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Method for performing regenerating treatment on alkylated waste sulfuric acid

A technology for alkylating waste sulfuric acid and treatment methods, which is applied in the direction of sulfur trioxide/sulfuric acid, chemical instruments and methods, ferric sulfate, etc., can solve the problems of high equipment maintenance cost, difficult to handle, and waste residue that cannot be handled, and achieve good results Environmental benefits and economic benefits, the realization of resource recycling, the effect of low sulfuric acid reduction decomposition rate

Pending Publication Date: 2019-12-10
3R ENVIRONMENTAL TECH CO LTD
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  • Abstract
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  • Claims
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Problems solved by technology

[0004] The freeze crystallization method uses frozen isobutane to contact waste sulfuric acid countercurrently to crystallize and separate the sulfuric acid, but the filtrate obtained by this method has complex components and high acid ester content, which is difficult to handle; although the solvent extraction method can make the alkylated acid The consumption is reduced by 65% ​​to 75%, but the solvent loss is large and the regeneration cost is high
The method of producing ammonium sulfate and phosphate fertilizer is to dilute, separate, deodorize, and neutralize the alkylated waste sulfuric acid to obtain phosphate fertilizer, but the separation effect of organic matter is poor, the fertilizer efficiency is not high, and there is a large amount of waste residue that cannot be processed
The high-temperature cracking method cracks waste sulfuric acid at a high temperature of 1000°C to 1100°C, and then produces qualified sulfuric acid products through washing, contact conversion and absorption, but the process is complicated, high energy consumption, large investment, and equipment maintenance costs are relatively high high
Although the method of producing white carbon black and petroleum antirust agent is relatively thorough in the treatment of waste sulfuric acid, the process route is complicated and the product market is very general, which is gradually replaced by the alkylation regeneration process technology
The oxidation method uses a strong oxidant to oxidize the reducing substances of the alkylated waste sulfuric acid to realize the regeneration of the alkylated waste sulfuric acid. This method requires a large amount of oxidant, and the cost is high. Nitric acid oxidation will also produce nitrogen oxide pollution.
In short, the current regeneration technology of alkylation waste sulfuric acid is complicated and the production cost is high

Method used

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  • Method for performing regenerating treatment on alkylated waste sulfuric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 100 g of alkylated waste sulfuric acid into a three-necked flask with a capacity of 500 ml, heat up to a temperature of 150° C. for 30 min, stop heating and lower the temperature. Add 100g of clear water to the reactor for stirring and washing, the stirring speed is 100r / min, and the stirring time is 30min, filter off the solution, and repeatedly wash with clear water to neutral filtrate. Carry out oxidation treatment to brown waste sulfuric acid filtrate, adopt mass fraction to be 30% hydrogen peroxide as oxidant, its addition is 3% of waste sulfuric acid mass, be 80 ℃ at reaction temperature, reaction time is under the condition of 30min, make waste sulfuric acid filtrate It is treated as colorless and transparent regenerated sulfuric acid. The tail gas produced by the reaction is absorbed by the first-level absorption liquid as a ferrous sulfate solution with a ferrous iron content of 7% and the second-level absorption liquid with a mass fraction of 15% sodium hy...

Embodiment 2

[0037] Add 100 g of alkylated waste sulfuric acid into a three-necked flask with a capacity of 500 ml, heat up to a temperature of 200° C. for 5 min, stop heating and lower the temperature. Add 100g of clear water to the reactor for stirring and washing, the stirring speed is 300r / min, and the stirring time is 30min, filter off the solution, and repeatedly wash with clear water to neutral filtrate. The brown waste sulfuric acid filtrate is oxidized, and the mass fraction is 30% hydrogen peroxide as the oxidant, and its addition is 1% of the waste sulfuric acid mass. At a reaction temperature of 100°C and a reaction time of 60 minutes, the waste sulfuric acid filtrate is It is treated as colorless and transparent regenerated sulfuric acid. The tail gas produced by the reaction is absorbed by the first-level absorption liquid as a ferrous sulfate solution with a ferrous iron content of 9% and the second-level absorption liquid with a mass fraction of 20% sodium hydroxide solutio...

Embodiment 3

[0039] Add 100 g of alkylated waste sulfuric acid into a three-necked flask with a capacity of 500 ml, heat up to a temperature of 175° C. for 15 minutes, stop heating and lower the temperature. Add 100g of clear water to the reactor for stirring and washing, the stirring speed is 200r / min, and the stirring time is 30min, filter the solution, and repeatedly use clear water to neutralize the filtrate. Carry out oxidation treatment to brown waste sulfuric acid filtrate, adopt the hydrogen peroxide of mass fraction 30% as oxidant, its addition is 2% of waste sulfuric acid mass, be 90 ℃ at reaction temperature, reaction time is under the condition of 50min, make waste sulfuric acid filtrate It is treated as colorless and transparent regenerated sulfuric acid. The tail gas produced by the reaction is absorbed by the first-level absorption liquid as ferrous sulfate solution with a ferrous iron content of 8% and the second-level absorption liquid with a mass fraction of 18% sodium hy...

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Abstract

The invention relates to a method for performing regenerating treatment on alkylated waste sulfuric acid. The method for performing regenerating treatment on the alkylated waste sulfuric acid comprises the following steps: sequentially heating and carbonizing, washing, filtering and oxidizing the alkylated waste sulfuric acid to obtain regenerated sulfuric acid, performing absorbing treatment on tail gas generated through carbonizing treatment of the alkylated waste sulfuric acid by a ferrous sulfate solution and liquid caustic soda, wherein the absorbing liquid serving as a raw material is used for producing a polyferric sulfate water purifying agent; and filter residues generated through carbonizing, washing and filtering treatment of the alkylated waste sulfuric acid are used for processing and preparing fuel or activated carbon products. The method provided by the invention has the advantages of simple process, mild reaction condition, high organic matter removal rate, low treatment cost and the like; and harmless regeneration of the alkylated waste sulfuric acid is realized, waste is changed into treasures, the environmental hazard problem is solved and good economic benefit is achieved.

Description

technical field [0001] The invention relates to the technical field of regeneration treatment methods for waste sulfuric acid, in particular to a regeneration treatment method for alkylation waste sulfuric acid. Background technique [0002] At present, in the process of petroleum refining, concentrated sulfuric acid is generally used as a catalyst to produce high-octane alkylate oil. During the alkylation reaction process, as impurities such as moisture in raw materials and side reaction products are continuously incorporated into the concentrated sulfuric acid catalyst, the concentration of sulfuric acid gradually decreases. When the concentration of concentrated sulfuric acid is lower than 90%, it is discharged as waste acid to form alkylation waste. sulfuric acid. About 80kg-100kg of waste sulfuric acid is produced for every ton of alkylated oil produced, the concentration of sulfuric acid is about 85%-90%, and the rest is organic polymers and a small amount of water. O...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/92C01G49/14C02F1/52C10L5/48C01B32/324
CPCC01B17/92C01G49/14C02F1/5245C10L5/48C01B32/324Y02E50/30
Inventor 吴勇基丁德才王权永陈小哲赵英武关志红朱浩
Owner 3R ENVIRONMENTAL TECH CO LTD
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