CN101481098A - Method for processing sulphonation waste acid from reactive dye production - Google Patents
Method for processing sulphonation waste acid from reactive dye production Download PDFInfo
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- CN101481098A CN101481098A CNA2008101540904A CN200810154090A CN101481098A CN 101481098 A CN101481098 A CN 101481098A CN A2008101540904 A CNA2008101540904 A CN A2008101540904A CN 200810154090 A CN200810154090 A CN 200810154090A CN 101481098 A CN101481098 A CN 101481098A
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Abstract
The invention provides a method for treating and utilizing sulfonation waste acid, which comprises the following steps: firstly, collecting the waste acid generated by sulfonation in the reactive dye manufacture into a recycling pot; secondly, adding granular activated carbon inside the recycling pot to perform stirring adsorption or fixed bed adsorption; separating the waste acid solution from adsorbing agent after the adsorption, obtaining waste acid clear solution by using a filter press to filter the waste acid, and using the waste acid clear solution for adjusting the pH value of the diazotization reaction.
Description
Technical field
The processing of the spent acid that the present invention produces for sulfonation reaction in the reactive dyestuffs production process and utilize method, especially blue 3G, blue 8G, the processing of the sulphonation waste acid that sulfonation reaction produces in the red 6G isoreactivity DYE PRODUCTION process and utilize method.
Background technology
Sulfonation is the important reaction during fine chemistry industry is synthesized, and the general stronger oleum of sulfonation ability that adopts carried out sulfonation as sulphonating agent during reactive dyestuffs were synthetic.After sulfonation is finished, dilution, suction filtration, filtrate is sulphonation waste acid, the acid solution amount is big, is dark-brown, chemical composition complexity, acidity height (30%～40%).As not treated discharging, not only environment is caused severe contamination, and cause the waste of sour resource.
Neutralization is the most general spent acid solution treatment process.Sulfur waste acid neutralization is carried out landfill with the form of gypsum later.The very big defective of this method is that per 1 ton of spent acid generally needs 4 tons of alkali.Therefore, sulfuric acid per ton produces nearly 5 tons of waste liquids that need landfill to dispose after neutralization is disposed.
Also can adopt membrane technique (reverse osmosis method, diffusive dialysis method) to handle or dispose sulfuric acid at present.Reverse osmosis method need adopt expensive filtering system, and present reverse osmosis filtration system only can be handled small amount of liquid.Problems such as film pollution and film rupture easily take place in diffusive dialysis method.
Can also adopt to burn and dispose the sulfuric acid refuse.The same with evaporation, it is very high to burn cost, and can cause acid rain, thereby can not be accepted by environment.
Adopt other method: also exist problems such as energy consumption is big, cost is high, waste of human resource is big as ozone method, electrolytic process and strong oxidizer method.
Summary of the invention
Because the limitation of present various spent acid treatment processs, it is low to be necessary to seek cost, and the processing of environmental sound and utilize the method for sulfuric acid waste is to reduce the sulfur acid waste liquid amount that the ultimate demand landfill is disposed.Both economical feasible method is that the recycle sulfuric acid waste liquid is exercised usefulness again.Sulfuric acid is recycled the demand that also can reduce to landfill.Past has proposed many methods of recycle sulfuric acid, but do not have so far can be for the method for the recycle sulfuric acid waste liquid implemented in dyestuffs industries.
The report that does not also have at present discovery that the sulphonation waste acid in the reactive dyestuffs production is effectively handled and utilized.
For solving the problems of the technologies described above, the invention provides a kind of processing of sulphonation waste acid and utilize method, it comprises the steps:
(a), the spent acid that sulfonation in the reactive dyestuffs production is produced is collected in the withdrawing can;
(b), in withdrawing can, add grain active carbon, carry out whip attachment or ADSORPTION IN A FIXED BED;
(c), absorption separates spent acid solution after finishing with sorbent material, filter spent acid with pressure filter and obtain the spent acid clear liquid; Aforesaid method can also comprise the steps:
(d), the spent acid clear liquid that (c) step is obtained is used to regulate the pH value of diazotization reaction.
Wherein the collection of (a) step generally can be carried out under 5-50 ℃; other suitable temperature also can allow; (b) weight of the grain active carbon that adds in the step is 1 ‰-1% of spent acid weight; the amount that adds grain active carbon can increase or reduce; those skilled in the art can be according to the very few amount of determining to add activated carbon of impurity in the waste liquid; adsorption time is 3-6 hour generally speaking; the temperature of diazotization reaction generally is controlled under 0-5 ℃ carries out; reactive dyestuffs production wherein can be the production method of any reactive dyestuffs; as long as used the sulfonation reaction step in this reactive dyestuffs production, invention so of the present invention just is applicable to handles the sulphonation waste acid that produces in this reactive dyestuffs method production.
Grain active carbon in the aforesaid method is this area activated carbon commonly used, can obtain from the market, and it is not had specific requirement.
Diazotization reaction in the aforesaid method can be any diazotization reaction, as long as diazotization reaction takes place, the spent acid clear liquid of generation of the present invention just can be used in the basic solution of its generation of neutralization.
Method of the present invention in fact not only is confined to reactive dyestuffs production, and for other DYE PRODUCTION, as long as used sulfonation procedure and diazotization reaction step, method of the present invention just can be suitable for.Method of the present invention is applicable to that preferably reactive dyestuffs are blue 3G, and in the production of blue 8G or red 6G, these dyestuffs are known dyestuffs, and its production method also is known, and method of the present invention is particularly useful in the production of these dyestuffs.
