CN104193045B - Active bright blue waste water in dye production recycles technique - Google Patents
Active bright blue waste water in dye production recycles technique Download PDFInfo
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- CN104193045B CN104193045B CN201410330442.2A CN201410330442A CN104193045B CN 104193045 B CN104193045 B CN 104193045B CN 201410330442 A CN201410330442 A CN 201410330442A CN 104193045 B CN104193045 B CN 104193045B
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Abstract
The present invention proposes a kind of active bright blue waste water in dye production and recycle technique, comprise the following steps: (1) the waste water from dyestuff of colourity��50 times directly enters waste water holding tank, colourity > waste water from dyestuff of 50 times, entering decolouring pond and carry out physical decolorization process, after process, waste water from dyestuff enters waste water holding tank again; By step (1) waste water holding tank waste water from dyestuff add in neutralization reaction still, then slowly add milk of lime, stir while adding evenly, when pH value is 7.0��8.5, stopped reaction; (3) adopt pressure filter to carry out press filtration, obtain filtrate I and filter cake I; (4) gained filtrate I joins in replacement reaction kettle, adds sodium carbonate and carries out replacement(metathesis)reaction; (5) adopt pressure filter to carry out press filtration the material in step (4) replacement reaction kettle, obtain filtrate II and filter cake II. Waste water after this art breading can fully recovering in the bright blue DYE PRODUCTION of activity, it is achieved that the cleaner production target of DYE PRODUCTION process.
Description
Technical field
The present invention relates to active bright blue waste water in dye production and recycle technique.
Background technology
In Dyestuff synthesis production process, a large amount of mother liquor waste waters and washes can be produced, because its COD value and colourity are higher, such as not treated direct discharge, the destruction of water ecological setting can be caused, serious environment pollution. At present, the Treatment process of waste water in dye production has been reported by existing a lot of document, such as adsorption decoloring method, catalytic oxidation, biochemical process, Fe-C Micro Electrolysis Method etc. The improvement of waste water from dyestuff is all obtained certain effect by these methods, but the non-recovery of waste water. Waste water reclamation is applied mechanically the area for water scarcity and is seemed particularly important, yet there are no the report reaching process water zero release about active bright blue waste water in dye production recovery.
Summary of the invention
For solving above-mentioned prior art Problems existing, the present invention proposes a kind of active bright blue waste water in dye production and recycles technique, waste water after this art breading can fully recovering in the bright blue DYE PRODUCTION of activity, it is achieved that the cleaner production of DYE PRODUCTION process and the green production target of energy-saving and emission-reduction.
The technical scheme of the present invention is achieved in that
A kind of active bright blue waste water in dye production recycles technique, comprises the following steps:
(1) waste water from dyestuff processes respectively according to the difference of colourity, and the waste water from dyestuff of colourity��50 times directly enters waste water holding tank, colourity > waste water from dyestuff of 50 times, enter decolouring pond and carry out physical decolorization process, after process, waste water from dyestuff enters waste water holding tank again;
By step (1) waste water holding tank waste water from dyestuff add in neutralization reaction still, then slowly add milk of lime, stir while adding evenly, simultaneously the pH value in detection neutralization reaction still in real time, when pH value is 7.0��8.5, stop adding milk of lime;
(3) adopt pressure filter to carry out press filtration the material in step (2) neutralization reaction still, obtain filtrate I and filter cake I;
By step (3) gained filtrate I join in replacement reaction kettle, add sodium carbonate and carry out replacement(metathesis)reaction;
(5) adopt pressure filter to carry out press filtration the material in step (4) replacement reaction kettle, obtain filtrate II and filter cake II.
Further, the filtrate II reuse (5) of described step is to DYE PRODUCTION process, it is possible to uses as water at the bottom of sulfonation operation bath water and condensation operation, certainly also can be used as ice making water and filter cake rinse water; Filter cake II reuse to neutralization reaction still carries out neutralization reaction.
Further, described decolouring pond is provided with filter screen and main component is the molecular sieve of silicon-dioxide, described filter screen order number 200 order.
