CN219580555U - Anacardol continuous flow synthesizer - Google Patents
Anacardol continuous flow synthesizer Download PDFInfo
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- CN219580555U CN219580555U CN202320242806.6U CN202320242806U CN219580555U CN 219580555 U CN219580555 U CN 219580555U CN 202320242806 U CN202320242806 U CN 202320242806U CN 219580555 U CN219580555 U CN 219580555U
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The utility model discloses a cardanol continuous flow synthesis device. The utility model relates to a cardanol continuous flow synthesis device which comprises a temperature raising unit, a gas-liquid separation reaction unit and a cooling unit which are sequentially connected in series; wherein, the temperature raising unit and the temperature lowering unit are continuous reactors; the gas-liquid separation reaction unit has gas permeability; the cooling unit is used for cooling the product obtained by the decarboxylation reaction. The continuous flow synthesis device for cardanol can efficiently, safely and rapidly synthesize cardanol.
Description
Technical Field
The utility model relates to a cardanol continuous flow synthesis device.
Background
At present, cardanol is industrially obtained by pyrolyzing cashew nut shell oil, the temperature is an important factor influencing the reaction of cashew nut acid decarboxylation to generate cardanol, the higher the temperature is, namely the higher the energy provided by a reaction system is, and the reaction can be normally carried out only when the energy is high enough to destroy the carboxyl activation energy in cashew nut acid molecules. Therefore, the reaction does not occur at low temperature (130 ℃), and the cardanol content in the product gradually increases with the increase of the temperature, so that the cardanic acid is completely converted to 180 ℃. The decarboxylation reaction of the cardanol is rapid, the cardanol content in the product at the initial stage of the reaction can be rapidly increased, the peak value is reached when the reaction reaches 30min, and after 30min, the high temperature can cause the intermolecular self-polymerization of the cardanol, so that the cardanol content in the product is reduced, and the pyrolysis time is not suitable to be excessively long.
The traditional process of cardanol synthesis in the prior art is an intermittent process carried out in a reaction kettle, and the phenomenon of uneven mixing and heat transfer exists in a reaction system in the actual production process due to the amplification effect of the reaction kettle, so that the reaction is insufficient or excessive, the production process is unstable, and the quality of a product is further influenced. On the other hand, the reaction is decarboxylation reaction, a large amount of carbon dioxide gas is discharged after the reaction is initiated at high temperature, the hidden danger of flushing is caused, the reaction quantity needs to be limited for controlling the reaction risk, and the production efficiency is reduced. Finally, in order to avoid the risks of flushing, even explosion and the like caused by too severe reaction process, the temperature rise and the reaction time of the traditional process often need to be as long as 5-6 hours, and the product is kept at high temperature for a long time to cause side reactions such as polymerization and the like, so that the phenol content in the reaction liquid can be further reduced, and the quality and the yield are affected. Therefore, it is difficult to maintain a high temperature of 180 ℃ while securing safety in the conventional tank process, and to separate the product within a prescribed time under the high temperature condition.
Therefore, it is desirable to provide a continuous flow synthesis device for cardanol to achieve efficient, rapid and safe synthesis of cardanol.
Disclosure of Invention
The utility model provides a cardanol continuous flow synthesis device, which aims to solve the defects that the reaction process is unstable, the quality of products is further influenced, the flushing material exists in the reaction process and the like caused by uneven heating of reaction feed liquid in the process of preparing cardanol by the traditional kettle type process. The continuous flow synthesis device for cardanol can efficiently, safely and rapidly synthesize cardanol.
The utility model provides a cardanol continuous flow synthesis device, which comprises a temperature raising unit, a gas-liquid separation reaction unit and a cooling unit which are sequentially connected in series;
wherein, the temperature raising unit and the temperature lowering unit are continuous reactors; the gas-liquid separation reaction unit comprises a heating inner pipe, a reaction pipe and a gas collecting pipe, wherein the heating inner pipe, the reaction pipe and the gas collecting pipe are coaxially fixed in sequence from the center to the outside to form a sleeve, an annular gap between the outer wall surface of the heating inner pipe and the wall surface of the reaction pipe forms a micro-channel reaction zone, the micro-channel reaction zone is provided with a feed inlet and a discharge outlet, the wall surface of the reaction pipe adjacent to the gas collecting pipe in the micro-channel reaction zone is a gas selective permeable membrane, and the heating inner pipe is provided with a heat conducting medium inlet and a heat conducting medium outlet;
wherein the temperature raising unit is used for preheating the reaction feed liquid; the gas-liquid separation reaction unit is used for decarboxylation reaction of the reaction feed liquid; the cooling unit is used for cooling the product obtained by the decarboxylation reaction.
