CN112569880B - Microchannel reactor and application thereof - Google Patents

Microchannel reactor and application thereof Download PDF

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Publication number
CN112569880B
CN112569880B CN201910943504.XA CN201910943504A CN112569880B CN 112569880 B CN112569880 B CN 112569880B CN 201910943504 A CN201910943504 A CN 201910943504A CN 112569880 B CN112569880 B CN 112569880B
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channel
reaction
microchannel reactor
section
preheating
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CN112569880A (en
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储博钊
钟思青
何乐路
王菊
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
    • C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
    • C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D207/24—Oxygen or sulfur atoms
    • C07D207/26—2-Pyrrolidones
    • C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
    • C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00783—Laminate assemblies, i.e. the reactor comprising a stack of plates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00822—Metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00824—Ceramic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00853—Employing electrode arrangements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00873—Heat exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00889—Mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00891—Feeding or evacuation
    • B01J2219/00894—More than two inlets

Abstract

The invention relates to a microchannel reactor and application thereof, comprising a substrate (3) and a fluid channel (4), wherein the substrate (3) comprises an upper substrate and a lower substrate; the fluid channel (4) is formed by laminating the upper substrate and the lower substrate, and the fluid channel (4) comprises a preheating section channel (6), a mixing section channel (7) and a reaction section channel (8). The micro-channel reactor provided by the invention utilizes the micro-scale effect to effectively limit the size of bubbles in the multiphase fluid in the whole process, and can ensure high-efficiency mixing efficiency and good safety in the whole process flow.

Description

Microchannel reactor and application thereof
Technical Field
The invention belongs to the field of micro-channel devices, and particularly relates to a micro-channel reactor and application thereof.
Background
The microchannel technology is a process strengthening technology for carrying out chemical reaction, heat exchange, mixing and separation in a three-dimensional structure process fluid channel with a characteristic dimension of micron, can obviously improve the heat and mass transfer efficiency and the space utilization rate, realizes the accurate control of reaction conditions, and has intrinsic safety. In recent years, microchannel reaction technology has been rapidly developed in the fields of fine chemical engineering and pharmaceutical chemical engineering.
Because the microchannel reaction technology can realize the characteristics of high-efficiency conversion and continuous production, the method has obvious advantages and wide application prospect compared with the traditional batch kettle technology in the process of synthesizing fine chemicals with severe thermal effect. However, there are many heterogeneous reaction processes with complex processes in the fine chemical industry, and many production processes of high-added-value fine chemical products comprise various processes such as heat transfer, mixing, reaction, separation, and even external field strengthening, and although accurate regulation and control on the production process of the products can be realized in a microchannel reactor, the conventional continuous flow synthesis technology does not have very mature commercial products and process routes in the aspect of heterogeneous system multi-process coupling.
Chinese patent CN 101391974a discloses a method for synthesizing N-vinyl pyrrolidone by continuous flow, which strengthens gas-liquid mixing efficiency by using metal membrane tube material of a membrane dispersion type reactor, but a distributor made of metal membrane tube material is only arranged below the reactor, and micro-size limitation after fluid contact is absent above the reactor, so that gas phase raw materials are easy to form bubbles with larger scale by collision coalescence and other actions above the reactor, and therefore, the reactor has limited promotion degree compared with the traditional process in terms of process efficiency and safety.
Disclosure of Invention
In order to solve the above problems, the first aspect of the present invention provides a microchannel reactor, where the microchannel reactor uses the microscale effect to effectively limit the size of bubbles in a multiphase fluid, so as to ensure efficient mixing efficiency and good safety in the whole process.
The second aspect of the invention provides a method for strengthening the gas-liquid heterogeneous mixing-external electric field reaction coupling process based on the microchannel technology, which has better applicability, can be used for continuous processes of various gas-liquid reaction systems, and has more obvious effect especially for the process of synthesizing NVP by an acetylene method.
According to a first aspect of the invention, the microchannel reactor comprises a base plate (3) and a fluid channel (4), the base plate (3) comprising an upper base plate and a lower base plate; the fluid channel (4) is formed by laminating the upper substrate and the lower substrate, and the fluid channel (4) comprises a preheating section channel (6), a mixing section channel (7) and a reaction section channel (8).
