CN1295155C - Treatment of wastewater from production of p-phthalic acid and recoval of resources therewith - Google Patents
Treatment of wastewater from production of p-phthalic acid and recoval of resources therewith Download PDFInfo
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- CN1295155C CN1295155C CN200510037696.6A CN200510037696A CN1295155C CN 1295155 C CN1295155 C CN 1295155C CN 200510037696 A CN200510037696 A CN 200510037696A CN 1295155 C CN1295155 C CN 1295155C
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- terephthalic acid
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- 239000002351 wastewater Substances 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 title claims description 48
- 229920005989 resin Polymers 0.000 claims abstract description 55
- 239000011347 resin Substances 0.000 claims abstract description 55
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- 238000003795 desorption Methods 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 24
- 150000001555 benzenes Chemical class 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 230000008929 regeneration Effects 0.000 claims abstract description 9
- 238000011069 regeneration method Methods 0.000 claims abstract description 9
- 239000006227 byproduct Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 238000010521 absorption reaction Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000003463 adsorbent Substances 0.000 claims description 16
- 238000001179 sorption measurement Methods 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 238000011084 recovery Methods 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 229920001429 chelating resin Polymers 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 abstract 15
- -1 benzenethiol Chemical class 0.000 abstract 1
- 238000010828 elution Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 241000196324 Embryophyta Species 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 241000406668 Loxodonta cyclotis Species 0.000 description 2
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical compound CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- RVHSTXJKKZWWDQ-UHFFFAOYSA-N 1,1,1,2-tetrabromoethane Chemical compound BrCC(Br)(Br)Br RVHSTXJKKZWWDQ-UHFFFAOYSA-N 0.000 description 1
- 229920004935 Trevira® Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000005605 benzo group Chemical group 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 239000011297 pine tar Substances 0.000 description 1
- 229940068124 pine tar Drugs 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 150000003504 terephthalic acids Chemical class 0.000 description 1
Landscapes
- Water Treatment By Sorption (AREA)
Abstract
The present invention discloses a method for treating wastewater from benzenethiol production and recovering resources. Wastewater from benzenethiol production is filtered and passes through an adsorbing column loading macroporous resin, so that organic substances in benzene series, such as benzenethiol, intermediate bodies thereof, etc., are adsorbed on the resin. The resin after the adsorbing operation is eluted for regeneration by aqueous sodium hydroxide, the desorbed high-concentration organic substance solution in benzene series is acidified, cooled and filtered, and white solids which are filtered out return to the original production section or serve as by-products for selling. The filtered liquid returns to the original wastewater for circular treatment. Low-concentration desorption liquid is used for preparing aqueous sodium hydroxide for the desorption operation of the next batch. Compared with the prior art, the present invention realizes the effective separation of wastewater and organic substances in benzene series, such as benzenethiol, etc., and the resin can be used repeatedly after elution. The method of the present invention achieves the unification of treating wastewater and changing waste into resources and has a great economic value and a great practicability value during the treatment of wastewater from benzenethiol production.
Description
One, technical field
The present invention relates to the method for the recycling of pollutent in a kind of effective improvement of Production of Terephthalic Acid waste water and the waste water.
Two, background technology
Terephthalic acid (being called for short PTA) has another name called the pine tar phthalic acid, white, needle-shaped crystals or powder, and major part is used to produce polyester, is the important source material of trevira, film, insullac, also is used for the production of medicine, other products of dye well.
It is the high-temperature liquid-phase oxidation style of raw material that industrial production mainly adopts with the p-Xylol, and p-Xylol is a catalyzer with cobaltous acetate-manganous acetate, is promotor with the tetrabromoethane, and in 221～225 ℃, oxidation generates terephthalic acid under 2.5～3.0 MPas.Give off high concentrated organic wastewater in the above-mentioned production process, the about 4500～8000mg/L of CODcr wherein except containing a large amount of acetic acid, also contains the organism such as terephthalic acid of the 1000mg/L that has an appointment.The Production of Terephthalic Acid corporate boss will adopt the aerobic/anaerobic process integration to handle this waste water both at home and abroad at present.The shortcoming of this treatment process is: since water body in the benzene series organism than difficult for biological degradation, the investment and the running cost of biochemical processing process are higher, and portioned product and the intermediate in the water body is broken to small-molecule substance and causes the wasting of resources in treating processes simultaneously.
Three, summary of the invention
The purpose of this invention is to provide a kind of improvement of Production of Terephthalic Acid waste water and the recovery method of resource thereof, this method can effectively be administered Production of Terephthalic Acid waste water and therefrom be reclaimed the benzene series organism.
The objective of the invention is to be achieved through the following technical solutions:
A kind of improvement of Production of Terephthalic Acid waste water and the recovery method of resource thereof is characterized in that it may further comprise the steps:
A), remove suspended substance wherein with the Production of Terephthalic Acid waste water filtering.
