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Reaction strengthening method and device for producing lactide by lactic acid liquid-phase one-step method

A lactide and lactic acid solution technology, applied in chemical instruments and methods, separation methods, organic chemistry, etc., can solve the problems of increasing the mass transfer capacity of the two-liquid phase separation in the reflux liquid, low reaction rate and single-pass yield, etc. Achieve the effect of improving reaction rate and selectivity, continuous lactide production

Active Publication Date: 2022-08-05
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at the problem of low reaction rate and single-pass yield in the prior art, the present invention finds that it is related to the strict removal of trace moisture, and the salting-out phase separation technology can effectively increase the mass transfer capacity of the two-liquid phase separation in the reflux liquid

Method used

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  • Reaction strengthening method and device for producing lactide by lactic acid liquid-phase one-step method

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Experimental program
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Effect test

Embodiment 1

[0037] 80wt% L-lactic acid solution 1.25g, H-β catalyst 0.5g, toluene 30mL, liquid-liquid extraction tank volume 20mL, system pressure 100kpa, oil bath 140°C, reaction time 3 hours, liquid-liquid extraction tank pre-filled with excess CaCl 2 Salt, CaCl during the reaction 2 Salt is always supersaturated. The one-way yield was 75.0%.

Embodiment 2

[0039] 80wt% L-lactic acid solution 1.25g, H-β catalyst 0.5g, toluene 30mL, liquid-liquid extraction tank volume 20mL, system pressure 100kpa, oil bath 140°C, reaction time 3 hours, liquid-liquid extraction tank pre-filled with excess BaCl 2 Salt, BgCl in progress 2 Salt is always supersaturated. The one-way yield was 77.7%.

Embodiment 3

[0041] 80wt% L-lactic acid solution 1.25g, H-β catalyst 0.5g, toluene 30mL, liquid-liquid extraction tank volume 20mL, system pressure 100kpa, oil bath 140°C, reaction time 3 hours, liquid-liquid extraction tank pre-filled with excess NaCl salt , the NaCl salt is always in a supersaturated state during the reaction process. The one-way yield was 68.5%.

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Abstract

The invention discloses a reaction process strengthening method and device for producing lactide from lactic acid through a one-step method. The invention provides a means and a device for recycling an entrainer in the device and improving the conversion per pass of the reaction. L-lactic acid or D-lactic acid is used as a raw material, under the action of a catalyst, a lactic acid dehydration reaction is performed in an organic solvent in a boiling state, steam generated in the reaction process is condensed and then subjected to phase separation, one or a combination of a salt chemical and a physical water absorbent is added in the phase separation process, and the lactic acid is obtained. Continuously refluxing the evaporated organic solvent into the reactor to finally obtain an organic solvent dissolved with an L-lactide or D-lactide product; in the reaction process, the organic solvent continuously removes water generated in the reaction process through azeotropy; according to the method provided by the invention, the salt and the physical water absorbent are added, so that trace moisture in the reflux organic solvent can be removed, the conversion per pass and rate of the reaction are improved, and the production cost of one-step production of lactide from lactic acid is reduced.

Description

technical field [0001] The invention belongs to the technical field of polymer material production, and relates to a preparation method and device for a chemical intermediate, in particular to a method for strictly removing trace moisture in the reflux liquid in the process of catalyzing lactic acid to directly synthesize lactide, thereby improving the Method and device for enhancing the yield of lactide. Background technique [0002] Polylactic acid is a kind of degradable plastic with good mechanical strength and biocompatibility, and has a wide range of application prospects and fields of application. With the continuous maturity of polylactic acid production technology and the continuous increase of market demand, the production of polylactic acid by the route of non-food crops → lactic acid → lactide → polylactic acid has begun to enter a period of industrial development. At present, most of the high molecular weight polylactic acid produced at home and abroad is obtai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12B01D3/14B01D3/32B01D5/00B01D11/04B01J8/00B01J8/02
CPCC07D319/12B01J8/001B01J8/008B01J8/025B01J8/0285B01D3/14B01D3/32B01D5/006B01D11/04Y02P20/10
Inventor 李新刚宋松柳嘉澍田野丁彤
Owner TIANJIN UNIV
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