CN102951617B - Purifying treatment system and method of waste sulfuric acid - Google Patents
Purifying treatment system and method of waste sulfuric acid Download PDFInfo
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- CN102951617B CN102951617B CN201210398498.2A CN201210398498A CN102951617B CN 102951617 B CN102951617 B CN 102951617B CN 201210398498 A CN201210398498 A CN 201210398498A CN 102951617 B CN102951617 B CN 102951617B
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Abstract
The invention discloses a purifying treatment system and method of waste sulfuric acid. In the method, the purifying treatment system composed of a waste sulfuric acid tank, a sulfuric acid heat exchanger, a stripping tower and a finished product acid storage tank is utilized. The method comprises the following steps of: heating the air, directly contacting the air with the waste sulfuric acid to fully exchange heat to raise the temperature of the waste sulfuric acid to 150-200 DEG C, and performing steam stripping treatment on the waste sulfuric acid to blow out all volatile organic impurities, so that most part of soluble organic impurities and a part of oligomers in the waste sulfuric acid, the rest part of polymerized organic impurities generate a little part of carbon and increase the molecular weights of the polymers to disperse the polymers in the sulfuric acid at a solid state so as to purify the waste sulfuric acid generated in the production process of 1,4-butanediol. By utilizing the system and the method, the problems of high recycling treatment cost and complex technique process of waste sulfuric acid generated in the production process of 1,4-butanediol in the prior art are solved.
Description
Technical field
The invention belongs to chemical technology field, relate to a kind of Waste Sulfuric Acid cleaning treatment system and method.
Background technology
Adopting the Reppe method production 1 of Reppe method or improvement, in the process of 4 butyleneglycols (BDO), need to process and purify with the acetylene gas that sulfuric acid produces calcium carbide, purify Waste Sulfuric Acid after acetylene gas and be stable chocolate thick liquid and with strong impulse smell, after dilution, be brown or light brown, without obvious suspended substance.
Initial analysis purify after acetylene gas sulfuric acid become stablize the former of thick liquid because the vitriol oil in acetylene gas processing, high temperature acetylene gas contacts with the vitriol oil, except sulfuric acid, carry the impurity such as inorganics, also likely produce oxidation and polyreaction with acetylene, carbon black, inorganics that the oxidation of part acetylene produces are carried by the vitriol oil, make the sulfuric acid thickness that becomes, the polymer that polyreaction produces simultaneously is also carried secretly by sulfuric acid, makes the vitriol oil form stable black thick liquid.If directly discharge or discharge after simple neutralizing treatment, will cause great pollution to environment.If directly add phosphoric acid system to use as raw material sulphuric acid it, can cause phosphoric acid system to produce undesired, production environment deterioration, thereby cannot reclaim use.
The Waste Sulfuric Acid treatment process generally adopting both at home and abroad at present mainly contains high temperature pyrolytic cracking (HTP), high-temperature cracking method, oxidation style, extraction process etc., and wherein high-temperature cracking method decomposes Waste Sulfuric Acid SO processed at adopting 900-1100 ℃
2, then through the catalyzed oxidation vitriol oil processed, device input and production cost are higher; Oxidation style is to use oxygenant under suitable condition by the organic impurity oxygenolysis in Waste Sulfuric Acid, make it change carbonic acid gas, water, nitrogen oxide etc. into separates from sulfuric acid, thereby Waste Sulfuric Acid is purified, reclaim, conventional oxygenant has hydrogen peroxide, nitric acid, ozone etc.Extraction process is to utilize organic solvent fully to contact with Waste Sulfuric Acid, make the impurity in spent acid transfer to solvent, its technical requirements is higher, to the selection of extraction agent, requires harsher (if extraction agent is inertia for sulfuric acid,, with sulfuric acid react with, be not insoluble to sulfuric acid yet; Impurity in spent acid has very high partition ratio in extraction agent and sulfuric acid; Easily separated with impurity, during extraction, lose little etc.), and the working cost of extraction process is also higher.
In sum, although having several different methods in prior art can process for Waste Sulfuric Acid, but all there are problems, as installed, drop into and production cost is high, manufacturing requirements is high, working cost is high, complex technical process etc., or only carry out simple end processing (as neutralizing treatment), can cause so again the pollution of environment.
Summary of the invention
The object of this invention is to provide a kind of Waste Sulfuric Acid cleaning treatment system and method, solved in prior art producing the recycling input cost of the Waste Sulfuric Acid producing in the process of Isosorbide-5-Nitrae butyleneglycol high, the problem of complex technical process.
