CN101376747A - Method for recycling bipseudoindoxyl dye from indigo dyeing waste water - Google Patents

Method for recycling bipseudoindoxyl dye from indigo dyeing waste water Download PDF

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Publication number
CN101376747A
CN101376747A CNA2008101564186A CN200810156418A CN101376747A CN 101376747 A CN101376747 A CN 101376747A CN A2008101564186 A CNA2008101564186 A CN A2008101564186A CN 200810156418 A CN200810156418 A CN 200810156418A CN 101376747 A CN101376747 A CN 101376747A
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waste water
indigo
bipseudoindoxyl dye
dye
reclaims
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CN101376747B (en
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邱滔
徐圃清
张晟
石剑虹
刘子辉
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Liyang Chang Technology Transfer Center Co., Ltd.
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Jiangsu Polytechnic University
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Abstract

The invention discloses a method for recycling an indigo dye from the indigo waste coloring water. In the method, a proper filtration fabric is selected first for filtering the fibers and impurities in the waste water; then an acid liquid is added into the waste water the fibers and impurities of which are removed to adjust the pH value between 2 and 7; air is blown for oxidation to oxidize sodium salt of a water-soluble indigo leuco body into an insoluble solid indigo dye; finally the indigo dye and a condensed liquid which is rich in the dye are obtained through a microfiltration membrane device. The method has the advantages of less investment and simple device; the recycled indigo dye and the recycled condensed liquid can be recycled for coloring a fabric; besides, after the indigo waste coloring water is treated by the membrane, the chroma, the turbidity and the COD, and the like, are greatly reduced. The removing rate of effluent color dilution after the membrane treatment is larger than 98 percent; the turbidity is reduced by more than 97 percent and the COD removing rate is larger than 30 percent.

