CN102807279A - Method for treating wastewater produced in process of producing phenylacetic acid - Google Patents
Method for treating wastewater produced in process of producing phenylacetic acid Download PDFInfo
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- CN102807279A CN102807279A CN2012102312386A CN201210231238A CN102807279A CN 102807279 A CN102807279 A CN 102807279A CN 2012102312386 A CN2012102312386 A CN 2012102312386A CN 201210231238 A CN201210231238 A CN 201210231238A CN 102807279 A CN102807279 A CN 102807279A
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Abstract
The invention discloses a method for treating wastewater produced in the process of producing phenylacetic acid by hydrolyzing phenylacetonitrile. The wastewater comprises cyanide wastewater and hydrolysis wastewater. The method comprises the following steps of: regulating the pH of the cyanide wastewater to 0.5 to 2 by using acid, converting cyanide ions in the wastewater into hydrocyanic acid, bringing hydrocyanic acid gas out by blowing air, and absorbing the gas by using a sodium hydroxide solution; neutralizing the acidic cyanide wastewater from which cyanides are removed by using the alkaline hydrolysis wastewater until the pH is 6 to 7; and adsorbing a mixed solution of the cyanide wastewater from which the cyanides are removed and the hydrolysis wastewater by using activated carbon, and blowing the air with heating to oxidize iso-benzyl chloride contained in the hydrolysis wastewater. The whole treatment process is easy to operate, a cyanide removing effect and a deodorizing effect are good, and the treated wastewater is colorless and odorless, is nearly neutral, has high stability after being placed for a long time, and can be directly discharged.
Description
Technical field
The invention belongs to chemical field, relate to a kind of treatment process of Chemicals factory effluent.
Background technology
The type reaction of carboxyl, methylene radical hydrogen and phenyl ring can take place in toluylic acid (Phenylacetic acid), generates many useful intermediates, is a kind of important chemical material.At present, using the most widely, the toluylic acid working method is the benzyl cyanide hydrolysis method.This method is that Benzyl Chloride is generated benzyl cyanide with the sodium cyanide reaction under catalyst action, again benzyl cyanide is carried out basic hydrolysis and makes toluylic acid.This method mainly produces two portions waste water in process of production, and a part is the cyanide wastewater that in the process of preparation benzyl cyanide, produces, because the reaction raw materials sodium cyanide is excessive adding, so contains more deleterious cyanide ion in this part waste water; Another part is the hydrolyzed waste water that in the process of basic hydrolysis benzyl cyanide, produces, and this part waste water has foul smell owing to containing the isocyanide benzyl.Existing toluylic acid production wastewater treatment method is that above-mentioned two portions waste water is handled respectively: to cyanide wastewater, mainly adopt oxygenant such as ydrogen peroxide 50 etc. to fall cyanogen and handle; To hydrolyzed waste water, mainly adopt charcoal absorption to remove stink.But there is following shortcoming in this method of wastewater treatment: 1) fall cyanogen with oxygenant and handle, production cost is higher; 2) two portions waste water separate treatment, operating process are complicated; 3) two portions waste water can not directly discharge after treatment, also need carry out acid-base neutralisation and handle; 4) originally waste water be colourless transparent liquid after treatment, but place spend the night after, then become blue liquid.
Summary of the invention
In view of this, the objective of the invention is to the benzyl cyanide hydrolysis method produce the waste water research and development that produce in the toluylic acid process a kind of simply, efficiently, treatment process cheaply.
For achieving the above object, the present invention provides following technical scheme:
The toluylic acid factory effluent comprises cyanide wastewater and hydrolyzed waste water two portions, and its treatment process may further comprise the steps: with cyanide wastewater with acid for adjusting pH to 0.5-2, bubbling air carries out air-blowing; The hydrocyanic acid gas body and function sodium hydroxide solution that bloats absorbs; Temperature 75-85 ℃ of insulation air-blowing to system contains the cyanogen amount and reduces to below the 9ppm, during to keep system pH be 0.5-2, add hydrolyzed waste water regulation system pH to 6-7 then; Add the gac that is equivalent to liquid gross weight 1-5% again; Continue 75-85 ℃ of insulation of temperature air-blowing 30-50 minute, the filtered and recycled gac, filtrating is the toluylic acid factory effluent after the processing.
Further, the treating method comprises following steps: it is that 60% sulphuric acid soln is regulated pH to 0.5-2 that cyanide wastewater is used mass percentage concentration, and bubbling air carries out air-blowing; The hydrocyanic acid gas body and function mass percentage concentration that bloats is that 23% sodium hydroxide solution absorbs; Temperature 75-85 ℃ of insulation air-blowing to system contains the cyanogen amount and reduces to below the 9ppm, during to keep system pH be 0.5-2, add hydrolyzed waste water regulation system pH to 6-7 then; Add the gac that is equivalent to liquid gross weight 1-2% again; Continue 75-85 ℃ of insulation of temperature air-blowing 30-50 minute, the filtered and recycled gac, filtrating is the toluylic acid factory effluent after the processing.
