CN104529742A - Method for continuously treating waste acid of methanol low-pressure carbonyl process by scraper film evaporator - Google Patents
Method for continuously treating waste acid of methanol low-pressure carbonyl process by scraper film evaporator Download PDFInfo
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- CN104529742A CN104529742A CN201410802225.9A CN201410802225A CN104529742A CN 104529742 A CN104529742 A CN 104529742A CN 201410802225 A CN201410802225 A CN 201410802225A CN 104529742 A CN104529742 A CN 104529742A
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- 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
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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
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Abstract
The invention discloses a method for continuously treating waste acid of a methanol low-pressure carbonyl process by a scraper film evaporator, which comprises the following steps: (1) adding deionized water, which accounts for 0.5-2 wt% of the waste acetic acid, into the waste acetic acid raw material, and thoroughly mixing with the waste acetic acid; (2) introducing the waste acetic acid mixed with deionized water into a scraper film evaporator to perform evaporation treatment; (3) sending a liquid in a storage tank into a first rectification tower to perform rectification, distilling off crude acetic acid with the mass content of greater than 90% from the tower top of the first rectification tower, returning to an acetic acid production device for further rectification, and finally separating to obtain the acetic acid; and separating deep-color propionic acid from the tower kettle of the first rectification tower, sending the deep-color propionic acid into a second rectification tower for rectification, and distilling off colorless propionic acid with the mass content of greater than 99.5% from the tower top of the second rectification tower. The method can remove most organic inorganic salt and condensate heavy components capable of easily causing scarring and blockage of the equipment, thereby reducing the influence on the subsequent rectifier.
Description
Technical field
The present invention relates to a kind for the treatment of process of spent acid, particularly relate to the method for the acetic acid synthesized process spent acid of process low-pressure methanol carbonyl process.
Background technology
In the technique of synthesizing acetic acid by methanol low-pressure carbonylation, adopt rhodium or iridium and osmium as catalyzer, methyl iodide and hydrogen iodide are as promotor, the acetic acid of top grade product is obtained through three towers or four tower rectifying separation, but in the process of rectifying, in order to ensure quality product, need to discharge a certain amount of heavy component spent acid, what wherein content was higher is acetic acid and propionic acid, and other have the acetaldehyde of certain content, ritalin, organic salt and the high boiling point condensate such as inorganic salts, acetyloxypropanoic acid.
Disclosed useless acetic acid process patent CN200610147677.3 discloses a kind of by rectification process, is separated the method obtaining acetic acid and propionic acid.But in the process of actual production, owing to there is organic salt and inorganic salts in spent acid, acetic acid and propionic acid are in rectifying heating high temperature generation condensation reaction, generate anhydrides material, when using conventional rectifying device to carry out spent acid rectifying, easy generation, for the heat transfer tube blocking of heating, is difficult to the continuous rectification realizing spent acid.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art, a kind of stability that can improve distillation operation is provided, the colourless propionic acid mass content obtained can reach 99.5%, achieves the method processing the spent acid of low-pressure methanol carbonyl process with scrapper thin film evaporator continuously of the continuous operation of Waste acid treating device.
Scrapper thin film evaporator of the present invention processes the method for the spent acid of low-pressure methanol carbonyl process continuously, and it comprises the following steps:
(1) in useless acetic acid raw material, add the deionized water accounting for useless acetic acid content 0.5% ~ 2% in mass, fully mix with useless acetic acid;
(2) the useless acetic acid of mixing deionized water is passed into scrapper thin film evaporator and carry out evaporation process, controlling vaporization temperature is 141 ~ 146 DEG C, control evaporation residue amount by percentage to the quality and account for 8% ~ 12% of useless acetic acid total amount, in scrapper thin film evaporator, Light ends and most acetic acid and propionic acid vaporization become secondary steam and are discharged by vaporizer top and in addition condensation, condensed liquid storage is in storage tank, and base of evaporator is inorganic, organic salt and most heavy component flow out with liquid state and enter basin;
(3) liquid in storage tank is sent into the first rectifying tower and carry out rectifying, distillate at the first rectifying tower tower top the thick acetic acid that mass content is greater than 90%, return acetic acid production device and carry out further rectifying, be finally separated the acetic acid obtaining top grade product; Isolate the dark propionic acid of mass content more than 97.5% at the first tower bottom of rectifying tower, dark propionic acid is sent into Second distillation column rectifying, distillates the colourless propionic acid of mass content more than 99.5% at Second distillation column tower top.
