CN104692422B - Its Future about Alkaline Residue Treatment Unit and treatment process is mixed in indigo production - Google Patents
Its Future about Alkaline Residue Treatment Unit and treatment process is mixed in indigo production Download PDFInfo
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- CN104692422B CN104692422B CN201510077707.7A CN201510077707A CN104692422B CN 104692422 B CN104692422 B CN 104692422B CN 201510077707 A CN201510077707 A CN 201510077707A CN 104692422 B CN104692422 B CN 104692422B
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Abstract
The present invention relates to mixed base Slag treatment device and method in a kind of indigo production, comprise alkaline residue thinning tank, carburizing reagent still, the first whizzer, filtrate tanks, separator, aqueous phase storage tank, organic phase storage tank, aqueous phase still kettle, ageing reactor, the second whizzer, organic phase still kettle, rectifying tower and solvent tank, described carburizing reagent still connects alkaline residue thinning tank and carbonic acid gas supply, carburizing reagent still connects the first whizzer, first whizzer fluid connects filtrate tanks, and filtrate tanks connects aqueous phase storage tank and organic phase storage tank respectively through separator; Described aqueous phase storage tank connects ageing reactor through aqueous phase still kettle, the external mixed base storage tank of ageing reactor, and ageing reactor connects the second whizzer; Described organic phase storage tank connects rectifying tower through organic phase still kettle, tundish successively, rectifying tower connects solvent tank and water tank, solvent tank connects filtrate tanks or separator, second whizzer fluid connects the mixed base storage tank of water tank or alkaline residue thinning tank or indigo oxidation press filtration mother liquor concentrations, and water tank connects alkaline residue thinning tank and/carburizing reagent still.
Description
Technical field
The present invention relates to indigo its Future about Alkaline Residue Treatment Unit and treatment process, is the alkaline residue treatment of wastes produced device and treatment process that produce in KOH and NaOH mixed base recovery process in the indigo production of a kind of vat specifically.
Background technology
Indigo is a kind of vat, and it is with a long history, and before more than 4000 year, the mankind just start with natural indigo dye burlap.1880, since Germanization scholar Bayer success synthesizing indigo, indigo always lasting, be widely used in the painted of the dyeing of cloth, particularly denim.
Traditional indigo synthesis technique is: anilinoacetic acid potassium/sodium salt and sodium amide are react also condensation further in the system of solvent to generate indolol potassium/sodium, ammonia and sodium hydroxide with sodium amide at the mixed base of KOH and NaOH.After alkali fusion condenses is water-soluble, blowing air is oxidized, and obtains indigo after press filtration washing, and the mother liquor after press filtration is that KOH and NaOH containing alkali 12% also contains a small amount of benzene feedstock Glycinates and by product anthranilate mixed ammonium/alkali solutions.
When alkali fusion condensation reaction, the mixed base K/Na=1:1 of KOH and NaOH, due to when reacting, sodium in sodium amide is converted into NaOH, make the potassium sodium in mother liquor than being 0.5-0.6:1, the excessive requirement not reaching alkali fusion of sodium hydroxide, existing production technique adopts the method adding potassium hydroxide adjustment potassium sodium ratio in mixed alkali to cause mixed base more than needed and potassium hydroxide deficiency, an alkali part more than needed is at oxidation section because the carbonic acid gas absorbed in air becomes sodium carbonate, and in concentration process, precipitation becomes alkaline residue becomes solid waste.A part runs off with indigo wash water, and the diluted alkaline in wash water neutralizes through sulfuric acid, becomes salt, finally becomes waste water.Not only contaminate environment, and the loss causing potassium, waste potassium resource, causes also needing make-up potassium hydroxide in production process.
For listing problem, applicant has applied for and has obtained " staying potassium to remove sodium " and waste water applies mechanically patent.The alkali carried secretly in alkaline residue then runs off with alkaline residue, the alkaline residue being rich in about the 1000kg of potassium hydroxide of present indigo generation per ton can only cheap selling to paper mill, valuable potassium resource does not have potassium and effectively utilizes, and easily brings secondary pollution.
