CN1858007A - Treating and resourcing method for 4.4-diamido diphenyl propylene-2-disulfonic acid production oxide waste water - Google Patents
Treating and resourcing method for 4.4-diamido diphenyl propylene-2-disulfonic acid production oxide waste water Download PDFInfo
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- CN1858007A CN1858007A CN200610038630.3A CN200610038630A CN1858007A CN 1858007 A CN1858007 A CN 1858007A CN 200610038630 A CN200610038630 A CN 200610038630A CN 1858007 A CN1858007 A CN 1858007A
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- resin
- waste water
- desorption
- dsd
- dsd acid
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- 239000002253 acid Substances 0.000 title claims abstract description 39
- 239000002351 wastewater Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 235000010290 biphenyl Nutrition 0.000 title 1
- 239000004305 biphenyl Substances 0.000 title 1
- 125000006267 biphenyl group Chemical group 0.000 title 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 title 1
- 229920005989 resin Polymers 0.000 claims abstract description 53
- 239000011347 resin Substances 0.000 claims abstract description 53
- 238000003795 desorption Methods 0.000 claims abstract description 32
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 238000010521 absorption reaction Methods 0.000 claims description 20
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 14
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 14
- 239000003463 adsorbent Substances 0.000 claims description 13
- 150000002148 esters Chemical class 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229920001429 chelating resin Polymers 0.000 claims description 9
- 230000006872 improvement Effects 0.000 claims description 7
- 230000008929 regeneration Effects 0.000 claims description 7
- 238000011069 regeneration method Methods 0.000 claims description 7
- 238000002203 pretreatment Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 150000002895 organic esters Chemical class 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000004925 Acrylic resin Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000012467 final product Substances 0.000 description 3
- 230000000274 adsorptive effect Effects 0.000 description 2
- 238000009303 advanced oxidation process reaction Methods 0.000 description 2
- 230000031018 biological processes and functions Effects 0.000 description 2
- 238000001311 chemical methods and process Methods 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- PJANXHGTPQOBST-VAWYXSNFSA-N trans-stilbene Chemical group C=1C=CC=CC=1/C=C/C1=CC=CC=C1 PJANXHGTPQOBST-VAWYXSNFSA-N 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- ZPTVNYMJQHSSEA-UHFFFAOYSA-N 4-nitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1 ZPTVNYMJQHSSEA-UHFFFAOYSA-N 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 101100412856 Mus musculus Rhod gene Proteins 0.000 description 1
- 102000004316 Oxidoreductases Human genes 0.000 description 1
- 108090000854 Oxidoreductases Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000019600 saltiness Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical compound C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 235000021286 stilbenes Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000271 synthetic detergent Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention discloses oxide waste water treating and resourcing process for DSD acid production. The process includes the following steps: adsorption of the pre-treated oxide waste water from DSD acid production in apparatus filled with macroporous adsorbing acrylate resin at normal temperature and flow rate of 0.5-5 BV/hr; neutralizing with alkali before exhaust; desorption of the resin to regenerate at the temperature of 80-98 deg.c and flow rate of 0.5-3.0 BV/hr, returning the high concentration desorption solution to DSD acid production and using the low concentration desorption solution for next desorption. The said process can lower DNS acid content from 4500 mg/L to below 2.0 mg/L and lower CODCr from 15000 mg/L to below 100 mg/L reaching the exhaust standard, and has the advantages of capacity of separating out DSD acid, saving in material and no secondary pollution.
Description
One, technical field
The present invention relates to a kind of DSD acid and produce the improvement and the method for resource of oxidized waste water, particularly, be meant that adopting acrylic resin to reclaim DSD acid produces in the oxidized waste water other organic removal in DNS acid and the waste water.。
Two, background technology
DSD acid is a kind of important dyestuff intermediate, and being used for synthetic toluylene type white dyes and stilbene is substantive dyestuff, reactive dyestuffs.Synthetic detergent, textile industry, plastics, photograph and paper industry etc. have been widely used in by DSD acid synthetic white dyes.The synthetic route of DSD acid mainly is raw material with the para-nitrotoluene, finishes through oversulfonate, oxidation, reduction three big steps.Wherein produce a large amount of salt-containing organic wastewater (DSD acid per ton produces about 25～30 tons of waste water) in the oxidation operation, wherein main organism DNS acid content is about 4500mg/L, COD
CrContent is up to 15000mg/L, and colourity is about 15000 times, and pH is about 1.5～2.5, inorganic salt (Na
2SO
4) content is up to 14% (massfraction), is one of wastewater from chemical industry of at present refractory reason.If directly enter water body, not only with serious environment pollution, be detrimental to health, and the serious waste resource.
