CN101870648A - Method for recovering benzoic acid from PTA oxidation residue - Google Patents
Method for recovering benzoic acid from PTA oxidation residue Download PDFInfo
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- CN101870648A CN101870648A CN201010185826A CN201010185826A CN101870648A CN 101870648 A CN101870648 A CN 101870648A CN 201010185826 A CN201010185826 A CN 201010185826A CN 201010185826 A CN201010185826 A CN 201010185826A CN 101870648 A CN101870648 A CN 101870648A
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- formic acid
- crude benzol
- acid
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- water
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- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 33
- 230000003647 oxidation Effects 0.000 title claims abstract description 25
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 25
- 239000005711 Benzoic acid Substances 0.000 title abstract description 7
- 235000010233 benzoic acid Nutrition 0.000 title abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000004090 dissolution Methods 0.000 claims abstract description 9
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- IMXLQXHCHYKEEE-UHFFFAOYSA-N benzene;formic acid Chemical compound OC=O.C1=CC=CC=C1 IMXLQXHCHYKEEE-UHFFFAOYSA-N 0.000 claims description 25
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 21
- 239000012065 filter cake Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 6
- 229960004365 benzoic acid Drugs 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000002351 wastewater Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims 1
- 239000010865 sewage Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 230000018044 dehydration Effects 0.000 abstract description 4
- 238000006297 dehydration reaction Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 5
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 238000004821 distillation Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical class COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- RIAYZOZLIDBPNR-UHFFFAOYSA-N C(=O)O.C1(=CC=CC=C1)NC1=C(C(=O)O)C=CC=C1 Chemical compound C(=O)O.C1(=CC=CC=C1)NC1=C(C(=O)O)C=CC=C1 RIAYZOZLIDBPNR-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical compound CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- -1 dioctyl ester Chemical class 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 208000021302 gastroesophageal reflux disease Diseases 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for recovering benzoic acid from PTA oxidation residue, which belongs to the technical field of waste recycling. The method at least includes six processes, i.e. residue dissolution in hot water, filtration, hot filtrate cooling, crude benzoic acid slurry filtration, crude benzoic acid dehydration and crude benzoic acid rectification, and industrial benzoic acid and mixed phthalic acid can be produced. The method has the advantages of high yield, simple technique, low cost, little environment pollution and the like.
Description
Technical field: the invention belongs to the recovery and reuse of waste technical field, be specifically related to from the PTA oxidation residua, reclaim benzoic method.
Background technology: pure terephthalic acid's (be called for short PTA) is the important source material of polyester industrial, large-scale industrial production, and the production capacity of China PTA in 2009 is 1,800 ten thousand tons.The newly-increased single line industrial scale of PTA is to be not less than 600,000 tons at present.
PTA by p-Xylol through oxidation, refining forming.Except that generating the principal product terephthalic acid, still there is multiple by product to generate in the oxidizing reaction.In order to guarantee the quality of PTA product, prevent that objectionable impurities from accumulating in production system, oxidation section needs regularly to discharge oxidation residua, and per 1,000,000 tons of PTA discharge moisture 60% oxidation residua at 0.7～10,000 ton.The main component of oxidation residua has water, phenylformic acid, terephthalic acid, m-phthalic acid etc.
The present main method of disposal of oxidation residua has: (1) is it to be entered the PTA sink drainage after with alkali dissolution handle.Present method characteristics are to handle very thoroughly, but the cost height has high input the producer of employing few (warding off as Zhuhai is green).(2) be to carry out recycling, the solid of oxidation residua is partly separated, become useful product, enter PTA sink drainage COD amount like this and can reduce about 70%, significantly reduce processing cost through certain separating technology post-treatment.
Summary of the invention: the invention provides a kind of benzoic method that from the PTA oxidation residua, reclaims, a kind of method of oxidation residua recycling also is provided simultaneously.Through the residue behind the extraction phenylformic acid, can replace the part purposes of terephthalic acid and phthalic acid, as the raw material of producing low-grade unsaturated polyester, dioctyl ester.Advantages such as this is produced this method and has rate of recovery height, and technology is simple, and cost is low, and environmental pollution is little.
Method of the present invention comprises six processes such as residue hot water dissolving, filtration, hot filtrate cooling, crude benzol formic acid dope filtration, crude benzol formic acid dewater, the rectifying of crude benzol formic acid, makes technical benzene formic acid and pure mixed phthalic acid product.
