CN1129556C - Treatment and source recovering method for waste water of 1,4-dihydroxy anthraquinone produetion - Google Patents
Treatment and source recovering method for waste water of 1,4-dihydroxy anthraquinone produetion Download PDFInfo
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- CN1129556C CN1129556C CN00112386.6A CN00112386A CN1129556C CN 1129556 C CN1129556 C CN 1129556C CN 00112386 A CN00112386 A CN 00112386A CN 1129556 C CN1129556 C CN 1129556C
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- dihydroxyanthraquinone
- phthalic acid
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- desorbing agent
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- 239000002351 wastewater Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 16
- GUEIZVNYDFNHJU-UHFFFAOYSA-N quinizarin Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C(O)=CC=C2O GUEIZVNYDFNHJU-UHFFFAOYSA-N 0.000 title abstract description 6
- 229920005989 resin Polymers 0.000 claims abstract description 26
- 239000011347 resin Substances 0.000 claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000001179 sorption measurement Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 48
- 229960001156 mitoxantrone Drugs 0.000 claims description 30
- 238000003795 desorption Methods 0.000 claims description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000010521 absorption reaction Methods 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 9
- 239000003463 adsorbent Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 claims description 2
- PCWZHTGDXLRULT-UHFFFAOYSA-N buta-1,3-dienylbenzene styrene Chemical compound C(=C)C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 PCWZHTGDXLRULT-UHFFFAOYSA-N 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000008929 regeneration Effects 0.000 claims description 2
- 238000011069 regeneration method Methods 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 abstract 2
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical compound C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 abstract 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 abstract 1
- -1 anthraquinone compounds Chemical class 0.000 abstract 1
- 239000003480 eluent Substances 0.000 abstract 1
- LGRFSURHDFAFJT-UHFFFAOYSA-N phthalic anhydride Chemical compound C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229920001429 chelating resin Polymers 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- WXNZTHHGJRFXKQ-UHFFFAOYSA-N 4-chlorophenol Chemical compound OC1=CC=C(Cl)C=C1 WXNZTHHGJRFXKQ-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000001000 anthraquinone dye Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- XZKRXPZXQLARHH-UHFFFAOYSA-N buta-1,3-dienylbenzene Chemical compound C=CC=CC1=CC=CC=C1 XZKRXPZXQLARHH-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229940090668 parachlorophenol Drugs 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 150000003022 phthalic acids Chemical class 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Water Treatment By Sorption (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention discloses a method for treating waste water of 1, 4-dihydroxy anthraquinone production and recovering resources. Waste water passes through macroporous adsorption resin with styrene-divinyl benzene copolymerization so that phthalate and a small quantity of anthraquinone compounds in the waste water are adsorbed on the macroporous resin which is eluted by a sodium hydroxide solution and then is regenerated, and meanwhile, the phthalate is recovered after an eluent is acidified. After the present invention is used for treating, the colorless transparent CODcr content of effluent water is reduced to be less than 100 mg/L, the removing rate is more than 99.5%, the removing rate of the phthalandione is more than 99.5, the recovery rate is more than 90%, the crystal recovering purity is from 97.9% to 99.6%, and the removing rate of 1, 4-dihydroxy anthraquinone is 100%.
Description
One, technical field
The present invention relates to anthraquinone dye and intermediate 1, the improvement of 4-dihydroxyanthraquinone factory effluent specifically, is 1, the recycling of phthalic acid and other organic removal in the 4-dihydroxyanthraquinone factory effluent.
Two, background technology
1, the 4-dihydroxyanthraquinone is a kind of important dyestuff intermediate, itself also is a kind of important dyestuff.Domestic main employing at present is traditional is the synthetic route of raw material with the Resorcinol or is the raw material synthetic route with the para-chlorophenol, produces 1 ton 1, and the 4-dihydroxyanthraquinone will discharge 60~96 tons scarlet waste water, COD
CrUp to 7000~24000mg/L, wherein mainly contain the phthalic acid of 4700~12000mg/L and a spot of 1,4-dihydroxyanthraquinone, 1, product and by products thereof such as 5-dihydroxyanthraquinone also contain 0.5~20% sulfuric acid and a spot of boric acid in addition.
Literature search is the result show, do not relate to 1, the improvement and the resource recycling of 4-dihydroxyanthraquinone factory effluent in the existing domestic and foreign literature report.