B) with steps A) gained filtrate is by being filled with the adsorption tower of resin, and terephthalic acid and benzene series organism in the waste water optionally are adsorbed on the resin, obtains water white absorption effluent.Can be among the present invention at 0～35 ℃ with steps A) gained filtrate with the flow of 6～12BV/h (BV is the resin bed volume) by being filled with the macroporous resin absorption tower; Every batch of wastewater treatment capacity is 40～80BV.The absorption effluent water white transparency, COD
CrCan reduce to below the 2500mg/L, benzo pollutants concentration is lower than 50mg/L.Organism in the absorption effluent is mainly acetic acid, but adopts conventional aerobic biochemical treatment process qualified discharge.Described resin is to be the macroporous resin of basic framework with the polystyrene, it can be macroporous adsorbent resin NDA-101 resin (Jiangsu Nanda Gede Environmental Protection Technology Co., Ltd), JX-101 resin (Golden Elephant chemical plant, Danyang), the H-103 resin (Chemical Plant of Nankai Univ.) that home-made has high-specific surface area, also can be Amberlite XAD-2, the XAD-4 resin (Rohm Haas company) of the U.S., or the HP of Japan series macroporous adsorbent resin.Macroporous adsorbent resin NDA-101 preferably wherein.
C) when absorption reaches leakage point, stop absorption, carry out desorption and regeneration as desorbing agent with sodium hydroxide; Described polymeric adsorbent is to carry out the resin desorption and regeneration after having handled 40～80BV/ batch waste water.Described desorbing agent is that concentration is the aqueous sodium hydroxide solution of 0.5～4mol/L, and the flow with 0.5～2BV/h under 40～85 ℃ of temperature carries out desorption and regeneration.
D) with step C) high concentration desorption liquid that obtains carries out acidifying, and cold filtration, the white solid thing that obtains to return original working section after leaching or sell as by-product, filtrate comes back to the raw wastewater of processing to be recycled, and the light concentration desorption liquid after the acidifying is used to prepare the desorbing agent cover and is used for the next batch desorption manipulation.Adopt 50～70% sulfuric acid to carry out acidifying among the present invention, and to be acidified to the pH value be 2～4.
Resin absorption operation of the present invention can be adopted the operation scheme of double-column in series absorption, single tower desorption; I, II, three adsorption towers of III are set, and with I, II tower series connection following current absorption, the I tower is as first post earlier, the II tower after the absorption of I tower is saturated, switches to II, III tower series connection following current absorption as stern post, the II tower is as first post, and the III tower is as stern post, and the I tower carries out desorption and regeneration with desorbing agent simultaneously.Adopt the manner can guarantee that whole waste water treatment device moves continuously.
Beneficial effect of the present invention is: 1, Production of Terephthalic Acid waste water after resin absorption is separated, the water outlet water white transparency, the benzene series organic content is less than 50mg/L, COD
Cr＜2500mg/L handles through conventional aerobic biochemical again, and the CODcr＜100mg/L of waste water reaches the GB8978-1996 first discharge standard; 2, most terephthalic acids and intermediate thereof in the separable recovery raw wastewater are realized the resource recycling, can reclaim about 0.7～1.6 kilogram of terephthalic acid and intermediate thereof from every cubic metre of waste water; 3, the polymeric adsorbent regenerability is good, and is reusable.In sum, the present invention has realized the utilization of pollutent when administering waste water.
Four, embodiment
The invention will be further described by the following examples.
Embodiment 1
10mL (about 7.5 gram) macroporous adsorbent resin NDA-101 packed in the glass adsorption column of strap clamp cover, and (Φ 16 * 160mm).It is 900mg/L that waste water contains the organic concentration of benzene series, COD
CrBe 6000mg/L, after the filtration, in 25 ± 5 ℃, by resin bed, treatment capacity is that 600mL/ criticizes with the flow of 80mL/h with it.After resin absorption, the water outlet water white transparency, wherein the benzene series organism is 47mg/L, COD
CrReduce to 2200mg/L, again COD after conventional aerobic process is handled
CrBe 89mg/L.
Use the aqueous sodium hydroxide solution of 5mL 3.6mol/L and aqueous sodium hydroxide solution, the flow following current with 15mL/h under 75 ± 5 ℃ temperature of 20mL distilled water of 10mL 1.8mol/L to carry out desorption successively by resin bed.The high density benzene series organic solution that desorption gets off filters through sulfuric acid acidation, and the white solid thing that leaches returns original working section or sells as by-product, and filtrate is returned raw wastewater.Light concentration desorption liquid is used to prepare the used aqueous sodium hydroxide solution of next batch desorption.