Summary of the invention
The present invention is directed to the problems referred to above, in conjunction with existing soda balance technology and chemical recovery system, its Future about Alkaline Residue Treatment Unit and treatment process is mixed in the indigo production provided, adopt in carbonization be separated sodium carbonate, extracting and separating organics removal, filtrate cycle enters the potassium sodium that production material is settled out sodium carbonate further by ion-exchange and compares regulation strategy, achieve effective separation of three large components and the full recycling of recycle and potassium sodium resource in waste soda residue, reach reduction of discharging, reduce the consumption of potassium hydroxide, achieve the object turned waste into wealth.
The technical solution used in the present invention is: mix its Future about Alkaline Residue Treatment Unit in indigo production, comprise alkaline residue thinning tank, carburizing reagent still, the first whizzer, filtrate tanks, separator, aqueous phase storage tank, organic phase storage tank, aqueous phase still kettle, ageing reactor, the second whizzer, organic phase still kettle, rectifying tower and solvent tank, described carburizing reagent still connects alkaline residue thinning tank and carbonic acid gas supply, carburizing reagent still connects the first whizzer, first whizzer fluid connects filtrate tanks, and filtrate tanks connects aqueous phase storage tank and organic phase storage tank respectively through separator; Described aqueous phase storage tank connects ageing reactor through aqueous phase still kettle, the external mixed base storage tank of ageing reactor, and ageing reactor connects the second whizzer; Described organic phase storage tank connects rectifying tower through organic phase still kettle, tundish successively, rectifying tower connects solvent tank and water tank, solvent tank connects filtrate tanks or separator, second whizzer fluid connects the mixed base storage tank of water tank or alkaline residue thinning tank or indigo oxidation press filtration mother liquor concentrations, and water tank connects alkaline residue thinning tank and/carburizing reagent still.
Further, first and second whizzer described is slagged tap and is connected filter residue receiving tank.
Further, described organic phase still kettle is slagged tap and is connected the residual receiving tank of still.
Further, described aqueous phase still kettle connects ageing reactor through the 3rd whizzer.
Further, described second whizzer is slagged tap and is connected dry vaporizer.
Further, described rectifying tower connects alkaline residue thinning tank through water tank, or rectifying tower goes out vapour connection alkaline residue thinning tank.
Alkaline residue processing method is mixed in indigo production, first the alkaline residue solid waste of NaOH and the KOH mixed base being rich in sodium carbonate, organic impurity and being entrained with 20-30% of separating out in indigo oxidation press filtration mother liquor concentrations process is added in alkaline residue thinning tank, add water washing, water lotion flows in mixed base storage tank, add water after stirring in alkaline residue feeding carburizing reagent still after washing, pass into carbonic acid gas, until hydroxide radical all neutralizes, be separated through the first centrifuge, filter residue receiving tank reclaims filter residue sodium carbonate, as by-product sale; Filtrate sends into filtrate tanks, sends into organic solvent extraction by solvent tank in filtrate tanks, is separated organic phase and aqueous phase and sends into organic phase storage tank and aqueous phase storage tank respectively in separator; Organic phase is sent into the distillation of organic phase still kettle by organic phase storage tank, distillation residue send into the residual receiving tank of still, distillation steam sends into rectifying tower after tundish, the water vapor that rectifying goes out sends into water tank, water tank connects alkaline residue thinning tank and/or carburizing reagent still supplies water, the organic solvent that rectifying goes out sends into solvent tank, and solvent tank connects filtrate tanks or separator supplies organic solvent; Divided by the second whizzer after aqueous phase is sent into aqueous phase still kettle distillation and concentration by aqueous phase storage tank and isolate solid sodium carbonate, separating liquid sends into ageing reactor, the mixed base storage tank of indigo oxidation press filtration mother liquor concentrations is separated by ion-exchange, the second centrifuge ageing reactor supply mixed alkali liquor, be separated and receive solid sodium carbonate and send into dry vaporizer, be separated and receive parting liquid and send into water tank or alkaline residue thinning tank or mixed base storage tank.
Further, solid alkaline residue drops in reactor the solid content of the rear mixture of the stirring that adds water at 15.0%-85.0%; Logical carbonic acid gas has neutralized preferred PH=7-8, with free alkali lower than 0.1% for terminal; The temperature of charge 0-90 DEG C that described centrifuge is separated.