The treatment process of oxidized waste water mainly contained biological process, advanced oxidation processes and physico-chemical process etc. during DSD acid was at present produced, and wherein biological process is difficult to adapt to the high characteristics of DSD acid oxidase wastewater toxicity; Advanced oxidation processes requires harsh to reaction conditions, to the equipment requirements height, and working cost height, operational administrative complexity; Physico-chemical process exists the reagent consumption amount greatly, easily to produce shortcomings such as secondary pollution, poor processing effect.At present the resin that adopts resin adsorption method to handle high concentrated organic wastewater has ion exchange resin and superhigh cross-linking resin, but these two kinds of resins can't adapt to DSD acid produce in oxidized waste water acidity big, saltiness is high, contain the characteristics of high concentration organic contaminant.
Three, summary of the invention
The purpose of this invention is to provide a kind of DSD acid and produce the improvement and the method for resource of oxidized waste water, utilize the esters of acrylic acid macroporous adsorbent resin, raw material DNS acid that can the Separation and Recovery overwhelming majority can make the wastewater reduction, innoxious of final discharge again, realizes the target of recycling economy.
Technical scheme of the present invention is as follows:
The improvement and the method for resource of oxidized waste water produced in a kind of DSD acid, and it may further comprise the steps:
(a) DSD acid is produced oxidized waste water through after the pre-treatment, under the flow condition of 0～40 ℃ temperature and 0.5～5BV/h, by being filled with the device of esters of acrylic acid macroporous adsorbent resin, absorption effluent add in the alkali and after can discharge;
(b) the high-temperature water desorption and regeneration of organic esters of acrylic acid macroporous adsorbent resin with 80～98 ℃ will have been adsorbed in the step (a), eluting temperature is 80～98 ℃, the desorbing agent flow is 0.5～3.0BV/h, high concentration desorption liquid returns DSD acid production process as raw material, and light concentration desorption liquid can be used for preparing next batch desorbing agent recycled.
Pre-treatment is meant waste water is removed by filter wherein suspended matter earlier in the step (a), adsorption temp keeps getting final product at normal temperatures (0～40 ℃), after step (a) processing, absorption effluent is transparent light yellow, CODCr can reduce to about 100mg/L, the DNS acid content is reduced to below the 2.0mg/L, add in the alkali and after get final product qualified discharge.
Can separate out the DNS acid crystal of purity more than 80% in the desorption liquid in the step (b), the esters of acrylic acid macroporous adsorbent resin can use behind desorption and regeneration repeatedly.
Esters of acrylic acid macroporous adsorbent resin described in the step (a) is Amberlite XAD-6 resin, Amberlite XAD-7 resin, Amberlite XAD-8 resin, Diaion HP1MG resin, DiaionHP2MG resin, Diaion HP3MG resin (Amberlite XAD series is produced by U.S. Rhom and Hass, and Diaion HPMG series is produced by MIT) or esters of acrylic acid YWB-38 resin (Jiangsu Nanda Gede Environmental Protection Technology Co., Ltd's production).Preferred esters of acrylic acid macroporous adsorbent resin is the YWB-38 resin.
In the concrete operations step, the absorption of resin can be adopted double-column in series absorption, the operation scheme of single tower desorption, be that every kind of resin is provided with I, II, three adsorption towers of III, 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, the I tower carries out the following current desorption simultaneously, and so cyclical operation can guarantee the operation continuously all the time of whole device.
Beneficial effect
The present invention compared with prior art, its remarkable advantage is: (1) employed esters of acrylic acid macroporous adsorbent resin (the pH value is about 1.5～2.5) under the original acidity of waste water can obtain the maximal absorptive capacity to DNS acid, and raw wastewater need not acid adjustment and gets final product adsorption treatment.(2) after second resin absorption, the content of DNS is reduced to below the 2.0mg/L by 4500mg/L in the waste water, and the CODCr of waste water reduces to about 100mg/L by 15000mg/L, makes final factory effluent reach wastewater discharge standard.(3) having adsorbed organic esters of acrylic acid macroporous adsorbent resin such as DNS acid can separate out the DNS acid crystal of purity more than 80% directly with 80～98 ℃ water desorption in the desorption liquid, the rest high concentration desorption liquid returns production workshop section and reclaims DNS acid.Promptly save raw material, avoided secondary pollution again.(4) the esters of acrylic acid macroporous adsorbent resin can be high temperature resistant, long service life, and renewable performance is good, reusable advantage.
Four, embodiment
Further specify the present invention by the following examples.
