CN103556420A - Method for recycling mixed alkali liquor from after-treatment washing process of indigo - Google Patents

Method for recycling mixed alkali liquor from after-treatment washing process of indigo Download PDF

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Publication number
CN103556420A
CN103556420A CN201310523218.0A CN201310523218A CN103556420A CN 103556420 A CN103556420 A CN 103556420A CN 201310523218 A CN201310523218 A CN 201310523218A CN 103556420 A CN103556420 A CN 103556420A
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China
Prior art keywords
indigo
alkali liquor
mixed alkali
washing process
water
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CN201310523218.0A
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CN103556420B (en
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吴德生
李留德
毛永生
常青
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TAIFENG CHEMICAL CO Ltd JIANGSU
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TAIFENG CHEMICAL CO Ltd JIANGSU
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Abstract

The invention relates to a method for recycling mixed alkali liquor from an after-treatment washing process of indigo. According to the method for recycling the mixed alkali liquor from the after-treatment washing process of the indigo, after an indigo oxidation process, mixed alkali liquor is sent to a filter press for filter pressing, tap water is filled for washing, washing liquid is divided into two paths, one path returns back to the filter press to serve as washing water, and the other path returns back to the indigo oxidation process to serve as diluting water of alkali fusion materials according to the amount of the diluting water of the alkali fusion materials of the indigo oxidation process after being cooled. According to the method for recycling the mixed alkali liquor from the after-treatment washing process of the indigo, the requirements of the indigo oxidation process are combined, the characteristics of a alkali fusion process are utilized, a method of recycling and reusing is utilized, the filter-pressed washed low-concentration mixed alkali liquor is collected and reused as washing water and the diluting water of the kali fusion materials, full recycling of the low-concentration mixed alkali liquor and the utilization of surplus low-concentration mixed alkali liquor can be achieved, and the aims of emission reduction and fresh water tap water consumption reduction can be achieved.

Description

A kind of method that reclaims mixed alkali liquor from indigo post processing washing process
Technical field
The invention belongs to dye chemical industry raw materials recovery technology, is the method for mixed alkali liquor that reclaims in the post processing washing process for indigo reducing dye such as grade specifically.
Background technology
Indigo is a kind of environmental protection, time-honored reducing dye, 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 course of reaction comprises a certain amount of anilino-acetate, Sodamide and NaOH 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 post processing washing process, Washing of Filter Cake causes a large amount of alkali to run off, and need to a large amount of running water, to material, dilute and wash, the alkali of loss enters after sewage disposal device, need to neutralize with a large amount of acid, disposal cost and production cost are high, and the inorganic salts 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 present invention is in conjunction with indigo oxidation technology requirement, utilize alkali fusion operational characteristic, adopt the method for circulation recovery, low concentration mixed alkali liquor after press filtration washing is collected to cover as slurry and alkali fusion material thinned water, realize abundant recovery and more than needed utilization of low concentration mixed base, reach to reduce and discharge, reduce the object that fresh tap water consumes.
The technical solution used in the present invention is: a kind of method that reclaims mixed alkali liquor from indigo post processing washing process, its flow process is: after indigo oxidation operation, send into filter press press filtration, enter running water washing, cleaning solution divides two-way, one tunnel is returned to filter press and is made slurry, returns to indigo oxidation operation make alkali fusion material thinned water after another road is cooling by indigo oxidation operation alkali fusion material thinned water consumption.
Further, the mixed alkali liquor concentration of described cleaning solution is 0.5%-5.0%, and preferred concentration is at 1.0%-4.0%.
Further, another road of described cleaning solution cools to 0-70 ℃, preferably 5-45 ℃.
Further, the diluted concentration of described alkali fusion material requires 5%-30%, preferably at 8%-20%.
Again further, described cleaning solution is done to go successively suspended matter to filter and adsorb organic compound filtration before slurry and thinned water.
The washings that contain the mixed alkali liquor of NaOH and KOH in indigo post processing washing process are first all recycled in collecting tank, after going suspended matter and adsorb organic compound to filter, a part is returned to washing procedure as washings, another part is after cooling, be delivered to again in indigo oxidation reactor, as the thinned water of next group alkali fusion material, so toward circulation, thereby reach the object that reclaims low concentration NaOH and KOH mixed alkali liquor in washings.
Press filtration filtrate NaOH of the present invention and KOH mixed alkali liquor,, processed concentrated through alkali vapo(u)rization system, can be used as commodity and sell outward, or, CO concentrated through alkali vapo(u)rization system 2de-sodium regulates after potassium sodium ratio, processed, and cover is the solvent as reaction as alkali fusion procedure.
The method not only can also reduce the use of a large amount of running water by the whole recoveries of the alkali in indigo washings, have advantages of energy-efficient, reduce discharging significantly, clean environment firendly, Benefit.
Accompanying drawing explanation
Fig. 1 is the process chart of the inventive method.
The specific embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Shown in Fig. 1, a kind of method that reclaims mixed alkali liquor from indigo post processing washing process, its flow process is: after indigo oxidation operation, send into filter press press filtration, enter running water washing, press filtration filtrate is concentrated through alkali vapo(u)rization system, CO 2de-sodium regulates after potassium sodium ratio, processed, and cover is as the solvent of oxidation operation alkali fusion; Cleaning solution concentration is 0.5%-5.0%, preferred concentration is at 1.0%-4.0%, cleaning solution goes suspended matter to filter successively and adsorb organic compound filters rear minute two-way, one tunnel is returned to filter press and is made slurry, another road cools to 0-70 ℃, and preferably 5-45 ℃, returns to indigo oxidation operation by indigo oxidation operation alkali fusion material thinned water consumption and make alkali fusion material thinned water, the diluted concentration of alkali fusion requires 5%-30%, preferably at 8%-20%.