Beneficial effect of the present invention: 1, by the process of scrapper thin film evaporator, the organic-inorganic salt scabbed wherein easily causing equipment and block and the condenses heavy component overwhelming majority are removed, decrease the impact on subsequent fine distillation unit, thus achieve the continuous operation of Waste acid treating device.2, add the de-mineralized water accounting for spent acid total amount 0.5% ~ 2% in mass, suppress the generation of evaporation and rectifying condensation side reaction.3, device adopts continuous seepage mode, can reduce operation easier, and avoid periodical operation and frequently to heat up cooling, decrease energy expenditure, improve the stability of distillation operation, improve the stability of quality product, the shutting down frequently reducing operator is worked.4, after long-term (more than one month) is run, by adding aqueous sodium hydroxide solution in scrapper thin film evaporator, keeping scraper plate to rotate, carrying out clean, good cleaning performance can be obtained.Waste water after cleaning, adopts microbe fermentation method to carry out harmless treatment.
Accompanying drawing explanation
Accompanying drawing is the schematic flow sheet that scrapper thin film evaporator of the present invention processes the method for the spent acid of low-pressure methanol carbonyl process continuously.
Embodiment
Below in conjunction with drawings and embodiments example, the present invention is described in further detail.
Scrapper thin film evaporator of the present invention processes the method for the spent acid of low-pressure methanol carbonyl process continuously as shown in drawings, it comprises the following steps: (1) adds the deionized water accounting for useless acetic acid content 0.5% ~ 2% in mass in useless acetic acid raw material, fully mixes with useless acetic acid.In high temperature evaporation and follow-up rectifying, the condensation reaction that acetic acid and propionic acid dehydration occur can be suppressed.Useless acetic acid produces by low-pressure methanol oxo synthesis the useless acetic acid obtained in process of acetic acid, containing acetic acid, propionic acid, iodide, acetaldehyde, ritalin, the organic and condenses such as inorganic salts, acetyloxypropanoic acid heavy component in useless acetic acid.(2) the useless acetic acid of mixing deionized water is passed into scrapper thin film evaporator 1 and carry out evaporation process, controlling vaporization temperature is 141 ~ 146 DEG C, control evaporation residue amount by percentage to the quality and account for 8% ~ 12% of useless acetic acid total amount, in scrapper thin film evaporator 1, Light ends and most acetic acid and propionic acid vaporization become secondary steam and are discharged by vaporizer 1 top and in addition condensation, condensed liquid is (mainly containing acetic acid, propionic acid, water) leave in storage tank 3, vaporizer 1 bottom inorganic, organic salt and most heavy component flow out with liquid state and enter basin 2, (3) liquid in storage tank 3 is sent into the first rectifying tower 5 and carry out rectifying, distillate at the first rectifying tower tower top the thick acetic acid that mass content is greater than 90%, return acetic acid production device and carry out further rectifying, be finally separated the acetic acid obtaining top grade product, isolate the dark propionic acid of mass content more than 97.5% at the first tower bottom of rectifying tower, dark propionic acid is sent into Second distillation column 7 rectifying, distillates the colourless propionic acid of mass content more than 99.5% at Second distillation column 7 tower top.At the bottom of Second distillation column tower tower, liquid-phase outlet is connected with holding tank 8 by liquid phase pipeline.
Found when evaporation residue accounts for spent acid total amount 4% ~ 5.5% by research in the inventive method, in waste liquid, start have a large amount of solid waste to separate out.Therefore control evaporation residue when accounting for 8% ~ 12% of spent acid total amount, to guarantee that evaporation residue flows out smoothly with liquid state.