According to some embodiments of the invention, the upper and lower substrates have a matched groove structure.
According to some embodiments of the invention, the groove structure of the upper substrate and the groove structure of the lower substrate are symmetrical.
According to some embodiments of the invention, the groove structure of the upper substrate is the same as the groove structure of the lower substrate.
According to some embodiments of the invention, the groove structure may be referred to as a micro-scale structure.
According to some embodiments of the invention, the material of the substrate (3) is selected from one or more of metals and ceramics, preferably from one or more of alloys and ceramics, more preferably from one or more of stainless steel 316L, hastelloy C and silicon carbide ceramics.
According to some embodiments of the invention, the thickness of the substrate is 2-8cm.
According to some embodiments of the invention, the pre-heating stage channels (6) have a hydraulic diameter of 300-3000 μm, preferably 500-2000 μm, more preferably 1000-1500 μm.
According to some embodiments of the invention, the preheating section channels comprise a gas phase preheating channel (6 a) and a liquid phase preheating channel (6 b).
According to some embodiments of the invention, the length of the gas phase preheating passage is 2-20 cm, preferably 3-15 cm, more preferably 5-10 cm.
According to some embodiments of the invention, the length of the liquid phase preheating channels is 2-20 cm, preferably 3-15 cm, more preferably 5-10 cm.
According to some embodiments of the invention, the length of the gas phase preheating channel and the liquid phase preheating channel are the same.
According to some embodiments of the invention, the hydraulic diameter of the mixing section channel (7) is 200-2000 μm, preferably 300-1500 μm, more preferably 300-500 μm.
According to some embodiments of the invention, the mixing section channel comprises a gas phase inlet channel (7 a), a liquid phase inlet channel (7 b) and a mixing outlet channel (7 c), wherein an included angle between the gas phase inlet channel and the liquid phase inlet channel is 20-120 ℃, preferably 30-100 ℃, more preferably 60-90 ℃.
According to some embodiments of the invention, the length of the gas phase inlet passage is 1-10 cm, preferably 2-5 cm; and/or the length of the liquid phase inlet channel is 1-10 cm, preferably 2-5 cm; and/or the length of the mixing outlet channel is 1-10 cm, preferably 2-5 cm.
According to some embodiments of the invention, the lengths of the gas phase inlet channel, the liquid phase inlet channel and the mixing outlet channel are all the same.
According to some embodiments of the invention, the hydraulic diameter of the reaction zone channel (8) is 200-2000 μm, preferably 300-1500 μm, more preferably 300-800 μm.
According to some embodiments of the invention, the length of the reaction section channel (8) is 10-200 cm, preferably 30-150 cm, more preferably 50-100cm.
According to some embodiments of the invention, the hydraulic diameter of the preheating section channel (6) is larger than the hydraulic diameter of the mixing section channel (7), and the hydraulic diameter of the preheating section channel (6) is larger than the hydraulic diameter of the reaction section channel (8).
According to some embodiments of the invention, the hydrodynamic diameter of the mixing section channel (7) is equal to the hydrodynamic diameter of the reaction section channel (8)
According to some embodiments of the invention, further comprising a metal foam inner member (9).
According to some embodiments of the invention, the metal foam internals include a Y-shaped metal foam internals located in the mixing section channel and an I-shaped metal foam internals located in the reaction section channel.
According to some embodiments of the invention, the Y-shaped metal foam internals are sized to conform to the size of the mixing segment channels.
According to some embodiments of the invention, the length of the I-shaped metal foam internals in the reaction zone channel is 1-3cn, the spacing is 5-25cm, preferably 10-20cm.
According to some embodiments of the invention, the metal foam internals are selected from one or more of aluminum foam internals, iron foam internals, nickel foam internals, titanium foam internals and copper foam internals.
According to some embodiments of the invention, the micropores of the metal foam inner member have a hydraulic diameter of 10-100 μm, preferably 30-100 μm, and a porosity of 50% -95%, preferably 50% -90%.
According to some embodiments of the invention, an electrode arrangement (5) is also comprised, comprising two electrode plates, preferably with a spacing of 5-30cm, preferably 10-20cm.