Further, described organic solvent is ethanol.
Again further, the temperature 0-90 DEG C of ion-exchange.
Sodium carbonate is rich in by what separate out in indigo oxidation press filtration mother liquor concentrations process, the alkaline residue solid waste of organic impurity and NaOH and the KOH mixed base that is entrained with 20-30% is sent in alkaline residue thinning tank, solid alkaline residue adds in reactor, add appropriate water again, after stirring, pass into carbonic acid gas, until hydroxide radical all neutralizes, because sodium carbonate is at NaOH, in KOH mixed base, solubleness is less, through a centrifugation, isolate sediment fraction sodium carbonate, isolate in filtrate containing sodium carbonate, salt of wormwood and organic impurity, filtrate is through organic solvent extraction, isolate organic phase and aqueous phase, again aqueous phase after extraction and organic phase are carried out Distillation recovery respectively, the organic impurity overwhelming majority such as benzene feedstock Glycinates and by product anthranilate enter organic phase, reusable edible after Distillation recovery extraction solvent, turn back in the mixed base storage tank of indigo oxidation press filtration mother liquor concentrations after aqueous solution distillation, sodium carbonate is settled out further by the ion-exchange of salt of wormwood and NaOH, again through secondary separation, material potassium sodium after separation can turn back in the mixed base storage tank of indigo oxidation press filtration mother liquor concentrations than meeting production requirement, isolated solid sodium carbonate can be used as outside commodity and sells, we find under study for action, neutralized by carbonization, sodium carbonate can major part be precipitated out, and easily filter, the potassium carried secretly and organism little.
Further research is surprised to find that, be that the ethanol adding 2% in the solution of main component gets final product layering with salt of wormwood what remove sodium carbonate, and take most of organism out of, benzene feedstock Glycinates and the by product anthranilate of the aqueous solution more than 99% just can be removed with little ethanol, ethanol content in the aqueous solution only has about 15%, be easy to Distillation recovery, this discovery solves the enrichment of recycle stock organism ingeniously and simply affects general problem, COD after process can drop to below 2000ppm, meets and applies mechanically requirement.Removing organism and what be concentrated to about 40% concentration take salt of wormwood as the purification material of main component, can enter production system, carry out ion-exchange, precipitate and isolate further sodium carbonate, regulate the potassium sodium ratio meeting production requirement.
Present invention process has less investment, can be combined with existing alkali evaporization process well, and does not increase, do not introduce new impurity, can potassium sodium resource in effective recycling alkaline residue.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
In figure: alkaline residue thinning tank 1, carburizing reagent still 2, first whizzer 3, filter residue receiving tank 4, filtrate tanks 5, separator 6, aqueous phase storage tank 7, aqueous phase still kettle 8,3rd whizzer 9, ageing reactor 10, mixed base storage tank 11, second whizzer 12, dry vaporizer 13, organic phase storage tank 14, organic phase still kettle 15, the residual receiving tank 16 of still, tundish 17, rectifying tower 18, solvent tank 19, water tank 20.
Embodiment
below in conjunction with accompanying drawing, the invention will be further described.
Shown in Fig. 1, mix its Future about Alkaline Residue Treatment Unit in indigo production and comprise alkaline residue thinning tank 1, carburizing reagent still 2, first whizzer 3, filter residue receiving tank 4, filtrate tanks 5, separator 6, aqueous phase storage tank 7, aqueous phase still kettle 8, the 3rd whizzer 9, ageing reactor 10, mixed base storage tank 11, second whizzer 12, dry vaporizer 13, organic phase storage tank 14, organic phase still kettle 15, the residual receiving tank 16 of still, tundish 17, rectifying tower 18, solvent tank 19 and water tank 20.Alkaline residue thinning tank 1 connects carburizing reagent still 2, carburizing reagent still 2 connects carbonic acid gas supply, alkaline residue thinning tank 1 fluid connects mixed base storage tank 11, carburizing reagent still 2 connects the first whizzer 3, first whizzer 3 is slagged tap and is connected filter residue receiving tank 4, and filtrate tanks 5 connects aqueous phase storage tank 7 and organic phase storage tank 14 respectively through separator 6; Aqueous phase storage tank 7 connects ageing reactor 10 through aqueous phase still kettle 8, the 3rd whizzer 9, ageing reactor 10 connects the mixed base storage tank 11 of indigo oxidation press filtration mother liquor concentrations, ageing reactor 10 connects the second whizzer 12, second whizzer 12 and connects filter residue receiving tank and dry vaporizer 13; Organic phase storage tank 14 connects rectifying tower 18 through organic phase still kettle 15, tundish 17 successively, organic phase still kettle 15 is slagged tap and is connected the residual receiving tank 16 of still, rectifying tower 18 connects solvent tank 19 and water tank 20, solvent tank 19 connects filtrate tanks 5 or separator 6, second whizzer 12 fluid connects water tank 20, and water tank 20 connects alkaline residue thinning tank 1.