Three, summary of the invention
The purpose of this invention is to provide a kind of technology, can not only effectively administer 1,4-dihydroxyanthraquinone factory effluent is removed wherein most organic, the Organic Chemicals phthalic acid that can also enriching and recovering wherein runs off is realized the unification of waste water treatment and resource recycling.
Technical scheme of the present invention is as follows:
A kind of 1, the improvement of 4-dihydroxyanthraquinone factory effluent and resource recycling method, it is that factory effluent is carried out pre-treatment, promptly for containing 1, the 4-dihydroxyanthraquinone is lower than the waste water of 10mg/L, pre-treatment is a direct filtration, for containing 1, the 4-dihydroxyanthraquinone is higher than the waste water of 10mg/L, regulates PH to 3-4 earlier, refilter, remove wherein 1,4-dihydroxyanthraquinone and suspended substance are to guarantee the adsorption efficiency of resin in the governance process, improve the purity that reclaims phthalic acid simultaneously, will follow these steps to administer and recycle through pretreated factory effluent then:
A) will be through pretreated 1, the macroporous adsorbent resin of the waste water that discharges in 4-dihydroxyanthraquinone production process vinylbenzene one Vinylstyrene copolymerization by being filled with spheroidal particle under the flow of 0~60 ℃ temperature and 0.5~7BV/h also has the adsorption tower of heating jacket, make phthalic acid and remaining a small amount of 1, the 4-dihydroxyanthraquinone is adsorbed on the macroporous adsorbent resin, the absorption effluent water white transparency, COD
CrWith organic content all below 100mg/L, can requiring reuse to make production workshop section bath water or carry out the comprehensive utilization of spent acid or add in the alkali and directly discharging of back according to the difference of acid content wherein and producer's technology, economic dispatch each side factor.
B) with concentration be the NaOH solution of 0.5~4mol/L as desorbing agent, will adsorb phthalic acid and a small amount of 1, the macroporous adsorbent resin wash-out regeneration of 4-dihydroxyanthraquinone, eluting temperature is 20~95 ℃, the desorbing agent flow is 0.2~3.0BV/h.
C) the high density elutriant that elutes partly uses vitriol oil acid adjustment to pH<4~6, filter, obtain the O-phthalic acid crystal, filtrate is further reclaimed the O-phthalic acid crystal through concentrating again, and the crystal thorough drying that the operation of two steps is collected is to remove wherein moisture.Raffinate burning disposal after concentrating.The lower concentration of elutriant partly is used to prepare next batch desorbing agent recycled.
Above-mentioned vinylbenzene-Vinylstyrene copolymerization macroporous adsorbent resin can be homemade NDA-404 resin or CHA-101 or X-5 or H-103 resin, can also be AmberliteXAD-2, XAD-4, XAD-7 or the XAD-8 resin that U.S. Rohm-Haas company produces, or Mitsubishi changes into Diaion HP series macroporous adsorbent resin, the preferably NDA-404 or the CHA-101 resin of company's Development and Production.
Desorbing agent in the aforesaid method can also replace aqueous sodium hydroxide solution with methyl alcohol or ethanol, when doing desorbing agent with methyl alcohol or ethanol, desorption temperature is respectively 20~50 ℃ and 20~70 ℃, high concentration desorption liquid reclaims methyl alcohol or ethanol through rectifying, obtain phthalic acid and a small amount of 1 simultaneously, the mixture of 4-dihydroxyanthraquinone, dehydration obtains Tetra hydro Phthalic anhydride under 200 ℃, returns synthesizing section as raw material.The lower concentration of elutriant partly is used to prepare next batch desorbing agent recycled.
The present invention 1, the improvement of 4-dihydroxyanthraquinone factory effluent and resource recycling method can adopt double-column in series absorption, the operation method of single tower desorption, I, II, three adsorption towers of III promptly are set, earlier with I, II tower following current series connection absorption, the I tower is as the one-level adsorption tower, the II tower after the absorption of I tower is saturated, switches to II, III tower following current series connection absorption as the secondary absorption tower, the II tower is as the one-level adsorption tower, the III tower is as the secondary absorption tower, and the I tower carries out reverse desorption simultaneously, so cyclical operation, can guarantee the operation continuously all the time of whole device, raise the efficiency.