Beneficial effect of the present invention is: the present invention for the benzyl cyanide hydrolysis method produce the waste water that produces in the toluylic acid process provide a kind of simply, efficiently, treatment process cheaply; At first; Excessive cyanide ion in the cyanide wastewater is converted into prussic acid, takes hydrocyanic acid gas out of, absorb with sodium hydroxide solution through the mode that blasts air; Thereby the cyanide ion in the efficient recovery waste water reaches the purpose except that cyanogen and resource reutilization; Then, will be tart and be 6-7, reach the pH value that allows discharging, thereby realize the purpose that basis is applied mechanically hydrolyzed waste water except that the acidity maximization of cyanide wastewater behind the cyanogen except that cyanide wastewater behind the cyanogen uses the hydrolyzed waste water that is alkaline to be neutralized to pH; At last, will use charcoal absorption, and under 75-85 ℃ of condition, carry out air-blowing and handle, and make the different benzyl chloride oxidation that contains in the hydrolyzed waste water, thereby reach effective de-odorised effect except that the mixed solution of cyanide wastewater behind the cyanogen and hydrolyzed waste water; The entire treatment process operation is simple, and is low for equipment requirements, removes cyanogen, good deodorization effect, and production cost is low, the waste water colorless and odorless after the processing, and the pH value is near neutral, need not to carry out acid-base neutralisation again and handles, and long-time shelf-stability is good, can directly discharge.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer, will carry out detailed description to the preferred embodiments of the present invention below.Should be appreciated that preferred embodiment has been merely explanation the present invention, rather than in order to limit protection scope of the present invention.
Embodiment 1
In 1000 milliliters of there-necked flasks, add 300 gram cyanide wastewaters (containing the cyanogen amount is 0.85mg/L), the use mass percentage concentration is 60% sulphuric acid soln adjusting pH to 1, and bubbling air carries out air-blowing; Using mass percentage concentration is that 23% sodium hydroxide solution absorbs the hydrocyanic acid gas that bloats, and 80 ℃ of insulation air-blowing 5 hours (during keep system pH be 1) contain the cyanogen amount to system and reduce to 9ppm, in flask, add hydrolyzed waste water 400 grams then with regulation system pH to 6.5; Add the gac that accounts for liquid gross weight 1% again, continue 80 ℃ of insulation air-blowing 40 minutes, stop air-blowing; Waste water after suction filtration recovered carbon while hot, filtrating are promptly handled is through detecting; Containing the cyanogen amount is 4ppm; The cyanogen recovery is greater than 99.9%, and the liquid colorless and odorless still is colourless transparent liquid after placing a week.
The comparative example 1
In 1000 milliliters of there-necked flasks, add 300 gram cyanide wastewaters (containing the cyanogen amount is 0.85mg/L), the use mass percentage concentration is 60% sulphuric acid soln adjusting pH to 1, is heated with stirring to 80 ℃; Using mass percentage concentration is that 23% sodium hydroxide solution absorbs the hydrocyanic acid gas that produces, and 80 ℃ of insulated and stirred 5 hours (during keep system pH be 1) add hydrolyzed waste water 400g then with regulation system pH to 6-7 in flask; Add the gac account for liquid gross weight 1% again, 80 ℃ of insulated and stirred 40 minutes, suction filtration recovered carbon while hot at last; Waste water after filtrating is promptly handled, through detecting, containing the cyanogen amount is 170 ppm; The cyanogen recovery is 80%; Liquid is faint yellow, has certain foul smell, places the back liquid that spends the night and becomes blueness.
Embodiment 2
In 1000 milliliters of there-necked flasks, add 1000 gram cyanide wastewaters (containing the cyanogen amount is 1.0mg/L), the use mass percentage concentration is 60% sulphuric acid soln adjusting pH to 2, and bubbling air carries out air-blowing; Using mass percentage concentration is that 23% sodium hydroxide solution absorbs the hydrocyanic acid gas that bloats, and contains the cyanogen amount in 85 ℃ of insulation air-blowing 5 hours (during keep system pH be 2) to the system and reduces to 9ppm, in flask, adds hydrolyzed waste water 900 grams then with regulation system pH to 7; Add the gac that accounts for liquid gross weight 1% again, 80 ℃ are incubated air-blowing 40 minutes, stop air-blowing; Waste water after suction filtration recovered carbon while hot, filtrating are promptly handled is through detecting; Containing the cyanogen amount is 3.5ppm; The cyanogen recovery is greater than 99.9%, and the liquid colorless and odorless still is colourless transparent liquid after placing a week.
