CN103554995A - Method for recycling mixed alkali liquor in indigo production - Google Patents
Method for recycling mixed alkali liquor in indigo production Download PDFInfo
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- CN103554995A CN103554995A CN201310523139.XA CN201310523139A CN103554995A CN 103554995 A CN103554995 A CN 103554995A CN 201310523139 A CN201310523139 A CN 201310523139A CN 103554995 A CN103554995 A CN 103554995A
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- filtrate
- indigo
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- alkali liquor
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Abstract
The invention relates to a method for recycling mixed alkali liquor in indigo production, and the method comprises the following steps: feeding indigo into a filter press so as to be filter-pressed after an oxidation process, concentrating a filter-pressing filtrate to obtain caustic sludge, and feeding a filter-pressing concentrated liquor into a reaction still; washing the indigo filter-pressed in the step (1), adding the caustic sludge of the step (1) into washing water, warming and stirring until the caustic sludge is completely dissolved, naturally cooling to room temperature, filtering, concentrating the filtrate as a concentrated alkali liquor, and then feeding the concentrated alkali liquor into the reaction still; washing filter residue by using saturated Na2CO3, filtering to obtain a Na2CO3 solid, concentrating the filtrate as the concentrated alkali liquor, and then feeding the concentrated alkali liquor into the reaction still, introducing CO2 into the reaction still, stopping introducing CO2 when the reaction temperature is at 60-70 DEG C, cooling to room temperature, stirring for 1-2 hours, crystallizing, filtering to obtain mother liquor and crude product Na2CO3, concentrating the filtrate as the concentrated alkali liquor, and then feeding the concentrated alkali liquor into the reaction still in the step (3). By adopting the method of circularly recycling, the filter-pressed filtrate, the washing water and the KOH in the caustic sludge are effectively recycled.
Description
Technical field
The invention belongs to dye chemical industry raw materials recovery technology, is the method that mixed alkali liquor is reclaimed in indigo production specifically.
Background technology
Indigo is a kind of environmental protection, time-honored vat dyes, aspect the dyeing of cotton fabric dyeing process, the particularly warp thread of indigo jean goods, is being widely used.
Current industrial production is all indigo via 3-indoles phenates oxidation preparation, wherein reaction process comprises a certain amount of anilino-acetate, sodium amide and sodium hydroxide is reacted at 220 ~ 250 ℃ with the mixed base of potassium hydroxide, obtain the alkali fusion thing of the 3-indoles phenates of 20-30%, this alkali fusion thing is dissolved in large water gaging, after blowing air oxidation, then through press filtration, washing, dry obtain indigo.
In indigo synthetic alkali fusion, oxidation and postprocessing working procedures, the use of alkali is mainly at alkali fusion procedure, and after oxidation press filtration, diluted alkaline enters alkali reclaims, and the loss of alkali is mainly after press filtration in the washing process of product.According to following the tracks of Classified statistics, in indigo aftertreatment washing process, filter cake washing causes a large amount of alkali to run off, and need to a large amount of tap water, to material, dilute and wash, the alkali of loss enters after Sewage disposal device, need to neutralize with a large amount of acid, processing costs and production cost are high, and the inorganic salt that form are difficult to biochemical treatment, waste alkali resource, has caused compared with overall situation and has polluted.
Summary of the invention
For the problems referred to above, the invention provides a kind of method that adopts circulation recovery, the indigo production of KOH efficient recovery in press filtration filtrate, washing water and alkaline residue is reclaimed to the method for mixed alkali liquor.
The technical solution used in the present invention is: the method for mixed alkali liquor is reclaimed in a kind of indigo production, comprises the following steps:
(1) after indigo oxidation operation, send into pressure filter press filtration, press filtration filtrate thickening filtration goes out after alkaline residue, and press filtration concentrated solution is sent into reactor;
(2) indigo after washing step (1) press filtration adds alkaline residue in step (1) in washing water, heats up, is stirred to alkaline residue and dissolve completely, naturally is down to room temperature and filters, and filtrate is condensed into and concentrates alkali lye and send into reactor; Filter residue adopts saturated Na
2cO
3after washing, filter to obtain Na
2cO
3solid, filtrate is condensed into concentrated alkali lye and sends into reactor;
(3) to logical CO in reactor
2, temperature of reaction stops ventilation in the time of 60-70 ℃, is cooled to room temperature, stirs crystallization in 1-2 hour, filters to obtain mother liquor and crude product Na
2cO
3, mother liquor is concentrated into over dry and becomes dehydration alkali, and K/Na > 1 in dehydration alkali, directly applies mechanically back in indigo production;
(4) step (3) crude product Na
2cO
3adopt saturated Na
2cO
3washing, filters to obtain the Na of K/Na=0
2cO
3solid, filtrate is condensed into concentrated alkali lye and sends into step (3) reactor.
