CN215855852U - Device based on microchannel reactor serialization preparation acetic acid - Google Patents
Device based on microchannel reactor serialization preparation acetic acid Download PDFInfo
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Abstract
The utility model discloses a device for continuously preparing acetic acid based on a microchannel reactor, which comprises a prefabricated kettle, a gas mass flow meter, an injection pump A, an injection pump B, an injection pump C, a microchannel mixer A, a microchannel mixer B, CO preheater A, a methanol preheater B, a catalyst mother liquor preheater C, a microchannel reactor, a flash tank, a material circulating pump, a collecting tank, a rectifying tower and a material circulating pump, wherein a liquid phase component in the flash tank and a gas phase component in the rectifying tower are recycled into the prefabricated kettle for cyclic use through the material circulating pump, and the reaction is continuously carried out. According to the device for continuously preparing acetic acid based on the microchannel reactor, the reaction raw materials can be continuously fed, the contact is sufficient, the back mixing is less, a good environment is provided for synthesizing acetic acid by methanol carbonylation, the methanol conversion rate is high, the number of byproducts is less, and the acetic acid yield is high.
Description
Technical Field
The utility model relates to a device for continuously preparing acetic acid based on a microchannel reactor, belonging to the technical field of organic synthesis.
Background
Acetic acid is an important organic chemical raw material, is mainly used for producing vinyl acetate, acetic ester, acetic anhydride, chloroacetic acid, terephthalic acid and the like, and is widely applied to the fields of chemical industry, textile, medicine, printing and dyeing and the like. The industrial production method of acetic acid mainly comprises a light hydrocarbon liquid phase oxidation method, an acetaldehyde oxidation method, an ethylene direct oxidation method, a methanol carbonylation method and the like, wherein the methanol carbonylation method has the advantages of high methanol conversion rate, few byproducts and the like, and becomes one of the main methods for producing acetic acid. Currently, 60% of the world's acetic acid production is produced by methanol carbonylation.
In the traditional reaction process of synthesizing acetic acid by methanol low-pressure carbonylation, raw materials of methanol, carbon monoxide and separated return materials of a flash evaporation kettle are continuously introduced into a reactor, crude acetic acid is generated under the action of a main catalyst (mainly a rhodium catalyst and an iridium catalyst), a cocatalyst of methyl iodide and an additive (mainly alkali metal iodized salt or acetate), the crude acetic acid is flashed by an evaporator, a flashed vapor phase enters a rear-stage separation system to be purified to obtain an acetic acid product, and a liquid phase returns to the reactor again. The following problems exist in the process of synthesizing acetic acid by methanol carbonylation: 1) the reaction process is complex, byproducts such as formic acid, acetaldehyde and propionic acid are more, and the separation energy consumption is higher; 2) the heat is released violently in the reaction process, and if the heat is not transferred in time, the active catalytic species can be deactivated, so that the stability and the activity of the catalyst in the system are influenced; 4) the reaction is a typical gas-liquid reaction, and the generation efficiency of acetic acid is greatly influenced due to insufficient mass transfer; 5) the reaction system has strong corrosivity, and the reaction device needs to use special materials such as zirconium, hastelloy and the like, so that the investment cost is high.
Patent CN110835295A discloses a method for preparing acetic acid by using a microchannel reactor. The method comprises the steps of preparing acetic acid by taking ethanol as a raw material and nano gold, vanadium oxide and nano palladium oxide as catalysts, adding the catalysts into an ethanol water solution with the mass fraction of 30-70% to obtain a suspension for later use, wherein the mass content of the catalysts is 2-8%, the suspension is added into a microchannel reactor at the flow rate of 5-25 g/min and the flow rate of oxygen is added into the microchannel reactor at the flow rate of 3-10 g/10min, the temperature of the reactor is controlled to be 70-130 ℃, the reaction time is 50-150 s, collecting products through a condensing device, separating out the catalysts, and circulating mother liquor. The raw material adopted by the method is ethanol, at present, the price of the ethanol used as a bulk industrial raw material is about 7000 yuan/ton, and the price of the acetic acid is about 5000 yuan/ton, so that the process route for preparing the acetic acid by using the ethanol as the raw material is obviously not economical and is not suitable for industrial popularization. The price of the methanol raw material is about 2300 yuan/ton, the synthesis of the acetic acid by using the methanol as the raw material has good economic benefit, 60 percent of the existing acetic acid yield is produced by using a methanol carbonylation method, and the methanol carbonylation method is modified on the basis of the existing device as far as possible under the background that the acetic acid capacity is saturated, so that the cost is reduced and the energy is increased. If the process route of synthesizing acetic acid by an ethanol oxidation method is adopted, the compatibility of the process route with the existing reaction device for preparing acetic acid by methanol carbonylation is poor, and the process route is difficult to popularize.