Description

A kind of method that from indigo dyeing waste water, reclaims bipseudoindoxyl dye
Technical field
The present invention relates to a kind of method of wastewater treatment, particularly from indigo dyeing waste water, reclaim the method for bipseudoindoxyl dye.
Background technology
Indigo is the weaving synthetic dyestuff of consumption maximum in the world.What indigo dyeing was adopted is dip method yarn dyeing line.Indigo dye uptake is low, have near 20% bipseudoindoxyl dye can not on dye.Factory all adopts the repeatedly method of dip-dyes/oxidation earlier, obtaining colour fastness and dye level preferably, and then washing removal yam surface loose colour and color spot, can produce a large amount of dyeing waste-waters, this chroma in waste water is big, and the COD height belongs to one of difficult dyeing waste water.Treatment process is many at present is purpose with the water outlet emission compliance, indigo molecular structure stabilized, and intractability is big.
At present, the bipseudoindoxyl dye recovery method has: 1, reclaim indigo with the alum flocculation; 2, with the indigo waste water of electrolytic gas float glass process treating lab configuration, reclaim bipseudoindoxyl dye; 3, adopt acid neutralization, filtering method to reclaim indigo.But all not mentioned pre-treatment of these methods is removed fiber and solid impurity, is not had the recovering effect of clear and definite oxidizing condition, bipseudoindoxyl dye bad.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method that reclaims bipseudoindoxyl dye effectively from dyeing waste-water is provided, the bipseudoindoxyl dye in this method recoverable wastewater reduces the post-processing difficulty of waste water simultaneously.
The technical solution used in the present invention is to comprise the steps: in regular turn
1, select for use suitable filter cloth to remove by filter fiber and impurity in the waste water;
2, adding the acid solution adjust pH in the waste water after removing fiber and impurity is 2~7, and the drum atmospheric oxidation makes water miscible indigo leuco compound sodium salt be oxidized to insoluble solid bipseudoindoxyl dye;
3,, obtain bipseudoindoxyl dye and be rich in the concentrated solution of dyestuff by the microfiltration membrane device.
The invention has the beneficial effects as follows: invest little, equipment is simple.Bipseudoindoxyl dye that is reclaimed and concentrated solution can be back to textile dyeing, and indigo dyeing waste water is after film is handled, and colourity, turbidity, COD etc. reduce greatly.Film is handled back effluent color dilution clearance greater than 98%, and turbidity reduces more than 97%, and the COD clearance is more than 30%.
Embodiment
Collect yarn indigo dyeing after scouring water or dye vat waste liquid earlier, select for use suitable filter cloth to remove by filter fiber and impurity in the waste water, filter cloth is selected non-woven fabrics for use, classified processing or once filter to remove fiber and impurity can enter neutralization tank after PP25 (aperture is equivalent to the polypropylene filter cloth of 25 μ m) and PP5 (aperture is equivalent to the polypropylene filter cloth of 5 μ m) filter cloth prefiltration are removed fiber in the waste water and impurity.Add acid solution in the waste water after removing fiber and impurity and transfer pH to 2~7, be advisable, preferred pH=4 with slightly acidic.Rouse atmospheric oxidation then, water miscible indigo leuco compound sodium salt is oxidized to insoluble solid bipseudoindoxyl dye; Also can add acid solution control pH value in drum atmospheric oxidation process, oxidization time is 10min~4h, preferred 2 hours.In the oxidising process, the pH value rises, and adds acid solution control; At last by microfiltration membrane device commonly used, but the membrane pore size of microfiltration membrane is 0.1~1 μ m, microfiltration membrane device working pressure is 0~0.2MPa, wherein, the membrane pore size 0.2 μ m of preferred microfiltration membrane, preferred microfiltration membrane device working pressure 0.1Mpa utilizes the crown_interception of microfiltration membrane to reclaim bipseudoindoxyl dye, and effluent color dilution, turbidity, COD etc. reduce greatly behind the membrane filtration simultaneously.
Describe the present invention again in detail below by 5 embodiment:
Embodiment 1
Get 10L printing and dyeing mill indigo dyeing waste water, 1024 times of its colourities, turbidity 1430 NTU, COD 1800mg/L.Earlier after after non-woven fabrics PP25 and the PP5 filtration, with 1:1 sulphuric acid soln adjust pH, drum atmospheric oxidation 2 hours, control pH value is 4.Handle through 0.2 μ m PE membrane filtration then, working pressure is 0.08Mpa.The bipseudoindoxyl dye that reclaims can be used for textile dyeing.Film is handled in the water outlet of back and is not contained bipseudoindoxyl dye substantially, and its colourity is 8 times, clearance 99.2%; Turbidity 5 NTU reduce by 99.7%; COD 960mg/L, clearance 46.7%.
Embodiment 2
Get the indigo waste water of 8L printing and dyeing mill, 516 times of colourities, turbidity 932NTU, COD 1960mg/L.After non-woven fabrics PP25, PP5 filter, the sulphuric acid soln adjust pH, drum atmospheric oxidation 30min, control pH value is 2.Handle working pressure 0.05Mpa then through 0.1 μ m PE membrane filtration.The bipseudoindoxyl dye of holding back can be used for textile dyeing.Film is handled in the water outlet of back and is not contained bipseudoindoxyl dye, and its colourity is 8 times, clearance 98.5%, and turbidity 3.6 NTU reduce by 99.6%.COD 690mg/L, clearance 64.8%.
Embodiment 3
Get 8L printing and dyeing mill indigo dyeing waste water, 2024 times of its colourities, turbidity 3152 NTU, COD 2530mg/L.After non-woven fabrics PP25 and PP5 filtration, the sulphuric acid soln adjust pH, drum atmospheric oxidation 3 hours, control pH value is 6.Handle working pressure 0.1Mpa through 0.5 μ m PE micro-filtrate membrane filtration.The bipseudoindoxyl dye that reclaims can be used for textile dyeing.It is 32 times that film is handled the back effluent color dilution, clearance 98.4%, and turbidity 18.9 NTU reduce by 99.4%.COD1720mg/L, clearance 32%.
Example executes 4
Get 8L printing and dyeing mill indigo dyeing waste water, 2024 times of its colourities, turbidity 3560 NTU, COD 3920mg/L.After non-woven fabrics PP25, PP5 filter, the sulphuric acid soln adjust pH, drum atmospheric oxidation 4 hours, control pH value is 7.1.0 μ mPE micro-filtrate membrane filtration is handled, working pressure is to 0.2Mpa, and the bipseudoindoxyl dye that reclaims can be used for textile dyeing.Effluent color dilution is 64 times, clearance 96.8%, and turbidity 104.3 NTU reduce by 97.1%.COD 2730mg/L, clearance 30.4%.
Embodiment 5
Get 10L printing and dyeing mill indigo dyeing waste water, 2024 times of its colourities, turbidity 3560 NTU, COD 3920mg/L.After non-woven fabrics PP25, PP5 filter, atmospheric oxidation 10min is roused with 1:1 sulphuric acid soln adjust pH in the back earlier, and control pH value is 3.After 0.8 μ m PE micro-filtrate membrane filtration is handled working pressure 0.1Mpa.Film is held back bipseudoindoxyl dye and be can be used for textile dyeing.Effluent color dilution is 16 times, clearance 99.2%, and turbidity 24.8 NTU reduce by 99.3%.COD 2250mg/L, clearance 42.6%.

