CN101234829A - Method for treating copper-containing acid-containing waste liquid produced by glucide displacement reaction - Google Patents
Method for treating copper-containing acid-containing waste liquid produced by glucide displacement reaction Download PDFInfo
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- CN101234829A CN101234829A CNA2007101502132A CN200710150213A CN101234829A CN 101234829 A CN101234829 A CN 101234829A CN A2007101502132 A CNA2007101502132 A CN A2007101502132A CN 200710150213 A CN200710150213 A CN 200710150213A CN 101234829 A CN101234829 A CN 101234829A
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Abstract
The invention relates to a method for treating waste liquid containing copper and acid generated during substitution reaction of saccharine, wherein mainly the wastewater containing copper and acid is distilled, thus H<-> and CL <-> is azeotropied with water in an HCL manner; hydrochloric acid is condensed and reclaimed; solution A is obtained by utilizing water to dissolve remained matters in a container; then solution B is obtained by mixing alkali (sodium hydroxide, sodium sulfide, etc.) with water; after the solution B is filtered, copper hydroxide (or copper sulfide) and solution C are obtained; the solution C is added with active carbon, decolored and filtered to obtain solution D; the solution D is concentrate, crystallized and separated to obtain sodium sulfide of ten types of edema. The treatment method of the invention has the advantages that the wastewater containing copper and acid during the production of saccharine can be completely separated to obtain hydrochloric acid, copper hydroxide (or copper sulfide) and sodium sulfide of ten types of edema; during the treatment process, no acid gas or acid water exist to pollute the environment, thus the separated product can be used as chemical industrial material in saccharine, chemical industry and metallurgy industries; energy conservation, emission reduction and circulation economy are assured; as for enterprises producing the wastewater, the comprehensive benefits can reach 2 million to 3 million yuan a year, calculated by current price of chemical industrial material, thus the method has remarkable social and economic benefits.
Description
Technical field
The invention belongs to field of waste water treatment, particularly relate to the method that a kind of in asccharin and the soluble saccharin production handles the copper-containing acid-containing waste liquid that the asccharin replacement(metathesis)reaction produced.
Background technology
In the chemical industry building-up process, produce cupric, acidiferous waste water in its displacement, the chlorination reaction, metal ions such as a large amount of bivalent cupric ion that in this waste water, contains, monovalence chlorion, divalent sulfur acid ion, monovalence sodium ion, if contain the directly discharging of these metal ion solutions, can cause very big pollution to environment.Handle this waste water at present and adopt substitution method usually, its substitute mode is that iron filings are fed in the cupric sour water, replaces copper by chemical reaction with fe, and filtration drying obtains copper then.The deficiencies in the prior art part mainly is: still contain a large amount of CL in the filtrate after displacement 1.
-, SO4
2-H
+, Fe
2+, Fe
3+Na
+And Cu
2+Deng chemical element, can't reach the emission standard of regulation; In the replacement(metathesis)reaction process because of heating produces hydrogen chloride gas, this gas is contaminate environment not only, also because Fe+H
+=Fe
2++ H
2↑, the hydrogen danger that is produced is bigger, easily blasts; 3. energy expenditure is also big.
By retrieval, finding to have certain method is to adopt the distillation mode to obtain hydrochloric acid, again crystalline mixture by obtaining copper sulfate, sodium sulfate after concentrating or the oven dry moisture mixture that obtains copper sulfate and sodium sulfate.The shortcoming of this mode is a complex process, and is not easy to operate, can not get pure copper sulfate recycle, and exists the possibility of environmental pollution.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, provide a kind of technology simple, can decontamination, and a kind of method of handling the copper-containing acid-containing waste liquid that the asccharin replacement(metathesis)reaction produced that can handle cupric, acid-bearing wastewater in asccharin and the soluble saccharin production effectively up hill and dale; When disposing waste liquid, also can make discharge of wastewater up to standard, and obtain hydrochloric acid and 96% copper sulfate is applied to asccharin production, reach the recycling economy purpose.