The conventional kettle type reaction device for synthesizing acetic acid by methanol low-pressure carbonylation adopts a conventional mechanical stirring reactor, but a shaft seal and a bearing which adopt mechanical stirring are extremely easy to damage in long-term operation, so that the kettle type reaction device is stopped and maintained and is difficult to realize continuous and stable operation. Patent CN201010217347.3 discloses a reaction equipment for synthesizing acetic acid by methanol low pressure carbonylation, including retort and at the last discharge gate and the feed inlet of discharge gate and retort bottom on retort upper portion, the retort is connected with liquid circulation device and gas input device. Although the utility model avoids unstable factors existing in mechanical stirring and can realize effective mixing of materials in the reactor, the reaction equipment has complex structure and serious back mixing and influences the product yield. The micro-channel reactor is adopted to prepare the acetic acid, the heat transfer and mass transfer efficiency of the reactor is much higher than that of the traditional kettle type reactor, and the problems of poor material mixing effect, serious back mixing and more byproducts of the traditional kettle type reactor can be effectively solved.
Disclosure of Invention
The technical problem to be solved by the utility model is as follows: the existing reaction device for preparing acetic acid has the problems of complex structure, poor material mixing effect, serious back mixing, more byproducts and low acetic acid yield.
In order to solve the technical problems, the utility model provides a device for continuously preparing acetic acid based on a microchannel reactor, which comprises a catalyst mother liquor prefabricating system, a preheating system for preheating reaction materials, a microchannel mixing system for mixing the reaction materials, a reaction system for reaction, a separation system for separation and purification and a collection system for collecting products, wherein the preheating system is used for preheating the reaction materials; the reaction system comprises a micro-channel reactor (10), and a crude product is obtained by reaction in the micro-channel reactor (10); the separation system comprises:
a flash tank (11) for coarsely dividing the coarse product to obtain a first gas phase component and a first liquid phase component;
a rectifying tower (15) for rectifying the first gas phase component to obtain a second gas phase component and a liquid phase product after rectification;
a material circulating pump A (12) for conveying the first liquid-phase component back to the prefabrication system for recycling;
a material circulating pump B (16) for conveying the second gas-phase component back to the prefabricated system for recycling.
Preferably, the catalyst mother liquor prefabrication system comprises a prefabrication kettle (1) for preparing catalyst mother liquor; the preheating system comprises a CO preheater A (7), a methanol preheater B (8), a catalyst mother liquor preheater C (9), an injection pump A (3) for conveying CO to the preheater A for preheating, an injection pump B (2) for conveying raw material methanol to the preheater B for preheating, and an injection pump C (4) for conveying the catalyst mother liquor prepared by the prefabricating kettle (17) to the preheater C for preheating.
Preferably, the microchannel mixing system comprises:
a micro-channel mixer A (5) for mixing the preheated CO and the preheated catalyst mother liquor to obtain a reaction material A;
a microchannel mixer B (6) for mixing the reaction mass A and the preheated methanol.
Preferably, the separation system further comprises a condenser (13) for condensing the first gas-phase component and then rectifying the condensed first gas-phase component in a rectifying tower (15).