According to some embodiments of the invention, the electric field strength of the electrode arrangement is 10-100V/m, preferably 20-50V/m.
According to some embodiments of the invention, the substrate is disposed between two electrode plates of the electrode device, preferably the reaction section channel of the substrate is disposed between two electrode plates of the electrode device.
According to a second aspect of the invention, the method for strengthening the coupling process of the gas-liquid heterogeneous mixing reaction comprises the step of carrying out the gas-liquid heterogeneous mixing reaction in the reactor.
According to some embodiments of the invention, the method comprises the steps of:
(1) The gas-phase raw material and the liquid-phase raw material enter a fluid channel (4) of the substrate (3) from a gas-phase raw material inlet (1 a) and a liquid-phase raw material inlet (1 b) respectively and are preheated in a preheating section channel (6) of the fluid channel (4);
(2) The preheated gas phase raw material and the liquid phase raw material are dispersed and mixed in a mixing section channel (7) of the fluid channel (4) through a Y-shaped metal foam inner member (9);
(3) The mixed gas phase raw material and liquid phase raw material react in a reaction section channel (8) of the fluid channel (4), preferably, two-phase fluid in the reaction section channel (8) is subjected to the strengthening effect of an external electric field formed by the electrode device (5).
In some preferred embodiments of the present invention, the method for strengthening the coupling process of gas-liquid heterogeneous mixing-external electric field reaction adopts a microchannel reactor, which comprises the following steps:
(1) The gas phase raw material and the liquid phase raw material are preheated in the micro-channel reactor, wherein the gas phase raw material and the liquid phase raw material enter a fluid channel (4) of a substrate (3) through a gas phase raw material inlet (1 a) and a liquid phase raw material inlet (1 b) respectively, and are preheated to a certain temperature in a preheating section channel (6) of the fluid channel (4);
The microchannel reactor comprises: a raw material inlet (1), a product outlet (2), a substrate (3), a microfluidic channel (4) and an electrode device (5); the fluid channel includes: a preheating section channel (6), a mixing section channel (7), a reaction section channel (8) and a built-in metal foam inner member (9);
(2) The gas phase raw material and the liquid phase raw material are mixed in a micro-channel reactor, wherein the mixing process is that the preheated gas phase raw material and the liquid phase raw material are mutually contacted after being dispersed in a mixing section channel (7) of a micro-scale fluid channel (4) through a Y-shaped metal foam inner member (8);
(3) The gas phase raw material and the liquid phase raw material are reacted in the micro-channel reactor, wherein the reaction process is that the mixed two-phase fluid reacts in a reaction section channel (8) of a fluid channel (4), the two-phase fluid in the reaction section channel (8) is subjected to the strengthening effect of an external electric field formed by an externally loaded electrode device (5), and the reacted product is discharged from a product outlet (2).
The micro-channel reactor provided by the invention can be used for carrying out a mixed reaction coupling strengthening process of a heterogeneous system under the condition of an external electric field, heterogeneous raw materials enter the micro-reactor for carrying out mixed contact and carrying out a reaction process, the external electric field is formed in a reaction area by adopting an external electrode plate mode to improve the catalyst efficiency, the efficient implementation of a complex heterogeneous reaction process is realized, and the micro-channel reactor can be used for the fields of carrying out mixed reaction and strengthening the external electric field coupling process by a micro-channel technology.
In a third aspect of the invention, there is provided the use of a microchannel reactor as described above or of a process as described above in a gas-liquid heterogeneous mixing reaction, in particular in the synthesis of N-vinylpyrrolidone.
The above preferred conditions can be arbitrarily combined on the basis of not deviating from the common knowledge in the art, and thus, each preferred embodiment of the present invention can be obtained.
Drawings
FIG. 1 is a schematic diagram of a microchannel reactor according to the present invention.
Fig. 2 is a schematic view of a fluid channel structure according to the present invention.
In fig. 1: 1-a raw material inlet; 2-product outlet; 3-a substrate; 4-fluid channels; 5-electrode means.
