottom is provided with the outlet of polymeric adsorbent regenerated liquid；
The described top of filter 1 is provided with acetic acid waste liquid import, connection acetic acid waste liquid material conveying pipe W1；
A kind of technological process of the purification recovery system of described acetic acid waste liquid is：Acetic acid waste liquid is conveyed by acetic acid waste liquid material
The top of pipeline W1 connections filter 1 enters filter and removes fixed impurity, and less than 50 microns of granule foreign is removed by filtering
Afterwards, solid particle requirement prevents resin from blocking below 10 microns；The bottom of acetic acid waste liquid from filter 1 after filtering comes out,
Then the first adsorption tanks V1 or the second adsorption tanks V2 is alternately entered by material conveying pipe W2 after filtering and removes metal ion, drop
After resin adsorption saturation in low spent acid viscosity and colourity etc., two adsorption tanks alternate runs, adsorption tanks, carried out again with acid solution
It is raw, then it is rinsed with desalted water rear standby, more than 97% metal ion is by the first adsorption tanks 2 and the second adsorption tanks 3
Resin adsorption intercept after, concentration of metal ions be less than 1g/L waste liquids the first adsorption tanks 2 and the second adsorption tanks 3 lower part outlet simultaneously
Connection is delivered to distillation system by the 3rd spent acid material purging line W3 after converging and carries out recovery of acetic acid and propionic acid；First absorption
The top and bottom of 2 and second adsorption tanks of tank 3 are provided with polymeric adsorbent regenerated liquid inlet and outlet, and regenerated liquid is produced after polymeric adsorbent
Raw a small amount of regeneration and flushing waste water enters full factory's sewage disposal system by waste outflow pipe W6；
Described regenerated liquid is the acid and demineralized water that mass fraction is less than 10%；During resin regeneration, pass first into mass fraction and be less than
10% acid is regenerated, and mass fraction is less than the water treatment system of 10% acid Entry Firm after polymeric adsorbent；Work as outlet
The acidity of place's acid is stable to be stopped being passed through acid in certain value；Then, desalted water is passed through to be rinsed；When the acid of exit desalted water
Degree is stable to be stopped being passed through desalted water in certain value；The water treatment system of desalted water Entry Firm after polymeric adsorbent.
The operation of described the first adsorption tanks 2 and the second adsorption tanks 3 is routine operation, temperature≤120 DEG C.
Critical component constituent content（v%）：W1：Acetic acid 30%, propionic acid 70%, potassium content：40g/L；W3：Acetic acid 30%, propionic acid
70%, potassium content：1g/L；W4：Acid 5%, water 95%.
Embodiment 1
Henan chemical enterprise, the acetic acid waste liquid produced during production of acetic acid, is made up of following percentage by weight：Acetic acid
22.2%th, propionic acid 77.2%, potassium concentration 40g/l.Acetic acid waste liquid is passed through filter and carries out filtration treatment, afterwards with 0.5
BV/h flow velocity is passed through in the adsorption tanks filled with cation type resin, and potassium concentration is in the waste liquid come out by adsorption tanks
0.8g/l, sends waste liquid into distillation system, and recovery rate reaches 92.3%, and the propionic acid rate of recovery reaches 93.8%, distillation system fortune
Row is steady, line clogging situation does not occur.
Embodiment 2
Henan production of acetic acid enterprise, the quality hundred of the acetic acid waste liquid produced during production of acetic acid, wherein acetic acid and propionic acid
Fraction is respectively 30.7% and 68.8%, potassium concentration 30g/l.Acetic acid waste liquid is passed through filter and carries out filtration treatment, afterwards
It is passed through with 0.4BV/h flow velocity in the adsorption tanks filled with cation type resin, adsorption tanks outlet waste liquid potassium concentration 0.5g/
L, waste liquid is admitted to distillation system, and distillation system operates steadily, and does not find that heavy constituent crystallizes situation, recovery rate reaches
93.6%, the propionic acid rate of recovery reaches 94.1%.
