CN104478028A - Treatment method of saccharin production wastewater - Google Patents
Treatment method of saccharin production wastewater Download PDFInfo
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- CN104478028A CN104478028A CN201410771066.0A CN201410771066A CN104478028A CN 104478028 A CN104478028 A CN 104478028A CN 201410771066 A CN201410771066 A CN 201410771066A CN 104478028 A CN104478028 A CN 104478028A
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- Prior art keywords
- extraction
- phase
- asccharin
- agent
- factory effluent
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
Abstract
The invention belongs to the field of treatment of fine chemical production wastewater, and particularly relates to a treatment method of saccharin production wastewater. The method comprises the following steps: mixing an extracting agent with the saccharin production wastewater of which the pH value is adjusted to be 1-3 with sulfuric acid at the volume ratio of 1 to (8-15); carrying out single-stage extraction after mixing, and carrying out extracting reaction for 30-60 minutes, so that two phases reach the extraction balance; and separating a water phase from an extracting phase, so that the processed saccharin production wastewater can be discharged up to the standard. After treatment by the treatment method, toxic refractory organic matters in the wastewater are effectively reduced; meanwhile, o-aminobenzoic acid in the wastewater can be recycled; and the saccharin wastewater processed by the method can be discharged up to the standard after being biodegraded.
Description
Technical field
The invention belongs to fine chemistry industry production wastewater treatment field, be specifically related to a kind for the treatment of process of asccharin factory effluent.
Background technology
Asccharin is the synthetic sweetener of unique a large amount of manufacture and usage in the world, and product is mainly used in the industries such as food, beverage, medicine, agricultural chemicals, plating, uses extensively in countries in the world.Asccharin generative process Raw kind is many, complex process, and production stage is long, and the waste component of thus discharging is complicated, and COD is high, colourity is dark, and quantity discharged is large.Not only containing a large amount of poisonous hardly degraded organic substances (by-product aldehydes matter, methyl o-aminobenzoate, anthranilic acid, methyl alcohol etc.) in asccharin factory effluent, and the salt containing higher concentration, thus difficulty of governance is very large.
Chinese patent CN 101891699A describes a kind of method that resin adsorption method reclaims saccharin insoluble in acid waste water, and the method mainly utilizes the processes such as resin absorption, desorb, decolouring, filtration, acid out, drying, oven dry.Name be called the disclosed treatment step of the Chinese patent (CN103193665A) of " a kind of preparation method reclaiming anthranilic acid from saccharin wastewater " comprise the preparation-alkali of mantoquita molten-press filtration-decolouring-suction filtration-acid out and drying.Above-mentioned treatment process can reach its expected effect, but still has following weak point: the regeneration solution concentration 1) produced in resin regeneration process is relatively on the low side, makes reuse effect not remarkable, if carry out reprocessing to it, must cause the rising of cost; 2) mantoquita precipitation reclaims after anthranilic acid, and the saccharin wastewater after process, still containing poisonous hardly degraded organic substance, makes its waste water cannot qualified discharge.
Summary of the invention
The object of the invention is the treatment process providing a kind of asccharin factory effluent.
For achieving the above object, the technical solution used in the present invention is:
A kind for the treatment of process of asccharin factory effluent, by extraction agent be that the asccharin factory effluent of 1-3 is by volume for 1:8-15 mixes by sulfuric acid adjust ph, single-stage extraction is carried out after mixing, extractive reaction 30-60 minute, two-phase is made to reach extraction equilibrium, water phase separated and extraction (organic) phase, namely aqueous phase reaches can biochemical treatment standard.
Described extraction agent by volume percentages by 18-52% complexing agent, 5-35% solubility promoter, surplus be thinner composition; Its complexing agent is trialkylamine, and the isomery alcohol of solubility promoter to be carbochain be 14-25, thinner is kerosene.