Further, described step (3) dehydration alkali is directly applied mechanically back in indigo production, adopts the dilution of step (2) washing water.
Compared with prior art, advantage of the present invention is: the alkaline residue of separating out in indigo filter liquor is concentrated, and adopt K/Na to dissolve alkaline residue lower than the indigo washing water of alkaline residue, crystallization filtered liquid is concentrated, and crystallization is crossed filter solid and is adopted saturated Na
2cO
3filtrate concentration and recovery potassium resource after washing causticizing reaction, crossing filter solid is commodity Na
2cO
3directly commercial exploitation; Logical CO after the dissolving crystallized filtrate of indigo filter liquor and alkaline residue is concentrated
3, utilize Na
2cO
3, KCO
3dissolubility difference separate out Na
2cO
3, the K/Na ratio of adjusting concentrated solution, separates out Na
2cO
3adopt saturated Na
2cO
3the concentrated CO that applies mechanically of filtrate after washing causticizing reaction
3regulate K/Na than using, crossing filter solid is commodity Na
2cO
3directly commercial exploitation; When dehydration alkali is directly applied mechanically back in indigo production, directly adopt indigo washing water, effectively saving water resource, saves potassium resource recovery process, energy-saving and emission-reduction.
The present invention is led to CO by concentrated adjusting of each operation filtrate in indigo production
3regulate K/Na ratio, coordinate the low K/Na of alkaline residue than secondary dissolve, each operation filter residue causticizing reaction reaction reclaims potassium resource, can effectively prevent potassium resource waste in indigo production, have advantages of energy-efficient, reduce discharging significantly, clean environment firendly, Benefit.
Embodiment
The invention will be further described below.
A method for mixed alkali liquor is reclaimed in indigo production, comprises the following steps:
(1) after indigo oxidation operation, send into pressure filter press filtration, press filtration filtrate thickening filtration goes out after alkaline residue, and press filtration concentrated solution is sent into reactor;
(2) indigo after washing step (1) press filtration adds alkaline residue in step (1) in washing water, heats up, is stirred to alkaline residue and dissolve completely, naturally is down to room temperature and filters, and filtrate is condensed into and concentrates alkali lye and send into reactor; Filter residue adopts saturated Na
2cO
3after washing, filter to obtain Na
2cO
3solid, filtrate is condensed into concentrated alkali lye and sends into reactor;
(3) to logical CO in reactor
2, temperature of reaction stops ventilation in the time of 60-70 ℃, is cooled to room temperature, stirs crystallization in 1-2 hour, filters to obtain mother liquor and crude product Na
2cO
3, mother liquor is concentrated into over dry and becomes dehydration alkali, and K/Na > 1 in dehydration alkali, directly applies mechanically back in indigo production;
(4) step (3) crude product Na
2cO
3adopt saturated Na
2cO
3washing, filters to obtain the Na of K/Na=0
2cO
3solid, filtrate is condensed into concentrated alkali lye and sends into step (3) reactor.
Claims (2)
1. a method for mixed alkali liquor is reclaimed in indigo production, comprises the following steps:
After indigo oxidation operation, send into pressure filter press filtration, press filtration filtrate thickening filtration goes out after alkaline residue, and press filtration concentrated solution is sent into reactor;
Indigo after washing step (1) press filtration adds alkaline residue in step (1) in washing water, heats up, is stirred to alkaline residue and dissolve completely, naturally is down to room temperature and filters, and filtrate is condensed into and concentrates alkali lye and send into reactor; Filter residue adopts saturated Na
2cO
3after washing, filter to obtain Na
2cO
3solid, filtrate is condensed into concentrated alkali lye and sends into reactor;
To logical CO in reactor
2, temperature of reaction stops ventilation in the time of 60-70 ℃, is cooled to room temperature, stirs crystallization in 1-2 hour, filters to obtain mother liquor and crude product Na
2cO
3, mother liquor is concentrated into over dry and becomes dehydration alkali, and K/Na > 1 in dehydration alkali, directly applies mechanically back in indigo production;
Step (3) crude product Na
2cO
3adopt saturated Na
2cO
3washing, filters to obtain the Na of K/Na=0
2cO
3solid, filtrate is condensed into concentrated alkali lye and sends into step (3) reactor.