Embodiment 3
Henan petro-chemical corporation, the mass percent of the acetic acid waste liquid, wherein acetic acid and propionic acid that are produced during production of acetic acid
Respectively 33.7% and 65.5%, potassium concentration 36g/l.By acetic acid waste liquid be passed through filter carry out filtration treatment, afterwards with
0.5BV/h flow velocity is passed through in the adsorption tanks filled with chelate resin, and potassium concentration is in the waste liquid come out by adsorption tanks
0.6g/l, waste liquid continues to send into distillation system, and distillation system operates steadily, and line clogging situation, acetic acid recovery does not occur
Rate reaches 93.7%, and the propionic acid rate of recovery reaches 93.9%.
The present invention effectively reduces metal ion content before rectifying is carried out, and fundamentally solves the stifled of follow-up distillation system
Plug, on the one hand makes distillation system even running, on the other hand greatly improves the rate of recovery of acetic acid and propionic acid；The environmental protection effect of the present invention
It is beneficial notable：The scene that generation escape is caused during reducing spent acid storage/stock first is pungent, foul odour, and rainy weather is especially
Significantly；Secondly, spent acid low price is outer after sale, the metal ion being used for more by enterprise in the PH for adjusting chemical enterprise water system, spent acid
Enter water system therewith, finally discharged with the sewerage of enterprise and cause secondary pollution.The spent acid of current acetic acid enterprise
Rectifier unit majority is stopped production due to the blocking of metal ion, and spent acid is outer at a low price to be sold, about 500-800 yuan/ton；Rough estimation, 20
Ten thousand tons/year of acetic acid plant, produces about 3000 tons of spent acid, wherein acetic acid 30%, about 900 tons, propionic acid 70%, about 2100 tons per year.Using
After the present invention, at least 90% acetic acid is recovered, and is worth 1,620,000 yuan, 90% propionic acid is recovered, and value 18,900,000 amounts to 2052
The directly outer value sold of Wan Yuan, significantly larger than spent acid（About 1,500,000-240 ten thousand）.
Above case study on implementation is merely to illustrate the preferred embodiment of the present invention, but the present invention is not limited to above-mentioned embodiment party
Formula, in the knowledge that the field those of ordinary skill possesses, that is made within the spirit and principles in the present invention is any
Modification, equivalent substitute and improvement etc., are regarded as the protection domain of the application.
Claims (6)
1. a kind of purification recovery system of acetic acid waste liquid, it is characterised in that：It is arranged on before distillation system, including filter 1, mistake
Upper inlet of the filter 1 by material conveying pipe W2 after filtering respectively with the first adsorption tanks 2 and the second adsorption tanks 3 is connected；Institute
The first adsorption tanks 2 and the bottom of the second adsorption tanks 3 stated are provided with the 3rd spent acid material purging line W3；Described acetic acid spent acid thing
Expect discharge line W3 connection distillation systems.
2. a kind of purification recovery system of acetic acid waste liquid according to claim 1, it is characterised in that：The first described absorption
The adsorption tanks 3 of tank 2 and second are arranged in parallel, and top is connected to acid solution conveyance conduit W4 and desalted water conveyance conduit W5.
3. a kind of purification recovery system of acetic acid waste liquid according to claim 1 or 2, it is characterised in that：Described first
Resin is provided with the adsorption tanks 3 of adsorption tanks 2 and second, while top is provided with polymeric adsorbent regenerated liquid import, bottom is provided with
Polymeric adsorbent regenerated liquid is exported.
4. a kind of purification recovery system of acetic acid waste liquid according to claim 1, it is characterised in that：Described filter 1
Top is provided with acetic acid waste liquid import, connection acetic acid waste liquid material conveying pipe W1.