Claims (5)

1. a method that reclaims mixed alkali liquor from indigo post processing washing process, its flow process is: after indigo oxidation operation, send into filter press press filtration, enter running water washing, cleaning solution divides two-way, one tunnel is returned to filter press and is made slurry, returns to indigo oxidation operation make alkali fusion material thinned water after another road is cooling by indigo oxidation operation alkali fusion material thinned water consumption.
2. a kind of method that reclaims mixed alkali liquor from indigo post processing washing process according to claim 1, is characterized in that: the mixed alkali liquor concentration of described cleaning solution is 0.5%-5.0%, and preferred concentration is at 1.0%-4.0%.
3. a kind of method that reclaims mixed alkali liquor from indigo post processing washing process according to claim 1, is characterized in that: another road of described cleaning solution cools to 0-70 ℃, preferably 5-45 ℃.
4. a kind of method that reclaims mixed alkali liquor from indigo post processing washing process according to claim 1, is characterized in that: the diluted concentration of described alkali fusion material requires 5%-30%, preferably at 8%-20%.
5. according to the arbitrary a kind of described method that reclaims mixed alkali liquor from indigo post processing washing process of claims 1 to 3, it is characterized in that: described cleaning solution is done to go successively suspended matter to filter and adsorb organic compound filtration before slurry and thinned water.
CN201310523218.0A 2013-10-30 2013-10-30 A kind of method reclaiming mixed alkali liquor from indigo aftertreatment washing process Active CN103556420B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105648790A (en) * 2016-02-25 2016-06-08 苏州华良化纤纺织有限公司 Washing method capable of realizing water recycling

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5116996A (en) * 1991-07-17 1992-05-26 Basf Aktiengesellschaft Purification of indigo
JPH05112729A (en) * 1991-04-15 1993-05-07 Basf Ag Preparation of pure indigo
CN1234370A (en) * 1998-05-01 1999-11-10 黄中杰 Method for recovering waste liquid of industrial mixed alkali
US6767448B1 (en) * 1999-04-29 2004-07-27 Dystar Textilfarben Gmbh & Co. Deutschland Kg Method for producing aqueous alkaline solutions or reduced indigoid dyes
CN101314924A (en) * 2008-06-26 2008-12-03 晏永祥 Pulping paper-making process with zero discharge of sewage water
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

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05112729A (en) * 1991-04-15 1993-05-07 Basf Ag Preparation of pure indigo
US5116996A (en) * 1991-07-17 1992-05-26 Basf Aktiengesellschaft Purification of indigo
CN1234370A (en) * 1998-05-01 1999-11-10 黄中杰 Method for recovering waste liquid of industrial mixed alkali
US6767448B1 (en) * 1999-04-29 2004-07-27 Dystar Textilfarben Gmbh & Co. Deutschland Kg Method for producing aqueous alkaline solutions or reduced indigoid dyes
CN101314924A (en) * 2008-06-26 2008-12-03 晏永祥 Pulping paper-making process with zero discharge of sewage water
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 (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105648790A (en) * 2016-02-25 2016-06-08 苏州华良化纤纺织有限公司 Washing method capable of realizing water recycling

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