CN219272982U - Combined device for continuously preparing industrial glyoxylic acid - Google Patents

Combined device for continuously preparing industrial glyoxylic acid Download PDF

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Publication number
CN219272982U
CN219272982U CN202320103050.7U CN202320103050U CN219272982U CN 219272982 U CN219272982 U CN 219272982U CN 202320103050 U CN202320103050 U CN 202320103050U CN 219272982 U CN219272982 U CN 219272982U
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glyoxylic acid
glyoxal
gas
continuously preparing
industrial
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师红亮
张芦苇
刘超
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Xintiandi Pharmaceutical Co ltd
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Henan Newland Pharmaceutical Co Ltd
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Abstract

The utility model provides a combined device for continuously preparing industrial glyoxylic acid, and belongs to the technical fields of fine chemical equipment and glyoxylic acid synthesis. It comprises the following steps: a gas-liquid mixing injector, a micro-channel reactor, a micro-channel heat exchanger, a microporous membrane filter press and the like; the main innovation point of the combined device for continuously preparing industrial glyoxylic acid is that devices such as a micro-channel reactor, a microporous membrane filter press and the like are combined and introduced into a glyoxylic acid synthesis process, so that the combined device can quickly and effectively synthesize glyoxylic acid from air and glyoxal in one step; the method has the advantages of no generation of waste water, waste gas and waste solids, cyclic utilization of reuse water and environmental protection; it has the characteristic of obtaining higher content of glyoxylic acid without distillation and concentration; the combined device for continuously preparing the industrial glyoxylic acid has the characteristics of convenience in operation, high production efficiency and small occupied space.