The scrapper thin film evaporator equipment manufacturer adopted in the inventive method is on sale, the heating tube of this vaporizer is a thicker upright pipe, in, bottom is provided with two chucks and heats, rotor segment is equipped with at pipe center, scraper plate borrows rotary centrifugal force to press in liquid film surface, forces the flowing of feed liquid film-like by means of external force.The spent acid solution entered is distributed in heating tube inwall under the stirring of scraper plate, and flows downward in membranaceous rotation.Along with the evaporation of material, the concentrated solution that residual velocity concentration increases gradually, constantly flows downward, is finally discharged by base of evaporator under the effect of scraper plate.
The evaporation of the inventive method and rectification process adopt decompression or atmospheric operation, preferred atmospheric operation.
In present method inventive method after the first rectifying tower 5 is separated, Light ends contained in thick acetic acid, the materials such as ritalin, acetaldehyde, water, reaction cycle can be participated in the synthesis procedure of acetic acid production, therefore after slightly acetic acid enters the distillation system of production equipment, ritalin, acetaldehyde, water etc. can return synthesis procedure with Light ends material to be continued to participate in reaction.
In present method, the first rectifying tower heating source 4 and Second distillation column heating source 6 adopt autoclave well heater, and tube side leads to heating medium, to reduce the blocking that may occur.
The inventive method, by adding de-salted water, suppresses acetic acid and the reaction of propionic acid dehydration polymerization, the generation of high-viscosity material.The de-salted water added returns the distillation system of former acetic acid production device, and water consumption is fallen by side reaction by the synthesis system finally returning acetic acid production device.
When scrapper thin film evaporator 1 long-time running (more than one month) power consumption increases, adopt strong base solution to clean device, device can be washed preferably and to scab the material of fouling.
In the inventive method, the scraper plate of scrapper thin film evaporator selects the wherein one of hinge type scraper plate or fixed scraper plate, preferential hinge type scraper plate.The preferred high-temperature resistant polytetrafluoroethylmelt of scraper plate material.
The device that the inventive method adopts can comprise the scrapper thin film evaporator 1 that import is connected with feed line, described scrapper thin film evaporator 1 top gaseous phase outlet is connected with the first condenser and storage tank 3 successively by the first vapor delivery line, at the bottom of described scrapper thin film evaporator 1 tower, liquid-phase outlet is connected with basin 2 by the first liquid phase pipeline, the outlet of described storage tank is connected by the side line import of line of pipes with the first rectifying tower 5, the top gaseous phase outlet of the first described rectifying tower 5 is connected with acetic acid production device distillation system by being connected with the second condenser second vapor delivery line, liquid-phase outlet at the bottom of the first described rectifying tower is connected with the import of Second distillation column rectifying side line by second liquid phase pipeline, Second distillation column tower 7 is pushed up gaseous phase outlet and is connected with propionic acid finished pot by the 3rd vapor delivery line being connected with the 3rd condenser, at the bottom of described Second distillation column tower 7 tower, liquid-phase outlet is connected with holding tank 8 by the 3rd liquid phase pipeline.
Embodiment 1
(1) in useless acetic acid raw material, add the deionized water accounting for useless acetic acid content 0.5% in mass, fully mix with useless acetic acid;
(2) the useless acetic acid of mixing deionized water is passed into scrapper thin film evaporator and carry out evaporation process, controlling vaporization temperature is 142 DEG C, control evaporation residue amount by percentage to the quality and account for 10% of useless acetic acid total amount, in scrapper thin film evaporator, Light ends and most acetic acid and propionic acid vaporization become secondary steam and are discharged by vaporizer top and in addition condensation, condensed liquid storage is in storage tank, and base of evaporator is inorganic, organic salt and most heavy component flow out with liquid state and enter basin; Scrapper thin film evaporator heat interchanging area 5M
2, physical dimension φ 700* φ 600mm, H=6500mm, adopt hinge type scraper plate, vane material is high-temperature resistant polytetrafluoroethylmelt, and evaporator material is TA10.