Mixing alkaline residue processing method in indigo production is:
the removal of sodium carbonate in alkaline residue
By the alkaline residue 40Kg produced in a collection of indigo production, add 20Kg water, add and stir 30min, maintain temperature of reaction at 65-75 DEG C, pass into carbonic acid gas, until hydroxyl content is 0.1%, centrifugation obtains carbonic acid solid 7.9Kg, wherein potassium content is 1.10%, and sodium ions content is 32.91%, and organic content is 0.34%.Separation obtains carbonization filtrate 53Kg, and wherein potassium content is 6.30%, and sodium ions content is 10.30%, and organic content is 3.12%.
organism in embodiment 1 alcohol extraction carbodiimide solution
Get 20g carbodiimide solution, wherein anthranilic acid is 0.47g, and amino phenyl acetate is 0.17g, adds 3g ethanol, vibrates after 2 minutes and leaves standstill layering in 30 minutes.Upper strata quality is 5.32g, and wherein anthranilic acid is 0.45g, and amino phenyl acetate is 0.16g, and ethanol is 2.58g.Lower floor's quality is 17.47g, and wherein anthranilic acid is 0.02g, and amino phenyl acetate is 0.01g, and ethanol is 0.14g.Organic percentage extraction reaches more than 95%.
organism in embodiment 2 methanol extraction carbodiimide solution
Get 20g carbodiimide solution, wherein anthranilic acid is 0.47g, and amino phenyl acetate is 0.17g, adds 3g methyl alcohol, and vibrate after 2 minutes and leave standstill 2 hours, mixture cannot layering.
organism in embodiment 3 isopropyl alcohol extraction carbodiimide solution
Get 20g carbodiimide solution, wherein anthranilic acid is 0.47g, and amino phenyl acetate is 0.17g, adds 3.04g Virahol, vibrates after 2 minutes and leaves standstill layering in 30 minutes.Upper strata quality is 6.13g, and wherein anthranilic acid is 0.40g, and amino phenyl acetate is 0.16g, and Virahol is 3.03g.Lower floor's quality is 16.93g, and wherein anthranilic acid is 0.07g, and amino phenyl acetate is 0.01g, and Virahol is 0.05g.Organic percentage extraction reaches 87.5%.
organism in embodiment 4 n-butanol extraction carbodiimide solution
Get 20g carbodiimide solution, wherein anthranilic acid is 0.47g, and amino phenyl acetate is 0.17g, adds 3.01g propyl carbinol, vibrates after 2 minutes and leaves standstill layering in 30 minutes.Upper strata quality is 5.28g, and wherein anthranilic acid is 0.39g, and amino phenyl acetate is 0.14g, and propyl carbinol is 2.93g.Lower floor's quality is 17.90g, and wherein anthranilic acid is 0.08g, and amino phenyl acetate is 0.03g, and Virahol is 0.02g.Organic percentage extraction reaches 82.8%.
organism in embodiment 5 calcium phosphate+ forage carbodiimide solution
Get 20g carbodiimide solution, wherein anthranilic acid is 0.47g, and amino phenyl acetate is 0.17g, adds 3.09g tributyl phosphate, vibrates after 2 minutes and leaves standstill layering in 30 minutes.Upper strata quality is 3.24g, and wherein anthranilic acid is 0.11g, and amino phenyl acetate is 0.03g, and propyl carbinol is 3.05g.Lower floor's quality is 11.64g, and wherein anthranilic acid is 0.35g, and amino phenyl acetate is 0.14g, and tributyl phosphate is 0.04g.Organic percentage extraction reaches 23.4%.