Realize that technical scheme of the present invention is:
A kind of method of handling the copper-containing acid-containing waste liquid that the asccharin replacement(metathesis)reaction produced, the step of its treatment process is:
(1). with the distillation of copper-containing acid-containing waste water, make H
+, CL
-With HCL form and water azeotropic, hydrochloric acid is reclaimed in condensation, and the residuum of water dissolution vessel obtains A liquid;
(2). A liquid is mixed into B liquid with alkali and water; OH in the B liquid
-Or S
2-With Cu
2+Precipitin reaction taking place generate copper hydroxide or cupric sulfide, after filtering, obtains liquor C;
(3). add decolorizing with activated carbon, filtration to liquor C, obtain filtrate D;
(4). filtrate D obtains sal glauberi through concentrated, crystallization, separation.
And, when copper-containing acid-containing waste water was distilled, its distillation temperature was lower than 130 ℃, and calculated the container residuum at chloride 0.5% o'clock by the former sour water chloride ion-containing amount and the difference of the chloride ion-containing amount that steams hydrochloric acid, stop distillation heating, and with the water dissolution residuum to obtain A liquid.
And it is sodium hydroxide or sodium sulphite that described A liquid is mixed into the alkali that B liquid adopted with alkali and water.
And described B liquid is to be 30% solution with part dissolution of sodium hydroxide or to prepare 30% sodium sulfide solution with sodium sulphite or Sodium sulfhydrate and form to mix with A liquid behind the solution again and obtain.
And described filtrate D is liquor C to be heated up add decolorizing with activated carbon after 50～60 ℃ and stir 15 minutes after-filtration and obtain thus.
And described filtrate D concentrates and water is cooled to 20 ℃ and has crystallization to produce, and after filtration, drying or centrifuge dripping, obtains sal glauberi thus.
Advantage of the present invention and beneficial effect are:
1. treatment process of the present invention can be produced asccharin cupric, acid-bearing wastewater and thoroughly is separated into hydrochloric acid, copper sulfate or cupric sulfide, sal glauberi, and there are not acid gas, sour water contaminate environment in the treating processes, isolating product can be used as industrial chemicals, be used for asccharin, chemical industry and metallurgy industry, fully accomplish recycling economy, reached effects of energy saving and emission reduction.
2. the present invention can effectively improve the capability of environmental protection of enterprise, reaches 200～3,000,000 yuan/year for the 3000 tons of asccharin enterprises of annual output that produce this waste water by present its comprehensive benefit of industrial chemicals calculation of price, and social benefit, economic benefit are obvious.
Embodiment
The invention will be further described below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
At first need to prove: the various components that the embodiment of the invention is used are the commercially available prod.
A kind of method of handling the copper-containing acid-containing waste liquid that the asccharin replacement(metathesis)reaction produced, the step of its treatment process is:
1. with 1 part of the useless acid-bearing wastewater of cupric, in distil container, distill in 105～130 ℃, make H
+, CL
-With HCL form and water azeotropic, hydrochloric acid is reclaimed in condensation.Fore-running is divided into 4～8% hydrochloric acid, collecting amount is a former waste liquid 8～10% (volume percent), and second section is collected as 14～21% (volume percent) hydrochloric acid, and collecting amount is a former sour water 70～75% (volume percent), and in distil container, add water several times and distill, purpose is with unnecessary H
+, CL
-Steam, so that carry out the next step.Still-process obtains 2～5% hydrochloric acid for the third time, and collecting amount is 40～60% (volume percent) of former water.The hydrochloric acid that obtains 2～5% and 4～8% (volume percent) in the still-process can be used as pickling agent, and 14～21% hydrochloric acid can also also can be used as the synthetic doazo reaction of asccharin with sour as pickling agent, and distillation temperature is not above 130 ℃.Calculated the container residuum at chloride 0.5% o'clock by the former sour water chloride ion-containing amount and the difference of the chloride ion-containing amount that steams hydrochloric acid, stop heating,, obtain A liquid with 0.5～0.7 part of water dissolution residuum.
2. with 0.1～0.2 part of 30% sodium hydroxide solution or prepare 30% sodium sulphite (sodium hydrosulfide) with 0.022～0.03 part of sodium sulphite or Sodium sulfhydrate and form alkali lye, above-mentioned alkali lye is slowly added form B liquid in the A liquid, stir B liquid and regulate PH and make Cu
2+With OH
-Produce Cu (OH)
2↓ or Cu
2++ S
2-=CuS ↓ precipitation; Continue to add alkali lye and make PH＞＞9, sedimentation and filtration is obtained solid hydrogen cupric oxide or cupric sulfide and liquor C.