Above-mentioned (extraction) organic phase is placed in extractant regeneration device, be that the extraction phase of extraction equilibrium mixes with the alkali lye of mass percentage concentration 8-20% by 3-6:1 by volume, reaction 30-60 minute, after two-phase reaches extraction equilibrium, separate dense aqueous phase, upper strata regenerating extracting agent can be used for again processing in the extraction process of saccharin wastewater.
Described alkali lye is sodium hydroxide solution.
Compared with prior art, tool of the present invention has the following advantages:
1. achieve the recycling of waste water.The dense aqueous phase that the present invention is reclaimed by complexometric extraction, main component is anthranilic acid sodium, can be back to production workshop section after separation, achieves the recycle of resource, embodies certain economic benefit while pollutent minimizing.
2. the saccharin wastewater after process of the present invention again can qualified discharge after biological degradation.The present invention selects trialkylamine as complexing agent, the polar organic matter that in waste water, nearly all difficulty is fallen and aborning generate the organic by-products being soluble in organic phase and extract into organic phase, therefore the waste water after process is easy to biological degradation, decreases environmental risk.
Accompanying drawing explanation
The asccharin production wastewater treatment process flow sheet that Fig. 1 embodiment of the present invention provides.
Embodiment
Below by embodiment, the present invention is further elaborated.
In following examples, asccharin factory effluent COD is 13405mg/L, pH is 4, and colourity is 3000.
Embodiment 1
The method of process asccharin factory effluent:
Complexing agent, solubility promoter and thinner are mixed with extraction agent, and wherein trialkylamine volume accounts for 30%, isomery 14 alcohol volume accounts for 15%, kerosene volume accounts for 55%.By extraction agent and the waste water regulating pH value 1 by volume 1:10 join in extraction plant, mass transfer 45 minutes, makes two-phase reach extraction equilibrium; Left standstill in tripping device by solution after balance, phase-splitting, isolates organic phase and aqueous phase after 30 minutes, lower floor's aqueous phase sampling analysis again, and after making process, carried out can biochemical treatment for asccharin factory effluent.After testing, processed waste water COD is 5142mg/L, and colourity is 100.
By above-mentioned organic phase and 15% (mass percent) sodium hydroxide solution by volume 5:1 send into extractant regeneration device, react 30 minutes, leave standstill, phase-splitting, obtain regenerating extracting agent, regenerating extracting agent is cycled to used in the process of waste water.
Embodiment 2
The method of process asccharin factory effluent:
Complexing agent, solubility promoter and thinner are mixed with extraction agent, and wherein trialkylamine volume accounts for 20%, isomery 14 alcohol volume accounts for 8%, kerosene volume accounts for 72%.By extraction agent and the waste water regulating pH value 2 by volume 1:7 join in extraction plant, mass transfer 60 minutes, makes two-phase reach extraction equilibrium; Left standstill in tripping device by solution after balance, phase-splitting, is separated organic phase and aqueous phase after 30 minutes, lower floor's aqueous phase sampling analysis again, and after making process, carried out can biochemical treatment for asccharin factory effluent.After testing, processed waste water COD is 5446mg/L, and colourity is 150.
By above-mentioned organic phase and massfraction 20% sodium hydroxide solution by volume 8:1 send into extractant regeneration device, react 60 minutes, leave standstill, phase-splitting, obtain regenerating extracting agent, regenerating extracting agent can be reused for the process of waste water.
Embodiment 3
The method of process asccharin factory effluent:
Complexing agent, solubility promoter and thinner are mixed with extraction agent, and wherein trialkylamine volume accounts for 40%, isomery 20 alcohol volume accounts for 10%, kerosene volume accounts for 50%.By extraction agent and the waste water regulating pH value 1 by volume 1:20 join in extraction plant, mass transfer 60 minutes, makes two-phase reach extraction equilibrium; Left standstill in tripping device by solution after balance, phase-splitting, is separated organic phase and aqueous phase after 30 minutes, lower floor's aqueous phase sampling analysis again, and after making process, carried out can biochemical treatment for asccharin factory effluent.After testing, processed waste water COD is 5316mg/L, and colourity is 150.