The technical solution adopted in the present invention is that a kind of Waste Sulfuric Acid cleaning treatment system, comprises sulfur waste acid tank, Heat Exchanger for Sulphuric Acid Plant, stripping tower and finished acid storage tank; The blast inlet of stripping tower is connected with calorifier by hot air duct, and the acid inlet of stripping tower is connected with Heat Exchanger for Sulphuric Acid Plant by reflux line; The acid inlet on Heat Exchanger for Sulphuric Acid Plant top is connected with the acid mouth of stripping tower bottom by hot acid pipeline, and the spent acid entrance of Heat Exchanger for Sulphuric Acid Plant bottom is connected with sulfur waste acid tank by pipeline, between Heat Exchanger for Sulphuric Acid Plant and sulfur waste acid tank by being provided with pump; The acid mouth of Heat Exchanger for Sulphuric Acid Plant bottom is connected with finished acid storage tank by cold acid tube road.
Another technical scheme of the present invention is, a kind of Waste Sulfuric Acid purifying treatment method is specifically implemented according to following steps:
Step 1, by the Waste Sulfuric Acid in sulfur waste acid tank by pump delivery to Heat Exchanger for Sulphuric Acid Plant, then by pipeline, deliver to stripping tower inside, with calorifier, by pipeline, be that stripping tower passes into and adds warm air simultaneously;
Step 2 arrives 150-200 ℃ through warm air beating by Waste Sulfuric Acid in stripping tower, and be 1-3 hour heat-up time, and the sulfuric acid after purification is delivered to Heat Exchanger for Sulphuric Acid Plant;
Step 3 is carried out heat exchange with the Waste Sulfuric Acid in sulfur waste acid tank input Heat Exchanger for Sulphuric Acid Plant by purifying the sulfuric acid obtaining in step 2 in Heat Exchanger for Sulphuric Acid Plant, obtains cooling sulfuric acid;
Step 4, stores being delivered to finished acid storage tank through overcooled sulfuric acid in step 3.
The invention has the beneficial effects as follows, adopt present method can solve prior art high to the recycling input cost of the Waste Sulfuric Acid producing in the process of process for producing Isosorbide-5-Nitrae butyleneglycol, the problem of complex technical process.Simultaneously, present method technical requirements is relatively low, can realize economically heavy industrialization, the requirement of equipment material is reduced, device input and production cost are lower, have reduced working cost, both can greatly alleviate environmental pollution, recyclable sulfuric acid resource, has great economic benefit and environmental benefit again.
Accompanying drawing explanation
Fig. 1 is the cleaning treatment system of a kind of Waste Sulfuric Acid of the present invention and the structural representation of method.
In figure, 1. sulfur waste acid tank, 2. Heat Exchanger for Sulphuric Acid Plant, 3. stripping tower, 4. finished acid storage tank, 5. hot air duct, 6. calorifier, 7. reflux line, 8. hot acid pipeline, 9. cold acid tube road, 10. pump.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
A kind of Waste Sulfuric Acid cleaning treatment system of the present invention, its structure as shown in Figure 1, comprises sulfur waste acid tank 1, Heat Exchanger for Sulphuric Acid Plant 2, stripping tower 3 and finished acid storage tank 4; The blast inlet of stripping tower 3 is connected with calorifier 6 by hot air duct 5, and the acid inlet of stripping tower 3 is connected with Heat Exchanger for Sulphuric Acid Plant 2 by reflux line 7; The acid inlet on Heat Exchanger for Sulphuric Acid Plant 2 tops is connected with the acid mouth of stripping tower 3 bottoms by hot acid pipeline 8, and the spent acid entrance of Heat Exchanger for Sulphuric Acid Plant 2 bottoms is connected with sulfur waste acid tank 1 by pipeline, between Heat Exchanger for Sulphuric Acid Plant 2 and sulfur waste acid tank 1 by being provided with pump 10; The acid mouth of Heat Exchanger for Sulphuric Acid Plant 2 bottoms is connected with finished acid storage tank 4 by cold acid tube road 9.
A kind of Waste Sulfuric Acid purifying treatment method of the present invention, specifically according to following steps, implement:
Step 1, is delivered to the Waste Sulfuric Acid in sulfur waste acid tank 1 in Heat Exchanger for Sulphuric Acid Plant 2 by pump 9, then by pipeline, delivers to stripping tower 3 inside;
With calorifier 6, by pipeline, be that stripping tower passes into and adds warm air simultaneously;
Step 2 arrives 150-200 ℃ through warm air beating by Waste Sulfuric Acid in stripping tower 3, and be 1-3 hour heat-up time, and the sulfuric acid after purification is delivered to Heat Exchanger for Sulphuric Acid Plant 2;
Step 3 is carried out heat exchange with the Waste Sulfuric Acid in sulfur waste acid tank 1 input Heat Exchanger for Sulphuric Acid Plant 2 by purifying the sulfuric acid obtaining in step 2 in Heat Exchanger for Sulphuric Acid Plant 2, obtains cooling sulfuric acid;
Step 4, stores being delivered to finished acid storage tank through overcooled sulfuric acid in step 3.