Preferably, the catalyst mother liquor preparation system further comprises a syringe pump D (1) for delivering the base catalyst, methyl iodide, water, methyl acetate and additives to the preparation kettle (17) and a gas mass flow meter (18) for delivering CO to the preparation kettle (17); in the raw materials passing through the injection pump D (1), the concentration of a catalyst is 200-1000 ppm, the concentration of methyl iodide is 5-20 wt%, the concentration of water is 2-6 wt%, the concentration of methyl acetate is 1-15 wt%, and the concentration of an additive is 5-15 wt%; the pressure of the CO conveyed to the prefabricating kettle 17 through the gas mass flow meter (18) is 0.5-1 Mpa.
Preferably, the catalyst is at least one of rhodium iodide, rhodium oxide, rhodium chloride, iridium iodide and iridium chloride; the additive is at least one of potassium iodide, potassium acetate, lithium iodide, lithium acetate, barium iodide and zinc iodide.
Preferably, the reaction temperature of the prefabricating kettle (1) is set to be 110-140 ℃, and the reaction time is set to be 1-3 h.
Preferably, the preheating temperature of the CO preheater A (7)/the methanol preheater B (8)/the catalyst mother liquor preheater C (9) is set to be 80-140 ℃.
Preferably, in the reaction materials passing through the injection pump A (3), the injection pump B (2) and the injection pump C (4), the mass ratio of the raw material methanol to the catalyst mother liquor prepared by the pre-preparation kettle (1) is 1: 3-1: 10, and the mass ratio of CO to the raw material methanol is 1: 1-1: 5.
Preferably, the reaction temperature of the microchannel reactor (10) is set to be 130-180 ℃, the reaction pressure is set to be 1.5-3 MPa, and the reaction time is set to be 30-180 s.
Preferably, the collection system includes a product collection tank (14).
Compared with the prior art, the utility model has the beneficial effects that:
1. according to the device for continuously preparing acetic acid based on the microchannel reactor, the reaction raw materials can be continuously fed, the contact is sufficient, the back mixing is less, a good environment is provided for synthesizing acetic acid by methanol carbonylation, the methanol conversion rate is high, the number of byproducts is less, and the acetic acid yield is high;
2. the micro-channel reactor adopted by the utility model has large specific surface area and high mass and heat transfer efficiency; inside the reactor, the gas contacts with the liquid film of the absorption liquid in the form of countless small bubbles to react, so that the problem that the production efficiency of acetic acid is not fully influenced by insufficient gas-liquid mass transfer in the traditional reactor is solved. Meanwhile, the microchannel reactor has large specific surface area and high heat transfer efficiency, so that the problem of inactivation of active catalyst species caused by untimely heat transfer in the reaction process is avoided;
3. the device of the utility model does not need to amplify the scale of the microchannel reactor, and only needs to correspondingly increase the number of modules to realize the numerical amplification of the reaction scale;
4. the utility model adopts the microchannel reactor, has small liquid holdup, can remove a large amount of heat in time, can reduce the possibility of accidents to the maximum extent and has high safety.
Drawings
FIG. 1 is a schematic structural diagram of a device for continuously preparing acetic acid based on a microchannel reactor;
reference numerals: 1. a syringe pump D; 2. an injection pump B; 3. an injection pump A; 4. an injection pump C; 5. a microchannel mixer A; 6. a microchannel mixer B; a CO preheater A; 8. a methanol preheater B; 9. a catalyst mother liquor preheater C; 10. a microchannel reactor; 11. a flash tank; 12. a material circulating pump A; 13. a condenser; 14. a product collection tank; 15. a rectifying tower; 16. a material circulating pump B; 17. prefabricating a kettle; 18. a gas mass flow meter.