Description

Combined device for continuously preparing industrial glyoxylic acid
Technical Field
The utility model belongs to the technical field of fine chemical equipment and glyoxylate synthesis, and particularly relates to a combined device for continuously preparing industrial glyoxylate.
Background
Glyoxylic acid (Glyoxylic acid) is also known as formaldehyde formic acid or dihydroxyacetic acid, and has the molecular formula CHOCOOH and a molecular weight of 74.04.
Glyoxylic acid has a special odor, is a corrosive acid, and is pale yellow in aqueous solution. Glyoxylic acid is soluble in water, slightly soluble in ethanol, diethyl ether, benzene, etc., and insoluble in lipid and aromatic solvents. The melting point of the crystal glyoxylic acid is 98 ℃, the relative density is 1.384,refractive index(n20D):1.403。
Glyoxylic acid is an important organic synthesis intermediate, and is widely applied to organic synthesis intermediates of perfumes, medicines, pesticides, foods, varnish raw materials, dyes, plastic additives and the like, and also can be applied to products of vanillin, ethyl vanillin, mandelic acid, p-hydroxyphenylglycine, p-hydroxyphenylacetic acid, allantoin and the like.
The synthesis of glyoxalic acid is basically classified into 2 kinds, namely chemical synthesis and electrochemical synthesis, wherein the chemical synthesis comprises a glyoxal nitric acid oxidation method, a maleic anhydride ozone oxidation method, a glyoxal hydrogen peroxide oxidation method and the like, and the electrochemical synthesis mainly comprises an oxalic acid electrolytic reduction method. At present, the production processes of glyoxal nitric acid oxidation method and oxalic acid electrolytic reduction method are mainly adopted in China.
The glyoxal nitric acid oxidation method is a glyoxylic acid synthesis method which is mature in the prior art and relatively low in cost, glyoxal is oxidized into glyoxylic acid by dilute nitric acid under the action of a composite catalyst, and a large amount of oxalic acid and nitric oxide are produced in the oxidation process.
The chemical reaction equation for glyoxal nitric acid oxidation is as follows:
3CHO-CHO+2HNO 3 →3CHO-COOH+2NO↑+H 2 O
3CHO-COOH+2HNO 3 →3HOOC-COOH+2NO↑+H 2 O。
the glyoxal nitric acid oxidation method is mainly used for synthesizing glyoxylic acid in an intermittent reaction kettle production mode, waste acid of the method is difficult to separate, and the product purity is low and cannot be used as a raw material of a high-end product. The technical defects are as follows: 1 nitric acid corrodes equipment, 2 is easy to have the dangers of bumping and the like when the concentration is high, 3 is unfavorable to the environment by nitric oxide and nitrogen dioxide gas generated by reaction, and 4 glyoxal residual energy interferes and limits the further application of glyoxylic acid.
Because of the adverse environmental effects of nitric oxide and nitrogen dioxide gas generated in the process operation, and the dangerous characteristic of easy bumping and pot overflow in the reaction process, the process is gradually strictly controlled by the national security department and replaced by manufacturers.
The conversion of "oxalic acid electroreduction" to glyoxylate is usually carried out in an electrolytic cell, the electrochemical reaction equation of which is as follows:
anode H 2 0–2e→2H+1/2O
Cathode HOOC-COOH+2H+2e→HOOC-CHO+H 2 O
Although the oxalic acid electrolytic reduction method is simple in process, the power consumption is high, the concentration of the produced glyoxylic acid is only 4.0-5.0%, the glyoxylic acid can be obtained by multistage distillation and concentration, and the energy consumption is too high.
Disclosure of Invention
The technical scheme of the utility model discloses a combined device for continuously preparing industrial glyoxylic acid, which mainly has the innovation points that devices such as a micro-channel reactor, a microporous membrane filter press, a gas-liquid mixing injector and the like are combined and introduced into a glyoxylic acid synthesis process, so that air and glyoxal can be quickly and effectively synthesized into glyoxylic acid in one step; the method has the advantages of no generation of waste water, waste gas and waste solids, cyclic utilization of reuse water and environmental protection; it also has the characteristic of obtaining higher content of glyoxylic acid without distillation and concentration; the combined device for continuously preparing the industrial glyoxylic acid has the characteristics of convenience in operation, high production efficiency and small occupied space. The utility model relates to a combined device for continuously preparing industrial glyoxylic acid, which comprises: the device is characterized in that the upper part of the glyoxal diluting tank is connected with a multiplexing water pipeline and a raw material glyoxal pipeline, the bottom of the glyoxal diluting tank is connected with the gas-liquid mixing injector from the side through a glyoxal delivery pump, the gas-liquid mixing injector is provided with three openings, one end inlet is connected with a high-pressure air pipeline, the side inlet is connected with the diluted glyoxal pipeline, one end outlet is connected with the microchannel reactor, the other end outlet of the microchannel reactor is connected with the microchannel heat exchanger through a back pressure pipe, the microchannel heat exchanger is connected with the gas-liquid separator through a built-in back pressure valve, the top of the gas-liquid separator is connected with a tail gas pipeline, the bottom of the gas-liquid separator is connected with the microporous membrane filter press through a booster pump, the side outlet is connected with the glyoxal collecting tank, the front end outlet is connected with the multiplexing water collecting tank, and the bottom outlet of the multiplexing water collecting tank is connected with the upper part of the glyoxal diluting tank through a pipeline, so that all components are organically combined to form the combined device.