5. a kind of technological process of the purification recovery system of acetic acid waste liquid as claimed in claim 1 is：Acetic acid waste liquid passes through vinegar
The top of acid waste liquid material conveying pipe W1 connections filter 1 enters filter, and less than 50 microns of granule foreign, which is crossed, to be filtered off
After removing, the bottom of acetic acid waste liquid from filter 1 after filtering comes out, and is then conveyed respectively by material conveying pipe W2 after filtering
To the upper inlet of the first adsorption tanks 2 and the second adsorption tanks 3, more than 97% metal ion is by the first adsorption tanks 2 and the second absorption
After resin adsorption in tank 3 is intercepted, concentration of metal ions is less than 1g/L waste liquids under the first adsorption tanks 2 and the second adsorption tanks 3
Portion's outlet parallel connection is delivered to distillation system after converging by the 3rd spent acid material purging line W3；First adsorption tanks 2 and second
The top and bottom of adsorption tanks 3 are provided with polymeric adsorbent regenerated liquid inlet and outlet, regenerated liquid Entry Firm after polymeric adsorbent
Water treatment system.
6. a kind of technique of the purification recovery system of acetic acid waste liquid according to claim 1, it is characterised in that：It is described again
Raw liquid is the acid and demineralized water that mass fraction is less than 10%；During resin regeneration, acid progress of the mass fraction less than 10% is passed first into
Regeneration, mass fraction is less than the water treatment system of 10% acid Entry Firm after polymeric adsorbent；When the acidity of exit acid is steady
Stop being passed through acid when being scheduled on certain value；Then, desalted water is passed through to be rinsed；When the acidity of exit desalted water is stable certain
Stop being passed through desalted water during value；The water treatment system of desalted water Entry Firm after polymeric adsorbent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710689124.9A CN107311856A (en) | 2017-08-13 | 2017-08-13 | A kind of purification recovery system of acetic acid waste liquid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710689124.9A CN107311856A (en) | 2017-08-13 | 2017-08-13 | A kind of purification recovery system of acetic acid waste liquid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111762920A (en) * | 2020-07-21 | 2020-10-13 | 河南城建学院 | Method for reducing concentration of potassium ions in acetic acid waste liquid |
| CN111847716A (en) * | 2020-07-21 | 2020-10-30 | 河南城建学院 | Purification device for acetic acid waste liquid |
| 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 |
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| CN1354139A (en) * | 2000-11-16 | 2002-06-19 | 亚新技术株式会社 | Method and device for treating waste water containing acetic acid |
| CN101234959A (en) * | 2008-03-07 | 2008-08-06 | 中国石化仪征化纤股份有限公司 | Method for reclaiming acetic acid from waste water containing dilute acetic acid |
| CN103241860A (en) * | 2013-04-27 | 2013-08-14 | 浙江晶泉水处理设备有限公司 | Combined treatment device and process for acid-washing wastewater of stainless steel |
| CN103298860A (en) * | 2010-12-30 | 2013-09-11 | 国际人造丝公司 | Purification of acetic acid product streams |
| CN105399236A (en) * | 2015-10-29 | 2016-03-16 | 钱中明 | Waste acid recovery apparatus |
| CN106745887A (en) * | 2016-12-20 | 2017-05-31 | 攀枝花市精研科技有限公司 | Industrial waste acid removal of impurities recovery process |
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2017
- 2017-08-13 CN CN201710689124.9A patent/CN107311856A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1354139A (en) * | 2000-11-16 | 2002-06-19 | 亚新技术株式会社 | Method and device for treating waste water containing acetic acid |
| CN101234959A (en) * | 2008-03-07 | 2008-08-06 | 中国石化仪征化纤股份有限公司 | Method for reclaiming acetic acid from waste water containing dilute acetic acid |
| CN103298860A (en) * | 2010-12-30 | 2013-09-11 | 国际人造丝公司 | Purification of acetic acid product streams |
| CN103241860A (en) * | 2013-04-27 | 2013-08-14 | 浙江晶泉水处理设备有限公司 | Combined treatment device and process for acid-washing wastewater of stainless steel |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111762920A (en) * | 2020-07-21 | 2020-10-13 | 河南城建学院 | Method for reducing concentration of potassium ions in acetic acid waste liquid |
| CN111847716A (en) * | 2020-07-21 | 2020-10-30 | 河南城建学院 | Purification device for acetic acid waste liquid |
| CN111847716B (en) * | 2020-07-21 | 2023-08-18 | 河南城建学院 | Purification device for acetic acid waste liquid |
| 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 |
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Application publication date: 20171103 |