A preferred embodiment of the present invention is:
1) with oxidation residua and water heating for dissolving, obtain the hot slurries of oxidation residua, solvent temperature is 70-140 ℃, Total Water is 0.7-1.5 times according to the theoretical consumption of phenylformic acid Calculation of Solubility gained in the pure water;
2) the hot slurries of oxidation residua remove the gred after filtration, and filtrate is cooled off in cooling vessel, are cooled to be no more than 10 ℃ of room temperatures, obtain thick this formic acid slurries; Filtration procedure preferentially adopts sealing pressure filtration, contains the leakage of micro-benzene formic acid water vapor with minimizing.The preferential still formula cooling apparatus that has stirrings, chuck that adopts of hot filtrate process of cooling, solution phenylformic acid are separated out in cooling and the fouling, the blockage problem that cause, the advantage of have stable operation, simple structure, being convenient to clear up.
3) crude benzol formic acid slurries obtain crude benzol formic acid filter cake and waste water through press filtration, and the big portion of waste water returns dissolution process, enter waste disposal plant after releasing on a small quantity and handle; Common filter type all can use, and preferential the employing analysed the frame pressure filter, to reduce the water content in the crude benzol formic acid as far as possible.
4) crude benzol formic acid filter cake distillation dehydration, the temperature terminal point is 115-130 ℃; Dehydration can be adopted methods such as drying and dewatering (loft drier, hot gas flow drying etc.) and dehydration by evaporation.The preferential vaporize water that adopts.Crude benzol formic acid filter cake moved to have among the reaction Fu that adds hot charging heat, remove after the water vapor.The preferential final material temperature that adopts is 125 ℃.
5) crude benzol formic acid rectifying, pressure-controlling are at 0.001～0.1mpa, and the still temperature is no more than 250 ℃.Preferential employing rectification under vacuum, periodical operation, the preferential 0.01～0.005mpa that adopts of rectifying pressure, the temperature prioritised employing of final material is no more than 200 ℃.
Need to prove that the residue solvent temperature can satisfy needs of the present invention at 70-140 ℃, but more than 80 ℃, along with temperature is high more, benzoic solubleness absolute value is exponential type and rises, the water of required adding is few more rapidly, and energy consumption descends obviously.But temperature surpasses 100 ℃, needs to use pressure exerting device, and equipment cost improves; Temperature improves, and water consumption descends, and the phenylformic acid concentration of ordinary dissolution is excessive, and the phenylformic acid that remains in the filter cake is too much, and the cleaning frequency of cooling apparatus fouling increases sharply in addition, also easier obstruction in the pipeline.In case high temperature benzoic acid solution leakage accident takes place, will increase greatly operator's hazardness.Having taken all factors into consideration a more excellent temperature province that obtains after the security of operation easier, whole technology and the economy is 95 ℃～100 ℃.
1), technology is simple, easy handling the present invention has the following advantages:; 2), phenylformic acid rate of recovery height, meet the requirement of technical benzene formic acid.3), about 70% COD changes into useful product in the oxidation residua, turn waste into wealth, the COD quantity discharged that has reduced significantly.
Embodiment: with reference to the following embodiment that only provides for explanation, further details of the present invention and advantage will become clearer.Need to prove that these embodiment also are used to limit protection scope of the present invention.
Embodiment 1:
Get oxidation residua 0.6kg (moisture 63.0%, phenylformic acid 17%), add water 1.662kg, stir, be heated to 95 ℃, constant temperature 10 minutes moves to press filtration while hot in the strainer (strainer need be preheating to 95 ℃), filter cake (moisture 37.0%) 98g.Filtrate is cooled to 25 ℃, and press filtration gets crude benzol formic acid 493g (moisture 67.5%).This is 98.2% for the dissolution process phenylformic acid rate of recovery.Crude benzol formic acid 493g is moved in two mouthfuls of burnings of 1 liter of glass, connect thermometer and condenser, connect water of condensation, heating.When temperature of charge reaches 125 ℃, stop heating.Get 157g dry raw phenylformic acid.
Get the dry raw phenylformic acid 700g of above-mentioned preparation, put into 1 liter of twoport flask, by the rectifier unit that connects shown in Figure 1.The rectifying column packed height is a 0.7-1 rice, adopt that University Of Tianjin produces, by φ 3 high efficiency packings of not Stainless Steel Wire coiling (down with).Take out straight sky the pressure of distillation system is dropped to 0.005mpa, check each sealing joint.If any gas leakage, need fix.Load thermal insulation layer, the insulation of rectifying shell of column initially fixes on 150 ℃, and temperature is consistent in back and the rectifying bottle; Rectifying column thermal insulation layer temperature is initially set in 120 ℃, and the back is suitably regulated according to phenylformic acid reflux rate and phenylformic acid output speed, makes reflux ratio roughly at 1: 2.Suitably regulate heater voltage according to distillation speed.When not having phenylformic acid to drip or rectification temperature when reaching 200 ℃, stop rectifying.Calculate phenylformic acid weight according to the weight difference of receiving bottle.Get phenylformic acid 384.6g, total recovery is 84.3%; Getting the rectifying slag is 315.4g (containing 15% phenylformic acid).
