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%.