Embodiment 1
By the Waste Sulfuric Acid in sulfur waste acid tank by pump delivery to Heat Exchanger for Sulphuric Acid Plant, then by pipeline, deliver to stripping tower inside; With calorifier, by pipeline, be that stripping tower passes into and adds warm air simultaneously; By Waste Sulfuric Acid in stripping tower through warm air beating to 150 ℃, be 1 hour heat-up time, the sulfuric acid after purification is delivered to Heat Exchanger for Sulphuric Acid Plant 2; The sulfuric acid that purification is obtained carries out heat exchange with the Waste Sulfuric Acid in sulfur waste acid tank input Heat Exchanger for Sulphuric Acid Plant in Heat Exchanger for Sulphuric Acid Plant, obtains cooling sulfuric acid; To be delivered to finished acid storage tank through overcooled sulfuric acid stores.
Embodiment 2
By the Waste Sulfuric Acid in sulfur waste acid tank by pump delivery to Heat Exchanger for Sulphuric Acid Plant, then by pipeline, deliver to stripping tower inside; With calorifier, by pipeline, be that stripping tower passes into and adds warm air simultaneously; By Waste Sulfuric Acid in stripping tower through warm air beating to 175 ℃, be 1.5 hours heat-up time, the sulfuric acid after purification is delivered to Heat Exchanger for Sulphuric Acid Plant; The sulfuric acid that purification is obtained carries out heat exchange with the Waste Sulfuric Acid in sulfur waste acid tank input Heat Exchanger for Sulphuric Acid Plant in Heat Exchanger for Sulphuric Acid Plant, obtains cooling sulfuric acid; To be delivered to finished acid storage tank through overcooled sulfuric acid stores.
Embodiment 3
By the Waste Sulfuric Acid in sulfur waste acid tank by pump delivery to Heat Exchanger for Sulphuric Acid Plant, then by pipeline, deliver to stripping tower inside; With calorifier, by pipeline, be that stripping tower passes into and adds warm air simultaneously; By Waste Sulfuric Acid in stripping tower through warm air beating to 200 ℃, be 2 hours heat-up time, then the sulfuric acid after purifying is delivered to Heat Exchanger for Sulphuric Acid Plant; The sulfuric acid that purification is obtained carries out heat exchange with the Waste Sulfuric Acid in sulfur waste acid tank input Heat Exchanger for Sulphuric Acid Plant in Heat Exchanger for Sulphuric Acid Plant, obtains cooling sulfuric acid; Then will be delivered to finished acid storage tank through overcooled sulfuric acid stores.
Utilize a kind of Waste Sulfuric Acid cleaning treatment system of the present invention and method to producing 1, the Waste Sulfuric Acid producing in the process of 4 butyleneglycols carries out after purifying treatment, the sulfuric acid obtaining is from outward appearance, acid look front without considerable change with processing, before processing, spent acid color is brown, sulfuric acid after processing is black, but sulfuric acid after purifying has been eliminated strong impulse smell.
The index analysis result of Waste Sulfuric Acid before and after purifying is as shown in table 1:
| Analysis project | Acid dense (%) | Ash content (%) | Solid content (%) | Fe（%） | As（%） |
| Spent acid before purifying | 90～92 | 0.2～0.4 | 0～0.02 | 0.014～0.023 | 0.0002 |
| Sulfuric acid after purifying | 90～92 | 0.2～0.8 | 1～2 | 0.028 | 0.0001～0.0002 |
Table 1
Sulfuric acid after purification is as the raw material sulphuric acid of phosphoric acid production, and production system is used extracting system, the filtering system leading indicator of front and back to contrast situation as shown in table 2 and table 3:
Table 2
Table 3
Adopt the inventive method can solve prior art high to the recycling input cost of the Waste Sulfuric Acid producing in the process of process for producing Isosorbide-5-Nitrae butyleneglycol, the problem of complex technical process.Simultaneously, the inventive method technical requirements is relatively low, can realize economically heavy industrialization, the requirement of equipment material is reduced, device input and production cost are lower, have reduced working cost, both can greatly alleviate environmental pollution, recyclable sulfuric acid resource, has great economic benefit and environmental benefit again.Utilize the BDO Waste Sulfuric Acid of the inventive method purifying treatment, can be used as the raw material sulphuric acid of phosphoric acid production with certified products sulfuric acid after according to certain ratio blending completely, can't cause disadvantageous effect to the production environment of phosphoric acid system and state of arts.