Further, (2) described step detects the pH value in neutralization reaction still in real time, when pH value is 7.5��8.5, stops adding milk of lime, is conducive to follow-up replacement(metathesis)reaction like this.
Further, described step, (2) after waste water from dyestuff neutralization reaction, is 0.5��1:10 according to liquid mass ratio in polyacrylamide and neutralization still4Ratio, in neutralization reaction still, add polyacrylamide solid, the speed of pressure filter press filtration can be accelerated like this.
Further, described replacement(metathesis)reaction adopts sodium carbonate to carry out, the object carrying out replacement(metathesis)reaction be in active bright blue dyestuff calcium salt there is the Saline alkali tolerance on dyestuff and the impact of solubleness index bigger.
Waste water from dyestuff colourity of the present invention measures according to extension rate method and draws, described extension rate method refers to that getting a certain amount of sewage sample is placed in 100mL or 50mL colorimetric cylinder, repeatedly it is diluted to till just can't see color with distilled water, i.e. color the same as distilled water, the multiple of dilution water is the colourity of water sample, unit is that doubly the method is applicable to the contaminated surface water and industrial sewage color measurenent.
The useful effect of the present invention:
The active bright blue waste water in dye production recovery method of the present invention, first carries out desolventing technology by waste water from dyestuff, it is possible to effectively avoid post precipitation thing to need desolventing technology step, saved program, and waste water and tap water after decolouring is close, colourity��50 times; After adopting lime slurry neutralization to process, the COD value of waste water, lower than 100mg/L, adopts lime slurry neutralization instead of neutralization with lime, is that the pH value after neutralization is more accurate because the pH of lime slurry neutralization reaction more easily controls; Obtained filtrate I and filter cake I after neutralization by pressure filter press filtration, filter cake I main component is calcium sulfate, it is possible to for adjusting the additive of cement index; Filtrate I is not directly discharged into sewage work, and it is through sodium carbonate replacement(metathesis)reaction, and carry out pressure filter press filtration and obtain filtrate II and filter cake II, filtrate II reuse is to DYE PRODUCTION process, filter cake II carries out neutralization reaction in calcium carbonate reuse to neutralization reaction still, it is achieved that the complete-reclaiming of waste water and dregs.
Embodiment
Embodiment 1
The factory effluent of Qu Naiman Mingzhou Chemical Industry Science Co., Ltd active bright blue 21 carries out colorimetric detection, and colourity is 210 times, puts it into decolouring pond and carries out decolorization filtering. Decolouring pond comprises order number 200 object filter screen, filter screen has main component be the molecular sieve of silicon-dioxide. Waste water after decolouring collects waste water holding tank, after collection, waste water in waste water holding tank is joined in the neutralization reaction still of 10 tons, then milk of lime is slowly added, stir while adding evenly, detect the pH value in neutralization reaction still simultaneously in real time, when pH value is 7.5, stop adding milk of lime. Then, adopting pressure filter to carry out press filtration the material in neutralization reaction still, obtain filtrate I and filter cake I, filter cake I is for adjusting the additive of cement index, and filtrate I joins replacement reaction kettle and sodium carbonate carries out replacement(metathesis)reaction; Then, adopt pressure filter to carry out press filtration the material in replacement reaction kettle, obtain filtrate II and filter cake II, filter cake II can carry out neutralization reaction in reuse to neutralization reaction still, filtrate II naked eyes look the same with tap water, and colourity is 40 times after testing, and COD value is 90mg/L. Filtrate II is all for bright blue 21 production processes of activity, and products obtained therefrom solubleness reaches 155 grams per liters, and resistance to saline and alkaline index reaches 16 minutes, reaches the production standard of active bright blue dyestuff 21 completely.