Claims (7)

1. method that reclaims bipseudoindoxyl dye from indigo dyeing waste water, it is characterized in that: this method comprises the steps: in regular turn
(1) select for use suitable filter cloth to remove by filter fiber and impurity in the waste water;
(2) adding the acid solution adjust pH in the waste water after removing fiber and impurity is 2~7, and the drum atmospheric oxidation makes water miscible indigo leuco compound sodium salt be oxidized to insoluble solid bipseudoindoxyl dye;
(3), obtain bipseudoindoxyl dye and be rich in the concentrated solution of dyestuff by the microfiltration membrane device.
2. a kind of method that reclaims bipseudoindoxyl dye from indigo dyeing waste water according to claim 1, it is characterized in that: the filter cloth in the step (1) is selected non-woven fabrics for use, classified processing or once filter and remove fiber and impurity.
3. a kind of method that reclaims bipseudoindoxyl dye from indigo dyeing waste water according to claim 1 is characterized in that: pH=4 in the step (2).
4. a kind of method that reclaims bipseudoindoxyl dye from indigo dyeing waste water according to claim 1 is characterized in that: add acid solution control pH value in the step (2) in drum atmospheric oxidation process, oxidization time is 10min~4h.
5. a kind of method that reclaims bipseudoindoxyl dye from indigo dyeing waste water according to claim 1, it is characterized in that: the membrane pore size of microfiltration membrane is 0.1~1 μ m in the step (3), and microfiltration membrane device working pressure is 0~0.2MPa.
6. a kind of method that reclaims bipseudoindoxyl dye from indigo dyeing waste water according to claim 4, it is characterized in that: oxidization time is 2h.
7. a kind of method that reclaims bipseudoindoxyl dye from indigo dyeing waste water according to claim 5, it is characterized in that: the membrane pore size of microfiltration membrane is 0.2 μ m, and microfiltration membrane device working pressure is 0.1Mpa.
CN2008101564186A 2008-10-10 2008-10-10 Method for recycling bipseudoindoxyl dye from indigo dyeing waste water Active CN101376747B (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102516817A (en) * 2011-12-28 2012-06-27 河北化工医药职业技术学院 Method for preparing indigo white solution
CN102531224A (en) * 2010-12-22 2012-07-04 常州市环境保护研究所 Method and device for recovering indigoid dye
CN104792598A (en) * 2015-03-25 2015-07-22 塔里木大学 Reduction liquid for treating waste alcohol generated after HE staining and preparation method of reduction liquid
CN105295444A (en) * 2015-11-10 2016-02-03 杭州天马思宏染织有限公司 High-purity salt-free reactive dye and manufacturing method thereof
CN106630307A (en) * 2016-09-30 2017-05-10 航天长征化学工程股份有限公司 System and method for treating coal gasification grey water
CN113231044A (en) * 2021-05-20 2021-08-10 南京工业大学 High-efficiency environment-friendly adsorption fiber for removing indigo in wastewater and preparation method thereof
CN113416967A (en) * 2021-06-17 2021-09-21 武汉纺织大学 Method for recycling indigo dye in waste jeans and fabric dyeing method
CN113549938A (en) * 2021-06-17 2021-10-26 武汉纺织大学 Method for recycling indigo in waste denim laser waste ash

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102531224A (en) * 2010-12-22 2012-07-04 常州市环境保护研究所 Method and device for recovering indigoid dye
CN102531224B (en) * 2010-12-22 2015-12-02 江苏常环环境科技有限公司 A kind of method that bipseudoindoxyl dye reclaims and device
CN102516817A (en) * 2011-12-28 2012-06-27 河北化工医药职业技术学院 Method for preparing indigo white solution
CN102516817B (en) * 2011-12-28 2013-12-11 河北化工医药职业技术学院 Method for preparing indigo white solution
CN104792598A (en) * 2015-03-25 2015-07-22 塔里木大学 Reduction liquid for treating waste alcohol generated after HE staining and preparation method of reduction liquid
CN105295444A (en) * 2015-11-10 2016-02-03 杭州天马思宏染织有限公司 High-purity salt-free reactive dye and manufacturing method thereof
CN106630307A (en) * 2016-09-30 2017-05-10 航天长征化学工程股份有限公司 System and method for treating coal gasification grey water
CN113231044A (en) * 2021-05-20 2021-08-10 南京工业大学 High-efficiency environment-friendly adsorption fiber for removing indigo in wastewater and preparation method thereof
CN113416967A (en) * 2021-06-17 2021-09-21 武汉纺织大学 Method for recycling indigo dye in waste jeans and fabric dyeing method
CN113549938A (en) * 2021-06-17 2021-10-26 武汉纺织大学 Method for recycling indigo in waste denim laser waste ash
CN113549938B (en) * 2021-06-17 2022-06-21 武汉纺织大学 Method for recycling indigo in waste denim laser waste ash

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