Preferably, the technical scheme of the combined device for continuously preparing the industrial glyoxal is characterized in that the gas-liquid mixing ejector takes high-pressure air as power, the design working pressure is 1.0-2.0 MPa, and the high-pressure air nozzle is perpendicular to the diluted glyoxal inlet and extends forwards for 20-50 mm.
Preferably, the technical scheme of the utility model provides a combined device for continuously preparing industrial glyoxylic acid, which is characterized in that a catalyst module taking aluminum oxide or a molecular sieve as a carrier is arranged in the micro-channel reactor.
Preferably, the technical scheme of the utility model provides a combined device for continuously preparing industrial glyoxylic acid, which is characterized in that the working pressure of the microchannel reactor is 0.5-2.5 MPa.
Preferably, the technical scheme of the utility model provides a combined device for continuously preparing industrial glyoxylic acid, which is characterized in that the pressure range of the back pressure communicating pipe connecting the microchannel reactor and the microchannel heat exchanger from high pressure to low pressure is 2.5-0.5 MPa.
Preferably, the technical scheme of the utility model provides a combined device for continuously preparing industrial glyoxylic acid, which is characterized in that the volume of the micro-channel heat exchanger is 1.0-2.0 m 3 The heat exchange area is 600-1200 m 2 The working pressure range from high pressure to low pressure of the back pressure valve arranged in the micro-channel heat exchanger is 0.5MPa to normal pressure.
Preferably, the combined device for continuously preparing industrial glyoxylic acid is characterized in that the upper part of the gas-liquid separator is provided with a liquid-blocking grid layer, the liquid-blocking grid layer consists of oblique corrugated filler or PE, PP, PTFE spherical filler, and the thickness of the module is 200-400 mm.
Preferably, the combined device for continuously preparing industrial glyoxylic acid is characterized in that the flow rate of the microporous membrane filter press is 8-12 t/h, the precision is 0.10-1.0 nm, 15-30 microporous membrane columns are arranged in the microporous membrane filter press, and the effective membrane area is 100-120 m 2 . The purpose of this design is to use a high-precision, large surface area microporous membrane filter press to facilitate rapid removal of more water from the reaction solution.
The technical scheme of the utility model provides a combined device for continuously preparing industrial glyoxylic acid, which has the obvious beneficial effects that the combined device comprises the following 4 aspects: (1) The method can quickly and effectively synthesize the glyoxylic acid by air and glyoxal in one step; (2) The method has the advantages of no waste water, waste gas and waste solids, and (3) reuse of water energy, and is very beneficial to environmental protection; (3) It also has the characteristic of obtaining higher content of glyoxylic acid without distillation and concentration;
the combined device for continuously preparing the industrial glyoxylic acid has the characteristics of convenience in operation, high production efficiency and small occupied space.
Drawings
In order to more clearly illustrate the embodiments of the present utility model or the technical solutions of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are only some embodiments of the present utility model, and other drawings may be obtained according to these drawings for a person having ordinary skill in the art. FIG. 1 is a schematic diagram of the structure and process flow of a combined device for continuously preparing industrial glyoxylic acid according to an embodiment of the present utility model.
In fig. 1: glyoxal diluting tank 01, gas-liquid mixing ejector 02, microchannel reactor 03, back pressure communicating pipe 04, microchannel heat exchanger 05, gas-liquid separator 06, booster pump 07, microporous membrane filter press 08, glyoxylate collecting tank 09, reuse water collecting tank 10, raw material glyoxal inlet 102, reuse water inlet 101, glyoxal delivery pump 103, air inlet 201, dilution glyoxal inlet 202, back pressure valve 501, tail gas pipe 601, liquid blocking mesh layer 602, nano column 801, small molecule outlet 802, macromolecule outlet 803, glyoxylate outlet 901, reuse water outlet 1001.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present utility model more apparent, embodiments of the present utility model will be further described with reference to the accompanying drawings.
Referring to fig. 1, an apparatus for continuously preparing industrial glyoxylic acid according to an embodiment of the present utility model comprises:
glyoxal diluting tank 01, gas-liquid mixing ejector 02, microchannel reactor 03, back pressure communicating pipe 04, microchannel heat exchanger 05, gas-liquid separator 06, booster pump 07, microporous membrane filter press 08, glyoxylate collecting tank 09, reuse water collecting tank 10, raw material glyoxal inlet 102, reuse water inlet 101, glyoxal delivery pump 103, air inlet 201, dilution glyoxal inlet 202, back pressure valve 501, liquid blocking mesh layer 602 of tail gas pipeline 601, nano column 801, small molecule outlet 802, macromolecule outlet 803, glyoxylate outlet 901, reuse water outlet 1001.
The combination device for continuously preparing industrial glyoxal according to the embodiment of the present utility model is characterized in that the upper portion of the glyoxal diluting tank 01 is connected with a multiplexing water pipe 101 and a raw material glyoxal pipe 102, the bottom is connected with a gas-liquid mixing injector 02 from the side through a glyoxal delivery pump 103, the gas-liquid mixing injector 02 is provided with three openings, one end inlet is connected with a high-pressure air pipe 201, the side inlet is connected with a diluted glyoxal pipe, one end outlet is connected with a micro-channel reactor 03, the other end outlet of the micro-channel reactor 03 is connected with a micro-channel heat exchanger 05 through a back pressure pipe 04, the micro-channel heat exchanger 05 is connected with a gas-liquid separator 06 through a built-in back pressure valve 501, the top of the gas-liquid separator 06 is connected with a tail gas pipe 601, the bottom of the gas-liquid separator 06 is connected with a microporous membrane filter press 08 through a booster pump 04, the microporous membrane filter press 08 is provided with 2 outlets, the side outlet is connected with a glyoxal collecting tank 09, the front end outlet is connected with a multiplexing water collecting tank 10, the bottom outlet 1001 of the multiplexing water collecting tank 10 is connected with the glyoxal diluting tank 01 through a pipe, and thus the components are organically combined to form the combination device.
