Technique for comprehensive treatment of diesel oil alkaline residue by using circulating technology

A comprehensive treatment and diesel oil technology, applied in the petroleum industry, refining with alkaline aqueous solution, preparation of organic compounds, etc., can solve the problems of low product purity, low raw material utilization rate, high energy consumption, etc., to improve economic benefits, The effect of high product quality and improved yield

Inactive Publication Date: 2008-09-03
SHANDONG UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0011] In order to solve the shortcomings of the traditional process such as high energy consumption, low raw material utilization rate, and low purity of the obtained product, the present invention provides a comprehensive treatment and utilization technology of diesel alkali residue. The process mainly includes: synergistic method to quickly and completely remove neutral oil; Acidification to control the pH value, separate and recover naphthenic acid and phenol step by step; the waste liquid is prepared into alkali washing solution and the recovered Glauber's salt is reused as demulsifier

Method used

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  • Technique for comprehensive treatment of diesel oil alkaline residue by using circulating technology

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Effect test

Embodiment 1

[0034] Diesel soda residue contains 10% oil, 13% naphthenic acid, 5% creosote and 336700mg / l COD.

[0035] Add high-efficiency polymeric demulsifier, Glauber's salt and sulfuric acid to the diesel soda slag, the amount of demulsifier and Glauber's salt is 0.012% and 50% of the weight of the soda slag respectively, control the pH value at 7.0, stand for 2 hours to demulsify and separate Waste alkaline water and diesel oil. Control the temperature in a water bath, add 1 mol / L sulfuric acid to control the pH value at 5 when the waste alkaline water reaches 60°C, stir for 0.5 hours at a stirring speed of 500r / min, let stand in the separatory funnel for 2.5 hours to recover phenol, and use the same method Add 1 mol / L sulfuric acid to control the pH value at 3, let it stand for 2.5 hours to recover naphthenic acid, and separate the water phase. The aqueous phase is neutralized to neutral by adding NaOH, concentrated, cooled to 15°C, crystallized and filtered to obtain Glauber’s sal...

Embodiment 2

[0037] Diesel soda residue contains 10% oil, 13% naphthenic acid, 5% creosote and 336700mg / l COD.

[0038] Add high-efficiency polymeric demulsifier, Glauber's salt and sulfuric acid to the diesel soda slag, the amount of demulsifier and Glauber's salt is 0.010% and 60% of the weight of the soda slag respectively, control the pH value at 7.0, stand for 2 hours to demulsify and separate Waste alkaline water and diesel oil. Control the temperature in a water bath, add 1mol / L sulfuric acid to control the pH value at 6 when the waste alkaline water reaches 55°C, stir for 0.5 hours at a stirring speed of 500r / min, and let stand in a separatory funnel for 2.5 hours to recover phenol, use the same method Add 1 mol / L sulfuric acid to control the pH value at 4, let it stand for 2.5 hours to recover naphthenic acid, and separate the water phase. The aqueous phase is neutralized to neutral by adding NaOH, concentrated, cooled to 15°C, crystallized and filtered to obtain Glauber’s salt, ...

Embodiment 3

[0040] Diesel soda residue contains 10% oil, 13% naphthenic acid, 5% creosote and 336700mg / l COD.

[0041] Add high-efficiency polymeric demulsifier, Glauber's salt and sulfuric acid to the diesel soda slag, the amount of demulsifier and Glauber's salt is 0.015% and 70% of the weight of the soda slag respectively, control the pH value at 8.0, stand for 2 hours to demulsify and separate Waste alkaline water and diesel oil. Control the temperature in a water bath, add 1 mol / L sulfuric acid to control the pH value at 4 when the waste alkaline water reaches 50°C, stir for 0.5 hours at a stirring speed of 500r / min, let stand in a separatory funnel for 2.5 hours to recover phenol, and use the same method Add 1 mol / L sulfuric acid to control the pH value at 2, let stand for 2.5 hours to recover naphthenic acid, and separate the water phase. The aqueous phase is neutralized to neutral by adding NaOH, concentrated, cooled to 15°C, crystallized and filtered to obtain Glauber’s salt, wh...

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Abstract

The invention discloses a comprehensive processing alkaline residue of diesel oil by circulation technology, which solves conventional process's shortcomings of low raw material utilization, high cost, and provides a highly efficient energy saving process. The process includes steps of: water-bathing with temperature controlled in 50-100 DEG C, demulsifying with highly effective polymerized demulsifying agent for alkaline residue, mirabilite, vitriol assisted by thermal method, demulsifying agent and mirabilite has a weight of 0.003%-0.03% and 10%-80% of alkaline residue respectively, standing for 5-6 hours for stratification to separate alkali waste water and diesel oil, adding vitriol to alkali waste water for acidizing, controlling temperature between 50 DEG C and 80 DEG C, and pH value between 4-6, standing for 1 and 8 hours to recycle phenol, acidizing to reach pH value of 2-4, standing for 1-8 hours to recycle naphthenic acid, obtaining mirabilite from waste alkali water after condensing and cooling to 10-30 DEG C for crystallization, which is recycling used, adding 1-5ppm polyacrylamide into waste alkali water after crystallization, and adding NaOH to prepare alkaline wash liquor to be cycled in alkaline wash process of diesel.

Description

technical field [0001] The invention relates to a process for comprehensively treating diesel soda slag by using a circulation technology. Background technique [0002] Diesel soda residue generally contains free alkali, oil, naphthenic acid and phenol, among which naphthenic acid is an organic acid, which accounts for the main part of petroleum acid, and is also a valuable fine chemical raw material, which is widely used in the synthesis of Rubber, petroleum product additives, paint driers, surfactants, antiseptics, plasticizers, rare earth metal extractants, plant growth promoters and corrosion inhibitors, etc. In addition, it is also used in food, metallurgy, machinery manufacturing, paint and dye industry, agriculture and construction. The content of naphthenic acid in diesel soda residue is relatively high, if it is recycled, it will definitely improve the overall economic benefits of petrochemical industry. [0003] The naphthenic saline in the alkali slag is a stron...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G19/02C10G19/08C10G33/00C07C61/06C07C37/68
Inventor 曹成波
Owner SHANDONG UNIV
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