Embodiment 2:
Get oxidation residua 0.6kg (moisture 63.0%, phenylformic acid 17%), add water 1.75kg, stir, be heated to 95 ℃, constant temperature 10 minutes, move to press filtration while hot in the strainer (strainer need be preheating to 95 ℃), press dry (pressurized air), get filter cake (moisture 37.1%) 93.6g.Filtrate is cooled to 25 ℃, and press filtration gets crude benzol formic acid 498g (moisture 67.5%).This is 98.3% for the dissolution process phenylformic acid rate of recovery.Crude benzol formic acid 351g is moved in two mouthfuls of burnings of 1 liter of glass, connect thermometer and condenser, connect water of condensation, heating.When temperature of charge reaches 125 ℃, stop heating.Get 159.8g dry raw phenylformic acid.Get dry raw phenylformic acid 700g, press rectificating method rectifying among the embodiment 1, get phenylformic acid 376.3g, the phenylformic acid total recovery is 84.2%; Getting the rectifying slag is 323.7g (containing 15% phenylformic acid).
Embodiment 3:
Get oxidation residua 0.6kg (moisture 63.0%, phenylformic acid 17%), add water 1.05kg, stir, be heated to 95 ℃, constant temperature 10 minutes, move to press filtration while hot in the strainer (strainer need be preheating to 95 ℃), press dry (pressurized air), get filter cake (moisture 37%) 179.6g.Filtrate is cooled to 25 ℃, and press filtration gets crude benzol formic acid 335g (moisture 67.5%).This is 66.7% for the dissolution process phenylformic acid rate of recovery.Crude benzol formic acid 351g is moved in two mouthfuls of burnings of 1 liter of glass, connect thermometer and condenser, connect water of condensation, heating.When temperature of charge reaches 125 ℃, stop heating.Get 106.6g dry raw phenylformic acid.Get dry raw phenylformic acid 700g, press rectificating method rectifying among the embodiment 1, get phenylformic acid 384.3g, the phenylformic acid total recovery is 57.4%; Getting the rectifying slag is 315.6g (containing 15% phenylformic acid).
Embodiment 4:
Get oxidation residua 0.6kg ((moisture 63%, phenylformic acid 17%), add water 1.66kg, be heated to 90 ℃, constant temperature 10 minutes, press filtration while hot (pressurized air), filter cake (moisture 38.3%) 222g.Filtrate is cooled to 25 ℃, and press filtration gets crude benzol formic acid 83.2g (moisture 68.2%).This is 54.6% for the dissolution process phenylformic acid rate of recovery.Crude benzol formic acid 267.4g is moved in two mouthfuls of burnings of 1 liter of glass, connect thermometer and condenser, connect water of condensation, heating.When temperature of charge reaches 125 ℃, stop heating.Get 101g dry raw phenylformic acid.Get dry raw phenylformic acid 700g, press rectificating method rectifying among the embodiment 1, get phenylamino benzoic acid formic acid 408.2g, the phenylformic acid total recovery is 47.6%; Getting the rectifying slag was 291.8 (containing 15.5% phenylformic acid).
Claims (5)
1. one kind is reclaimed benzoic method from pure terephthalic acid's oxidation residua, it is characterized in that comprising that residue hot water dissolving, filtration, hot filtrate cooling, crude benzol formic acid dope filtration, crude benzol formic acid dewater, six processes of crude benzol formic acid rectifying, make technical benzene formic acid and pure mixed phthalic acid product.
2. the method for claim 1 is characterized in that comprising following consecutive steps:
A), with oxidation residua and water heating for dissolving, obtain the hot slurries of oxidation residua, solvent temperature is 70-140 ℃, Total Water is according to the 0.7-1.5 of the theoretical consumption of phenylformic acid Calculation of Solubility gained in the pure water doubly;
B), the hot slurries of oxidation residua remove the gred after filtration, filtrate is cooled off in cooling vessel, is cooled to be no more than 10 ℃ of room temperatures, obtains crude benzol formic acid slurries;
C), crude benzol formic acid slurries get crude benzol formic acid filter cake and waste water through press filtration, the waste water major part is returned dissolution process, enters the sewage disposal dress after releasing on a small quantity and handles;
D), crude benzol formic acid filter cake distilled water, the temperature terminal point is 115～130 ℃;
E), the rectifying of crude benzol formic acid, pressure-controlling is at 0.001～0.1mpa, the still temperature is no more than 250 ℃.