The simple process operation flow of the combined device for continuously preparing industrial glyoxylic acid disclosed in the embodiment of the utility model is as follows: firstly, raw material glyoxal and reuse water are pumped into a glyoxal diluting tank 01 through inlets 101 and 102 to prepare 30-35% concentration, the raw material glyoxal and reuse water are pumped into a gas-liquid mixing injector 02 through a glyoxal delivery pump 103 to be mixed with high-pressure air flow and sent into a microchannel reactor 03, the technology conditions of catalysis, pressurization, heating and the like are adopted to synthesize the glyoxylic acid of 35% in one step, the glyoxylic acid is slightly depressurized through a back pressure communicating pipe 04 and enters a microchannel heat exchanger 05, after the glyoxylic acid is cooled, the glyoxylic acid is reduced to normal pressure through a back pressure valve 501 and then enters a gas-liquid separator 06, tail gas is subjected to further purification treatment through a pipeline 601, crude glyoxylic acid is sent into a microporous membrane filter press 08 through a booster pump 07 to be concentrated and dehydrated, most of the contained water is pressed into a reuse water collecting tank 10, and the reuse water is transferred into the glyoxal diluting tank 01 through an outlet 1001 for recycling; high-concentration glyoxylate is injected into the glyoxylate collection tank 09 and then is transferred to the next working procedure for concentration or crystallization through the outlet 901.
Further, the combination device for continuously preparing industrial glyoxal according to the embodiment of the present utility model is characterized in that the gas-liquid mixing ejector uses high-pressure air as power, the design working pressure is 1.0-2.0 MPa, and the high-pressure air nozzle is perpendicular to the diluted glyoxal inlet and extends forward for 20-50 mm.
Further, the combination device for continuously preparing industrial glyoxylic acid according to the embodiment of the present utility model is characterized in that a catalyst module using alumina or molecular sieve as a carrier is disposed in the microchannel reactor.
Further, the combination device for continuously preparing industrial glyoxylic acid according to the embodiment of the present utility model is characterized in that the working pressure of the microchannel reactor is 0.5-2.5 MPa, and the working pressure of the microchannel heat exchanger is 0.1-0.5 MPa
Further, the combination device for continuously preparing industrial glyoxylic acid according to the embodiment of the present utility model is characterized in that the pressure range of the back pressure pipe connecting the microchannel reactor and the microchannel heat exchanger from high pressure to low pressure is 2.5-0.5 MPa.
Further, the combination device for continuously preparing industrial glyoxylic acid according to the embodiment of the present utility model is characterized in that the volume of the microchannel heat exchanger is 1.0-2.0 m 3 The heat exchange area is 600-1200 m 2 The working pressure range from high pressure to low pressure of the back pressure valve arranged in the micro-channel heat exchanger is 0.5MPa to normal pressure.
Further, the combination device for continuously preparing industrial glyoxylic acid according to the embodiment of the utility model is characterized in that the upper part of the gas-liquid separator is provided with a liquid-blocking grid layer, the liquid-blocking grid layer consists of oblique corrugated filler or PE, PP, PTFE spherical filler, and the thickness of the module is 200-400 mm.
Further, the combined device for continuously preparing industrial glyoxylic acid according to the embodiment of the utility model is characterized in that the flow rate of the microporous membrane filter press is 8-12 t/h, the precision is 0.10-1.0 nm, 15-30 microporous membrane columns are arranged in the microporous membrane filter press, and the effective membrane area is 100-120 m 2 . The purpose of this design is to use a high-precision, large surface area microporous membrane filter to facilitate rapid removal of more water from the reaction solution.
By designing in this way, the technical scheme of the utility model discloses a combined device for synthesizing glyoxylic acid by using a microchannel reactor, which has the following 4 obvious beneficial effects: (1) The method can quickly and effectively synthesize the glyoxylic acid by air and glyoxal in one step; (2) The method has the advantages of no waste water, waste gas and waste solids, and (3) reuse of water energy, and is very beneficial to environmental protection; (4) It also has the characteristic of obtaining higher content of glyoxylic acid without distillation and concentration;
by means of the design, the combined device for continuously preparing the industrial glyoxylic acid has the characteristics of convenience in operation, high production efficiency and small occupied space. The generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the utility model. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present utility model should be included in the protection scope of the present utility model. The scope of the present utility model is to be accorded the widest scope consistent with the principles and novel features described herein.