3. the solid hydrogen cupric oxide is added sulfuric acid to PH=1～2 and regulate proportion 1.2～1.5, crystallisation by cooling obtains 96% copper sulfate then; Can sell according to content after the cupric sulfide washing, be used for copper smelting.Liquor C heated up to add 0.003～0.007 part of decolorizing with activated carbon after 50～60 ℃ and stirs 15 minutes after-filtration, obtains carbon and filtrate D, and carbon can regeneration.
4. filtrate D concentrates, crystallization, centrifugation obtain sal glauberi and mother liquor, and sal glauberi detects qualified back and sells mother liquid recycle.
By aforesaid method treatment effect the best, both can reach energy-saving and emission-reduction, can reclaim useful matter again, accomplish recycling economy fully, produce cupric when making in the chemical industry building-up process displacement, chlorination reaction, acid-bearing wastewater is effectively administered.
The specification of each raw material and consumption in the technological process
| Operation | Material name | Specification | Weight part | Remarks |
| Still-process | Copper-containing acid-containing water | 1 | ||
| Water | 0.5～0.7 | |||
| B liquid | Sodium hydroxide sodium sulphite | More than 30% 60% | 0.1～0.2 0.022～0.03 | Be made into 30% solution |
| Decolouring | Gac | 0.003～0.007 |
Provide specific examples of the present invention below:
Specific examples 1:
1. copper-containing acid-containing water 500ml with the electric mantle heating, comes to life at 105 ℃ in the 1000ml matrass, and 106 ℃ of condensations have distillate, collects its content 5.6% of 50ml salt acidity test; Change receiving flask, continue distillation, 360ml salt acidity test content 18.8% is reclaimed in condensation, this moment residuum near evaporate to dryness, add 15ml water after, distill again and amount to 18 times, collect 180ml hydrochloric acid altogether, measure content 3.6%.With 350ml water dissolution residuum, chlorine detection ion content 0.5% obtains A liquid.
2. get 40g, 30% sodium hydroxide solution, this alkali lye is slowly added formation B liquid in the A liquid, stir and produce black precipitate; Continue to add alkali lye and do not produce to there being precipitation, this moment PH＞＞9, about 20 minutes of whole process will precipitate to filter in the suction funnel again and obtain copper hydroxide and liquor C.
3. filter cake 20ml water washing, wash water mix the back and amount to 420ml with liquor C, obtain copper hydroxide 8.3 grams after measured; Be neutralized to PH＜2 with adding 92.5% sulfuric acid, 8.3 grams in the copper hydroxide, water is regulated proportion 1.15, and crystallization obtains 18 gram copper sulfate and mother liquor 20ml.The mixed solution of wash water and liquor C is warming up to 55 ℃ and adds the 2g activated carbon, stirs 15 minutes after-filtration and obtains activated carbon and filtrate D.
4. filtrate D is concentrated into 280ml, and water is cooled to 20 ℃ has crystallization to produce, filter, dry, obtain sal glauberi and mother liquor, sal glauberi 256g.
Specific examples 2:
1. copper-containing acid-containing water 3500L with adding the cover steam heating, comes to life at 105 ℃ in the 5000L enamel pot, and 106 ℃ of condensations have distillate, collects its content 5.8% of 350L salt acidity test, and phlegma is imported the concentrated hydrochloric acid tourie; Continue distillation, 2600L hydrochloric acid is reclaimed in condensation, measures content 18.6%.This moment, residuum was near evaporate to dryness, add 120L water after, distill again and amount to 8 times and collect 960L salt acidity test content 3.8% altogether.With 2000L water dissolution residuum, chlorine detection ion content 0.5% obtains A liquid.
2. get 280 kilogram of 30% sodium hydroxide solution, this alkali lye is slowly added in the A liquid to form B liquid, stirring generation black precipitate; Continue to add alkali lye and do not produce to there being precipitation, this moment PH＞＞9, about 20 minutes of whole process.To precipitate again to filter in the suction funnel and obtain copper hydroxide and liquor C.
3. filter cake 140L water washing, wash water mix the back and amount to 2500L with liquor C, obtain the 58kg copper hydroxide after measured.With adding 92.5% sulfuric acid 60kg in the copper hydroxide, be neutralized to PH＜2, water is regulated proportion 1.12, and crystallization obtains 126kg copper sulfate and mother liquor 140L.The mixed solution of wash water and liquor C is warming up to 55 ℃ and adds the 20kg activated carbon, stirs 15 minutes after-filtration and obtains activated carbon and filtrate D.