In fig. 2: 1 a-a gas phase feed inlet; 1 b-liquid phase raw material inlet; 2-product outlet; 6-preheating section channel; 6 a-a gas phase preheating channel; 6 b-a liquid phase preheating channel; 7-mixing section channels; 7 a-a gas phase inlet channel; 7 b-a liquid phase inlet channel; 7 c-a mixing outlet channel; 8-reaction section channels; 9-metal foam inner member.
Detailed Description
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The following examples were carried out in microreactors according to the requirements of the process of the invention.
The preparation method of the catalyst pyrrolidone potassium salt comprises the following steps:
1. Mixing a certain amount of potassium hydroxide with pyrrolidone, and rapidly placing in a rotary evaporator;
2. the rotary evaporator is started to carry out reduced pressure distillation for 2 hours at 120 ℃ under the vacuum environment (50 mbar), and nitrogen purging is carried out once every 30 minutes to carry out residual moisture;
3. and rapidly taking out the liquid phase product after the reduced pressure distillation is finished, and sealing the liquid phase product in a wide-mouth bottle for standby.
[ example 1 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 2 percent and the mass fraction of the auxiliary is 2 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 30V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 500ms, and the residence time of the reaction section is controlled to be 20min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis showed an acetylene conversion of 82.2% and an N-vinylpyrrolidone selectivity of 95.6%.
[ example 2 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1500 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis showed an acetylene conversion of 81.2% and an N-vinylpyrrolidone selectivity of 95.7%.
[ example 3 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 5 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis shows that the conversion of acetylene is 80.8% and the selectivity of N-vinyl pyrrolidone is 95.4%.
[ example 4 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the channel hydraulics diameter of the mixing section is 1000 micrometers, the total length of the gas phase inlet channel and the liquid phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the micropore hydraulics diameter of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the mixing section inlet channel and the outlet channel; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis showed a conversion of acetylene of 76.1% and a selectivity of 94.4% for N-vinylpyrrolidone.
[ example 5 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 5 centimeters, the total length of the mixing outlet channel is 5 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis showed an acetylene conversion of 83.2% and an N-vinylpyrrolidone selectivity of 95.1%.
[ example 6 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 90 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron inner member arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis showed an acetylene conversion of 81.0% and an N-vinylpyrrolidone selectivity of 94.3%.
[ example 7 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the channel hydraulics diameter of the mixing section is 500 micrometers, the total length of the gas phase inlet channel and the liquid phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 30 ℃, the micropore hydraulics diameter of the Y-shaped foam iron inner member arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the mixing section inlet channel and the outlet channel; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis shows that the conversion rate of acetylene is 80.8% and the selectivity of N-vinyl pyrrolidone is 93.6%.
TABLE 1
Figure SMS_1
[ example 8 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 100 micrometers, the porosity is 80 percent, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis showed that the conversion of acetylene was 78.2% and the N-vinylpyrrolidone selectivity was 92.6%.
[ example 9 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 50%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis shows that the conversion of acetylene is 75.7% and the selectivity of N-vinyl pyrrolidone is 93.3%.
[ example 10 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 800 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis showed a conversion of acetylene of 76.8% and a selectivity of 94.3% for N-vinylpyrrolidone.
[ example 11 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the channel hydraulics diameter of the mixing section is 300 micrometers, the total length of the gas phase inlet channel and the liquid phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the micropore hydraulics diameter of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the mixing section inlet channel and the outlet channel; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis showed that the conversion of acetylene was 84.8% and the N-vinylpyrrolidone selectivity was 95.4%.
[ example 12 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 50 centimeters, the microporous hydraulic diameter and the porosity of the I-type foam iron inner member arranged in the channel are consistent with those of the Y-type foam iron inner member, the length of each I-type foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis shows that the conversion of acetylene is 75.3% and the selectivity of N-vinyl pyrrolidone is 95.1%.
[ example 13 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 1 centimeter, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis shows that the conversion of acetylene is 79.0% and the selectivity of N-vinyl pyrrolidone is 93.8%.
[ example 14 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 20 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis showed an acetylene conversion of 80.2% and an N-vinylpyrrolidone selectivity of 94.3%.