Organic solvent extraction isolates organic phase and aqueous phase, again aqueous phase after extraction and organic phase are carried out Distillation recovery respectively, the organic impurity overwhelming majority such as benzene feedstock Glycinates and by product anthranilate enter organic phase, reusable edible after Distillation recovery extraction solvent; Turn back in the mixed base storage tank of indigo oxidation press filtration mother liquor concentrations after aqueous solution distillation, sodium carbonate is settled out further by the ion-exchange of salt of wormwood and NaOH, again through secondary separation, material potassium sodium ratio after separation meets production requirement and can turn back in indigo production soda balance system, and isolated solid sodium carbonate can be used as outside commodity and sells.
Claims (1)
1. mix its Future about Alkaline Residue Treatment Unit in an indigo production, it is characterized in that: comprise alkaline residue thinning tank, carburizing reagent still, the first whizzer, filtrate tanks, separator, aqueous phase storage tank, organic phase storage tank, aqueous phase still kettle, ageing reactor, the second whizzer, organic phase still kettle, rectifying tower and solvent tank, described carburizing reagent still connects alkaline residue thinning tank and carbonic acid gas supply, carburizing reagent still connects the first whizzer, first whizzer fluid connects filtrate tanks, and filtrate tanks connects aqueous phase storage tank and organic phase storage tank respectively through separator, described aqueous phase storage tank connects ageing reactor through aqueous phase still kettle, the external mixed base storage tank of ageing reactor, and ageing reactor connects the second whizzer, described organic phase storage tank is successively through organic phase still kettle, tundish connect rectifying tower, rectifying tower connects solvent tank and water tank, solvent tank connects filtrate tanks or separator, second whizzer fluid connects the mixed base storage tank of water tank or alkaline residue thinning tank or indigo oxidation press filtration mother liquor concentrations, water tank connects alkaline residue thinning tank and/or carburizing reagent still, described first, two whizzers are slagged tap and are connected filter residue receiving tank, described organic phase still kettle is slagged tap and is connected the residual receiving tank of still, described aqueous phase still kettle connects ageing reactor through the 3rd whizzer, described second whizzer is slagged tap and is connected dry vaporizer, described rectifying tower connects alkaline residue thinning tank through water tank, or rectifying tower goes out vapour connection alkaline residue thinning tank.
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| CN201510077707.7A CN104692422B (en) | 2015-02-13 | 2015-02-13 | Its Future about Alkaline Residue Treatment Unit and treatment process is mixed in indigo production |
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| CN104692422B true CN104692422B (en) | 2016-03-30 |
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| CN104692423B (en) * | 2015-02-13 | 2016-01-06 | 内蒙古泰兴泰丰化工有限公司 | Its Future about Alkaline Residue Treatment Unit is mixed in indigo production |
| CN115520918B (en) * | 2022-06-27 | 2024-05-03 | 山东科技大学 | Comprehensive treatment process of alkaline residue waste liquid by ammonia-soda process |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557708A (en) * | 2004-01-19 | 2004-12-29 | 升 贾 | Comprehensive process for recovering and treating indigo blue powder waste slag |
| CN102350435A (en) * | 2011-09-09 | 2012-02-15 | 韩扶军 | Novel process for treating indigo alkaline residue |
| 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 |
| 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 |
| CN204508823U (en) * | 2015-02-13 | 2015-07-29 | 内蒙古泰兴泰丰化工有限公司 | Its Future about Alkaline Residue Treatment Unit is mixed in indigo production |
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- 2015-02-13 CN CN201510077707.7A patent/CN104692422B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557708A (en) * | 2004-01-19 | 2004-12-29 | 升 贾 | Comprehensive process for recovering and treating indigo blue powder waste slag |
| 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 |
| CN102350435A (en) * | 2011-09-09 | 2012-02-15 | 韩扶军 | Novel process for treating indigo alkaline residue |
| 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 |
| CN204508823U (en) * | 2015-02-13 | 2015-07-29 | 内蒙古泰兴泰丰化工有限公司 | Its Future about Alkaline Residue Treatment Unit is mixed in indigo production |
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