3. method as claimed in claim 1 or 2 is characterized in that the hot slurries of residue adopt the sealing press filtration.
4. method as claimed in claim 1 or 2 is characterized in that cooling off the still formula cooling apparatus that employing has stirring, chuck.
5. method as claimed in claim 3 is characterized in that using washing, filtering and drying machine.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101858261A CN101870648B (en) | 2010-05-28 | 2010-05-28 | Method for recovering benzoic acid from PTA oxidation residue |
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| CN2010101858261A CN101870648B (en) | 2010-05-28 | 2010-05-28 | Method for recovering benzoic acid from PTA oxidation residue |
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| CN101870648A true CN101870648A (en) | 2010-10-27 |
| CN101870648B CN101870648B (en) | 2013-11-20 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336659A (en) * | 2011-07-07 | 2012-02-01 | 山西大学 | Method for separating diphenic acid from tower bottom waste for preparing benzoic acid |
| CN102381963A (en) * | 2011-08-04 | 2012-03-21 | 绍兴县金程针纺有限公司 | Method and device for preparing benzoic acid by utilizing waste PX (paraxylene) oxidation residues |
| CN102965506A (en) * | 2012-12-14 | 2013-03-13 | 葛新芳 | Method for removing aluminum from rare earth solution by benzoate precipitation method |
| CN104003453A (en) * | 2014-04-17 | 2014-08-27 | 绍兴县远程树脂科技有限公司 | Technological method for recovery of oxidation residue solid waste valuable mixture |
| CN110836378A (en) * | 2019-11-29 | 2020-02-25 | 沈福昌 | Resource recovery incineration treatment method for fine terephthalic acid residue |
| CN110864308A (en) * | 2019-11-29 | 2020-03-06 | 沈福昌 | Harmless recovery and incineration treatment method for residue of purified terephthalic acid |
| WO2021103338A1 (en) * | 2019-11-29 | 2021-06-03 | 沈福昌 | Purified terephthalic acid residue recylcing recovery incineration treatment method |
| CN113387794A (en) * | 2021-07-22 | 2021-09-14 | 常州德诚环境科技有限公司 | Method for recovering benzoic acid in PTA oxidation residue |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402564A (en) * | 2008-05-15 | 2009-04-08 | 厦门海湾化工有限公司 | Dissolution processing method for CTA draff in PTA production |
-
2010
- 2010-05-28 CN CN2010101858261A patent/CN101870648B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402564A (en) * | 2008-05-15 | 2009-04-08 | 厦门海湾化工有限公司 | Dissolution processing method for CTA draff in PTA production |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336659A (en) * | 2011-07-07 | 2012-02-01 | 山西大学 | Method for separating diphenic acid from tower bottom waste for preparing benzoic acid |
| CN102336659B (en) * | 2011-07-07 | 2013-09-04 | 山西大学 | Method for separating diphenic acid from tower bottom waste for preparing benzoic acid |
| CN102381963A (en) * | 2011-08-04 | 2012-03-21 | 绍兴县金程针纺有限公司 | Method and device for preparing benzoic acid by utilizing waste PX (paraxylene) oxidation residues |
| CN102965506A (en) * | 2012-12-14 | 2013-03-13 | 葛新芳 | Method for removing aluminum from rare earth solution by benzoate precipitation method |
| CN102965506B (en) * | 2012-12-14 | 2015-07-22 | 葛新芳 | Method for removing aluminum from rare earth solution by benzoate precipitation method |
| CN104003453A (en) * | 2014-04-17 | 2014-08-27 | 绍兴县远程树脂科技有限公司 | Technological method for recovery of oxidation residue solid waste valuable mixture |
| CN110836378A (en) * | 2019-11-29 | 2020-02-25 | 沈福昌 | Resource recovery incineration treatment method for fine terephthalic acid residue |
| CN110864308A (en) * | 2019-11-29 | 2020-03-06 | 沈福昌 | Harmless recovery and incineration treatment method for residue of purified terephthalic acid |
| WO2021103338A1 (en) * | 2019-11-29 | 2021-06-03 | 沈福昌 | Purified terephthalic acid residue recylcing recovery incineration treatment method |
| CN110836378B (en) * | 2019-11-29 | 2021-11-23 | 沈福昌 | Resource recovery incineration treatment method for fine terephthalic acid residue |
| CN113387794A (en) * | 2021-07-22 | 2021-09-14 | 常州德诚环境科技有限公司 | Method for recovering benzoic acid in PTA oxidation residue |
| CN113387794B (en) * | 2021-07-22 | 2023-09-26 | 常州德诚环境科技有限公司 | Method for recycling benzoic acid in PTA oxidation residues |
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