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One-step impurity removal method for preparing ammonium sulfate from alkylated waste acid through

A technology of alkylating waste acid and ammonium sulfate, which is applied in the direction of ammonium sulfate, etc., can solve the problems of unable to adsorb and remove the color and odor of ammonium sulfate, easy to block pipes and valves, and reduce product purity, so as to avoid frequent shutdowns The effect of cleaning the pipeline, realizing continuous production and improving production efficiency

Active Publication Date: 2020-06-19
云南云天化石化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of product generation, due to the occlusion and entrainment of ammonium sulfate, other impurities are often added to the ammonium sulfate product, which reduces the purity of the product and has peculiar smell. Only by adding activated carbon to the product, ammonium sulfate cannot be adsorbed and removed. All abnormal colors and odors in the product
[0004] However, the decomposition temperature used in the high-temperature incineration method is too high, and the decomposition temperature of this method is only applicable to ammonium sulfate products whose decomposition temperature is higher than 700°C. For ammonium sulfate products whose decomposition temperature is below 700°C, the high-temperature incineration method cannot be used to remove impurities
[0005] In addition, during the production process, as the product concentration becomes higher and higher, a supersaturated solution is gradually formed, and the entire supersaturated solution is paste-like, which is easy to block pipes and valves

Method used

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  • One-step impurity removal method for preparing ammonium sulfate from alkylated waste acid through
  • One-step impurity removal method for preparing ammonium sulfate from alkylated waste acid through
  • One-step impurity removal method for preparing ammonium sulfate from alkylated waste acid through

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The preparation of embodiment 1 ammonium sulfate sample 1

[0044] 1) add carbon tetrachloride in the neutralization reaction vessel, submerge the bottom of reaction vessel to carbon tetrachloride solution and form the carbon tetrachloride solution layer that thickness is 20mm;

[0045]2) Dilute the alkylated waste acid with an organic content of 10% and add water until the mass concentration of the alkylated waste acid is 30%, to obtain a diluted solution of the spent acid, add the diluted solution of the spent acid to the reaction vessel, and then add 25% of the mass concentration Ammonia, carry out the neutralization reaction at normal temperature and pressure for 15 minutes.

[0046] 3) After the neutralization reaction is completed, add anhydrous methanol solution to the reaction vessel, and add according to the volume ratio of anhydrous methanol solution and waste acid dilution solution at 10:1; after standing for 10 minutes, flow into the centrifuge through the p...

Embodiment 2

[0048] The preparation of embodiment 2 ammonium sulfate sample 2

[0049] 1) Add tetrachlorethylene in the neutralization reaction vessel until the tetrachlorethylene solution submerges the bottom of the reaction vessel and forms a tetrachlorethylene solution layer with a thickness of 30 mm;

[0050] 2) Add water to dilute the alkylated waste acid with an organic content of 13% until the mass concentration of the alkylated waste acid is 30%, to obtain a diluted solution of the spent acid, add the diluted solution of the spent acid to the reaction vessel, and then add 25% of the mass concentration Ammonia, neutralization reaction was carried out at normal temperature and pressure for 10 minutes.

[0051] 3) After the neutralization reaction is completed, add the second extractant solution (mixture of acetone and ethanol in a volume ratio of 1:1) to the reaction vessel, and add it according to the volume ratio of the second extractant solution to the waste acid dilution solution...

Embodiment 3

[0052] The preparation of embodiment 3 ammonium sulfate sample 3

[0053] 1) Add and mix the first extractant (carbon trichloride and chloroform in a volume ratio of 1:1) in the neutralization reaction vessel until the first extractant solution submerges the bottom of the reaction vessel and forms a solution with a thickness of 20-30mm The first extractant solution layer;

[0054] 2) Dilute the alkylation waste acid with an organic content of 10% to 13% with water until the mass concentration of the alkylation waste acid is 30%, to obtain a diluted solution of the spent acid, add the diluted solution of the spent acid to the reaction vessel, and then add the diluted solution with a mass concentration of 25% % ammonia water, carry out the neutralization reaction at normal temperature and pressure for 10 to 15 minutes.

[0055] 3) After the neutralization reaction is completed, add absolute ethanol solution to the reaction vessel, and add according to the volume ratio of absolu...

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Abstract

The invention discloses a one-step impurity removal method for preparing ammonium sulfate from alkylated waste acid, which comprises the following steps: arranging a first extraction agent solution layer with the thickness of 20-30mm at the bottom of a reaction container, sequentially adding a dilute solution of alkylated waste acid and ammonia water, and carrying out neutralization reaction at normal temperature and normal pressure for 10-15 minutes; after the neutralization reaction is finished, and adding a second extraction agent, wherein the addition amount of the second extraction agentmeets the condition that the volume ratio of the second extraction agent to the dilute solution of the alkylated waste acid is 10: 1; and after standing for 10-30 minutes, enabling the mixture to enter a centrifugal machine through a pipeline to be centrifuged to obtain an ammonium sulfate solid, wherein the first extraction agent is selected from at least one of carbon tetrachloride, tetrachloroethylene, carbon trichloride, trichloromethane or dichloromethane. Through organic solvent extraction, different-color and peculiar-smell substances in a waste acid-to-ammonium sulfate product can be thoroughly extracted and separated, and it is ensured that the ammonium sulfate product is not decomposed by heating.

Description

technical field [0001] The application relates to a one-step impurity-removing method for producing ammonium sulfate from alkylated waste acid, which belongs to the field of industrial wastewater treatment and recycling. Background technique [0002] In the existing process, 80-90 kg of waste sulfuric acid with a concentration of 85%-90% is produced for every 1 ton of alkylated oil, and its composition contains 8%-14% of complex organic matter and water in addition to sulfuric acid. The waste sulfuric acid has a high concentration and has a pungent smell, and direct discharge wastes resources and pollutes the environment. [0003] At present, using alkylation waste acid to produce ammonium sulfate products, for the abnormal color and odor in the product, the commonly used treatment methods include high-temperature incineration and activated carbon adsorption. In the process of product generation, due to the occlusion and entrainment of ammonium sulfate, other impurities are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C1/24
CPCC01C1/24
Inventor 杨亚乔钱树伟陈举
Owner 云南云天化石化有限公司
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