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CN221816151U - Loop reaction system for continuously producing 1, 3-propylene glycol by glycerol hydrogenation - Google Patents

Loop reaction system for continuously producing 1, 3-propylene glycol by glycerol hydrogenation Download PDF

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Publication number
CN221816151U
CN221816151U CN202322664122.8U CN202322664122U CN221816151U CN 221816151 U CN221816151 U CN 221816151U CN 202322664122 U CN202322664122 U CN 202322664122U CN 221816151 U CN221816151 U CN 221816151U
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reaction
separator
buffer tank
reaction system
glycerol
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CN202322664122.8U
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俞健
宋鑫颖
潘莉
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Nanjing Shu Yi Hui Scientific Instruments Co ltd
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Nanjing Shu Yi Hui Scientific Instruments Co ltd
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Abstract

The utility model provides a loop reaction system for continuously producing 1, 3-propylene glycol by glycerol hydrogenation, which comprises the following components: the device comprises a buffer tank, a venturi reactor, a heat exchanger, a separator, a circulating pump, a rectifying tower and a circulating pipeline; the discharge port of the Venturi reactor is communicated with the feed port of the buffer tank, and the feed port of the Venturi reactor is communicated with the circulating pipeline behind the separator; materials in the buffer tank are sequentially cooled by the heat exchanger along the material conveying direction through the circulating pump, separated by the separator and distilled and purified by the rectifying tower. The product enters a rectification system for purification treatment after being subjected to solid removal by a membrane separator, and the solvent and byproducts after separation and purification continuously enter a circulating pipeline for reaction by a circulating pump. The system is simple and efficient, is easy to operate, has high production efficiency, ensures that the whole reaction process continuously carries out catalytic reaction in a steady state, realizes the recycling and efficient utilization of the solvent and the catalyst, and reduces the production cost.

