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Method for intensified neutral oil removal of diesel alkaline residue and stepwise reclamation of naphthenic acids and phenols

A neutral oil and naphthenic acid technology, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid compounds, etc., can solve the problems of low utilization rate of raw materials, low product purity, low deoiling rate, etc. problem, to achieve the effect of rapid and thorough deoiling, improved purity and remarkable effect

Inactive Publication Date: 2011-03-16
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the disadvantages of high energy consumption, low raw material utilization rate, low deoiling rate and low product purity in the existing process, the present invention proposes a high-efficiency and energy-saving method. Sexual oil; acidification control pH value step-by-step separation and recovery of naphthenic acid and phenol

Method used

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  • Method for intensified neutral oil removal of diesel alkaline residue and stepwise reclamation of naphthenic acids and phenols
  • Method for intensified neutral oil removal of diesel alkaline residue and stepwise reclamation of naphthenic acids and phenols

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Effect test

Embodiment 1

[0016] Diesel soda residue contains 10% oil, 13% naphthenic acid, 5% creosote and 336700mg / l COD.

[0017] 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. Add sulfuric acid dropwise to control the pH value at 7.0, and stand for 2 hours to break the demulsification and stratify , to separate waste alkaline water and diesel oil. Control the temperature of the waste alkaline water in a water bath. When the waste alkaline water reaches 60°C, add 1 mol / L sulfuric acid dropwise to control the pH value at 5.5, stir for 0.5 hours at a stirring speed of 500 r / min, and stand in a separating funnel for 2 hours to recover phenol , add sulfuric acid in the same way to control the pH value at 3.5, let stand for 2 hours to recover naphthenic acid, and separate the water phase.

Embodiment 2

[0019] Diesel soda residue contains 10% oil, 13% naphthenic acid, 5% creosote and 336700mg / l COD.

[0020] 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 0.01% and 60% of the weight of the soda slag respectively. Add sulfuric acid dropwise to control the pH value at 7.0, and let it stand for 2 hours to break the demulsification and stratify , to separate waste alkaline water and diesel oil. Control the temperature of the waste alkaline water in a water bath. When the waste alkaline water reaches 55°C, add 1 mol / L sulfuric acid dropwise to control the pH value at 5. Stir for 0.5 hours at a stirring speed of 500 r / min. Stand still in a separatory funnel for 2.5 hours to recover Phenol, add sulfuric acid in the same way to control the pH value at 3, let it stand for 2.5 hours to recover naphthenic acid, and separate the water phase.

Embodiment 3

[0022] Diesel soda residue contains 10% oil, 13% naphthenic acid, 5% creosote and 336700mg / l COD.

[0023] 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 0.01% and 60% of the weight of the soda slag respectively. Add sulfuric acid dropwise to control the pH value at 8.0, and let it stand for 2 hours to break the demulsification and stratify , to separate waste alkaline water and diesel oil. Control the temperature of the waste alkaline water in a water bath, and when the waste alkaline water reaches 60°C, add 1 mol / L sulfuric acid dropwise to control the pH value at 4, stir for 0.5 hours at a stirring speed of 500 r / min, and stand in a separatory funnel for 2.5 hours to recover Phenol, use the same method to add sulfuric acid to control the pH value at 2, let it stand for 2.5 hours to recover naphthenic acid, and separate the water phase.

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Abstract

The invention discloses a method for reclaiming naphthenic acid and hydroxybenzene in steps from diesel oil alkaline residue, solves the disadvantages that the use ratio of raw material, the deoiling ratio and product purity are low, and provides a highly effective and energy-saving method to produce a high-purity product. The invention comprises: controlling the temperature at 50-100 degree C, emulsion breaking of the diesel oil alkaline residue by using polymerization-type emulsion breaker, mirabilite and sulfuric acid and by heat method, wherein the dosages of emulsion breaker, and mirabilite are 0. 003 03and 10% by weight of alkaline residue respectively, adding 1mol / L sulfuric acid to control the pH value between 6-10, stewing for 0. 5-6h to break emulsion and values stratify, and separating out alkali waste water and diesel oil; adding 1mol / L sulfuric acid to the alkali waste water, acidizing and stirring, controlling the temperature at 50-80 degree C, controlling the pH value at 4-6, stewing for 1-8h, dissociating and reclaiming hydroxybenzene, then acidizing with a pH value from 2 to 4, stewing for 1-8h, and dissociating and reclaiming naphthenic acid.

Description

technical field [0001] The invention relates to a method for strengthening deneutral oil by diesel alkali slag and recovering naphthenic acid and phenol step by step. 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. The naphthenic saline in alkali slag is a strong emulsifier, if it is not properly treated and recovered, it will affect the subsequent treatment. Therefore, naphthenic acid must be extracted from alkali residue. [0003] In order to improve the purity and yield of recovered naphthenic acid, the neutral oil in the alkali residue must be removed to reduce the oil content in the alkali residue and prepare for the recovery of naphthenic acid in the next acidification reaction. Demulsification treatment can be carried out to eliminate or reduce the sol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/42C07C51/02C07C61/00C07C37/68C07C39/00
Inventor 曹成波唐文
Owner SHANDONG UNIV