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Removal method of carboxylic acid in aqueous material containing carboxylic acid impurity

A carboxylic acid removal technology, applied in chemical instruments and methods, water pollutants, water/sewage treatment, etc., can solve the problems of low deacidification efficiency, saturation failure of adsorbents, etc., and achieve good technical effects.

Active Publication Date: 2014-12-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is that in the existing deacidification technology, the adsorption method is prone to adsorbent saturation failure, and the esterification deacidification method needs to add alcohol and water when the deacidification efficiency is low.

Method used

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  • Removal method of carboxylic acid in aqueous material containing carboxylic acid impurity
  • Removal method of carboxylic acid in aqueous material containing carboxylic acid impurity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Catalyst preparation

[0028] 1) Add 0.75 mol MgSO 4 and 0.125 mol Al 2 (SO 4 ) 3 Dissolve in 1 L of water to prepare a uniform mixed salt solution; add dropwise sodium carbonate and sodium hydroxide mixed alkali solution (the concentration of sodium carbonate is 2.5 mol / L, and the concentration of sodium hydroxide is 1.25 mol / L, that is, sodium carbonate and hydrogen The molar ratio of sodium oxide is 2), and the pH value of the control reaction solution is 8.5.

[0029] 2) Aging at room temperature for 6 hours, raising the temperature to 130 °C, keeping it for 24 hours, quenching, filtering, washing with deionized water, and drying at 120 °C overnight to obtain a nano-sized magnesium aluminum hydrotalcite precursor.

[0030] 3) Combine step 2) magnesium aluminum hydrotalcite precursor, 2.5 grams of 30wt% silica sol, 116 grams of 42wt% Mg(Ac) 2 Aqueous solution (i.e. 0.35 mol Mg(Ac) 2 , that is, the ratio of step 1) the number of moles of Mg salt in terms of M...

Embodiment 2

[0039] 1. Catalyst preparation

[0040] According to the catalyst preparation steps in Example 1, a cylindrical (length×diameter: 5 mm×2 mm) magnesium-aluminum composite oxide catalyst was still obtained.

[0041] 2. Catalyst evaluation

[0042] Take 5 grams of the above-mentioned catalyst, and investigate its effect on removing carboxylic acid in the raw material in a fixed-bed continuous microreactor.

[0043] Raw material composition: water 50wt%, p-xylene 50wt%; carboxylic acid content 500 ppmw, wherein carboxylic acid is acetic acid.

[0044] Specific investigation conditions: reaction pressure, 0.5 MPa; reaction temperature, 400 °C; raw material mass space velocity, 2 h -1 .

[0045] The amount of residual carboxylic acid in the reaction product was determined by ion chromatography to be 22.5 ppmw.

[0046] For the convenience of comparison, the catalyst composition, raw material composition, reaction pressure, reaction temperature, raw material mass space velocity, ...

Embodiment 3

[0049] 1. Catalyst preparation

[0050] According to the catalyst preparation steps in Example 1, a cylindrical (length×diameter: 5 mm×2 mm) magnesium-aluminum composite oxide catalyst was still obtained.

[0051] 2. Catalyst evaluation

[0052] Take 5 grams of the above-mentioned catalyst, and investigate its effect on removing carboxylic acid in the raw material in a fixed-bed continuous microreactor.

[0053] Raw material composition: water 50wt%, p-xylene 50wt%; carboxylic acid content 500 ppmw, wherein carboxylic acid is acetic acid.

[0054] Specific investigation conditions: reaction pressure, 0.5 MPa; reaction temperature, 500 °C; raw material mass space velocity, 2 h -1 .

[0055] The amount of residual carboxylic acid in the reaction product was determined by ion chromatography to be 18.8 ppmw.

[0056] For the convenience of comparison, the catalyst composition, raw material composition, reaction pressure, reaction temperature, raw material mass space velocity, ...

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Abstract

The invention relates to a removal method of carboxylic acid in aqueous material containing carboxylic acid impurity. The invention mainly solves the problems in the prior art of such as adsorbent saturation and failure in adsorption method, and additional alcohol requirement and low deacidification efficiency when water exists in the esterification method. The method for removing carboxylic acid in aqueous material containing carboxylic acid impurities is as below: the raw materials contact with the catalyst at the reaction temperature of 300-600 DEG C to remove the carboxylic acid impurity; the catalyst comprises a magnesium aluminum composite oxide with the molar ratio of Mg to Al being 1-5, and the magnesium aluminum composite oxide has XRD characteristic peak I at 2 theta of 43 + / - 2 DEG and XRD characteristic peak II at 2 theta of 63 + / - 2 DEG, and the characteristic peak I and the characteristic peak II have peak height ratio of 1-3. The technical scheme solves the technical problems and can be used for removal of impurities in the production of carboxylic acid.

Description

technical field [0001] The present invention relates to the removal of carboxylic acids from aqueous feedstocks containing carboxylic acid impurities. Background technique [0002] At present, there are two most commonly used methods for removing carboxylic acid from reaction materials in industry: the one is adsorption separation method, as Chinese patent CN101054245A discloses a kind of under the condition lower than 100 ℃, utilizes metal chelate resin adsorbent A method for separating and recovering fatty acids in water, but this method has the problem of adsorption saturation when metal chelating resins are used for a long time. The first is the neutralization precipitation method, such as the Chinese patent CN102107985A, which oxidizes the organic oxygen-containing compounds in the waste water to corresponding acids, then neutralizes the acids with calcium oxide or calcium hydroxide to form calcium salt precipitates, and then filters and incinerates the precipitates , ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F1/00B01J21/10C02F101/34
Inventor 姜丽燕孔德金邹薇郑均林管卉周亚新
Owner CHINA PETROLEUM & CHEM CORP
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