Embodiment 2
The factory effluent of Qu Naiman Mingzhou Chemical Industry Science Co., Ltd active bright blue 14 carries out colorimetric detection, colourity is 40 times, collected waste water holding tank, after collection, the waste water in waste water holding tank is joined in the neutralization reaction still of 10 tons, then slowly add milk of lime, stir while adding evenly, detect the pH value in neutralization reaction still simultaneously in real time, when pH value is 7.0, stop adding milk of lime. Then, adding according to polyacrylamide and liquid mass ratio in neutralization still in neutralization reaction still is 0.5:104Ratio add polyacrylamide solid; Then, adopting pressure filter to carry out press filtration, obtain filtrate I and filter cake I, filter cake I is for adjusting the additive of cement index, and filtrate I joins replacement reaction kettle and sodium carbonate carries out replacement(metathesis)reaction; Then, adopt pressure filter to carry out press filtration the material in replacement reaction kettle, obtain filtrate II and filter cake II, filter cake II can carry out neutralization reaction in reuse to neutralization reaction still, filtrate II naked eyes look the same with tap water, and colourity is 40 times after testing, and COD value is 100mg/L. Filtrate II is all for bright blue 14 production processes of activity, and products obtained therefrom solubleness reaches 150 grams per liters, reaches the production standard of active bright blue dyestuff 14 completely.
Embodiment 3
The factory effluent of Qu Naiman Mingzhou Chemical Industry Science Co., Ltd active bright blue 72 carries out colorimetric detection, and colourity is 160 times, puts it into decolouring pond and carries out decolorization filtering. Decolouring pond comprises order number 300 object filter screen, filter screen has main component be the molecular sieve of silicon-dioxide. Waste water after decolouring collects waste water holding tank, after collection, waste water in waste water holding tank is joined in the neutralization reaction still of 10 tons, then milk of lime is slowly added, stir while adding evenly, detect the pH value in neutralization reaction still simultaneously in real time, when pH value is 8.0, stop adding milk of lime. Then, adding according to polyacrylamide and liquid mass ratio in neutralization still in neutralization reaction still is 1:104Ratio add polyacrylamide solid; Then, adopting pressure filter to carry out press filtration, obtain filtrate I and filter cake I, filter cake I is for adjusting the additive of cement index, and filtrate I joins replacement reaction kettle and sodium carbonate carries out replacement(metathesis)reaction; Then, adopt pressure filter to carry out press filtration the material in replacement reaction kettle, obtain filtrate II and filter cake II, filter cake II can carry out neutralization reaction in reuse to neutralization reaction still, filtrate II naked eyes look the same with tap water, and colourity is 30 times after testing, and COD value is 85mg/L. Filtrate II is all for bright blue 72 production processes of activity, and products obtained therefrom solubleness reaches 165 grams per liters, reaches the production standard of active bright blue dyestuff 72 completely.
Embodiment 4
The factory effluent of Qu Naiman Mingzhou Chemical Industry Science Co., Ltd active bright blue 21 carries out colorimetric detection, colourity is 40 times, collected waste water holding tank, after collection, the waste water in waste water holding tank is joined in the neutralization reaction still of 10 tons, then slowly add milk of lime, stir while adding evenly, detect the pH value in neutralization reaction still simultaneously in real time, when pH value is 8.5, stop adding milk of lime. Then, adding according to polyacrylamide and liquid mass ratio in neutralization still in neutralization reaction still is 0.8:104Ratio add polyacrylamide solid; Then, adopting pressure filter to carry out press filtration, obtain filtrate I and filter cake I, filter cake I is for adjusting the additive of cement index, and filtrate I joins replacement reaction kettle and sodium carbonate carries out replacement(metathesis)reaction; Then, adopt pressure filter to carry out press filtration the material in replacement reaction kettle, obtain filtrate II and filter cake II, filter cake II can carry out neutralization reaction in reuse to neutralization reaction still, filtrate II naked eyes look the same with tap water, and colourity is 40 times after testing, and COD value is 80mg/L. Filtrate II is all for bright blue 21 production processes of activity, and products obtained therefrom solubleness reaches 155 grams per liters, and resistance to saline and alkaline index reaches 16 minutes, reaches the production standard of active bright blue dyestuff 21 completely.