By above-mentioned organic phase and massfraction 10% sodium hydroxide solution by volume 4:1 send into extractant regeneration device, react 45 minutes, leave standstill, phase-splitting, obtain regenerating extracting agent, regenerating extracting agent can be reused for the process of waste water.
Embodiment 4
The method of process asccharin factory effluent:
Complexing agent, solubility promoter and thinner are mixed with extraction agent, and wherein trialkylamine volume accounts for 50%, isomery 20 alcohol volume accounts for 8%, kerosene volume accounts for 42%.By extraction agent and the waste water regulating pH value 2 by volume 1:25 join in extraction plant, mass transfer 90 minutes, makes two-phase reach extraction equilibrium; Left standstill in tripping device by solution after balance, phase-splitting, is separated organic phase and aqueous phase after 30 minutes, lower floor's aqueous phase sampling analysis again, and after making process, carried out can biochemical treatment for asccharin factory effluent.After testing, processed waste water COD is 5046mg/L, and colourity is 100.
By above-mentioned organic phase and massfraction 25% sodium hydroxide solution by volume 6:1 send into extractant regeneration device, react 30 minutes, leave standstill, phase-splitting, obtain regenerating extracting agent, regenerating extracting agent can be reused for the process of waste water.
Embodiment 5
The method of process asccharin factory effluent:
Complexing agent, solubility promoter and thinner are mixed with extraction agent, and wherein trialkylamine volume accounts for 45%, isomery 18 alcohol volume accounts for 5%, kerosene volume accounts for 50%.By extraction agent and the waste water regulating pH value 2 by volume 1:15 join in extraction plant, mass transfer 60 minutes, makes two-phase reach extraction equilibrium; Left standstill in tripping device by solution after balance, phase-splitting, is separated organic phase and aqueous phase after 30 minutes, lower floor's aqueous phase sampling analysis again, and after making process, carried out can biochemical treatment for asccharin factory effluent.After testing, processed waste water COD is 5142mg/L, and colourity is 100.
By above-mentioned organic phase and massfraction 12% sodium hydroxide solution by volume 3:1 send into extractant regeneration device, react 45 minutes, leave standstill, phase-splitting, obtain regenerating extracting agent, regenerating extracting agent can be reused for the process of waste water.
Embodiment 6
The method of process asccharin factory effluent:
By the regenerating extracting agent in embodiment 5 and the waste water regulating pH value 1 by volume 1:16 join in extraction plant, mass transfer 30 minutes, makes two-phase reach extraction equilibrium; Left standstill in tripping device by solution after balance, phase-splitting, is separated organic phase and aqueous phase after 30 minutes, lower floor's aqueous phase sampling analysis again, and after making process, carried out can biochemical treatment for asccharin factory effluent.After testing, processed waste water COD is 5264mg/L, and colourity is 100.
By above-mentioned organic phase and massfraction 20% sodium hydroxide solution by volume 7:1 send into extractant regeneration device, react 60 minutes, leave standstill, phase-splitting, obtain regenerating extracting agent, regenerating extracting agent can be reused for the process of waste water.
Claims (3)
1. the treatment process of an asccharin factory effluent, it is characterized in that: by extraction agent be that the asccharin factory effluent of 1-3 is by volume for 1:8-15 mixes by sulfuric acid adjust ph, single-stage extraction is carried out after mixing, extractive reaction 30-60 minute, two-phase is made to reach extraction equilibrium, water phase separated and extraction phase, namely aqueous phase reaches can biochemical treatment standard;
Described extraction agent by volume percentages is 18-52% complexing agent, 5-35% solubility promoter, and surplus is thinner composition; Its complexing agent is trialkylamine, and solubility promoter is the isomery alcohol of carbochain at 14-25, and thinner is kerosene.