Embodiment 2
100mL (about 75 gram) macroporous adsorbent resin NDA-101 packed in the glass adsorption column of strap clamp cover, and (Φ 32 * 260mm).It is 850mg/L that waste water contains the organic concentration of benzene series, COD
CrBe 5800mg/L, after the filtration, in 5 ± 5 ℃, by resin bed, treatment capacity is that 8000mL/ criticizes with the flow of 1000mL/h with it.After resin absorption, the water outlet water white transparency, wherein the benzene series organism is about 45mg/L, COD
CrReduce to 2450mg/L, again COD after conventional aerobic process is handled
CrBe 96mg/L.
Use the aqueous sodium hydroxide solution of 50mL 4mol/L and aqueous sodium hydroxide solution, the flow following current with 50mL/h under 65 ± 5 ℃ temperature of 200mL distilled water of 100mL1mol/L to carry out desorption successively by resin bed.The high density benzene series organic solution that desorption gets off filters through sulfuric acid acidation, and the white solid thing that leaches returns original working section or sells as by-product, and filtrate is returned raw wastewater.Light concentration desorption liquid is used to prepare the used aqueous sodium hydroxide solution of next batch desorption.
Embodiment 3
500mL (about 375 gram) macroporous adsorbent resin NDA-101 packed in the glass adsorption column of strap clamp cover, and (Φ 100 * 360mm).Waste water contains the organic concentration of benzene series and is about 1250mg/L, COD
CrBe 8100mg/L, after the filtration, in 15 ± 5 ℃, by resin bed, treatment capacity is that 20000mL/ criticizes with the flow of 5000mL/h with it.After resin absorption, the water outlet water white transparency, wherein the benzene series organism is about 48mg/L, COD
CrReduce to 2300mg/L, again COD after conventional aerobic process is handled
CrBe 92mg/L.
Use the aqueous sodium hydroxide solution of 250mL 3.6mol/L and aqueous sodium hydroxide solution, the flow following current with 500mL/h under 75 ± 5 ℃ temperature of 500mL distilled water of 500mL2.5mol/L to carry out desorption successively by resin bed.The high density benzene series organic solution that desorption gets off filters through sulfuric acid acidation, and the white solid thing that leaches returns original working section or sells as by-product, and filtrate is returned raw wastewater.Light concentration desorption liquid is used to prepare the used aqueous sodium hydroxide solution of next batch desorption.
Embodiment 4
Select that three specifications are identical, material is 316L stainless steel adsorption tower for use (Φ 550 * 3500mm), compile Shang number be respectively I, II and III, every tower loads 375 kilograms of (about 0.5m of NDA-101 polymeric adsorbent
3).Waste water contains the organic concentration of benzene series and is about 1050mg/L, COD
CrBe 6100mg/L, after the filtration, with it in 20 ± 5 ℃, with 4m
3The flow of/h is squeezed into adsorption tower with pump, and the mode of I, II tower double-column in series following current absorption is adopted in absorption, and treatment capacity is 25m
3/ batch.After resin absorption, the water outlet water white transparency, wherein the benzene series organism is about 38mg/L, COD
CrReduce to 2100mg/L, again COD after conventional aerobic process is handled
CrBe 85mg/L.
To adsorb 25m
3The first post I adsorption tower of waste water breaks away from absorption system and carries out desorption manipulation; And the next batch adsorption operations changes II, the series operation of III tower into, post headed by the II tower becomes.
Earlier raffinate in the I adsorption tower is drained, more successively with 0.25m
3The aqueous sodium hydroxide solution of 4mol/L and 0.5m
32.5mol/L aqueous sodium hydroxide solution, 0.5m
3Distilled water is under 80 ± 5 ℃ temperature, with 1m
3The flow following current of/h is carried out desorption by resin bed.The high density benzene series organic solution that desorption gets off filters through sulfuric acid acidation, and the white solid thing that leaches returns original working section or sells as by-product, and filtrate is returned raw wastewater.Light concentration desorption liquid is used to prepare the used aqueous sodium hydroxide solution of next batch desorption.
I adsorption tower after desorption finishes will be as the stern post of the 3rd batch of adsorption operations.Can guarantee that by the present invention whole waste water treatment device moves continuously.
Embodiment 5
Change the macroporous adsorbent resin NDA-101 macroporous adsorbent resin (Jiangsu Nanda Gede Environmental Protection Technology Co., Ltd) among the embodiment 2 into JX-101 resin (Golden Elephant chemical plant, Danyang), H-103 resin (Chemical Plant of Nankai Univ.'s production) and AmberliteXAD-2, XAD-4 (RohmHass company) and HP series macroporous adsorbent resin, other operational conditions remain unchanged, except that every batch processing volume and absorption effluent water quality decreased, other effects substantially roughly the same.