TABLE 2
Figure SMS_2
[ example 15 ]
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary agent diethylene glycol dimethyl ether (wherein the mass fraction of the catalyst is 2%, and the mass fraction of the auxiliary agent is 2%); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 30V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 500ms, and the residence time of the reaction section is controlled to be 20min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis showed an acetylene conversion of 81.2% and an N-vinylpyrrolidone selectivity of 94.6%.
[ example 16 ]
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 5 percent and the mass fraction of the auxiliary is 5 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 30V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 500ms, and the residence time of the reaction section is controlled to be 20min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis showed that the conversion of acetylene was 84.5% and the N-vinylpyrrolidone selectivity was 96.0%.
[ example 17 ]
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 2 percent and the mass fraction of the auxiliary is 2 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 80%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 30V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 500ms, and the residence time of the reaction section is controlled to be 20min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis showed an acetylene conversion of 84.8% and an N-vinylpyrrolidone selectivity of 94.1%.
Example 18
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 2 percent and the mass fraction of the auxiliary is 2 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.2:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 30V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 500ms, and the residence time of the reaction section is controlled to be 20min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis showed 68.2% conversion of acetylene and 91.1% selectivity to N-vinylpyrrolidone.
[ example 19 ]
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 2 percent and the mass fraction of the auxiliary is 2 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 150 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 30V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 500ms, and the residence time of the reaction section is 20min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis showed an acetylene conversion of 82.5% and an N-vinylpyrrolidone selectivity of 95.3%.
[ example 20 ]
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 2 percent and the mass fraction of the auxiliary is 2 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 150 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 30V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 500ms, and the residence time of the reaction section is 20min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis shows that the conversion of acetylene is 70.1% and the selectivity of N-vinyl pyrrolidone is 95.8%.
[ example 21 ]
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 2 percent and the mass fraction of the auxiliary is 2 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.5MPa, the strength of an external electric field is 30V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 500ms, and the residence time of the reaction section is controlled to be 20min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis shows that the conversion of acetylene is 74.3% and the selectivity of N-vinyl pyrrolidone is 93.7%.
TABLE 3 Table 3
Figure SMS_3
[ example 22 ]
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 2 percent and the mass fraction of the auxiliary is 2 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 10V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 500ms, and the residence time of the reaction section is controlled to be 20min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis showed 75.2% conversion of acetylene and 94.6% selectivity to N-vinylpyrrolidone.
Example 23
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 2 percent and the mass fraction of the auxiliary is 2 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 30V/m, the flow of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 200ms, and the residence time of the reaction section is controlled to be 20min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis shows that the conversion of acetylene is 80.5% and the selectivity of N-vinyl pyrrolidone is 95.0%.
[ example 24 ]
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 2 percent and the mass fraction of the auxiliary is 2 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 30V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 800ms, and the residence time of the reaction section is controlled to be 20min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis showed an acetylene conversion of 83.8% and an N-vinylpyrrolidone selectivity of 95.2%.
[ example 25 ]
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 2 percent and the mass fraction of the auxiliary is 2 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 30V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 500ms, and the residence time of the reaction section is controlled to be 10min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis shows that the conversion of acetylene is 72.8% and the selectivity of N-vinyl pyrrolidone is 96.0%.
[ example 26 ]
(1) Building a device: the same as in example 1.
(2) NVP synthesis: a metering pump is used for conveying liquid-phase raw materials, and the raw materials comprise alpha-pyrrolidone, catalyst pyrrolidone potassium salt and catalyst auxiliary polytetrahydrofuran (wherein the mass fraction of the catalyst is 2 percent and the mass fraction of the auxiliary is 2 percent); the gas phase feed was delivered using a mass flow meter and consisted of feed acetylene with inert gas nitrogen (where the acetylene volume fraction was 50%). The molar flow ratio of the main raw materials in the metering pump and the mass flowmeter is set as acetylene: pyrrolidone=0.1:1. The two materials are preheated to 120 ℃ in a preheating section of a microscale fluid channel, enter a mixing section for full contact, enter a reaction section for pyrrolidone vinyl reaction, the reaction temperature is set to be 180 ℃, the reaction pressure is 0.8MPa, the strength of an external electric field is 30V/m, the flow rate of a metering pump and a mass flowmeter is regulated, the residence time of the reaction materials in the mixing section is controlled to be 500ms, and the residence time of the reaction section is 30min. The material at the outlet of the micro-channel reactor product can be separated by gas-liquid separation to obtain crude N-vinyl pyrrolidone. The product analysis showed an acetylene conversion of 85.5% and an N-vinylpyrrolidone selectivity of 94.2%.
