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A kind of method for preparing anhydrous peroxy organic carboxylic acid solution

A technology of anhydrous peroxy organic carboxylic acid and organic carboxylic acid, applied in the direction of organic chemistry, peroxygen compound preparation, chemical instruments and methods, etc., can solve the problem of long rectification time, reduction of device production capacity, and consumption of large circulating cooling water and other problems, to achieve high reactivity and thermal stability, reduce by-product production, and save steam consumption

Active Publication Date: 2018-03-06
HUNAN JUREN CHEM NEW MATERIAL TECH CO LTD
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  • Abstract
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Problems solved by technology

The technology needs to be improved in terms of safety, and there is no industrialization
[0009] In 2013, Jiangsu Feixiang Chemical Co., Ltd. cooperated with Sun Yat-sen University to use magnesium or tin porphyrin complexes as catalysts to react with benzaldehyde through air or oxygen in ester solvents. The conversion rate of cyclohexanone and ε-hexyl The yield of lactone is greater than 95%, but the by-product benzoic acid and caprolactone are difficult to separate
[0011] In the process of preparing ε-caprolactone by the indirect method of hydrogen peroxide, firstly, peroxycarboxylic acid is prepared. Since hydrogen peroxide contains a large amount of water, water is also generated during the preparation process, so the peroxycarboxylic acid solution contains a large amount of water. In order to reduce the impact on the oxidation reaction of cyclohexanone, it is required that the prepared peroxycarboxylic acid solution does not contain water. Generally, an organic solvent is selected to remove the moisture in the peroxycarboxylic acid solution through azeotropic distillation, but due to the azeotropic distillation During the process, the evaporated azeotropic solvent has a certain compatibility with water, and the weight content of saturated water generally reaches 2-3%. In this way, when preparing anhydrous peroxycarboxylic acid solution, the reflux ratio of rectification separation is very high, and the product can The consumption is very high. To prepare one ton of ε-caprolactone product, it needs to consume more than 10 tons of steam in the process of preparing anhydrous peroxycarboxylic acid, and also consumes a large amount of circulating cooling water
Not only that, but also in order to remove the moisture in the peroxycarboxylic acid solution by azeotropic rectification, the rectification time required is very long, and generally a batch reaction needs rectification time 24 hours, which seriously reduces the production capacity of the device

Method used

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  • A kind of method for preparing anhydrous peroxy organic carboxylic acid solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Preparation of peracetic acid solution

[0050] First, 100 g of bissulfonic acid-based polystyrene resin was charged into a reactor with a volume of 2 L, and then 600 g of acetic acid and 440 g of ethyl acetate were added into the reactor.

[0051] The reactor has a packed distillation column and a reflux condenser with a settling tank. Stir this solution at about 20kPa (absolute pressure), heat it to about 40°C with steam, and add a total amount of 220g of 50% (by weight) hydrogen peroxide solution into the reactor. Control the temperature of the reactor at about 40-45°C, introduce the organic phase in the heterogeneous azeotrope condensed by the low-temperature system in the reflux condenser into the adsorption tower, which is equipped with molecular sieves, and the organic phase passes through the molecular sieves Adsorption dehydration, the water content is reduced to below 1000ppm (mass), and returned to the rectification tower; the water phase is continuously dra...

Embodiment 2

[0060] Preparation of peroxypropionic acid solution

[0061] 100g bissulfonic acid polystyrene resin is charged in advance in the reactor that volume is 2L, then 600g propionic acid, 400g ethyl propionate and 1kg tributyl phosphate are charged in the reactor. Stir this solution at about 10kPa (absolute pressure), heat it to about 50°C with steam, and add a total of 220g of 50% (weight) hydrogen peroxide aqueous solution into the reactor. Control the reaction temperature at about 50-55°C, introduce the organic phase in the heterogeneous azeotrope condensed by the low-temperature system in the reflux condenser into the adsorption tower, the adsorption tower is equipped with molecular sieves, and the organic phase is dehydrated by molecular sieve adsorption , the water content drops below 1000ppm (mass), and returns to the rectifying tower; the water phase is continuously drained and the organic solvent is recovered through the organic solvent recovery device and returned to the ...

Embodiment 3

[0071] Preparation of long-term peroxypropionic acid solution

[0072] In advance, 100 g of bissulfonic acid-based polystyrene resin was loaded into a reactor with a volume of 2 L, and then 600 g of propionic acid, 400 g of ethyl propionate and 1 kg of tributyl phosphate were loaded into the reactor. Stir this solution at about 10kPa (absolute pressure), heat it to about 50°C with steam, and add a total of 220g of 50% (weight) hydrogen peroxide aqueous solution into the reactor. Control the reaction temperature at about 50-55°C, introduce the organic phase in the heterogeneous azeotrope condensed by the low-temperature system in the reflux condenser into the adsorption tower, the adsorption tower is equipped with molecular sieves, and the organic phase is dehydrated by molecular sieve adsorption , the water content drops below 1000ppm (mass), and returns to the rectifying tower; the water phase is continuously drained and the organic solvent is recovered by the organic solvent...

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Abstract

The invention discloses a method for preparing an anhydrous peroxide organic carboxylic acid solution. The method comprises the following steps: in the presence of a catalyst, oxidizing an organic carboxylic acid and organic solvent-containing mixed solution with hydrogen peroxide in a stirring reaction kettle with a rectifying tower; distilling the water carried by the hydrogen peroxide solution and water generated during reaction from the tower top through an azeotropic distillation manner, so as to obtain an organic solvent-containing peroxide carboxylic acid solution from the tower kettle, wherein the organic solvent-containing peroxide carboxylic acid solution is characterized by azeotropic distillation and dehydration; and condensing top gaseous azeotrope through a condenser, separating free water in a settling separation tank, entering an adsorption tower with an adsorbent so as to remove saturated water from the azeotrope solvent, and returning to the rectifying tower. According to the method, the adsorption tower is additionally arranged, the distillation time is shortened to 4-8 hours from original 18-24 hours once, the consumption of a great amount of vapor can also be saved, only 5-6 tonnage of vapor is needed to produce one tonnage of caprolactone during the preparation of peroxide carboxylic acid, the vapor can be saved by 50%, and the consumption of cooling water can also be decreased by more than 40%.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a method for preparing anhydrous organic peroxycarboxylic acid, in particular to a method for preparing anhydrous organic peroxycarboxylic acid used for the preparation of ε-caprolactone. Background technique [0002] ε-caprolactone (ε-CL) is a versatile chemical intermediate, mainly used as a monomer for high-performance polymer materials. Polycaprolactone (PCL) is obtained by self-polymerization of ε-caprolactone. PCL has good thermoplasticity and molding processability, and can be made into environmentally friendly plastic products for various purposes, and can also be made into biodegradable biomedical materials; ε - Caprolactone is triggered by polyol to obtain polycaprolactone polyol, polycaprolactone polyol reacts with diisocyanate to prepare high-performance material polycaprolactone polyurethane, which is widely used as a special polyurethane in synthetic leather,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C407/00C07C409/24C07C409/26C07D313/04
CPCC07C407/00C07C407/003C07D313/04C07C409/24C07C409/26
Inventor 王函宇王国兵张光旭李韶峰
Owner HUNAN JUREN CHEM NEW MATERIAL TECH CO LTD
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