Its medium blue 3G (C.I. Reactive blue 69) is the product that can obtain on the market, and it is Ciba (China) company limited that its commodity hair by name is used Reactive blue 3G, manufacturer, Tianjin Dek Chemical Company Ltd. etc.
Its medium blue 8G (C.I. Reactive blue 185) is the product that can obtain on the market, and its commodity are called acid bright blue 8G, and manufacturer is Ciba (China) company limited, Tianjin Dek Chemical Company Ltd. etc.
Wherein red 6G (C.I. reactive red 84) is the product that can obtain on the market, and it is Ciba (China) company limited that its commodity hair by name is used reactive red 6G, manufacturer, Tianjin Dek Chemical Company Ltd. etc.
Embodiment
Describe method of the present invention in detail below by specific embodiment, the following examples only are the explanations to technical scheme of the present invention, be not any limitation of the invention, by the following examples, those skilled in the art can round Realization technical scheme content of the present invention.
Embodiment 1:
Sulphonation waste acid 20m with sulfonation process generation in the blue 3G production
3Under 20 ℃, collect in the vinyon jar by acid proof pump; to the granulated active carbon that wherein adds 20kg; after the whip attachment 4 hours; by acid proof pump mixed solution is got to the pressure filter press filtration; leach colourless dilute sulphuric acid clear liquid; concentration is about 30%, this dilute sulphuric acid is used to regulate the pH value of diazotization reaction.
Embodiment 2:
Sulfonation process in the blue 8G production is produced sulphonation waste acid 15m
3Under 40 ℃, collect in the vinyon jar by acid proof pump; to the granulated active carbon that wherein adds 150kg; after stirring at a slow speed, adsorb 3 hours; get to the pressure filter press filtration by acid proof pump; leach colourless dilute sulphuric acid clear liquid; concentration is about 27%, this dilute sulphuric acid is used to regulate the pH value of diazotization reaction.
Embodiment 3:
Sulfonation process in the red 6G production is produced sulphonation waste acid 18m
3Collect in the vinyon jar under 5 ℃ by acid proof pump, add the granulated active carbon of 90kg, after stirring at a slow speed, adsorb 6 hours; get to the pressure filter press filtration by acid proof pump; leach colourless dilute sulphuric acid clear liquid, concentration is 30～35%, this dilute sulphuric acid is used to regulate the pH value of diazotization reaction.
Claims (3)
1, the processing of sulphonation waste acid and utilize method in the blue 3G preparation of a kind of reactive dyestuffs, it comprises the steps:
Sulphonation waste acid 20m with sulfonation process generation in the blue 3G production
3Under 20 ℃, collect in the vinyon jar by acid proof pump; to the granulated active carbon that wherein adds 20kg, whip attachment was got to the pressure filter press filtration by acid proof pump with mixed solution after 4 hours; leach colourless dilute sulphuric acid clear liquid, this dilute sulphuric acid is used to regulate the pH value of diazotization reaction.
2, the processing of sulphonation waste acid and utilize method in the blue 8G preparation of a kind of reactive dyestuffs, it comprises the steps:
Sulfonation process in the blue 8G production is produced sulphonation waste acid 15m
3Under 40 ℃, collect in the vinyon jar by acid proof pump; granulated active carbon to wherein adding 150kg after stirring at a slow speed, adsorb 3 hours, is got to the pressure filter press filtration by acid proof pump; leach colourless dilute sulphuric acid clear liquid, this dilute sulphuric acid is used to regulate the pH value of diazotization reaction.
3, the processing of sulphonation waste acid and utilize method in the red 6G of a kind of reactive dyestuffs preparation, it comprises the steps:
Sulfonation process in the red 6G production is produced sulphonation waste acid 18m
3Under 5 ℃, collect in the vinyon jar by acid proof pump; add the granulated active carbon of 90kg, after stirring at a slow speed, adsorb 6 hours, get to the pressure filter press filtration by acid proof pump; leach colourless dilute sulphuric acid clear liquid, this dilute sulphuric acid is used to regulate the pH value of diazotization reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101540904A CN101481098A (en) | 2008-12-12 | 2008-12-12 | Method for processing sulphonation waste acid from reactive dye production |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008101540904A CN101481098A (en) | 2008-12-12 | 2008-12-12 | Method for processing sulphonation waste acid from reactive dye production |
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| CNA2008101540904A Pending CN101481098A (en) | 2008-12-12 | 2008-12-12 | Method for processing sulphonation waste acid from reactive dye production |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641568A (en) * | 2013-12-11 | 2014-03-19 | 青岛奥盖克化工股份有限公司 | Comprehensive treatment method for waste sulfuric acid of sulfonated products |
| CN104725286A (en) * | 2015-04-17 | 2015-06-24 | 上海天坛助剂有限公司 | Method for using waste acid to produce sulfonated oil |
| CN105482495A (en) * | 2015-11-27 | 2016-04-13 | 天津德凯化工股份有限公司 | Preparation method of red reactive dye |
-
2008
- 2008-12-12 CN CNA2008101540904A patent/CN101481098A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641568A (en) * | 2013-12-11 | 2014-03-19 | 青岛奥盖克化工股份有限公司 | Comprehensive treatment method for waste sulfuric acid of sulfonated products |
| CN103641568B (en) * | 2013-12-11 | 2015-04-15 | 青岛奥盖克化工股份有限公司 | Comprehensive treatment method for waste sulfuric acid of sulfonated products |
| CN104725286A (en) * | 2015-04-17 | 2015-06-24 | 上海天坛助剂有限公司 | Method for using waste acid to produce sulfonated oil |
| CN105482495A (en) * | 2015-11-27 | 2016-04-13 | 天津德凯化工股份有限公司 | Preparation method of red reactive dye |
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Open date: 20090715 |