TABLE 4 Table 4
Figure SMS_4
[ example 27 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 500 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. The product analysis showed an acetylene conversion of 83.3% and an N-vinylpyrrolidone selectivity of 95.2%.
[ example 28 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 2000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 79.8%, and the N-vinylpyrrolidone selectivity was 96.0%.
[ example 29 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 3 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 78.8%, and the N-vinylpyrrolidone selectivity was 96.5%.
[ example 30 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 15 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 83.6%, and the N-vinylpyrrolidone selectivity was 95.1%.
Example 31
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 100 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80 percent, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 80.4%, and the N-vinylpyrrolidone selectivity was 93.9%.
[ example 32 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 300 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 82.9%, and the N-vinylpyrrolidone selectivity was 95.4%.
[ example 33 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 1500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 83.6%, and the N-vinylpyrrolidone selectivity was 94.9%.
TABLE 3 Table 3
Figure SMS_5
Example 34
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 100 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80 percent, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 30 centimeters, the micropore hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 70.8%, and the N-vinylpyrrolidone selectivity was 96.5%.
[ example 35 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 150 centimeters, the microporous hydraulic diameter and the porosity of the I-type foam iron inner member arranged in the channel are consistent with those of the Y-type foam iron inner member, the length of each I-type foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 84.4%, and the N-vinylpyrrolidone selectivity was 94.4%.
Example 36
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 30 micrometers, the porosity is 80%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 84.1%, and the N-vinylpyrrolidone selectivity was 95.8%.
Example 37
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the microporous hydraulic diameter of the Y-shaped foam iron internal component arranged in the channel is 150 micrometers, the porosity is 80 percent, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 75.4%, and the N-vinylpyrrolidone selectivity was 93.1%.
[ example 38 ]
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 30%, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 73.2%, and the N-vinylpyrrolidone selectivity was 92.7%.
Example 39
(1) Building a device: the micro-channel reactor main body is formed by processing stainless steel 316L, micron-sized notch grooves are manufactured on a stainless steel substrate through precision machining, the substrates at the two sides are pressed and sealed to form a micron-sized channel, foam iron inner components are arranged in part of channel positions, and the specific arrangement and the specific size are as follows: the channel hydraulic diameter of the preheating section is 1000 micrometers, and the total length of the gas phase preheating channel and the liquid phase preheating channel is 10 cm; the hydraulic diameter of the channel of the mixing section is 500 micrometers, the total length of the gas-phase inlet channel and the liquid-phase inlet channel is 2 centimeters, the total length of the mixing outlet channel is 2 centimeters, the included angle of the inlet channel is 60 ℃, the hydraulic diameter of the micropore of the Y-shaped foam iron internal component arranged in the channel is 50 micrometers, the porosity is 90 percent, and the size is consistent with the length of the inlet channel and the outlet channel of the mixing section; the hydraulic diameter of the channel of the reaction section is 500 micrometers, the total length of the reaction channel is 100 centimeters, the microporous hydraulic diameter and the porosity of the I-shaped foam iron inner member arranged in the channel are consistent with those of the Y-shaped foam iron inner member, the length of each I-shaped foam iron inner member in the reaction channel is 2 centimeters, and the interval is 10 centimeters.
Referring to the schematic diagram of the device shown in fig. 1, a microchannel reactor is built to synthesize an NVP device, a microchannel reaction substrate of a microscale fluid channel is arranged in the middle of an electrode device, the electrode device applies an external electric field to a reaction section of the microscale fluid channel, the microchannel reaction substrate is subjected to temperature control through a cold and hot integrated machine, and a crude NVP product can be collected from a product outlet.
(2) NVP synthesis: the same as in example 1. As a result of analysis of the product, the conversion of acetylene was 84.2%, and the N-vinylpyrrolidone selectivity was 95.3%.