Claims (8)
1, the recovery method of a kind of improvement of Production of Terephthalic Acid waste water and resource thereof is characterized in that it may further comprise the steps:
A), remove suspended substance wherein with the Production of Terephthalic Acid waste water filtering;
B) with steps A) gained filtrate is by being filled with the adsorption tower of resin, and terephthalic acid and benzene series organism in the waste water optionally are adsorbed on the resin, obtains water white absorption effluent;
C) when absorption reaches leakage point, stop absorption, carry out desorption and regeneration as desorbing agent with sodium hydroxide;
D) with step C) desorption liquid that obtains carries out acidifying, and cold filtration, the white solid thing that obtains returning original working section after leaching or sell as by-product, filtrate comes back to the raw wastewater of processing to be recycled, and the desorption liquid after the acidifying is used to prepare desorbing agent and is used for the next batch desorption manipulation.
2, the recovery method of the improvement of Production of Terephthalic Acid waste water according to claim 1 and resource thereof is characterized in that: step B) at 0～35 ℃ with steps A) gained filtrate with the flow of 6～12 resin bed volumes per hour by being filled with the macroporous resin absorption tower.
3, the recovery method of the improvement of Production of Terephthalic Acid waste water according to claim 1 and resource thereof, it is characterized in that: the resin step B) is to be the macroporous resin of basic framework with the polystyrene, it can be a kind of in the macroporous adsorbent resin NDA-101 resin of home-made with high-specific surface area, JX-101 resin, the H-103 resin, or the Amberlite XAD-2 of the U.S., XAD-4 resin, or the HP of Japan series macroporous adsorbent resin.
4, the recovery method of the improvement of Production of Terephthalic Acid waste water according to claim 3 and resource thereof is characterized in that: described resin is polymeric adsorbent NDA-101.
5, the recovery method of the improvement of Production of Terephthalic Acid waste water according to claim 1 and resource thereof is characterized in that: step C) in polymeric adsorbent be in every batch processed carry out the resin desorption and regeneration behind the waste water of 40～80 resin bed volumes.
6, the recovery method of the improvement of Production of Terephthalic Acid waste water according to claim 1 and resource thereof, it is characterized in that: desorbing agent is that concentration is the aqueous sodium hydroxide solution of 0.5～4mol/L step C), carries out desorption and regeneration with the flow of 0.5～2 resin bed volume per hour under 40～85 ℃ of temperature.
7, the recovery method of the improvement of Production of Terephthalic Acid waste water according to claim 1 and resource thereof is characterized in that: adopt 50～70% sulfuric acid to carry out acidifying step D), and to be acidified to the pH value be 2～4.
8, the recovery method of the improvement of Production of Terephthalic Acid waste water according to claim 1 and resource thereof, it is characterized in that: the operation scheme that adopts double-column in series absorption, single tower desorption, I, II, three adsorption towers of III promptly are set, and with I, II tower series connection following current absorption, the I tower is as first post earlier, the II tower is as stern post, after the absorption of I tower is saturated, switch to II, III tower series connection following current absorption, the II tower is as first post, the III tower is as stern post, and the I tower carries out desorption and regeneration with desorbing agent simultaneously.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510037696.6A CN1295155C (en) | 2005-01-13 | 2005-01-13 | Treatment of wastewater from production of p-phthalic acid and recoval of resources therewith |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510037696.6A CN1295155C (en) | 2005-01-13 | 2005-01-13 | Treatment of wastewater from production of p-phthalic acid and recoval of resources therewith |
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| CN1295155C true CN1295155C (en) | 2007-01-17 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101058467B (en) * | 2006-04-19 | 2010-09-22 | 中国石油化工股份有限公司 | Method for treating waste water generated in production of refined terephthalic acid |
| WO2009115888A1 (en) * | 2008-03-20 | 2009-09-24 | Dow Italia S.R.L. | Process for the recovery of water and valuable organics from wastewater in the production of aromatic carboxylic acids |
| CN101254985B (en) * | 2008-04-02 | 2010-06-02 | 中国纺织工业设计院 | PTA refined mother liquor reclaiming method and system |
| CN103241857B (en) * | 2012-10-11 | 2014-12-17 | 大连凯信石化科技有限公司 | Method for treating waste water discharged from refining process of purified terephthalic acid production device |
| CN104512943B (en) * | 2013-09-29 | 2016-05-11 | 中国石油化工股份有限公司 | Oxidized waste water reuse technology in a kind of aromatic carboxylic acid production process |
| CN103663758B (en) * | 2013-11-28 | 2015-10-21 | 亚东石化(上海)有限公司 | A kind of recoverying and utilizing method of water from refined p-benzene dicarboxylic acid production |
| CN105152389A (en) * | 2015-07-18 | 2015-12-16 | 常州大学 | Method for recovering purified terephthalic acid in chemical wastewater |
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