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Method for separating and purifying 1, 2, 4-butantriol based on bifunctional ionic liquid

An ionic liquid, separation and purification technology, applied in the separation/purification of hydroxyl compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve problems such as equipment corrosion, complex extraction methods, and poor industrial practice, and achieve the reduction of aldehydes The effect of low dosage, easy recycling, and long catalytic life

Pending Publication Date: 2022-02-25
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has two disadvantages: one is that the catalyst is easy to lose activity; the other is that valeraldehyde is easily oxidized to carboxylic acid if the amount is too large, causing equipment corrosion
(Meng Q Y, Yu J M, Yang L R, Li Y Q, Xian M, Liu H Z. Efficient recovery of bio-based 1,2,4-butanetriol by using boronic acidanionic reactive extraction. Separation and Purification Technology, 2021,255: 117728) The extraction method is too complicated and the industrial practice is not strong

Method used

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  • Method for separating and purifying 1, 2, 4-butantriol based on bifunctional ionic liquid
  • Method for separating and purifying 1, 2, 4-butantriol based on bifunctional ionic liquid
  • Method for separating and purifying 1, 2, 4-butantriol based on bifunctional ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Take 20ml of pretreated 21g / L 1,2,4-butanetriol fermentation broth and put it in the reactor, add [SO 3 HC 8 MIM][HSO 4 ] ionic liquid 10ml, the reaction temperature is 25 ℃, the reaction extraction time is 1h, the conversion rate of 1,2,4-butanetriol is 95%, 96.5%, 97.2% respectively, the recovery rate of acetal in the ionic liquid phase is respectively 98%, 98.6%, 99.1%, the water phase only contains 0.02% n-butyraldehyde, no ionic liquid;

[0031] (2) Put the ionic liquid phase in step (1) in a hydrolysis reactor, add 2ml of water, and perform hydrolysis reaction at 80°C for 50 minutes to form a two-phase product of the ionic liquid phase and the water phase. After testing, the hydrolysis conversion rate of acetal was 100%. The aqueous phase only contains 0.01% n-butyraldehyde and does not contain ionic liquids;

[0032] (3) The ionic liquid phase in step (2) is distilled under reduced pressure, and used for recycling in the reactor. The water phase was distil...

Embodiment 2

[0034] (1) Take 20ml of pretreated 21g / L 1,2,4-butanetriol fermentation broth and put it in the reactor, add [SO4] containing 4mmol n-butyraldehyde 3 HC 8 MIM][HSO 4 ] 10 ml of ionic liquid, the reaction temperatures were 5°C, 25°C, 50°C, the reaction extraction time was 1h, the conversion rates of 1,2,4-butanetriol were 95.1%, 96.3%, 97.0%, and the acetal The recovery rate in the ionic liquid phase is above 99%, and the aqueous phase only contains 0.01% n-butyraldehyde, and does not contain ionic liquid;

[0035] (2) Put the ionic liquid phase in step (1) in a hydrolysis reactor, add 2ml of water, and perform hydrolysis reaction at 80°C for 50 minutes to form a two-phase product of the ionic liquid phase and the water phase. After testing, the hydrolysis conversion rate of acetal was 100%. The aqueous phase only contains 0.01% n-butyraldehyde and does not contain ionic liquids;

[0036] (3) The ionic liquid phase in step (2) is distilled under reduced pressure, and used f...

Embodiment 3

[0038] (1) Take 20ml of pretreated 21g / L 1,2,4-butanetriol fermentation broth and put it in the reactor, add [SO4] containing 4mmol n-butyraldehyde 3 HC 8 MIM][HSO 4 ] ionic liquid 10 ml, the reaction temperature is 25 ℃, the reaction extraction time is 0.5h, 2h, 4h, the conversion rate of 1,2,4-butanetriol is 95.5%, 96.3%, 97.1%, respectively, the acetal in The recovery rate of the ionic liquid phase is above 97%, and the aqueous phase only contains 0.01% n-valeraldehyde and does not contain ionic liquid;

[0039] (2) Put the ionic liquid phase in step (1) in a hydrolysis reactor, add 2ml of water, and perform hydrolysis reaction at 80°C for 50 minutes to form a two-phase product of the ionic liquid phase and the water phase. After testing, the hydrolysis conversion rate of acetal was 100%. The aqueous phase only contains 0.01% n-valeraldehyde and does not contain ionic liquids;

[0040] (3) The ionic liquid phase in step (2) is distilled under reduced pressure, and used ...

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Abstract

The invention discloses a method for separating and purifying 1, 2, 4-butantriol based on a bifunctional ionic liquid. A hydrophobic acidic ionic liquid is taken as a catalyst and an extracting agent, an acetal reaction of a water phase is catalyzed, acetal generated by the reaction is extracted into an ionic liquid phase, and the ionic liquid phase can hydrolyze acetal to release 1, 2, 4-butantriol without adding an additional catalyst; and the ionic liquid used as the catalyst and the extracting agent is a quaternary phosphorus ionic liquid, a quaternary ammonium ionic liquid, an imidazole ionic liquid, a pyridine ionic liquid and a pyrrolidine ionic liquid which are functionalized by hydrophobic sulfonic acid, and the selected aldehydes are C4-C6 fatty aldehydes. The defects that in the prior art, (1) the active life of the catalyst is short, (2) the equipment is easy to corrode; and (3) serious environmental pollution caused by a large amount of volatile organic solvent and the like are overcome.

Description

technical field [0001] The invention belongs to the technical field of polyol chemical separation and purification, and in particular relates to a separation and purification method for extracting 1,2,4-butanetriol from a dilute solution. Background technique [0002] 1,2,4-Butanetriol (BT) is an important platform compound widely used in fields such as military industry, explosives, cosmetics, papermaking, cigarettes and materials. 1,2,4-Butanetriol is an important precursor for the synthesis of 1,2,4-Butanetriol Nitrate (BTTN), and BTTN can replace nitroglycerin as a high-quality propellant and plasticizer. 1,2,4-Butanetriol is also the building block of several synthetic drugs, such as Crestor and Zetia3. In addition, it can be used to synthesize polyurethane foams with higher elastic properties and compression bending characteristics. 1,2,4-Butanetriol can also reduce the toxicity of nitro compounds to the human body, so it is used as a cigarette additive in the tobacc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/88C07C29/86C07C29/74C07C29/92C07C31/22
CPCC07C29/88C07C29/92C07C29/86C07C29/74C07C31/22
Inventor 罗海燕李英波王晓天李敏唐斌
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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