The present invention 1, and the improvement and the resource recycling method of 4-dihydroxyanthraquinone factory effluent can make COD
CrBe 7000~24000mg/L, contain 4700~12000mg/L phthalic acid and 7~120mg/L1, the organic scarlet strongly acid wastewater of 4-dihydroxyanthraquinone and other minute quantities is after treatment, water outlet water white transparency, COD
CrReduce to below the 100mg/L, clearance is more than 99.5%, and the clearance of phthalic acid is more than 99.5%, and the rate of recovery reaches more than 90%, and reclaiming crystal purity is 97.9~99.6%, 1, and the clearance of 4-dihydroxyanthraquinone is 100%.Water outlet can be according to wherein the difference of acid content and the requirement of producer turn back to comprehensive utilization or the direct neutralization back discharging that production workshop section is used as washing water or carries out spent acid.According to 4.23~10.8 kilograms of recyclable phthalic acids in this method waste water per ton.
Four, embodiment
Further specify the present invention by the following examples.
Embodiment 1: the glass adsorption column (among the Φ 24 * 320mm) that 60ml (about 45g) NDA-404 resin is packed into and had insulation jacket, (10 ℃~25 ℃) allow the filtering workshop of process waste discharge pass through resin bed with the flow of 125ml/h under the room temperature, wastewater treatment capacity is that 600ml/ criticizes waste water COD
CrConcentration is 11325.8mg/L, and the O-phthalic acid concentration is 8174.8mg/L, 1, and 4-dihydroxyanthraquinone concentration is 7mg/L, the absorption effluent water white transparency wherein contains phthalic acid 37.6mg/L, COD
CrConcentration is 64.0mg/L, and clearance all is higher than 99.5%; 1, the 4-dihydroxyanthraquinone does not detect, and clearance is 100%.
NaOH aqueous solution flow adverse current with 30ml/h under 70 ± 5 ℃ temperature with 120ml 1mol/L is carried out desorption by resin bed, and organic desorption rate is 100%.100ml high concentration desorption liquid before collecting, through acid out---concentrate the operation of two steps and reclaim the O-phthalic acid crystal, yield is 4.51g, and the rate of recovery reaches 92.0%.Raffinate burning disposal after concentrating.Back 20ml light concentration desorption liquid is as the preparation of next batch desorbing agent.
Embodiment 2: adsorption column and operational condition are with embodiment 1, but filling Amberlite XAD-4 resin 60ml (about 45g), the O-phthalic acid content is reduced to 70.9mg/L from 7554.3mg/L in the waste water, clearance reaches 99.1%, the water outlet water white transparency, 1, the 4-dihydroxyanthraquinone does not detect.
NaOH aqueous solution flow adverse current with 30ml/h under 90 ± 5 ℃ temperature with 120ml 2mol/L is carried out desorption by resin bed, and organic desorption rate is 100%.High concentration desorption liquid reclaims the O-phthalic acid crystal, and yield is 4.15g, and the rate of recovery reaches 91.6%.Light concentration desorption liquid is as the preparation of next batch desorbing agent.
Embodiment 3: (Φ 250 * 3500mm) to adopt three identical band insulation jacket stainless steel adsorption columns of specification, every column bottom and pre-portion cover with stainless (steel) wire (50 order), fill with thick quartz sand (about 20L) at the bottom of the post, every post filling 90 kilograms of resins of NDA-404 (about 120L), twin columns series connection absorption, the single-column desorption.With COD
CrBe 7000~24000mg/L, the O-phthalic acid concentration is 4700~12000mg/L, 1, and 4-dihydroxyanthraquinone concentration is that the factory effluent of 6~120mg/L is removed the wherein suspended substance and the overwhelming majority 1 through pre-treatment earlier, the 4-dihydroxyanthraquinone uses pump with 0.35m again
3The flow of/h is squeezed into adsorption column from capital, and adsorption column adopts the mode of I, II twin columns following current series connection absorption, and every batch processing amount is controlled at 1.5m
3About, water outlet drains into storage tank from the II column bottom.Waste water water white transparency after the processing, average COD
CrLess than 100mg/L, the mean concns of phthalic acid is less than 50mg/L, and 1, the 4-dihydroxyanthraquinone does not detect, and can directly turn back to production workshop section and fully utilize as the washing water or the vitriolic that give up.
After every batch of absorption finished, the I post carried out desorption manipulation, and II, III proceed adsorption operations, at this moment post headed by the II post.After the raffinate emptying, in chuck, inject hot water in the I post, make resin be preheated to 90 ± 5 ℃, use 0.36m again
38% NaOH solution with 0.12m
3The flow of/h carries out desorption by resin bed from bottom to top, and desorption liquid enters storage tank, and is stand-by.After desorption finishes, use 0.25m
3Steam condensate clean resin to neutrality or weakly alkaline.