TABLE 4 Table 4
Figure SMS_6
It should be noted that the above-described embodiments are only for explaining the present invention and do not limit the present invention in any way. The invention has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the invention as defined in the appended claims, and the invention may be modified without departing from the scope and spirit of the invention. Although the invention is described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, as the invention extends to all other means and applications which perform the same function.

Claims (39)

1. A microchannel reactor comprises a metal foam inner member (9), a base plate (3), an electrode device (5) and a fluid channel (4),
the base plate (3) comprises an upper base plate and a lower base plate, the fluid channel (4) is formed by pressing the upper base plate and the lower base plate,
the fluid channel (4) comprises a preheating section channel (6), a mixing section channel (7) and a reaction section channel (8),
the electrode device (5) comprises two electrode plates, the substrate (3) is arranged between the two electrode plates of the electrode device (5),
the metal foam inner member (9) comprises a Y-shaped metal foam inner member positioned in the mixing section channel and an I-shaped metal foam inner member positioned in the reaction section channel, wherein the hydraulic diameter of micropores of the Y-shaped metal foam inner member and the hydraulic diameter of micropores of the I-shaped metal foam inner member are 30 mu m.
2. The microchannel reactor of claim 1, wherein the upper and lower base plates have a conforming groove structure; and/or the number of the groups of groups,
the material of the substrate is one or more selected from metal and ceramic; and/or the number of the groups of groups,
the thickness of the substrate is 2-8cm.
3. The microchannel reactor of claim 2, wherein the substrate is of a material selected from one or more of an alloy and a ceramic.
4. The microchannel reactor of claim 2, wherein the substrate is of a material selected from one or more of stainless steel 316L, hastelloy C, and silicon carbide ceramic.
5. Microchannel reactor according to any one of claims 1 to 4, characterized in that the hydraulic diameter of the preheating section channels (6) is 300-3000 μm.
6. The microchannel reactor according to claim 5, characterized in that the pre-heating stage channels (6) have a hydraulic diameter of 500-2000 μm.
7. The microchannel reactor according to claim 5, characterized in that the hydraulic diameter of the preheating section channels (6) is 1000-1500 μm.
8. The microchannel reactor according to any one of claims 1 to 4, wherein the preheating section channels comprise a gas phase preheating channel (6 a) and a liquid phase preheating channel (6 b), the length of the gas phase preheating channel being 2 to 20 cm; and/or the number of the groups of groups,
the length of the liquid phase preheating channel is 2-20 cm.
9. The microchannel reactor of claim 8, wherein the gas phase preheating channels have a length of 3-15 cm.
10. The microchannel reactor of claim 8, wherein the gas phase preheating channels have a length of 5-10 cm.
11. The microchannel reactor of claim 8, wherein the length of the liquid phase preheat channel is 3-15 cm.
12. The microchannel reactor of claim 8, wherein the length of the liquid phase preheat channel is from 5 to 10 cm.
13. The microchannel reactor of claim 8, wherein the gas phase preheating channels and the liquid phase preheating channels are the same length.
14. Microchannel reactor according to any of claims 1-4, characterized in that the hydrodynamic diameter of the mixing section channel (7) is 200-2000 μm.
15. Microchannel reactor according to claim 14, characterized in that the hydrodynamic diameter of the mixing section channel (7) is 300-1500 μm.
16. Microchannel reactor according to claim 14, characterized in that the hydrodynamic diameter of the mixing section channel (7) is 300-500 μm.
17. The microchannel reactor according to any one of claims 1-4, wherein the mixing section channel comprises a gas phase inlet channel (7 a), a liquid phase inlet channel (7 b) and a mixing outlet channel (7 c), the gas phase inlet channel and the liquid phase inlet channel having an angle of 20 ℃ to 120 ℃.
18. The microchannel reactor according to claim 17, wherein the angle between the gas phase inlet channel and the liquid phase inlet channel is 30 ℃ to 100 ℃; and/or the number of the groups of groups,
the length of the gas phase inlet channel is 1-10 cm; and/or the number of the groups of groups,
the length of the liquid phase inlet channel is 1-10 cm; and/or the number of the groups of groups,
the length of the mixing outlet channel is 1-10 cm.