Detailed Description
In order to make the utility model more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
The utility model provides a device for continuously preparing acetic acid based on a microchannel reactor, which comprises a catalyst mother liquor prefabricating system, a preheating system for preheating reaction materials, a microchannel mixing system for mixing the reaction materials, a reaction system for reaction, a separation system for separation and purification and a collection system for collecting products, wherein the preheating system is used for preheating the reaction materials; the reaction system comprises a micro-channel reactor 10, and a crude product is obtained by reaction in the micro-channel reactor 10; the reaction temperature of the microchannel reactor 10 is set to be 130-180 ℃, the reaction pressure is set to be 1.5-3 Mpa, and the reaction time is set to be 30-180 s; the separation system comprises:
a flash tank 11 for roughly dividing the crude product to obtain a first gas phase component and a first liquid phase component;
a condenser 13 for condensing the first gas phase component;
a rectifying tower 15 for rectifying the first gas phase component condensed by the condenser 13 to obtain a second gas phase component and a liquid phase product;
a material circulating pump A12 for conveying the first liquid-phase component back to the prefabrication system for recycling;
a material circulating pump B16 for conveying the second gas-phase component back to the prefabricated system for recycling.
The catalyst mother liquor prefabrication system comprises a prefabrication kettle 17 for preparing catalyst mother liquor, an injection pump D1 for conveying a base liquor catalyst, methyl iodide, water, methyl acetate and an additive to the prefabrication kettle 17, and a gas mass flow meter 18 for conveying CO to the prefabrication kettle 17; the CO pressure conveyed into the prefabricating kettle 17 through the gas mass flowmeter 18 is 0.5-1 Mpa, the reaction temperature of the prefabricating kettle 17 is set to be 110-140 ℃, and the reaction time is set to be 1-3 h; in the raw materials passing through the injection pump D1, the concentration of a catalyst is 200-1000 ppm, the concentration of methyl iodide is 5-20 wt%, the concentration of water is 2-6 wt%, the concentration of methyl acetate is 1-15 wt%, and the concentration of an additive is 5-15 wt%; the catalyst is at least one of rhodium iodide, rhodium oxide, rhodium chloride, iridium iodide and iridium chloride; the additive is at least one of potassium iodide, potassium acetate, lithium iodide, lithium acetate, barium iodide and zinc iodide.
The preheating system comprises a CO preheater A7, a methanol preheater B8, a catalyst mother liquor preheater C9, an injection pump A3 for conveying the CO of the synthesis gas to the preheater A for preheating, an injection pump B2 for conveying the methanol as the raw material to the preheater B for preheating and an injection pump C4 for conveying the catalyst mother liquor prepared by the pre-preparation kettle 17 to the preheater C for preheating; the preheating temperature of the CO preheater A7, the methanol preheater B8 and the catalyst mother liquor preheater C9 is set to be 80-140 ℃; in the reaction materials passing through the injection pump A3, the injection pump B2, the injection pump C4 and the gas mass flow meter 18, the mass ratio of the raw material methanol to the catalyst mother liquor prepared by the pre-preparation kettle 17 is 1: 3-1: 10, and the mass ratio of CO to the raw material methanol is 1: 1-1: 5.
The microchannel mixing system comprises:
a micro-channel mixer A5 for mixing the preheated CO and the preheated catalyst mother liquor to obtain a reaction material A;
a microchannel mixer B6 for mixing the reactant material A and the preheated methanol.
The collection system includes a product collection tank 14.
Application example 1
The device for continuously preparing the acetic acid based on the microchannel reactor is used for preparing the acetic acid and comprises the following steps:
rhodium iodide (800ppm), methyl iodide (10 wt%), lithium iodide (8 wt%), methyl acetate (6 wt%), water (4 wt%) and acetic acid are conveyed into a prefabricating kettle 17 through an injection pump D1, CO is introduced into the prefabricating kettle 17 through a mass flow meter 18, the reaction temperature is kept at 110 ℃, the system pressure is kept at 1Mpa, prefabrication is carried out for 2 hours, and the prefabricated part is reserved. And respectively sending the CO and the catalyst mother liquor into a corresponding CO preheater A7 and a corresponding catalyst mother liquor preheater C9 for preheating through an injection pump A3 and an injection pump C4, and then introducing into a microchannel mixer A5 for mixing. Then the methanol is sent into a methanol preheater B8 through an injection pump B2 for preheating and is uniformly mixed with the catalyst mother liquor in a micro-channel mixer B6, and the temperature of the preheater is controlled at 130 ℃. Then the preheated mixed liquid is sent into a micro-channel reactor 10 for reaction. The reaction product is fed into a flash tank 11 for separation, gas-phase components in the flash process are fed into a condenser 13, condensate is separated in a rectifying tower 15, and an acetic acid product is fed into a product collecting tank 14. Wherein, the liquid phase component (mainly catalyst mother liquor component) separated by flash evaporation is sent into the prefabricated kettle 17 for recycling through the material circulating pump A12, and the gas phase light component obtained by rectification is sent into the prefabricated kettle 17 for recycling through the material circulating pump B16; controlling the mass ratio of CO to methanol introduced into the microchannel reactor 10 to be 2: 1, the mass ratio of methanol to the catalyst mother liquor is 1:3, the temperature of the microchannel reactor is 140 ℃, the pressure is 1.8Mpa, and the reaction time is 100 s. After the reaction is completed, collecting the reaction product for chromatographic analysis, and obtaining the following results: the methanol conversion was 98% and the space-time yield of acetic acid was 15.3mol AcOH/(L.h).