Enter material composition change before and after vaporizer as follows:
| Light ends % | Water % | Acetic acid % | Propionic acid % | Heavy component % | Salt % | |
| Raw material after adding water | 0.5 | 0.6 | 34.1 | 58.7 | 3.6 | 2.5 |
| Condensation fraction | 0.55 | 0.65 | 36.7 | 60.6 | 1.5 | ≤0.0001 |
| Residue | ≤0.1 | ≤0.1 | 10.6 | 41.7 | 22.5 | 25 |
(3) material in storage tank 3 is entered in rectifying tower 5 by pump 10.Packing tower selected by rectifying tower 5, and adopt Pall ring filler, material is 316L, tower diameter φ 600mm, height 20000mm, divides three sections and evenly places filler, every layer of packed height is 4500mm, and by charging between first paragraph and second segment filler, feeding liquid enters in tower after sparger dispersion.Tower top temperature 114.8 DEG C ~ 115.6 DEG C, reflux ratio 3:1, the acetic acid that output quality content is greater than 90%.Bottom temperature 140.4 DEG C ~ 141.4 DEG C, tower reactor output quality content more than 97.5% propionic acid.
Material bottom rectifying tower 5 enters in rectifying tower 7 through pump 11, packing tower selected by rectifying tower 7, adopt Pall ring filler, material is 316L, tower diameter φ 600mm, height 17000mm, divide three sections and evenly place filler, every layer of packed height is 4500mm, and by charging between first paragraph and second segment filler, feeding liquid enters in tower after sparger dispersion.Tower top temperature 139.5 DEG C ~ 140.1 DEG C, reflux ratio 4:1, the colourless propionic acid of output (content >=99.5%).Bottom temperature 140.4 DEG C ~ 141 DEG C, when temperature uprises, intermittent discharge heavy component, enters tank 8.
Complete assembly spent acid enters from pump 9, and complete assembly continuously-running is produced, and sends the thick acetic acid of full scale plant back to, and through the separation of acetic acid plant, wherein the acetic acid component of more than 99.5% can as the extraction of acetic acid top grade product, therefore acetic acid yield >=96%; Propionic acid content >=99.5%, propionic acid yield >=88%.
Embodiment 2
(1) in useless acetic acid raw material, add the deionized water accounting for useless acetic acid content 2% in mass, fully mix with useless acetic acid;
(2) the useless acetic acid of mixing deionized water is passed into scrapper thin film evaporator and carry out evaporation process, controlling vaporization temperature is 146 DEG C, control evaporation residue amount by percentage to the quality and account for 8% of useless acetic acid total amount, in scrapper thin film evaporator, Light ends and most acetic acid and propionic acid vaporization become secondary steam and are discharged by vaporizer top and in addition condensation, condensed liquid storage is in storage tank, and base of evaporator is inorganic, organic salt and most heavy component flow out with liquid state and enter basin 3;
Enter material composition change before and after vaporizer as follows:
| Light ends % | Water % | Acetic acid % | Propionic acid % | Heavy component % | Salt % | |
| Raw material after adding water | 0.5 | 0.6 | 34.1 | 58.7 | 3.6 | 2.5 |
| Condensation fraction | 0.55 | 0.65 | 36.4 | 60.8 | 1.6 | ≤0.0001 |
| Residue | ≤0.1 | ≤0.1 | 7.8 | 34.1 | 26.6 | 31.3 |
(3) material in storage tank 3 is entered in rectifying tower 5 by pump 10.Packing tower selected by rectifying tower 5, and adopt Pall ring filler, material is 316L, tower diameter φ 600mm, height 20000mm, divides three sections and evenly places filler, every layer of packed height is 4500mm, and by charging between first paragraph and second segment filler, feeding liquid enters in tower after sparger dispersion.Tower top temperature 114.8 DEG C ~ 115.6 DEG C, reflux ratio 3:1, the thick acetic acid that output quality content is greater than 90%.Bottom temperature 140.4 DEG C ~ 141.4 DEG C, tower reactor output quality content more than 97.5% propionic acid.
