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Method for recovery of organic acid from dilute aqueous solution

A technology of organic acid and aqueous solution, applied in the field of separation and recovery of one or more organic acids, to achieve the effect of high carboxylic acid yield

Inactive Publication Date: 2013-12-04
KEMIRA OY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0018] A further problem is the separation of mixtures of organic acids from dilute aqueous solutions

Method used

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  • Method for recovery of organic acid from dilute aqueous solution
  • Method for recovery of organic acid from dilute aqueous solution
  • Method for recovery of organic acid from dilute aqueous solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] The boiling points of the free acid and methyl ester forms of selected water-soluble C1-C5 carboxylic acids are depicted in Table 1 for the pure compounds. At atmospheric pressure, the boiling point interval within the mixture is 84°C for the free acid form and 95°C for the methyl ester form, indicating the greater separation achievable for the latter group. Acid recovery in the methyl ester form was achieved at lower temperatures and with better separation compared to recovery of the free acid form, even without complexation with the extractant.

[0073] This is evidence for a significantly more energetically favorable recovery of acid in the ester form compared to the recovery of the acid form.

[0074] Table 1

[0075] sour

Embodiment 2-5

[0077] extract

[0078] The Scheibel column was filled with an aqueous solution containing 3.5 wt-% formic acid (Kemira) from the top of the column at a rate of 3.93 kg / h. Cyanex 932 (Cytec) solution was fed to the bottom of the column at a rate of 0.998 kg / h. The stirring speed was 350 rpm, and the column temperature range was 25-28°C. The extraction solution was separated and withdrawn from the column at a rate of 1.08 kg / h. In Cyanex 923, it contains 9.9 wt-% formic acid (in pure form) and 3.4 wt-% water. The recovery rate of formic acid in Cyanex923 was 78%.

[0079] Esterification

[0080] In a glass reactor heated with circulating silicone oil, 500.23 g of the resulting extraction solution were mixed with 105.73 g of methanol. The reactor was equipped with a fractionation column with structured packing and a cooler with isopropanol. The solution was warmed to 70°C with continuous mixing at ambient pressure. The distillate containing methyl formate in methanol was ...

Embodiment 3

[0092] extract

[0093] Similar to Example 2, the extraction was carried out.

[0094] The extraction solution coming out of the column contained 9.0 wt-% formic acid (in pure form) and 3.1 wt-% water in Cyanex 923.

[0095] Esterification

[0096] Similar to Example 2, 500.00 g of the obtained extraction solution was mixed with 96.0 g of methanol. The solution was warmed to 90°C at ambient pressure with continuous mixing. A distillate containing methyl formate in methanol was collected and more methanol was gradually introduced into the reactor below the liquid level. Keep the solution at about 90°C and continue the distillation until a distillate is obtained.

[0097] The consumption of methanol was recorded and the formation of methyl formate was quantified using GC both from the distillate and from the distillation bottoms. Table 4 shows the homogeneous quality of the distillate and Table 5 shows the final results.

[0098] Table 4

[0099]

[0100] table 5

[0...

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Abstract

The present invention relates to a method and an arrangement for recovery of at least one organic acid from a dilute aqueous solution thereof. In this method a complex between said organic acid and an extractant is formed by contacting the solution with a reactive extractant and dissolving the formed complex into said extractant thus forming an extractant phase. The organic acid is removed from the formed complex by esterification using an alcohol.

Description

field of invention [0001] The present invention relates to a method for separating and recovering one or more organic acids from aqueous solutions low in organic acids. In particular, the method of the invention relates to the separation of pure carboxylic acids from dilute aqueous solutions. Background of the invention [0002] Several industrial-scale processes are known to produce dilute wastewater solutions containing low levels of carboxylic acids. Recovery of these acid components is becoming increasingly important for environmental reasons. Recovery of these economically valuable by-products is typically by distillation or extractive distillation, which are efficient but energy-intensive and technically challenging processes because it forms azeotropes or stable emulsions that make Processing is uneconomical or provides the product in an undesired form, eg a solution that is too dilute to be used in further processes. [0003] In many cases, carboxylic acids produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/04C07C51/48C07C67/08
CPCC07C51/493B01D11/0434B01D11/0492B01D11/043C07C53/02C07C53/08
Inventor E·蒂洛宁J·海塔拉R·阿克塞拉
Owner KEMIRA OY
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