Application example 2
The device for continuously preparing the acetic acid based on the microchannel reactor is used for preparing the acetic acid and comprises the following steps:
rhodium iodide (800ppm), methyl iodide (10 wt%), lithium iodide (8 wt%), methyl acetate (6 wt%), water (2 wt%), and acetic acid are conveyed into a prefabricating kettle 17 through an injection pump D1, CO is introduced into the prefabricating kettle 17 through a mass flow meter 18, the reaction temperature is kept at 130 ℃, the system pressure is 1Mpa, prefabrication is carried out for 3 hours, and the prefabricated part is ready for use. And sending the CO and the catalyst mother liquor into a corresponding CO preheater A7 and a corresponding catalyst mother liquor preheater C9 for preheating through an injection pump A3 and an injection pump C4 respectively, and then sending the mixture into a microchannel mixer A5 for mixing. Then the methanol is sent into a methanol preheater B8 through an injection pump B2 for preheating and is uniformly mixed with the catalyst mother liquor in a micro-channel mixer B6, and the temperature of the preheater is controlled at 130 ℃. Then the preheated mixed liquid is sent into a micro-channel reactor 10 for reaction. The reaction product is fed into a flash tank 11 for separation, gas-phase components in the flash process are fed into a condenser 13, condensate is separated in a rectifying tower 15, and an acetic acid product is fed into a product collecting tank 14. Wherein, the liquid phase component (mainly catalyst mother liquor component) separated by flash evaporation is sent into the prefabricated kettle 17 for recycling through the material circulating pump A12, and the gas phase light component obtained by rectification is sent into the prefabricated kettle 17 for recycling through the material circulating pump B16; controlling the mass ratio of CO to methanol introduced into the microchannel reactor 10 to be 2: 1, the mass ratio of methanol to the catalyst mother liquor is 1:3, the temperature of the microchannel reactor is 140 ℃, the pressure is 1.8Mpa, and the reaction time is 100 s. After the reaction is completed, collecting the reaction product for chromatographic analysis, and obtaining the following results: the methanol conversion was 99% and the space-time yield of acetic acid was 16.2mol AcOH/(L.h).
Application example 3
The device for continuously preparing the acetic acid based on the microchannel reactor is used for preparing the acetic acid and comprises the following steps:
rhodium iodide (800ppm), methyl iodide (15 wt%), lithium iodide (10 wt%), methyl acetate (10 wt%), water (2 wt%), acetic acid and CO are introduced into a prefabricating kettle 17, the reaction temperature is kept at 130 ℃, the system pressure is 1Mpa, prefabrication is carried out for 3 hours, and the prefabricated product is ready for use. The reaction scheme and purification procedure were as described in example 1. Wherein the temperature of the preheater is controlled to be 130 ℃, and the mass ratio of CO to methanol introduced into the microchannel reactor is controlled to be 2: 1, the mass ratio of methanol to the catalyst mother liquor is 1:3, the temperature of the microchannel reactor is 140 ℃, the pressure is 1.8Mpa, and the reaction time is 100 s. After the reaction is completed, collecting the reaction product for chromatographic analysis, and obtaining the following results: the methanol conversion was 99% and the space-time yield of acetic acid was 18.7mol AcOH/(L.h).