Claims (8)

1. A combination unit for the continuous preparation of industrial glyoxylic acid comprising: the device is characterized in that the upper part of the glyoxal diluting tank is connected with a multiplexing water pipeline and a raw material glyoxal pipeline, the bottom of the glyoxal diluting tank is connected with the gas-liquid mixing injector from the side through a glyoxal delivery pump, the gas-liquid mixing injector is provided with three openings, one end inlet is connected with a high-pressure air pipeline, the side inlet is connected with the diluted glyoxal pipeline, the outlet of the other end is connected with the microchannel reactor, the outlet of the other end of the microchannel reactor is connected with the microchannel heat exchanger through a back pressure communicating pipe, the microchannel heat exchanger is connected with the gas-liquid separator through a built-in back pressure valve, the top of the gas-liquid separator is connected with a tail gas pipeline, the bottom of the microporous membrane filter press is connected with the microporous membrane filter press through a booster pump, the side outlet is connected with the glyoxal collecting tank, the front end outlet is connected with the multiplexing water collecting tank, and the outlet of the bottom of the multiplexing water collecting tank is connected with the upper part of the glyoxal diluting tank through a pipeline.
2. The combination device for continuously preparing industrial glyoxal according to claim 1, wherein the gas-liquid mixing ejector is powered by high-pressure air, the design working pressure is 1.0-2.0 MPa, and the high-pressure air nozzle is perpendicular to the diluted glyoxal inlet and extends forward for 20-50 mm.
3. The combination unit for continuously preparing industrial glyoxylic acid according to claim 1, wherein a catalyst module taking aluminum oxide or molecular sieve as a carrier is arranged in the micro-channel reactor.
4. The combination unit for continuously producing industrial glyoxylic acid according to claim 1, wherein the microchannel reactor is designed to have a working pressure of 0.5 to 2.5MPa.
5. The combination unit for continuously preparing industrial glyoxylic acid as set forth in claim 1, wherein the back pressure communication tube connecting the microchannel reactor and the microchannel heat exchanger has a pressure range from high pressure to low pressure of 2.5 to 0.5MPa.
6. The combination unit for continuously producing industrial glyoxylic acid as set forth in claim 1, in which the volume of the microchannel heat exchanger is 1.0 to 2.0m 3 The heat exchange area is 600-1200 m 2 The working pressure range from high pressure to low pressure of the back pressure valve arranged in the micro-channel heat exchanger is 0.5MPa to normal pressure.
7. The combination device for continuously preparing industrial glyoxylic acid according to claim 1, wherein the upper part of the gas-liquid separator is provided with a liquid-blocking grid layer, and the liquid-blocking grid layer consists of oblique corrugated fillers or PE, PP, PTFE spherical fillers and has a thickness of 200-400 mm.
8. The combined device for continuously preparing industrial glyoxylic acid according to claim 1, wherein the flow rate of the microporous membrane filter press is 8-12 t/h, the precision is 0.10-1.0 nm, 15-30 nano columns are arranged in the microporous membrane filter press, and the effective membrane area is 100-120 m 2
CN202320103050.7U 2023-02-02 2023-02-02 Combined device for continuously preparing industrial glyoxylic acid Active CN219272982U (en)

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CN202320103050.7U CN219272982U (en) 2023-02-02 2023-02-02 Combined device for continuously preparing industrial glyoxylic acid

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Application Number Priority Date Filing Date Title
CN202320103050.7U CN219272982U (en) 2023-02-02 2023-02-02 Combined device for continuously preparing industrial glyoxylic acid

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CN219272982U true CN219272982U (en) 2023-06-30

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Address after: 461500 eastern part of Wei Wu Road, Changge, Xuchang, Henan

Patentee after: Xintiandi Pharmaceutical Co.,Ltd.

Address before: 461500 eastern part of Wei Wu Road, Changge, Xuchang, Henan

Patentee before: HENAN NEWLAND PHARMACEUTICAL Co.,Ltd.