I post after III post and desorption finish is formed the absorption of connect, post headed by the III post at this moment, and the II post carries out desorption manipulation.So circulation is carried out, but assurance device move continuously, raise the efficiency.
High concentration desorption liquid in the storage tank transfers to acidity with the vitriol oil earlier, has crystal to separate out, and filters and collects; Filtrate filtered is carried out evaporation concentration again, has the part crystal to separate out again, filters and collects, and is high-purity o phthalic acid solid after the oven dry.
Adopt technical finesse 1 of the present invention; the method of 4-dihydroxyanthraquinone factory effluent is effective and feasible; in removing waste water, reclaimed wherein useful industrial chemicals in the organic pollutant; water outlet after administering simultaneously can be overlapped to use and be made washing water in the production technique; can also carry out the comprehensive utilization of spent acid; greatly reduce discharged waste water and pollutant load, environment protection is had positive effect.
Embodiment 4: change the polymeric adsorbent among the embodiment 1 into Amberlite XAD-2, XAD-7, XAD-8 or Diaion HP-10, Diaion HP-20, Diaion HP-30 resin and homemade CHA-101, H-103, X-5 resin, except that the processing wastewater flow rate changed to some extent, other results substantially roughly the same.
Claims (3)
1. one kind 1, the improvement of 4-dihydroxyanthraquinone factory effluent and resource recycling method is characterized in that:
A) with 1, the waste water that discharges in the 4-dihydroxyanthraquinone production process after filtration or light regulate PH to 3~4, refilter, then under the flow of 0~60 ℃ temperature and 0.5~7BV/h by macroporous adsorbent resin that is filled with particulate vinylbenzene-Vinylstyrene copolymerization and the adsorption tower that has heating jacket, make phthalic acid and remaining a small amount of 1, the 4-dihydroxyanthraquinone is adsorbed on the macroporous adsorbent resin, absorption effluent water white transparency, COD
CrWith organic content all below 100mg/L,
B) with concentration be the NaOH solution of 0.5~4mol/L as desorbing agent, will adsorb phthalic acid and a small amount of 1, the macroporous adsorbent resin wash-out regeneration of 4-dihydroxyanthraquinone, eluting temperature is 20~95 ℃, the desorbing agent flow is 0.2~3.0BV/h,
C) the high density elutriant that elutes partly uses vitriol oil acid adjustment to pH<4~6, filter, obtain the O-phthalic acid crystal, filtrate is further reclaimed the O-phthalic acid crystal through concentrating again, the crystal thorough drying that two step operations are collected is to remove wherein moisture, raffinate burning disposal after concentrating, the lower concentration of elutriant partly is used to prepare next batch desorbing agent recycled.
2. method according to claim 1, it is characterized in that desorbing agent replaces aqueous sodium hydroxide solution with methyl alcohol or ethanol, when doing desorbing agent with methyl alcohol or ethanol, desorption temperature is respectively 20~50 ℃ and 20~70 ℃, high concentration desorption liquid reclaims methyl alcohol or ethanol through rectifying, obtain phthalic acid and a small amount of 1 simultaneously, the mixture of 4-dihydroxyanthraquinone, dehydration obtains Tetra hydro Phthalic anhydride under 200 ℃, return synthesizing section as raw material, the lower concentration of elutriant partly is used to prepare next batch desorbing agent recycled.
3. method according to claim 1, it is characterized in that being provided with I, II, three adsorption towers of III, with I, II tower following current series connection absorption, the I tower is as the one-level adsorption tower earlier, and the II tower is as the secondary absorption tower, after the absorption of I tower is saturated, switch to II, III tower following current series connection absorption, the II tower is as the one-level adsorption tower, and the III tower is as the secondary absorption tower, with the I tower being carried out reverse desorption, so cyclical operation.
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Cited By (1)
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CN100417634C (en) * | 2006-08-25 | 2008-09-10 | 南京大学 | Method of separating and recovering fumaric acid and phthalic acid in fumaric acid preparation wastewater |
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CN105693505A (en) * | 2014-11-27 | 2016-06-22 | 江苏华尔化工有限公司 | Treatment method of 1,4-dihydroxyanthraquinone industrial wastewater |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN100417634C (en) * | 2006-08-25 | 2008-09-10 | 南京大学 | Method of separating and recovering fumaric acid and phthalic acid in fumaric acid preparation wastewater |
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