Application example 4
The device for continuously preparing the acetic acid based on the microchannel reactor is used for preparing the acetic acid and comprises the following steps:
introducing rhodium iodide (1000ppm), methyl iodide (20 wt%), lithium iodide (10 wt%), methyl acetate (10 wt%), water (2 wt%), acetic acid and CO into a prefabricating kettle 17, keeping the reaction temperature at 130 ℃, keeping the system pressure at 1Mpa, prefabricating for 3 hours, and reserving for later use after prefabricating. The reaction scheme and purification procedure were as described in example 1. Wherein the temperature of the preheater is controlled to be 130 ℃, and the mass ratio of CO to methanol introduced into the microchannel reactor is controlled to be 2: 1, the mass ratio of methanol to the catalyst mother liquor is 1:3, the temperature of the microchannel reactor is 140 ℃, the pressure is 2Mpa, and the reaction time is 100 s. After the reaction is completed, collecting the reaction product for chromatographic analysis, and obtaining the following results: the methanol conversion was 99% and the space-time yield of acetic acid was 20.3mol AcOH/(L.h).
Application example 5
The device for continuously preparing the acetic acid based on the microchannel reactor is used for preparing the acetic acid and comprises the following steps:
introducing rhodium iodide (1000ppm), methyl iodide (20 wt%), lithium iodide (15 wt%), methyl acetate (15 wt%), water (2 wt%) and CO into a prefabricating kettle 17, keeping the reaction temperature at 130 ℃ and the system pressure at 1MPa, prefabricating for 3 hours, and reserving for later use after prefabricating. The reaction scheme and purification procedure were as described in example 1. Wherein the temperature of the preheater is controlled to be 130 ℃, and the mass ratio of CO to methanol introduced into the microchannel reactor is controlled to be 3: 1, the mass ratio of methanol to the catalyst mother liquor is 1:5, the temperature of the microchannel reactor is 150 ℃, the pressure is 2Mpa, and the reaction time is 80 s. After the reaction is completed, collecting the reaction product for chromatographic analysis, and obtaining the following results: the methanol conversion was 99% and the space-time yield of acetic acid was 22.1mol AcOH/(L.h).
Application example 6
The device for continuously preparing the acetic acid based on the microchannel reactor is used for preparing the acetic acid and comprises the following steps:
introducing rhodium iodide (1000ppm), methyl iodide (20 wt%), lithium iodide (15 wt%), methyl acetate (15 wt%), water (2 wt%) and CO into a prefabricating kettle 17, keeping the reaction temperature at 130 ℃ and the system pressure at 1MPa, prefabricating for 3 hours, and reserving for later use after prefabricating. The reaction scheme and purification procedure were as described in example 1. Wherein the temperature of the preheater is controlled to be 130 ℃, and the mass ratio of CO to methanol introduced into the microchannel reactor is controlled to be 5: 1, the mass ratio of methanol to the catalyst mother liquor is 1: 7, the temperature of the microchannel reactor is 160 ℃, the pressure is 2.5Mpa, and the reaction time is 80 s. After the reaction is completed, collecting the reaction product for chromatographic analysis, and obtaining the following results: the methanol conversion was 99% and the space-time yield of acetic acid was 24.5mol AcOH/(L.h).
Application example 7
The device for continuously preparing the acetic acid based on the microchannel reactor is used for preparing the acetic acid and comprises the following steps:
introducing rhodium iodide (1000ppm), methyl iodide (20 wt%), lithium iodide (15 wt%), methyl acetate (15 wt%), water (2 wt%) and CO into a prefabricating kettle 17, keeping the reaction temperature at 130 ℃ and the system pressure at 1MPa, prefabricating for 3 hours, and reserving for later use after prefabricating. The reaction scheme and purification procedure were as described in example 1. Wherein the temperature of the preheater is controlled to be 130 ℃, and the mass ratio of CO to methanol introduced into the microchannel reactor is controlled to be 5: 1, the mass ratio of methanol to the catalyst mother liquor is 1:10, the temperature of the microchannel reactor is 160 ℃, the pressure is 2.5Mpa, and the reaction time is 80 s. After the reaction is completed, collecting the reaction product for chromatographic analysis, and obtaining the following results: the methanol conversion was 99% and the space-time yield of acetic acid was 25.3mol AcOH/(L.h).