2., by the treatment process of asccharin factory effluent according to claim 1, it is characterized in that:
Extraction phase after above-mentioned extraction equilibrium is placed in extractant regeneration device, be that the extraction phase of extraction equilibrium mixes with the alkali lye of mass percentage concentration 8-20% by 3-6:1 by volume, reaction 30-60 minute, after two-phase reaches extraction equilibrium, upper strata regenerating extracting agent can be used for again processing in the extraction process of saccharin wastewater.
3., by the treatment process of asccharin factory effluent according to claim 2, it is characterized in that: described alkali lye is sodium hydroxide solution.
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| CN201410771066.0A CN104478028A (en) | 2014-12-11 | 2014-12-11 | Treatment method of saccharin production wastewater |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111732322A (en) * | 2020-07-10 | 2020-10-02 | 同济大学 | Sludge deep dehydration treatment technical method for recycling conditioner |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1309092A (en) * | 2001-03-16 | 2001-08-22 | 清华大学 | Complex extraction process for pre-treating waste water for intermediate of sulfornic dyes |
| US20090171116A1 (en) * | 2006-02-01 | 2009-07-02 | Carsten Berg | Treatment of Aqueous Liquids and the Preparation of Anthranilic Acid |
| CN101891699A (en) * | 2010-07-08 | 2010-11-24 | 平煤集团开封兴化精细化工厂 | Method for recovery of insoluble saccharin in acidic wastewater by resin adsorption method |
| CN102108055A (en) * | 2009-12-23 | 2011-06-29 | 天津大学 | Processing for recovering methyl anthranilate |
| CN102603025A (en) * | 2012-03-31 | 2012-07-25 | 中国中化股份有限公司 | Method for processing wastewater produced in reactive dye production by utilizing complexing extraction technology |
| CN103193665A (en) * | 2013-04-10 | 2013-07-10 | 天津市鑫卫化工有限责任公司 | Preparation method of anthranilic acid recovered from saccharin wastewater |
| CN104016871A (en) * | 2014-06-11 | 2014-09-03 | 广东顺德天新环保科技有限公司 | Method for recycling anthranilic acid from methyl anthranilate wastewater |
-
2014
- 2014-12-11 CN CN201410771066.0A patent/CN104478028A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1309092A (en) * | 2001-03-16 | 2001-08-22 | 清华大学 | Complex extraction process for pre-treating waste water for intermediate of sulfornic dyes |
| US20090171116A1 (en) * | 2006-02-01 | 2009-07-02 | Carsten Berg | Treatment of Aqueous Liquids and the Preparation of Anthranilic Acid |
| CN102108055A (en) * | 2009-12-23 | 2011-06-29 | 天津大学 | Processing for recovering methyl anthranilate |
| CN101891699A (en) * | 2010-07-08 | 2010-11-24 | 平煤集团开封兴化精细化工厂 | Method for recovery of insoluble saccharin in acidic wastewater by resin adsorption method |
| CN102603025A (en) * | 2012-03-31 | 2012-07-25 | 中国中化股份有限公司 | Method for processing wastewater produced in reactive dye production by utilizing complexing extraction technology |
| CN103193665A (en) * | 2013-04-10 | 2013-07-10 | 天津市鑫卫化工有限责任公司 | Preparation method of anthranilic acid recovered from saccharin wastewater |
| CN104016871A (en) * | 2014-06-11 | 2014-09-03 | 广东顺德天新环保科技有限公司 | Method for recycling anthranilic acid from methyl anthranilate wastewater |
Non-Patent Citations (2)
| Title |
|---|
| 张会敏，许光荣，毛冉: "连续萃取法回收酯化废液中邻氨基苯甲酸甲酯工艺研究", 《河南科技》, no. 16, 25 August 2014 (2014-08-25), pages 48 * |
| 戴猷元: "《新型萃取分离技术的发展及应用》", 31 August 2007, article "第2章 有机物稀溶液络合萃取技术", pages: 59-60 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111732322A (en) * | 2020-07-10 | 2020-10-02 | 同济大学 | Sludge deep dehydration treatment technical method for recycling conditioner |
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