Embodiment 1:
Embodiment 1: the YWB-38 resin of each 10mL is respectively charged into (Φ 12 * 160mm), are respectively I, II, three adsorption towers of III in the glass adsorption column of three strap clamps covers.The brown waste water of getting 150mL carries out pre-treatment, and feed glass chuck water temperature is 15 ± 1 ℃, with waste water with the flow of 1BV/h by the YWB-38 resin bed, treatment capacity is that 150mL/ criticizes, absorption effluent is light yellow, COD
CrReduce to 100mg/L, the DNS acid content is reduced to 2.0mg/L.Water outlet can reach corresponding sewage drainage standard through neutralization again.The absorption of resin can be adopted double-column in series absorption, the operation scheme of single tower desorption.Earlier with I, II tower series connection following current absorption, the I tower is as first post, 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, the I tower carries out the following current desorption simultaneously, and so cyclical operation can guarantee the operation continuously all the time of whole device.
YWB-38 resin after absorption carries out wash-out regeneration with the water of 35mL, and eluting temperature is 90 ℃, and the eluent flow is 1BV/h.Can separate out the DNS acid crystal of purity more than 80% in the desorption liquid, high density residue desorption liquid returns production workshop section, and lower concentration elutriant cover is used for following batch desorption manipulation, and resin can recover adsorptive power behind desorption and regeneration.
Embodiment 2: the YWB-38 resin of each 100mL is respectively charged into (Φ 32 * 250mm) in the glass adsorption column of three strap clamps covers.The brown waste water of getting 1500mL carries out pre-treatment, and feed glass chuck water temperature is 30 ± 1 ℃, with waste water with the flow of 1BV/h at first by the YWB-38 resin bed, treatment capacity is that 1500mL/ criticizes, absorption effluent is light yellow, COD
CrReduce to 100mg/L, the DNS acid content is reduced to 2.0mg/L.Water outlet can reach corresponding sewage drainage standard through neutralization again.
YWB-38 resin after absorption carries out wash-out regeneration with the water of 350mL, and eluting temperature is 90 ℃, and the eluent flow is 1BV/h.Can separate out the DNS acid crystal of purity more than 80% in the desorption liquid, high density residue desorption liquid returns production workshop section, and lower concentration elutriant cover is used for following batch desorption manipulation, and resin can recover adsorptive power behind desorption and regeneration.
Embodiment 3: change the second resin among the embodiment 1 into Amberlite XAD-6 resin, AmberliteXAD-7 resin, Amberlite XAD-8 resin, Diaion HP1MG resin, Diaion HP2MG resin or Diaion HP3MG resin, other operational conditions remain unchanged, and every batch processing amount and effluent quality all slightly are inferior to embodiment 1.
Embodiment 4: the adsorption temp among the embodiment 1 is substituted with 40 ℃, and desorption temperature substitutes with 70 ℃, and other operational conditions remain unchanged, and every batch processing amount and effluent quality all slightly are inferior to embodiment 1.
Embodiment 5: the absorption flow among the embodiment 1 is substituted with 6BV/h, and the desorption flow substitutes with 4BV/h, and other operational conditions remain unchanged, and every batch processing amount and effluent quality all slightly are inferior to embodiment 1.
Embodiment 6: the absorption flow among the embodiment 1 is substituted with 0.5BV/h, and the desorption flow substitutes with 0.5BV/h, and other operational conditions remain unchanged, and every batch processing amount and effluent quality all slightly are inferior to embodiment 1.
Embodiment 7: the adsorption temp among the embodiment 1 is substituted with 25 ℃, and desorption temperature substitutes with 98 ℃, and other operational conditions remain unchanged, and every batch processing amount and effluent quality are similar to Example 1.
Embodiment 8: the adsorption temp among the embodiment 1 is substituted with 5 ℃, and desorption temperature substitutes with 80 ℃, and other operational conditions remain unchanged, and every batch processing amount and effluent quality slightly are inferior to embodiment 1.
Claims (3)
1. the improvement and the method for resource of oxidized waste water produced in DSD acid, it is characterized in that may further comprise the steps:
(a) DSD acid is produced oxidized waste water through after the pre-treatment, under the flow condition of 0～40 ℃ temperature and 0.5～5BV/h, by being filled with the device of esters of acrylic acid macroporous adsorbent resin, absorption effluent add in the alkali and after can discharge;
(b) the high-temperature water desorption and regeneration of organic esters of acrylic acid macroporous adsorbent resin with 80～98 ℃ will have been adsorbed in the step (a), eluting temperature is 80～98 ℃, the desorbing agent flow is 0.5～3.0BV/h, high concentration desorption liquid returns DSD acid production process as raw material, and light concentration desorption liquid can be used for preparing next batch desorbing agent recycled.