In the present utility model, the heating inner tube is preferably a metal tube.
In the present utility model, the gas collecting pipe is preferably a metal pipe.
In the present utility model, the heat conducting medium may be a heat conducting oil.
The gas-liquid separation reaction unit can enable carbon dioxide gas generated in the decarboxylation reaction process to continuously move out of a reaction system through the gas selective permeable membrane under the promotion of external negative pressure, so that the forward movement of the decarboxylation reaction balance is promoted, and the influence of the gas on the effective residence time of the reaction is eliminated.
In the present utility model, the temperature raising unit is preferably one or more of a microreactor, a tubular reactor and a static mixer, for example, a microreactor.
According to the utility model, the temperature raising unit can uniformly heat the materials to the temperature required by the reaction in a short time, so that the energy dissipation can be reduced, and the reaction efficiency can be improved.
In the present utility model, the cooling unit is preferably a microreactor and/or a tubular reactor, for example, a microreactor is used.
In the utility model, the temperature raising unit and the temperature lowering unit independently further comprise a heat exchanger.
The heat exchange medium of the heat exchanger can be heat conduction oil.
In the utility model, the cardanol continuous flow synthesis device can also comprise a feed pump.
The feed pump may be a device conventional in the art, such as a plunger pump, a diaphragm pump, or a syringe pump.
Wherein, the feed pump is arranged at the upstream of the temperature raising unit.
In the utility model, the reaction feed liquid is connected into the temperature raising unit through the feed pump.
In the utility model, the cooling unit can further comprise a pressure controller and a collecting unit.
Wherein the collection unit is preferably arranged downstream of the pressure controller.
Wherein the collecting unit is used for collecting reaction products.
Wherein the collection unit may be a collection unit conventional in the art, such as a collector.
In the present utility model, the pressure controller may use a device conventional in the art, such as a back pressure valve.
In the utility model, the cardanol continuous flow synthesis device is preferably connected in series in the following order: the device comprises a feeding pump, a temperature raising unit, a gas-liquid separation reaction unit, a cooling unit, a pressure controller and a collecting unit.
The utility model also provides a cardanol continuous flow synthesis process, which is carried out by adopting the cardanol continuous flow synthesis device, and comprises the following steps: the cardanol can be prepared after the reaction feed liquid flows through the temperature raising unit, the gas-liquid separation reaction unit and the cooling unit for treatment;
wherein the reaction feed liquid is cashew nut shell oil or anacardic acid;
wherein the temperature of the gas-liquid separation reaction unit is 150-210 ℃;
wherein the reaction residence time of the reaction feed liquid in the gas-liquid separation reaction unit is 7-15 min;
wherein the pressure of the reaction system in the reaction process is 7-11 bar.
In the present utility model, the temperature of the gas-liquid separation reaction unit is preferably 160 to 200 ℃, more preferably 180 to 200 ℃. When the reaction temperature of the reaction feed liquid in the gas-liquid separation reaction unit is 160-200 ℃, the total phenol content of cardanol in the prepared product is higher.
In the present utility model, the reaction residence time of the reaction feed liquid in the gas-liquid separation reaction unit is preferably 7 to 9 minutes. When the reaction residence time of the reaction feed liquid in the gas-liquid separation reaction unit is 7-9 min, the cardanol content in the prepared product is higher.
In the present utility model, the pressure of the reaction system during the reaction is preferably 8 to 10bar, for example 9bar. When the pressure of a reaction system is 8-10 bar in the reaction process, the total phenol content of cardanol in the prepared product is higher.
In the present utility model, the temperature of the temperature raising unit may be 140 to 200 ℃.
In the utility model, the residence time of the reaction feed liquid in the cooling unit can be 20-30 s.
In the utility model, the temperature of the cooling unit can be 50-60 ℃.
