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Method for recycling butyric acid by treating butanol and octanol waste lye

A waste lye, adsorption treatment technology, applied in chemical instruments and methods, water/sewage multi-stage treatment, water/sludge/sewage treatment, etc., can solve the problem of low CODCr removal rate, environmental friendliness and economic benefits. , the extraction technology is difficult to achieve the effect and other problems, to achieve the effect of significant environmental and economic benefits, increase product value, and low investment and operation costs

Active Publication Date: 2014-12-24
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that COD Cr Lower removal rate
[0010] Chinese patent CN1530334A adopts acidification heat separation technology to treat octanol waste lye. This method acidifies the waste lye to pH less than 4.5, heats the emulsion formed after acidification to a temperature of 95-100°C, and heats it for less than 0.5h, then statically Set the layers to form the oil-water two-phase. By setting the outlet height of the oil-water two-phase, the two phases can be separated automatically, and the organic phase can be recycled. This method does not need to add an extraction agent, but the COD Cr The removal rate is only about 50%, and the energy consumption is high
However, this process has high infrastructure investment, complex operating conditions, and high operating costs. It is still in the experimental stage and there are no reports of industrial applications.
[0016] Comprehensively analyzing the gains and losses of the above methods, it can be seen that although there are many recycling methods for octanol waste lye at present, and each has its own characteristics, it is still impossible to find a treatment method that is both environmentally friendly and economically beneficial.
Although the acidification method is the simplest and most economical and effective method for removing oily substances in spent octanol lye, it is difficult to recover the high value-added butyric acid in spent lye, and the existing extraction technology is also difficult to achieve the desired effect
And although concentration method and rectification method effect are better, processing cost is high, and the sodium butyrate quality that concentration method reclaims is poor simultaneously, is difficult to purify; Rectification method can only obtain the butyric acid that water content is about 81.4% (mass content) Azeotropic liquid, there is no relevant technical report on further concentration and purification

Method used

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  • Method for recycling butyric acid by treating butanol and octanol waste lye
  • Method for recycling butyric acid by treating butanol and octanol waste lye
  • Method for recycling butyric acid by treating butanol and octanol waste lye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1~5

[0051] Use 98% concentrated sulfuric acid to acidify the waste lye, adopt the method of standing and floating to separate layers, recover the upper organic phase, and measure the COD of the lower acidic water phase Cr . See the specific treatment effect

[0052] Table 1:

[0053] Table 1 Acidification treatment effect of butyl octanol waste lye

[0054]

Embodiment 6

[0056] COD with 30% waste sulfuric acid Cr Acidify the spent lye with a concentration of 104651mg / L. The pH after acidification is 3. After standing and floating for 2 hours, the upper organic phase is recovered, and the COD of the lower acidic aqueous phase is measured. Cr 27137mg / L, COD Cr The removal rate was 74.1%.

Embodiment 7~12

[0058] Use 98% concentrated sulfuric acid for COD Cr Carry out acidification treatment for 104651 mg / L octanol waste lye, adjust pH = 3, adopt static floatation method to stratify for 2 hours, recover the upper organic phase, and the lower acidic water phase enters the resin tower for adsorption treatment, and the adsorption adopts resin tower 3A and resin tower 3B two towers alternate adsorption regeneration operation form (see figure 2 ). The specific treatment effect is shown in Table 2:

[0059] Table 2 Effect of two towers alternate adsorption treatment

[0060]

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Abstract

The invention relates to a method for recycling butyric acid by treating butanol and octanol waste lye. The method comprises the following steps: acidizing butanol and octanol lye through inorganic acid, and recycling an organic phase in the upper layer; absorbing acidic water in the lower layer through a resin tower; when the pH of resin tower acidic outlet water subjected to adsorption treatment is neutralized to be 6 to 9 through lye, and feeding the resin tower acidic outlet water into a sewage treatment plant to be treated or utilizing the resin tower acidic outlet water as acid for neutralization; when resin adsorption is saturated, adsorption is stopped, performing desorption regeneration treatment on the resin, and recycling butyric acid; and performing desorption by virtue of a desorbent flowing back to the resin tower, feeding a desorption solution into a rectifying tower to be subjected to rectification treatment, so as to separate desorbent and coarse butyric acid, recycling the desorbent, and recycling the coarse which serves as a product. The method has the advantages that the CODCr (Chemical Oxygen Demand) of the butanol and octanol waste lye is reduced to lower than 300 mg / L, the total removal rate of CODCr reaches more than 99.0 percent, and treated outlet water can be used as acid for neutralization or can be directly discharged to the sewage treatment plant so as to be subjected to biochemical treatment after being neutralized through alkali, so as to realize up-to-standard release.

Description

technical field [0001] The invention relates to a method for recovering butyric acid from waste lye of butanol and octanol. Background technique [0002] my country's existing butanol production process is mainly propylene oxo synthesis method. In the method, propylene and synthesis gas are used as raw materials to synthesize butyraldehyde, and then the butyraldehyde is condensed under the catalysis of 2% sodium hydroxide to generate octenal. Butyraldehyde and octenal are finally hydrogenated to butanol and octanol. While butyraldehyde is condensed to form octenal, Cannizzaro reaction (Cannizzaro Reaction) also occurs at the same time, and the reaction formulas are as follows: [0003] [0004] 2CH 3 CH 2 CH 2 CHO+NaOH→CH 3 CH 2 CH 2 COONa+CH 3 CH 2 CH 2 OH (2) [0005] As can be seen from the above reaction formula, on the one hand, n-butyraldehyde is condensed to generate octenal while generating equimolar water; on the other hand, sodium hydroxide is consum...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/124C07C51/42C02F9/08
Inventor 马克存杜龙弟张春燕李彩霞王薇李欣王桂芝王斯晗邵正宏胥占风陆野冯成江郭丽娜朱宝莲
Owner PETROCHINA CO LTD
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