Description

Loop reaction system for continuously producing 1, 3-propylene glycol by glycerol hydrogenation
Technical Field
The utility model belongs to the technical field of 1, 3-propylene glycol production equipment, and particularly relates to a loop reaction system for continuously producing 1, 3-propylene glycol by glycerol hydrogenation.
Background
The glycerol can be used as renewable resources to prepare the organic chemical raw material 1, 3-propanediol with high added value through chemical hydrogenolysis reaction. 1, 3-propanediol is an important chemical raw material and has important applications in medicine, food, cosmetics and organic synthesis. Can be used as solvent, antifreeze agent, emulsifier, plasticizer, detergent, preservative, lubricant and the like, and has wide application prospect. At present, main methods for producing 1, 3-propylene glycol from glycerol include a biological fermentation method, an ethylene oxide oxo synthesis method, an acrolein hydration hydrogenation method, a one-step hydrogenation method and the like. The one-step hydrogenolysis method has the advantages of wide raw material adaptability, short process flow, less environmental pollution, low toxicity and the like, and has important application prospect.
The existing technology for preparing 1, 3-propylene glycol by glycerol hydrogenation mostly adopts fixed bed or intermittent kettle type process equipment, the mass transfer speed between gas and liquid is low, the glycerol conversion rate is low, the reactant selectivity is low and the production efficiency is low. To ameliorate the above problems, technicians are continually updating the improvement technology. Such as: the patent CN111333488a uses a loop reaction process to combine a venturi reactor with a reaction vessel to intermittently produce 1, 3-propanediol. According to the method, the reaction raw materials are put into a reaction kettle at one time, the reactants are gradually reduced along with the progress of the reaction, the products are gradually increased, and the products are discharged from the bottom end of the reaction kettle after the reaction is finished. The method has the advantages of simple process, low cost and high reaction rate, but the reaction is an unsteady intermittent reaction process, and the production efficiency is low. In CN103524302a, glycerin and hydrogen are simultaneously introduced into a fixed bed reactor to react, and then by-products of the reaction, i.e., 1, 2-propanediol, n-propanol, isopropanol and unreacted glycerin are recycled back to the reactor to react. In the method, although a fixed bed reactor can realize a continuous process, the reaction proportion is small, the glycerol is not completely converted, the heat transfer of a catalytic bed layer is poor, and side reactions are easy to generate.
In view of the above problems, a reaction system that simplifies the preparation process, reduces the production cost, improves the conversion of the reactants and the selectivity of 1, 3-propanediol is an important research point for researchers.
Disclosure of Invention
The utility model aims to provide a loop reaction system for continuously producing 1, 3-propylene glycol by glycerol hydrogenation, and the system can be used for producing 1, 3-propylene glycol by continuous catalytic hydrogenation. The system is simple and efficient, is easy to operate, has high production efficiency, ensures that the whole reaction process continuously carries out catalytic reaction in a steady state, realizes the recycling and efficient utilization of the solvent and the catalyst, and reduces the production cost.
In order to achieve the above purpose, the technical scheme of the utility model is as follows:
A loop reaction system for continuously producing 1, 3-propylene glycol by glycerol hydrogenation is characterized by comprising a buffer tank, a venturi reactor, a heat exchanger, a separator, a circulating pump, a rectifying tower and a circulating pipeline; the discharge port of the Venturi reactor is communicated with the feed port of the buffer tank, and the feed port of the Venturi reactor is communicated with the circulating pipeline behind the separator; materials in the buffer tank are sequentially cooled by the heat exchanger along the material conveying direction through the circulating pump, separated by the separator and distilled and purified by the rectifying tower.
Further, the flow ratio of the reaction liquid to the circulating pump in the system is 1:20-1:100.
Further, the discharge port of the Venturi reactor is communicated with the feed port of the buffer tank, the reaction material immediately undergoes hydrogenation reaction when passing through the jet port of the Venturi reactor, and the product enters the buffer tank.
Further, the reaction pressure in the buffer tank is 0.5-5 MPa, and the reaction temperature is 80-200 ℃.
Further, the whole reaction system controls the pressure of the reaction system by controlling the pressure of the reaction liquid feeding, the mixed liquid discharging and the hydrogen.
Further, the heat exchanger is a tubular heat exchanger.
Further, the separator is a metal-based ceramic composite membrane filtration system.
When the utility model is implemented, the solvent and the catalyst are added into the buffer tank, the circulating pump is started, and then the reaction liquid composed of glycerol and the solvent is added into the circulating pipeline behind the separator. The reaction liquid circulates in the loop, the Venturi reactor sprays at high speed, the glycerol and the hydrogen react rapidly to generate the 1, 3-propanediol which enters the buffer tank, the materials in the buffer tank enter the heat exchanger through the circulating pump, and the heat exchanger provides or transfers the heat absorbed or released in the reaction process, so as to control the reaction temperature. And (3) starting a membrane separator to discharge, separating the product from the solvent and byproducts, removing solid from the product by the membrane separator, purifying the product by a rectification system, and continuously feeding the separated and purified solvent and byproducts into a circulating pipeline by a circulating pump for reaction.
The utility model has the beneficial effects that:
1. The utility model adopts a loop reaction process, carries out reaction through a Venturi reactor and is matched with a membrane separation process to continuously produce 1, 3-propanediol, and a steady-state continuous reaction process is adopted. Meanwhile, the temperature distribution in the loop reaction system is very uniform due to the forced circulation of the circulating pump, no local overheating phenomenon exists, few byproducts are generated, and the selectivity of target products is high.
2. The utility model carries out reaction through the Venturi reactor, the Venturi reactor can provide high gas-liquid mixing ratio, the gas-liquid-solid three-phase mass transfer speed is high, and the reaction efficiency is high.
Drawings
FIG. 1 is a schematic structural diagram of a loop reaction system for continuous production of 1, 3-propanediol by hydrogenating glycerol according to the present utility model.
Detailed Description
The utility model will be further described with reference to specific examples and drawings, to which, however, the scope of the utility model is not limited.
Referring to fig. 1, a loop reaction system for continuous production of 1, 3-propanediol by glycerol hydrogenation comprises a buffer tank (1), a venturi reactor (2), a heat exchanger (3), a separator (4), a circulating pump (5), a rectifying tower (6) and a circulating pipeline (7); the discharge port of the Venturi reactor (2) is communicated with the feed port of the buffer tank (1), the feed port of the Venturi reactor (2) is communicated with the circulating pipeline (7) behind the separator (4), the reaction liquid in the circulating pipeline (7) is subjected to hydrogenation reaction when passing through the Venturi reactor (2), and the product enters the buffer tank (1); the material in the buffer tank (1) is subjected to material cooling through the heat exchanger (3) sequentially through the circulating pump (5) along the material conveying direction, the separator (4) is used for carrying out liquid-solid separation on the material, the separated material enters the rectifying tower (6) for rectifying and purifying, and the solvent and byproducts after the separation and purification continuously enter the circulating pipeline through the circulating pump for reaction. In this example, the whole reaction system controls the pressure of the reaction system by controlling the pressure of the reaction liquid feed, the mixed liquid discharge and the hydrogen.
Further, the heat exchanger is a tubular heat exchanger, and the separator is a metal-based ceramic composite membrane filtration system.
The flow ratio of the reaction liquid in the loop reaction system to the circulating pump is 1:20-1:100; the reaction pressure is 0.5-5 MPa, and the reaction temperature is 80-200 ℃.
When the embodiment is implemented, the solvent and the catalyst are added into a buffer tank, a circulating pump is started, and then the reaction liquid consisting of the glycerol and the solvent is added into a circulating pipeline behind the metal matrix ceramic composite membrane filtration system. The reaction liquid circulates in the loop, the Venturi reactor sprays at high speed, glycerin reacts with hydrogen rapidly, the product 1, 3-propanediol enters a buffer tank, materials in the buffer tank enter a tubular heat exchanger through a circulating pump, and the tubular heat exchanger provides or transfers heat absorbed or released in the reaction process, so that the reaction temperature is controlled. The whole reaction system controls the pressure of the reaction system by controlling the pressure of the reaction liquid feeding, the mixed liquid discharging and the hydrogen. And (3) starting a membrane separator to discharge, separating the product from the solvent and byproducts, removing solids by the separator, purifying by a rectification system, and continuously feeding the separated and purified solvent and byproducts into a circulating pipeline by a circulating pump for reaction.
The present embodiment is only a preferred embodiment of a loop reaction system for continuous production of 1, 3-propanediol by hydrogenation of glycerin, and is not intended to limit the scope of the utility model. It will be understood by those skilled in the art that various modifications and equivalent substitutions may be made to the technical solution of the present utility model without departing from the spirit and scope of the technical solution of the present utility model.