4. filtrate D is concentrated into 1600L in the 3000L concentration tank, and water is cooled to 20 ℃ has crystallization to produce, and centrifuge dripping in ∮=1000mm whizzer obtains sal glauberi and mother liquor, sal glauberi 1560kg.Recycling Mother Solution is used.
Specific examples 3:
1. copper-containing acid-containing water 500ml with the electric mantle heating, comes to life at 105 ℃ in the 1000ml matrass, and 106 ℃ of condensations have distillate, collect 50ml hydrochloric acid, measure its content 5.6%; Change receiving flask, continue distillation, 360ml hydrochloric acid is reclaimed in condensation, measures content 18.8%; This moment, residuum was near evaporate to dryness, add 15ml water after, distill again, amount to 18 times and collect 180ml altogether, salt acidity test content 3.6%.With 350ml water dissolution residuum, chlorine detection ion content 0.008% obtains A liquid.
2. get 11g sodium sulphite and prepare 30% sodium sulfide solution, this alkali lye is slowly added formation B liquid in the A liquid, stir and produce black precipitate; Continue to add alkali lye and do not produce to there being precipitation, about 20 minutes of whole process will precipitate to filter in the suction funnel again and obtain cupric sulfide and liquor C.
3. filter cake 20ml water washing, wash water mix the back and amount to 420ml with liquor C, obtain moisture 50% cupric sulfide 15.5g after measured; The mixed solution of wash water and liquor C is warming up to 55 ℃, adds the 2g activated carbon and stirs 15 minutes after-filtration, obtains activated carbon and filtrate D.
4. filtrate D is concentrated into 280ml, and water is cooled to 20 ℃ has crystallization to produce, filter, dry, obtain sal glauberi and mother liquor, sal glauberi 256g.
Specific examples 4:
1. copper-containing acid-containing water 3500L with adding the cover steam heating, comes to life at 105 ℃ in the 5000L enamel pot, and 106 ℃ of condensations have distillate, collects 350L hydrochloric acid, measures its content 5.8%, and phlegma is imported the concentrated hydrochloric acid tourie; Continue distillation, 2600L hydrochloric acid is reclaimed in condensation, measures content 18.6%; This moment, residuum was near evaporate to dryness, added to distill behind the 120L water to amount to 8 times and collect 960L hydrochloric acid altogether again, measured content 3.8%.With 2000L water dissolution residuum, chlorine detection ion content 0.008% obtains A liquid.
2. get 66kg sodium sulphite and prepare 30% sodium sulfide solution, this alkali lye is slowly added formation B liquid in the A liquid, stir and produce black precipitate; Continue to add alkali lye and do not produce about 20 minutes of whole process to there being precipitation.To precipitate again in the suction funnel and filter, obtain cupric sulfide and liquor C.
3. filter cake 120L water washing, wash water mix the back and amount to 2500L with liquor C, obtain moisture 50% cupric sulfide 96kg after measured; The mixed solution of wash water and liquor C is warming up to 55 ℃, adds the 20kg activated carbon and stirs 15 minutes after-filtration, obtains activated carbon and filtrate D.
4. filtrate D is concentrated into 1600L in the 3000L concentration tank, and water is cooled to 20 ℃ has crystallization to produce, and centrifuge dripping in ∮=1000mm whizzer obtains sal glauberi and mother liquor, sal glauberi 1560kg.Recycling Mother Solution is used.
Claims (6)
1. method of handling the copper-containing acid-containing waste liquid that the asccharin replacement(metathesis)reaction produced, it is characterized in that: the step of its treatment process is:
(1). with the distillation of copper-containing acid-containing waste water, make H
+, CL
-With HCL form and water azeotropic, hydrochloric acid is reclaimed in condensation, and the residuum of water dissolution vessel obtains A liquid;
(2). A liquid is mixed into B liquid with alkali and water; OH in the B liquid
-Or S
2-With Cu
2+Precipitin reaction taking place generate copper hydroxide or cupric sulfide, after filtering, obtains liquor C;
(3). add decolorizing with activated carbon, filtration to liquor C, obtain filtrate D;
(4). filtrate D obtains sal glauberi through concentrated, crystallization, separation.