Claims (4)
1. the bright blue waste water in dye production of activity recycles technique, it is characterised in that, comprise the following steps:
(1) waste water from dyestuff processes respectively according to the difference of colourity, the waste water from dyestuff of colourity��50 times directly enters waste water holding tank, colourity > waste water from dyestuff of 50 times, enter decolouring pond and carry out physical decolorization process, after process, waste water from dyestuff enters waste water holding tank again, described decolouring pond is provided with filter screen and main component is the molecular sieve of silicon-dioxide, described filter screen order number 200 order;
By step (1) waste water holding tank waste water from dyestuff add in neutralization reaction still, then slowly add milk of lime, stir while adding evenly, simultaneously the pH value in detection neutralization reaction still in real time, when pH value is 7.0��8.5, stop adding milk of lime;
(3) adopt pressure filter to carry out press filtration the material in step (2) neutralization reaction still, obtain filtrate I and filter cake I;
By step (3) gained filtrate I join in replacement reaction kettle, add sodium carbonate and carry out replacement(metathesis)reaction;
(5) adopt pressure filter to carry out press filtration the material in step (4) replacement reaction kettle, obtain filtrate II and filter cake II.
2. waste water reclamation according to claim 1 utilizes technique, it is characterised in that, the filtrate II reuse (5) of described step, to DYE PRODUCTION process, carries out neutralization reaction in filter cake II reuse to neutralization reaction still.
3. waste water reclamation according to claim 1 and 2 utilizes technique, it is characterised in that, (2) described step detects the pH value in neutralization reaction still in real time, when pH value is 7.5��8.5, stops adding milk of lime.
4. waste water reclamation according to claim 1 and 2 utilizes technique, it is characterised in that, described step, (2) after waste water from dyestuff neutralization reaction, is 0.5��1:10 according to liquid mass ratio in polyacrylamide and neutralization still4Ratio, in neutralization reaction still, add polyacrylamide solid.
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| CN104674570B (en) * | 2015-02-13 | 2017-04-19 | 绍兴文理学院 | Recycling dyeing method of dyeing wastewater of reactive dyes |
| CN105836921B (en) * | 2016-05-04 | 2019-06-25 | 浙江闰土研究院有限公司 | A kind of processing method of dye wash waste water |
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| CN103880210A (en) * | 2014-03-14 | 2014-06-25 | 浙江迪邦化工有限公司 | Treating and recycling process of acid wastewater generated in disperse dye production |
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| JPS61141995A (en) * | 1984-12-14 | 1986-06-28 | Shinyuu Kasei Kk | Treatment of waste water containing water-soluble dye |
| CN1280206C (en) * | 2004-04-14 | 2006-10-18 | 南京大学 | Method for treatng wastewater of producing reactive dyes in class of bromamine acid, and for reclaiming resources |
| ES2350074B1 (en) * | 2009-05-22 | 2011-11-04 | Universitat Politècnica De Catalunya | APPLICATION OF BIOPOLIMERO QUITOSAN IN THE ELIMINATION OF THE COLOR OF RESIDUAL LASAGUAS THROUGH THE COMBINED PROCESS OF COAGULATION-FLOCULATION AND ADSORTION. |
| US20110017098A1 (en) * | 2009-07-03 | 2011-01-27 | Board Of Regents, The University Of Texas System | Removal and recovery of dye waste from effluents using clay |
| CN103588318A (en) * | 2012-08-17 | 2014-02-19 | 浙江中辉皮草有限公司 | Processing method used for multiple recycling of fur dyeing effluent |
| CN103214116B (en) * | 2013-03-15 | 2014-03-12 | 浙江闰土股份有限公司 | Recycling method of sulfuric acid-containing wastewater from disperse dye production |
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| "内电解法处理染料生产废水试验研究";孙华 等;《工业用水与废水》;20011231;第32卷(第3期);第22-25页 * |
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Effective date of registration: 20180713 Address after: 063611 Hebei Tangshan City harbor development area, Zhongshan Avenue, north of Sinoma road. Patentee after: Tangshan minzhou science and Technology Co., Ltd. Address before: 028306 Tongliao City, the Inner Mongolia Autonomous Region, Naiman Banner, Da qinla town south suburb Chemical District Patentee before: NAIMAN MINGZHOU CHEMICAL TECHNOLOGY CO., LTD. |
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