Comparative example 1
A method for preparing acetic acid by adopting a traditional reaction kettle comprises the following steps:
introducing rhodium iodide (1000ppm), methyl iodide (20 wt%), lithium iodide (15 wt%), methyl acetate (15 wt%), water (2 wt%) and CO into a prefabricated kettle, keeping the reaction temperature at 130 ℃, keeping the system pressure at 1Mpa, and prefabricating for 3 hours. And proportionally introducing the prepared catalyst mother liquor, CO and methanol into a reaction kettle for reaction, and controlling the mass ratio of the CO to the methanol introduced into the reaction kettle to be 5: 1, the mass ratio of methanol to the catalyst mother liquor is 1:10, the temperature of the reaction kettle is 190 ℃, the pressure is 2.8Mpa, the stirring is 1500r/min, and the reaction time is 30 min. And after the reaction is finished, the reaction liquid is sent into a flash tank for separation, the gas-phase component obtained by flash evaporation is sent into a rectifying tower for separation and purification after being condensed, and the acetic acid product is obtained after collection. Returning the liquid phase component separated by flash evaporation to the reaction kettle to continue reacting. The chromatographic analysis is carried out on the collected acetic acid product, and the result is as follows: the methanol conversion was 99% and the space-time yield of acetic acid was 16.3mol AcOH/(L.h).
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way and substantially, it should be noted that those skilled in the art may make several modifications and additions without departing from the scope of the present invention, which should also be construed as a protection scope of the present invention.
Claims (4)
1. A device for continuously preparing acetic acid based on a microchannel reactor is characterized by comprising a catalyst mother liquor prefabricating system, a preheating system for preheating reaction materials, a microchannel mixing system for mixing the reaction materials, a reaction system for reaction, a separation system for separation and purification and a collection system for collecting products; the reaction system comprises a micro-channel reactor (10), and a crude product is obtained by reaction in the micro-channel reactor (10); the separation system comprises:
a flash tank (11) for coarsely dividing the coarse product to obtain a first gas phase component and a first liquid phase component;
a rectifying tower (15) for rectifying the first gas phase component to obtain a second gas phase component and a liquid phase product after rectification;
a material circulating pump A (12) for conveying the first liquid-phase component back to the prefabrication system for recycling;
a material circulating pump B (16) for conveying the second gas-phase component back to the prefabricated system for recycling.
2. The microchannel reactor-based continuous production apparatus of acetic acid according to claim 1, wherein the catalyst mother liquor preparation system comprises a preparation tank (17) for preparing the catalyst mother liquor; the preheating system comprises a CO preheater A (7), a methanol preheater B (8), a catalyst mother liquor preheater C (9), an injection pump A (3) for conveying CO to the preheater A for preheating, an injection pump B (2) for conveying raw material methanol to the preheater B for preheating, and an injection pump C (4) for conveying the catalyst mother liquor prepared by the prefabricating kettle (17) to the preheater C for preheating.
3. The apparatus for the continuous production of acetic acid based on a microchannel reactor according to claim 2, wherein the microchannel mixing system comprises:
a micro-channel mixer A (5) respectively connected with the CO preheater A (7) and the catalyst mother liquor preheater C (9);
and the micro-channel mixer B (6) is respectively connected with the micro-channel mixer A (5) and the methanol preheater B (8).
4. The device for continuously preparing the acetic acid based on the microchannel reactor is characterized in that the separation system further comprises a condenser (13) arranged between the flash tank (11) and the rectifying tower (15), and the flash tank (11), the condenser (13) and the rectifying tower (15) are connected in series; the catalyst mother liquor prefabricating system also comprises an injection pump D (1) and a gas mass flow meter (18) which are respectively connected with the prefabricating kettle (17).
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