CN101481097A - Method for processing waste acid from sulphonation ester production - Google Patents
Method for processing waste acid from sulphonation ester production Download PDFInfo
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- CN101481097A CN101481097A CNA2008101540891A CN200810154089A CN101481097A CN 101481097 A CN101481097 A CN 101481097A CN A2008101540891 A CNA2008101540891 A CN A2008101540891A CN 200810154089 A CN200810154089 A CN 200810154089A CN 101481097 A CN101481097 A CN 101481097A
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- waste acid
- sulfonation
- acid
- ester production
- sulphonation
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- Separation Using Semi-Permeable Membranes (AREA)
- Water Treatment By Sorption (AREA)
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 sulfonated para-ester manufacture into a recycling pot; secondly, adding granular activated carbon inside the recycling pot into 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 present invention is the processing of the spent acid that sulfonation reaction produces in sulfonation para-ester (PS) production process and utilizes 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 sulfonation para-ester was 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 sulfonation para-ester production is effectively handled and utilized.
For solving the problems of the technologies described above, the invention provides the processing of the sulphonation waste acid in a kind of sulfonation para-ester production and utilize method, it comprises the steps:
(a), the spent acid that sulfonation in the sulfonation para-ester 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;
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, and the temperature of diazotization reaction generally is controlled under 0-5 ℃ carries out.
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.
Method of the present invention in fact not only is confined to sulfonation para-ester production, for other DYE PRODUCTION, just can be suitable for as long as used sulfonation procedure method of the present invention.
Wherein the structure of sulfonation para-ester is can buy the product that obtains on the market as shown in the formula (I), and its commodity are called sulfonation para-ester (PS), and manufacturer is Tianjin Dek Chemical Company Ltd. etc.Its production method is disclosed in number of patent application 200710058731.1.
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 the sulfonation process generation in PS (sulfonation para-ester) production
3Collect in the withdrawing can under 50 ℃ by acid proof pump; to wherein adding the 60kg granulated active carbon; 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 40%, this dilute sulphuric acid is used for regulating the pH value of reactive dyestuffs production process diazotization reaction.
Claims (1)
1, the processing of the spent acid that sulfonation reaction produces in a kind of sulfonation para-ester production process and utilize method, it comprises the steps:
Sulphonation waste acid 20m with the sulfonation process generation in the sulfonation para-ester production
3Under 50 ℃, collect in the vinyon jar by acid proof pump; to wherein adding the 60kg granulated active carbon; 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, this dilute sulphuric acid is used for regulating the pH value of reactive dyestuffs production process diazotization reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101540891A CN101481097A (en) | 2008-12-12 | 2008-12-12 | Method for processing waste acid from sulphonation ester production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101540891A CN101481097A (en) | 2008-12-12 | 2008-12-12 | Method for processing waste acid from sulphonation ester production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101481097A true CN101481097A (en) | 2009-07-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008101540891A Pending CN101481097A (en) | 2008-12-12 | 2008-12-12 | Method for processing waste acid from sulphonation ester production |
Country Status (1)
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| CN (1) | CN101481097A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504587A (en) * | 2011-10-18 | 2012-06-20 | 褚平忠 | Method for recovering waste acid from sulfonation of para-ester |
| CN102531246A (en) * | 2011-11-22 | 2012-07-04 | 启东金美化学有限公司 | Method for recycling waste acid |
| 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 |
| CN110066230A (en) * | 2018-08-30 | 2019-07-30 | 内蒙古利元科技有限公司 | A kind of novel sulfonated para-ester production system and technique |
-
2008
- 2008-12-12 CN CNA2008101540891A patent/CN101481097A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504587A (en) * | 2011-10-18 | 2012-06-20 | 褚平忠 | Method for recovering waste acid from sulfonation of para-ester |
| CN102531246A (en) * | 2011-11-22 | 2012-07-04 | 启东金美化学有限公司 | Method for recycling waste acid |
| 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 |
| CN110066230A (en) * | 2018-08-30 | 2019-07-30 | 内蒙古利元科技有限公司 | A kind of novel sulfonated para-ester production system and technique |
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Open date: 20090715 |