2. the method for mixed alkali liquor is reclaimed in indigo production according to claim 1, it is characterized in that: described step (3) dehydration alkali is directly applied mechanically back in indigo production, adopts the dilution of step (2) washing water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310523139.XA CN103554995A (en) | 2013-10-30 | 2013-10-30 | Method for recycling mixed alkali liquor in indigo production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310523139.XA CN103554995A (en) | 2013-10-30 | 2013-10-30 | Method for recycling mixed alkali liquor in indigo production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103554995A true CN103554995A (en) | 2014-02-05 |
Family
ID=50009368
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310523139.XA Pending CN103554995A (en) | 2013-10-30 | 2013-10-30 | Method for recycling mixed alkali liquor in indigo production |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104624617A (en) * | 2015-02-13 | 2015-05-20 | 内蒙古泰兴泰丰化工有限公司 | Method for treating mixed alkali residues in production of indigo |
| CN104624616A (en) * | 2015-02-13 | 2015-05-20 | 内蒙古泰兴泰丰化工有限公司 | Device and method for treating mixed alkaline residue in indigotin production |
| CN104692423A (en) * | 2015-02-13 | 2015-06-10 | 内蒙古泰兴泰丰化工有限公司 | Mixed alkaline residue treatment device in indigo blue production |
| CN104761483A (en) * | 2015-02-13 | 2015-07-08 | 内蒙古泰兴泰丰化工有限公司 | Mixed alkaline residue treatment method during indigo production |
| CN104876247A (en) * | 2015-04-30 | 2015-09-02 | 浙江奇彩环境科技有限公司 | Method for resource recycling processing of indigo alkaline residue |
| CN105568721A (en) * | 2016-02-25 | 2016-05-11 | 苏州华良化纤纺织有限公司 | Alkaline-agent-recycling dyeing process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1234370A (en) * | 1998-05-01 | 1999-11-10 | 黄中杰 | Method for recovering waste liquid of industrial mixed alkali |
| CN102127307A (en) * | 2010-12-29 | 2011-07-20 | 梅剑平 | Recovered mixed alkali solution from production of indigo, and recovering method and use thereof |
| CN102924956A (en) * | 2011-08-09 | 2013-02-13 | 江苏泰丰化工有限公司 | Recovery, balance adjustment and comprehensive utilization technology for mixing alkali in indigo blue production |
-
2013
- 2013-10-30 CN CN201310523139.XA patent/CN103554995A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1234370A (en) * | 1998-05-01 | 1999-11-10 | 黄中杰 | Method for recovering waste liquid of industrial mixed alkali |
| CN102127307A (en) * | 2010-12-29 | 2011-07-20 | 梅剑平 | Recovered mixed alkali solution from production of indigo, and recovering method and use thereof |
| CN102924956A (en) * | 2011-08-09 | 2013-02-13 | 江苏泰丰化工有限公司 | Recovery, balance adjustment and comprehensive utilization technology for mixing alkali in indigo blue production |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104624617A (en) * | 2015-02-13 | 2015-05-20 | 内蒙古泰兴泰丰化工有限公司 | Method for treating mixed alkali residues in production of indigo |
| CN104624616A (en) * | 2015-02-13 | 2015-05-20 | 内蒙古泰兴泰丰化工有限公司 | Device and method for treating mixed alkaline residue in indigotin production |
| CN104692423A (en) * | 2015-02-13 | 2015-06-10 | 内蒙古泰兴泰丰化工有限公司 | Mixed alkaline residue treatment device in indigo blue production |
| CN104761483A (en) * | 2015-02-13 | 2015-07-08 | 内蒙古泰兴泰丰化工有限公司 | Mixed alkaline residue treatment method during indigo production |
| CN104876247A (en) * | 2015-04-30 | 2015-09-02 | 浙江奇彩环境科技有限公司 | Method for resource recycling processing of indigo alkaline residue |
| CN105568721A (en) * | 2016-02-25 | 2016-05-11 | 苏州华良化纤纺织有限公司 | Alkaline-agent-recycling dyeing process |
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Application publication date: 20140205 |