2. the improvement and the method for resource of oxidized waste water produced in a kind of DSD acid according to claim 1, it is characterized in that the esters of acrylic acid macroporous adsorbent resin described in the step (a) is Amberlite XAD-6 resin, Amberlite XAD-7 resin, Amberlite XAD-8 resin, Diaion HPIMG resin, HP2MG resin, HP3MG resin or YWB-38 resin.
3. the improvement and the method for resource of oxidized waste water produced in a kind of DSD acid according to claim 2, it is characterized in that the esters of acrylic acid macroporous adsorbent resin described in the step (a) is the YWB-38 resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100386303A CN100560512C (en) | 2006-03-06 | 2006-03-06 | A kind of 4,4-diaminobenzil-2, the 2-disulfonic acid is produced the improvement and the method for resource of oxidized waste water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100386303A CN100560512C (en) | 2006-03-06 | 2006-03-06 | A kind of 4,4-diaminobenzil-2, the 2-disulfonic acid is produced the improvement and the method for resource of oxidized waste water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1858007A true CN1858007A (en) | 2006-11-08 |
| CN100560512C CN100560512C (en) | 2009-11-18 |
Family
ID=37296969
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100386303A Active CN100560512C (en) | 2006-03-06 | 2006-03-06 | A kind of 4,4-diaminobenzil-2, the 2-disulfonic acid is produced the improvement and the method for resource of oxidized waste water |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100560512C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295393A (en) * | 2011-08-22 | 2011-12-28 | 山西阳煤丰喜肥业(集团)有限责任公司 | Treatment process for production wastewater of DSD acid |
| CN103910454A (en) * | 2014-04-24 | 2014-07-09 | 山西阳煤丰喜肥业(集团)有限责任公司 | Device and method for decreasing temperature of DSD (4,4'-diamido diphenylethylene-disulfonic acid) wastewater |
| CN104512943A (en) * | 2013-09-29 | 2015-04-15 | 中国石油化工股份有限公司 | Reuse technology for oxidized wastewater in production process of aromatic carboxylic acids |
| CN108727858A (en) * | 2018-06-07 | 2018-11-02 | 连云港莱亚化学有限公司 | A method of the oxidized waste water generated using production DSD acid prepares direct yellow dye |
-
2006
- 2006-03-06 CN CNB2006100386303A patent/CN100560512C/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295393A (en) * | 2011-08-22 | 2011-12-28 | 山西阳煤丰喜肥业(集团)有限责任公司 | Treatment process for production wastewater of DSD acid |
| CN102295393B (en) * | 2011-08-22 | 2012-09-05 | 山西阳煤丰喜肥业(集团)有限责任公司 | Treatment process for production wastewater of DSD acid |
| CN104512943A (en) * | 2013-09-29 | 2015-04-15 | 中国石油化工股份有限公司 | Reuse technology for oxidized wastewater in production process of aromatic carboxylic acids |
| 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 |
| CN103910454A (en) * | 2014-04-24 | 2014-07-09 | 山西阳煤丰喜肥业(集团)有限责任公司 | Device and method for decreasing temperature of DSD (4,4'-diamido diphenylethylene-disulfonic acid) wastewater |
| CN108727858A (en) * | 2018-06-07 | 2018-11-02 | 连云港莱亚化学有限公司 | A method of the oxidized waste water generated using production DSD acid prepares direct yellow dye |
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| Publication number | Publication date |
|---|---|
| CN100560512C (en) | 2009-11-18 |
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Assignee: Hebei Hua-chem Dye Chemical Co., Ltd. Assignor: Nanjing University|Jiangsu NTU Godwin Environmental Technology Co. Ltd. Contract record no.: 2010130000113 Denomination of invention: Method for preparing 4,4'- bi (4 - carboxyl phthalimide group) 3,3'- dimethyl diphenylmothane Granted publication date: 20091118 License type: Exclusive License Open date: 20061108 Record date: 20101119 |
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Address after: 210093 Hankou Road, Jiangsu, China, No. 22, No. Patentee after: Nanjing University Patentee after: Jiangsu NJU Environmental Technology Co., Ltd. Address before: 210093 Hankou Road, Jiangsu, China, No. 22, No. Patentee before: Nanjing University Patentee before: Jiangsu N&J Environmental Technology Co., Ltd. |
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Application publication date: 20061108 Assignee: Choi Yue chemical (Dong Guang) Limited Assignor: Jiangsu NANDA environmental protection science and Technology Co., Ltd.|Nanjing University Contract record no.: 2015320000022 Denomination of invention: Method for preparing 4,4'- bi (4 - carboxyl phthalimide group) 3,3'- dimethyl diphenylmothane Granted publication date: 20091118 License type: Exclusive License Record date: 20150203 |