Material bottom rectifying tower 5 enters in rectifying tower 7 through pump 11, packing tower selected by rectifying tower 7, adopt Pall ring filler, material is 316L, tower diameter φ 600mm, height 17000mm, divide three sections and evenly place filler, every layer of packed height is 4500mm, and by charging between first paragraph and second segment filler, feeding liquid enters in tower after sparger dispersion.Tower top temperature 139.5 DEG C ~ 140.1 DEG C, reflux ratio 3.9:1, the colourless propionic acid of output (content >=99.5%).Bottom temperature 140.4 DEG C ~ 141 DEG C, after temperature raises, intermittent discharge heavy component, enters tank 8.
Complete assembly spent acid enters from pump 9, and complete assembly continuously-running is produced, and sends the thick acetic acid of full scale plant back to, through the separation of acetic acid plant, and acetic acid yield >=97%; Propionic acid content >=99.5%, propionic acid yield >=89%.
Embodiment 3
(1) in useless acetic acid raw material, add the deionized water accounting for useless acetic acid content 1% in mass, fully mix with useless acetic acid;
(2) the useless acetic acid of mixing deionized water is passed into scrapper thin film evaporator and carry out evaporation process, controlling vaporization temperature is 141 DEG C, control evaporation residue amount by percentage to the quality and account for 12% of useless acetic acid total amount, in scrapper thin film evaporator, Light ends and most acetic acid and propionic acid vaporization become secondary steam and are discharged by vaporizer top and in addition condensation, condensed liquid storage is in storage tank, and base of evaporator is inorganic, organic salt and most heavy component flow out with liquid state and enter basin 3;
Enter material composition change before and after vaporizer as follows:
| Light ends % | Water % | Acetic acid % | Propionic acid % | Heavy component % | Salt % | |
| Raw material after adding water | 0.5 | 0.6 | 34.1 | 58.7 | 3.6 | 2.5 |
| Condensation fraction | 0.55 | 0.65 | 36.4 | 60.8 | 1.6 | ≤0.0001 |
| Residue | ≤0.1 | ≤0.1 | 7.8 | 34.1 | 26.6 | 31.3 |
(3) material in storage tank 3 is entered in rectifying tower 5 by pump 10.Packing tower selected by rectifying tower 5, and adopt Pall ring filler, material is 316L, tower diameter φ 600mm, height 20000mm, divides three sections and evenly places filler, every layer of packed height is 4500mm, and by charging between first paragraph and second segment filler, feeding liquid enters in tower after sparger dispersion.Tower top temperature 114.8 DEG C ~ 115.6 DEG C, reflux ratio 3:1, the thick acetic acid that output quality content is greater than 90%.Bottom temperature 140.4 DEG C ~ 141.4 DEG C, tower reactor output quality content more than 97.5% propionic acid.
Material bottom rectifying tower 5 enters in rectifying tower 7 through pump 11, packing tower selected by rectifying tower 7, adopt Pall ring filler, material is 316L, tower diameter φ 600mm, height 17000mm, divide three sections and evenly place filler, every layer of packed height is 4500mm, and by charging between first paragraph and second segment filler, feeding liquid enters in tower after sparger dispersion.Tower top temperature 139.5 DEG C ~ 140.1 DEG C, reflux ratio 3.9:1, the colourless propionic acid of output (content >=99.5%).Bottom temperature 140.4 DEG C ~ 141 DEG C, after temperature raises, intermittent discharge heavy component, enters tank 8.
Complete assembly spent acid enters from pump 9, and complete assembly continuously-running is produced, and sends the thick acetic acid of full scale plant back to, through the separation of acetic acid plant, and acetic acid yield >=97%; Propionic acid content >=99.5%, propionic acid yield >=89%.