Claims (7)

1. A loop reaction system for continuously producing 1, 3-propylene glycol by glycerol hydrogenation, which is characterized by comprising a buffer tank (1), a venturi reactor (2), a heat exchanger (3), a separator (4), a circulating pump (5), a rectifying tower (6) and a circulating pipeline (7); the discharge port of the Venturi reactor (2) is communicated with the feed port of the buffer tank (1), and the feed port of the Venturi reactor (2) is communicated with the circulating pipeline behind the separator (4); materials in the buffer tank (1) are cooled by the heat exchanger (3) through the circulating pump (5) along the material conveying direction, and are separated by the separator (4), and are rectified and purified by the rectifying tower (6).
2. The loop reaction system for continuously producing 1, 3-propanediol by hydrogenating glycerol according to claim 1, wherein the flow ratio of the reaction liquid to the circulating pump in the system is 1:20-1:100.
3. The loop reaction system for continuous production of 1, 3-propanediol by hydrogenating glycerol according to claim 1, wherein the outlet of the venturi reactor is communicated with the inlet of the buffer tank, the reaction material is immediately hydrogenated when passing through the jet orifice of the venturi reactor, and the product enters the buffer tank.
4. The loop reaction system for continuous production of 1, 3-propanediol by glycerol hydrogenation according to claim 1, wherein the reaction pressure in the system is 0.5-5 MPa and the reaction temperature is 80-200 ℃.
5. The loop reaction system for continuous production of 1, 3-propanediol by hydrogenating glycerol according to claim 1, wherein the pressure of the reaction system is controlled by controlling the pressure of the reaction liquid feed, the mixed liquid discharge and the hydrogen.
6. The loop reaction system for the continuous production of 1, 3-propanediol by the hydrogenation of glycerol of claim 1 wherein said heat exchanger is a tubular heat exchanger.
7. The loop reaction system for the continuous production of 1, 3-propanediol by the hydrogenation of glycerol of claim 1 wherein said separator is a metal matrix ceramic composite membrane filtration system.
CN202322664122.8U 2023-10-07 2023-10-07 Loop reaction system for continuously producing 1, 3-propylene glycol by glycerol hydrogenation Active CN221816151U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202322664122.8U CN221816151U (en) 2023-10-07 2023-10-07 Loop reaction system for continuously producing 1, 3-propylene glycol by glycerol hydrogenation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202322664122.8U CN221816151U (en) 2023-10-07 2023-10-07 Loop reaction system for continuously producing 1, 3-propylene glycol by glycerol hydrogenation

Publications (1)

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CN221816151U true CN221816151U (en) 2024-10-11

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