Claims (1)
1. a Waste Sulfuric Acid purifying treatment method, is characterized in that, based on a kind of Waste Sulfuric Acid cleaning treatment system,
Comprise sulfur waste acid tank (1), Heat Exchanger for Sulphuric Acid Plant (2), stripping tower (3) and finished acid storage tank (4);
The blast inlet of described stripping tower (3) is connected with calorifier (6) by hot air duct (5), and the acid inlet of described stripping tower (3) is connected with Heat Exchanger for Sulphuric Acid Plant (2) by reflux line (7);
The acid inlet on described Heat Exchanger for Sulphuric Acid Plant (2) top is connected with the acid mouth of stripping tower (3) bottom by hot acid pipeline (8), the spent acid entrance of described Heat Exchanger for Sulphuric Acid Plant (2) bottom is connected with described sulfur waste acid tank (1) by pipeline, between described Heat Exchanger for Sulphuric Acid Plant (2) and described sulfur waste acid tank (1) by being provided with pump (10);
The acid mouth of described Heat Exchanger for Sulphuric Acid Plant (2) bottom is connected with finished acid storage tank (4) by cold acid tube road (9);
Specifically according to following steps, implement:
Step 1, is delivered to the Waste Sulfuric Acid in sulfur waste acid tank (1) in Heat Exchanger for Sulphuric Acid Plant (2) by pump (10), and then delivers to stripping tower (3) inside by pipeline;
Use calorifier (6) is that stripping tower passes into and adds warm air by pipeline simultaneously;
Step 2 arrives 150-200 ℃ through warm air beating by Waste Sulfuric Acid in stripping tower (3), and be 1-3 hour heat-up time, and the sulfuric acid after purification is delivered to Heat Exchanger for Sulphuric Acid Plant (2);
Step 3 is carried out heat exchange with the Waste Sulfuric Acid in sulfur waste acid tank (1) input Heat Exchanger for Sulphuric Acid Plant (2) by purifying the sulfuric acid obtaining in step 2 in Heat Exchanger for Sulphuric Acid Plant (2), obtains cooling sulfuric acid;
Step 4, stores being delivered to finished acid storage tank through overcooled sulfuric acid in step 3.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210398498.2A CN102951617B (en) | 2012-10-18 | 2012-10-18 | Purifying treatment system and method of waste sulfuric acid |
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| CN201210398498.2A CN102951617B (en) | 2012-10-18 | 2012-10-18 | Purifying treatment system and method of waste sulfuric acid |
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| CN102951617A CN102951617A (en) | 2013-03-06 |
| CN102951617B true CN102951617B (en) | 2014-10-22 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104627967A (en) * | 2013-11-13 | 2015-05-20 | 雷永诚 | System and method of normal temperature recovery of waste sulfuric acid |
| CN103570081B (en) * | 2013-11-18 | 2015-05-06 | 南通宝聚颜料有限公司 | Titanium dioxide waste acid recycling and processing system |
| CN108069406B (en) * | 2016-11-15 | 2019-12-13 | 中国石油化工股份有限公司 | Regeneration method of alkylation waste sulfuric acid |
| CN107201527A (en) * | 2017-06-07 | 2017-09-26 | 浙江康盛股份有限公司 | A kind of hydrochloric acid pickler mode of heating |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094013A (en) * | 1993-03-15 | 1994-10-26 | 气体产品与化学公司 | Sulfuric acid purifying and concentration technology |
| CN101607700A (en) * | 2008-06-20 | 2009-12-23 | 南通江山农药化工股份有限公司 | Process for recycling waste sulfuric acid as byproduct of trichloroacetaldehyde |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094013A (en) * | 1993-03-15 | 1994-10-26 | 气体产品与化学公司 | Sulfuric acid purifying and concentration technology |
| CN101607700A (en) * | 2008-06-20 | 2009-12-23 | 南通江山农药化工股份有限公司 | Process for recycling waste sulfuric acid as byproduct of trichloroacetaldehyde |
Non-Patent Citations (2)
| Title |
|---|
| 钽材换热器及玻璃设备在废硫酸浓缩中的应用;雷馨;《硫磷设计与粉体工程》;20120331(第2期);24-27 * |
| 雷馨.钽材换热器及玻璃设备在废硫酸浓缩中的应用.《硫磷设计与粉体工程》.2012,(第2期),24-27. |
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