Claims (5)
1. process the method for the spent acid of low-pressure methanol carbonyl process with scrapper thin film evaporator continuously, it is characterized in that it comprises the following steps:
(1) in useless acetic acid raw material, add the deionized water accounting for useless acetic acid content 0.5% ~ 2% in mass, fully mix with useless acetic acid;
(2) the useless acetic acid of mixing deionized water is passed into scrapper thin film evaporator and carry out evaporation process, controlling vaporization temperature is 141 ~ 146 DEG C, control evaporation residue amount by percentage to the quality and account for 8% ~ 12% of useless acetic acid total amount, in scrapper thin film evaporator, Light ends and most acetic acid and propionic acid vaporization become secondary steam and are discharged by vaporizer top and in addition condensation, condensed liquid storage is in storage tank, and base of evaporator is inorganic, organic salt and most heavy component flow out with liquid state and enter basin;
(3) liquid in storage tank is sent into the first rectifying tower and carry out rectifying, distillate at the first rectifying tower tower top the thick acetic acid that mass content is greater than 90%, return acetic acid production device and carry out further rectifying, be finally separated the acetic acid obtaining top grade product; Isolate the dark propionic acid of mass content more than 97.5% at the first tower bottom of rectifying tower, dark propionic acid is sent into Second distillation column rectifying, distillates the colourless propionic acid of mass content more than 99.5% at Second distillation column tower top.
2. scrapper thin film evaporator according to claim 1 processes the method for the spent acid of low-pressure methanol carbonyl process continuously, it is characterized in that: the evaporation process in described step (2) and the rectifying in step (3) adopt atmospheric operation.
3. scrapper thin film evaporator according to claim 1 and 2 processes the method for the spent acid of low-pressure methanol carbonyl process continuously, it is characterized in that: the first rectifying tower heating source and Second distillation column heating source adopt autoclave well heater, and tube side leads to heating medium.
4. scrapper thin film evaporator according to claim 3 processes the method for the spent acid of low-pressure methanol carbonyl process continuously, it is characterized in that: hinge type scraper plate selected by the scraper plate of described scrapper thin film evaporator.
5. scrapper thin film evaporator according to claim 4 processes the method for the spent acid of low-pressure methanol carbonyl process continuously, it is characterized in that: described hinge type scraper plate material is high-temperature resistant polytetrafluoroethylmelt.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324427A (en) * | 2017-07-26 | 2017-11-07 | 江苏迈克化工机械有限公司 | A kind of method for reclaiming inorganic salts material |
| CN107973712A (en) * | 2017-11-28 | 2018-05-01 | 天津渤化永利化工股份有限公司 | A kind of system and method for improving propionic acid yield |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1995001A (en) * | 2006-12-21 | 2007-07-11 | 上海吴泾化工有限公司 | Method for separating and extracting acetic acid and propanoic acid from waste acetic acid produced from methanol low pressure carbonyl method |
| CN102126943A (en) * | 2010-11-19 | 2011-07-20 | 南京扬池工业气体有限公司 | Recycling and separating process of heavy component residual liquid in carbonylation production process of acetic acid |
| CN103772185A (en) * | 2014-02-07 | 2014-05-07 | 烟台国邦化工机械科技有限公司 | Device and method for removing moisture and heteroacids in acetic acid |
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2014
- 2014-12-19 CN CN201410802225.9A patent/CN104529742A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1995001A (en) * | 2006-12-21 | 2007-07-11 | 上海吴泾化工有限公司 | Method for separating and extracting acetic acid and propanoic acid from waste acetic acid produced from methanol low pressure carbonyl method |
| CN102126943A (en) * | 2010-11-19 | 2011-07-20 | 南京扬池工业气体有限公司 | Recycling and separating process of heavy component residual liquid in carbonylation production process of acetic acid |
| CN103772185A (en) * | 2014-02-07 | 2014-05-07 | 烟台国邦化工机械科技有限公司 | Device and method for removing moisture and heteroacids in acetic acid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324427A (en) * | 2017-07-26 | 2017-11-07 | 江苏迈克化工机械有限公司 | A kind of method for reclaiming inorganic salts material |
| CN107973712A (en) * | 2017-11-28 | 2018-05-01 | 天津渤化永利化工股份有限公司 | A kind of system and method for improving propionic acid yield |
| CN107973712B (en) * | 2017-11-28 | 2023-09-12 | 天津渤化永利化工股份有限公司 | System and method for improving propionic acid yield |
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Application publication date: 20150422 |