Embodiment 3
In 1000 milliliters of there-necked flasks, add 1200 gram cyanide wastewaters (containing the cyanogen amount is 0.90mg/L), the use mass percentage concentration is 60% sulphuric acid soln adjusting pH to 0.5, and bubbling air carries out air-blowing; Using mass percentage concentration is that 23% sodium hydroxide solution absorbs the hydrocyanic acid gas that bloats, and contains the cyanogen amount in 80 ℃ of insulation air-blowing 5 hours (during keep system pH be 0.5) to the system and reduces to 9ppm, in flask, adds hydrolyzed waste water 1600 grams then with regulation system pH to 6; Add the gac that accounts for liquid gross weight 2% again, 75 ℃ are incubated air-blowing 40 minutes, stop air-blowing; Waste water after suction filtration recovered carbon while hot, filtrating are promptly handled is through detecting; Containing the cyanogen amount is 3ppm; The cyanogen recovery is greater than 99.9%, and the liquid colorless and odorless still is colourless transparent liquid after placing a week.
Claims (2)
1. the treatment process of toluylic acid factory effluent, said toluylic acid factory effluent comprises cyanide wastewater and hydrolyzed waste water two portions, it is characterized in that; The treatment process of said toluylic acid factory effluent comprises the steps: cyanide wastewater with acid for adjusting pH to 0.5-2; Bubbling air carries out air-blowing, and the hydrocyanic acid gas body and function sodium hydroxide solution that bloats absorbs, and temperature 75-85 ℃ of insulation air-blowing to system contains the cyanogen amount and reduce to below the 9ppm; Keeping system pH during this time is 0.5-2; Add hydrolyzed waste water regulation system pH to 6-7 then, add the gac that is equivalent to liquid gross weight 1-5% again, continue 75-85 ℃ of insulation of temperature air-blowing 30-50 minute; The filtered and recycled gac, filtrating is the toluylic acid factory effluent after the processing.
2. the treatment process of toluylic acid factory effluent according to claim 1; It is characterized in that it is that 60% sulphuric acid soln is regulated pH to 0.5-2 that cyanide wastewater is used mass percentage concentration, bubbling air carries out air-blowing; The hydrocyanic acid gas body and function mass percentage concentration that bloats is that 23% sodium hydroxide solution absorbs; Temperature 75-85 ℃ of insulation air-blowing to system contains the cyanogen amount and reduces to below the 9ppm, during to keep system pH be 0.5-2, add hydrolyzed waste water regulation system pH to 6-7 then; Add the gac that is equivalent to liquid gross weight 1-2% again; Continue 75-85 ℃ of insulation of temperature air-blowing 30-50 minute, suction filtration recovered carbon while hot, filtrating is the toluylic acid factory effluent after the processing.
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| CN201210231238.6A CN102807279B (en) | 2012-07-05 | 2012-07-05 | Method for treating wastewater produced in process of producing phenylacetic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113185265A (en) * | 2021-07-01 | 2021-07-30 | 北京矿冶研究总院 | Cyanide sludge sintering cyanogen removal process, cyanide-free brick, cyanide sludge sintering cyanogen removal system and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1274684A (en) * | 2000-07-10 | 2000-11-29 | 南京大学 | Method of treating waste water from production of phenylacetic acid and reusing resouce |
| CN101514330A (en) * | 2008-12-18 | 2009-08-26 | 浙江工业大学 | Achromobacter capable of degrading aniline and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1274684A (en) * | 2000-07-10 | 2000-11-29 | 南京大学 | Method of treating waste water from production of phenylacetic acid and reusing resouce |
| CN101514330A (en) * | 2008-12-18 | 2009-08-26 | 浙江工业大学 | Achromobacter capable of degrading aniline and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 《黄金》 20070930 马红周等 "活性炭吸附酸化后的含氰废水试验研究" 第56-58页 1-2 第28卷, 第9期 * |
| 马红周等: ""活性炭吸附酸化后的含氰废水试验研究"", 《黄金》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113185265A (en) * | 2021-07-01 | 2021-07-30 | 北京矿冶研究总院 | Cyanide sludge sintering cyanogen removal process, cyanide-free brick, cyanide sludge sintering cyanogen removal system and application |
| CN113185265B (en) * | 2021-07-01 | 2021-11-05 | 北京矿冶研究总院 | Cyanide sludge sintering cyanogen removal process, cyanide-free brick, cyanide sludge sintering cyanogen removal system and application |
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| CN102807279B (en) | 2014-01-22 |
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