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Method for recovering organic acid and inorganic salt from oxidized and saponified cyclohexane waste lye

A technology of waste lye and organic acid, which is applied in the recycling process of cyclohexane waste lye, can solve the problems of unsatisfactory and high cost of economic calculation, and achieve high recovery rate, low economic cost, both economic benefits and environmental protection benefit effect

Inactive Publication Date: 2005-09-28
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the economic calculation cost of this process is relatively high, and it is not very ideal from the perspective of industrialization.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 150g cyclohexane oxidative saponification waste lye and 6g sodium hydroxide into an autoclave with a volume of 0.3 liters, and react for 6 hours at 280-300°C. 60g for neutralization, and the temperature is controlled at 10-30°C. Solid-liquid phase separation after acidification. After centrifugal filtration, 162 g of sodium sulfate aqueous solution and 40 g of muddy solid were obtained respectively. Sodium sulfate aqueous solution was extracted to obtain 0.9 g of succinic acid, 2.2 g of glutaric acid and 0.3 g of adipic acid. The muddy solid was dissolved in 65 g of water at a temperature of 100° C., and 18.7 g of black oil was separated and subjected to vacuum distillation to recover the unit acid. The aqueous solution was crystallized, and 7.9 g of adipic acid crystals were obtained after crystallization, with a content of 98.6%.

Embodiment 2

[0016] Add 150g cyclohexane oxidative saponification waste lye and 10g sodium hydroxide into an autoclave with a volume of 0.3 liters, react at 280-300°C for 6 hours, cool after the reaction, take out the obtained alkali fusion product, and use 98% sulfuric acid 60g for neutralization, and the temperature is controlled at 10-30°C. Solid-liquid phase separation after acidification. After centrifugal filtration, 154 g of sodium sulfate aqueous solution and 57 g of muddy solid were obtained respectively. Sodium sulfate aqueous solution was extracted to obtain 0.8 g of succinic acid, 2.1 g of glutaric acid and 0.4 g of adipic acid. Dissolve the muddy solid in the adipic acid crystallization mother liquor of Example 1 at 100° C., separate the black oil and carry out vacuum distillation to recover the unit acid. The aqueous solution was crystallized to obtain 12.9 g of adipic acid crystals with a content of 98.2%.

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Abstract

The present invention discloses a method for recovering organic acid and inorganic salt from cyclohexane oxidated saponified waste alkali liquor, including the following steps: making the recovered cyclohexane oxidated saponified waste alkali liquor implement alkali fusion reaction with sodium hydroxide to convert the carboxyhexanoic acid and its polymer into hexanedioic acid, then using inorganic acid to make neutralization, filtering to respectively obtain mud-like solid and sodium sulfate aqueous solution, using organic solvent to extract organic acid from sodium sulfate aqueous solution, treating extraction raffinate phase (water phase) and recovering sodium sulfate product, desolventizing extraction raffinate phase (oil phase) and recovering partial binary acid product; dissolving mud-like solid in water with 40-100 deg.C, and demixing, making upper layer hexanedioic acid aqueous solution undergo the once crystallization, drying crystal to obtain high-purity hexanedioic acid; making lower layer black oil-like liquor undergo the process of reduced prssure distillation so as to recover unitary acid product.

Description

technical field [0001] The invention relates to a process for recovering sodium sulfate, unit acid and dibasic acid in cyclohexane waste lye by treating hydroxycaproic acid and its polymer in cyclohexane waste lye by alkali fusion method . The process uses saponified waste lye as raw material, and after alkali fusion treatment, organic acid and inorganic salt are separated and recovered. Background technique [0002] Cyclohexane liquid-phase oxidation is the most commonly used process for preparing cyclohexanone in the world today. During the oxidation process, the selectivity of cyclohexane to produce alcohol and ketone products is about 75-85%, and the remaining 15-25% cyclohexane will inevitably undergo deep oxidation and turn into by-products. The composition of these by-products is very complex, including monobasic acids, dibasic acids, oxyacids, esters, polycondensates, and lower alcohols, ketones, aldehydes, etc., with 1 to 6 carbon atoms, which are formed after bei...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/90C07C51/487C07C55/14
Inventor 罗和安王良芥艾秋红胡湘群胡蓉蓉
Owner XIANGTAN UNIV