2. a kind of method of handling the copper-containing acid-containing waste liquid that the asccharin replacement(metathesis)reaction produced according to claim 1, it is characterized in that: when copper-containing acid-containing waste water is distilled, its distillation temperature is lower than 130 ℃, and calculated the container residuum at chloride 0.5% o'clock by the former sour water chloride ion-containing amount and the difference of the chloride ion-containing amount that steams hydrochloric acid, stop distillation heating, and with the water dissolution residuum to obtain A liquid.
3. a kind of method of handling the copper-containing acid-containing waste liquid that the asccharin replacement(metathesis)reaction produced according to claim 1 is characterized in that: it is sodium hydroxide or sodium sulphite that described A liquid is mixed into the alkali that B liquid adopted with alkali and water.
4. a kind of method of handling the copper-containing acid-containing waste liquid that the asccharin replacement(metathesis)reaction produced according to claim 1, it is characterized in that: described B liquid is to be 30% solution with part dissolution of sodium hydroxide or to prepare 30% sodium sulfide solution with sodium sulphite or Sodium sulfhydrate and form to mix with A liquid behind the solution again and obtain.
5. a kind of method of handling the copper-containing acid-containing waste liquid that the asccharin replacement(metathesis)reaction produced according to claim 1 is characterized in that: described filtrate D is liquor C to be heated up add decolorizing with activated carbon after 50～60 ℃ and stir 15 minutes after-filtration and obtain thus.
6. a kind of method of handling the copper-containing acid-containing waste liquid that the asccharin replacement(metathesis)reaction produced according to claim 1, it is characterized in that: the concentrated also water of described filtrate D is cooled to 20 ℃ has crystallization to produce, after filtration, drying or centrifuge dripping, obtain sal glauberi thus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101502132A CN101234829A (en) | 2007-11-19 | 2007-11-19 | Method for treating copper-containing acid-containing waste liquid produced by glucide displacement reaction |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101502132A CN101234829A (en) | 2007-11-19 | 2007-11-19 | Method for treating copper-containing acid-containing waste liquid produced by glucide displacement reaction |
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ID=39918772
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102134131A (en) * | 2011-01-18 | 2011-07-27 | 嘉兴市中华化工有限责任公司 | Method for treating wastewater generated in process of synthesizing vanillin by glyoxylic acid method |
| CN101774719B (en) * | 2009-01-09 | 2011-09-21 | 上海博丹环境工程技术有限公司 | Treatment method for sewage containing copper with medium or low concentration |
| CN101774724B (en) * | 2009-01-14 | 2011-09-21 | 上海博丹环境工程技术有限公司 | Method for treating production wastewater of glucide |
| CN104743725A (en) * | 2013-12-30 | 2015-07-01 | 西南大学 | Sodium saccharin wastewater and similar wastewater treatment method |
| CN107158804A (en) * | 2017-05-10 | 2017-09-15 | 上田环境修复股份有限公司 | A kind of filtering material, its preparation method and application for being used to filter copper ions and the exceeded foundation ditch water of nickel ion |
-
2007
- 2007-11-19 CN CNA2007101502132A patent/CN101234829A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774719B (en) * | 2009-01-09 | 2011-09-21 | 上海博丹环境工程技术有限公司 | Treatment method for sewage containing copper with medium or low concentration |
| CN101774724B (en) * | 2009-01-14 | 2011-09-21 | 上海博丹环境工程技术有限公司 | Method for treating production wastewater of glucide |
| 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 |
| CN101891699B (en) * | 2010-07-08 | 2012-12-26 | 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 |
| CN102134131A (en) * | 2011-01-18 | 2011-07-27 | 嘉兴市中华化工有限责任公司 | Method for treating wastewater generated in process of synthesizing vanillin by glyoxylic acid method |
| CN104743725A (en) * | 2013-12-30 | 2015-07-01 | 西南大学 | Sodium saccharin wastewater and similar wastewater treatment method |
| CN104743725B (en) * | 2013-12-30 | 2017-04-12 | 西南大学 | Sodium saccharin wastewater and similar wastewater treatment method |
| CN107158804A (en) * | 2017-05-10 | 2017-09-15 | 上田环境修复股份有限公司 | A kind of filtering material, its preparation method and application for being used to filter copper ions and the exceeded foundation ditch water of nickel ion |
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Open date: 20080806 |