19. The microchannel reactor according to claim 17, wherein the gas phase inlet channel and the liquid phase inlet channel have an included angle of 60 ℃ to 90 ℃; and/or the number of the groups of groups,
the length of the gas phase inlet channel is 2-5 cm; and/or the number of the groups of groups,
the length of the liquid phase inlet channel is 2-5 cm; and/or the number of the groups of groups,
the length of the mixing outlet channel is 2-5 cm.
20. The microchannel reactor of claim 17, wherein the gas phase inlet channel, liquid phase inlet channel, and mixing outlet channel are all the same length.
21. Microchannel reactor according to any of claims 1-4, characterized in that the hydrodynamic diameter of the reaction zone channel (8) is 200-2000 μm; the length of the reaction section channel is 10-200 cm; and/or;
the hydraulic diameter of the preheating section channel (6) is larger than that of the mixing section channel (7), and the hydraulic diameter of the preheating section channel (6) is larger than that of the reaction section channel (8).
22. The microchannel reactor according to claim 21, characterized in that the hydrodynamic diameter of the reaction zone channel (8) is 300-1500 μm; the length of the reaction section channel is 30-150 cm.
23. Microchannel reactor according to claim 21, characterized in that the hydrodynamic diameter of the reaction zone channel (8) is 300-800 μm; the length of the reaction section channel is 50-100cm.
24. Microchannel reactor according to any of claims 1-4, characterized in that the hydrodynamic diameter of the mixing section channel (7) is equal to the hydrodynamic diameter of the reaction section channel (8).
25. The microchannel reactor of any one of claims 1-4, wherein the Y-shaped metal foam internals are sized to correspond to the size of the mixing segment channels; and/or the length of the I-shaped metal foam inner member in the reaction section channel is 1-3cm, and the interval is 5-25cm.
26. The microchannel reactor of claim 25, wherein the distance between the inner members of the type I metal foam within the reaction zone channel is between 10 cm and 20cm.
27. The microchannel reactor of any one of claims 1-4, wherein the metal foam internals are selected from one or more of aluminum foam internals, iron foam internals, nickel foam internals, titanium foam internals, and copper foam internals.
28. The microchannel reactor of any one of claims 1-4, wherein the metal foam internals have a porosity of 50% -95%.
29. The microchannel reactor of claim 28, wherein the metal foam internals have a porosity of 50% -90%.
30. The microchannel reactor according to any one of claims 1-4, wherein the electrode arrangement has an electric field strength of 10-100V/m.
31. The microchannel reactor of any one of claims 1-4, wherein the electrode plate spacing is 5-30cm.
32. The microchannel reactor of any one of claims 1-4, wherein the electrode plate spacing is 10-20cm.
33. The microchannel reactor according to any one of claims 1-4, wherein the electrode arrangement has an electric field strength of 20-50V/m.
34. The microchannel reactor according to any one of claims 1 to 4, wherein the reaction zone channel of the substrate is disposed between two electrode plates of the electrode device.
35. A method for enhancing the coupling process of a gas-liquid heterogeneous mixing reaction, comprising carrying out the gas-liquid heterogeneous mixing reaction in the microchannel reactor of any one of claims 1-34.
36. The method according to claim 35, comprising the steps of:
(1) The gas-phase raw material and the liquid-phase raw material enter a fluid channel (4) of the substrate (3) from a gas-phase raw material inlet (1 a) and a liquid-phase raw material inlet (1 b) respectively and are preheated in a preheating section channel (6) of the fluid channel (4);
(2) The preheated gas phase raw material and the liquid phase raw material are dispersed and mixed in a mixing section channel (7) of the fluid channel (4) through a Y-shaped metal foam inner member;
(3) The mixed gas phase raw material and liquid phase raw material react in a reaction section channel (8) of the fluid channel (4).
37. A method according to claim 36, characterized in that the two-phase fluid in the reaction zone channel (8) is subjected to an applied electric field intensification by the electrode means (5).
38. Use of a microchannel reactor according to any one of claims 1-34 or a method according to any one of claims 35-37 in a gas-liquid heterogeneous mixing reaction.
39. The use according to claim 38, characterized in that it is in the synthesis of N-vinylpyrrolidone.
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