The utility model discloses a preferable cardanol continuous flow synthesis process, which comprises the following steps: after cashew nut shell oil or anacardic acid is input into the temperature raising unit through the plunger pump for preheating, the cashew nut shell oil or anacardic acid firstly flows through the gas-liquid separation reaction unit for reaction, then flows through the cooling unit for cooling, then the reaction feed liquid flows into the back pressure valve and the collector in sequence for collection, and finally the obtained product is subjected to liquid chromatography analysis and is compared with a cardanol standard substance;
wherein the temperature of the temperature raising unit is 140-200 ℃;
the temperature of the gas-liquid separation reaction unit is 160-200 ℃;
the reaction residence time of the reaction feed liquid in the gas-liquid separation reaction unit is 7-9 min;
the temperature of the cooling unit is 50-60 ℃;
the residence time of the reaction feed liquid in the cooling unit is 20-30 s;
the pressure of the back pressure valve is 8-10 bar.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred examples of the utility model.
The reagents and materials used in the present utility model are commercially available.
The utility model has the positive progress effects that:
the temperature raising unit can quickly raise the temperature of the reaction feed liquid, reduce the energy consumption in the reaction process, promote the forward movement of the reaction balance of the gas-liquid separation reaction unit with air permeability, eliminate the influence of the gas on the effective residence time of the reaction, and quickly lower the temperature of the materials after the high-temperature reaction. When the synthesis device is used for preparing cardanol, the high-temperature reaction time is short, the reaction feed liquid is heated uniformly, the local overheating of a reaction system can be effectively avoided, the intermolecular self-polymerization of cardanol under the high-temperature condition can be effectively prevented, the content of cardanol total phenol in a product is improved, the synthesis efficiency is high, the purity of the obtained product is higher, the problem that a polymer is formed by high-temperature polymerization in an intermittent kettle type reactor and a large amount of CO is released in the reaction process can be well solved 2 And the safety problem caused by the method improves the safety coefficient of the reaction.
Drawings
Fig. 1 is a schematic flow chart of a continuous flow synthesis apparatus for cardanol in example 1.
FIG. 2 is a schematic diagram showing the structure of a gas-liquid separation reaction unit used in example 1.
The reference numerals are explained as follows:
temperature raising unit 1
Gas-liquid separation reaction unit 2
Cooling unit 3
Feed pump 4
Back pressure valve 5
Collector 6
Heating inner tube 21
Reaction tube 22
Gas collection tube 23
Microchannel reaction zone 24
Gas-permselective membrane 25
Reaction tube feed inlet 26
Reaction tube discharge port 27
Conduction oil inlet 28
Conduction oil outlet 29
Detailed Description
The utility model is further illustrated by means of the following examples, which are not intended to limit the scope of the utility model. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
The devices used in examples 1 to 4 and comparative examples 1 to 4 in the present utility model were as follows:
and a temperature raising unit: SS0010WRBPA microreactor;
and (3) a reaction unit: a conventional sleeve reactor;
and a cooling unit: SS0010WRBPA microreactor;
back pressure valve: SSRBV1210NK4FMG back pressure regulator;
feeding pump: TBP5002SF type plunger pump;
the heat exchange medium of the heat exchangers of the temperature raising unit and the temperature lowering unit is heat conduction oil.
Examples 1 to 4
The connection mode of the cardanol continuous flow synthesis device is shown in figure 1, and the cardanol continuous flow synthesis device comprises a plunger pump 4, a temperature raising unit 1, a gas-liquid separation reaction unit 2, a cooling unit 3, a back pressure valve 5 and a collector 6 which are sequentially connected in series; the structure of the gas-liquid separation reaction unit 2 is shown in fig. 2, and the gas-liquid separation reaction unit comprises a sleeve formed by a heating inner tube 21, a reaction tube 22 and a gas collecting tube 23 which are coaxially fixed in sequence from the center to the outside, wherein an annular gap between the outer wall surface of the heating inner tube 21 and the wall surface of the reaction tube 22 forms a micro-channel reaction zone 24, the micro-channel reaction zone 24 is provided with a feed inlet 26 and a discharge outlet 27, the tube body material of the reaction tube 22 is a gas selective permeability membrane 25, and the heating inner tube 21 is provided with a heat conducting medium inlet 28 and a heat conducting medium outlet 29.
The continuous flow synthesis process of cardanol comprises the following steps: the raw material cashew nut shell oil is conveyed to the temperature raising unit 1 through the plunger pump 4, flows into the gas-liquid separation reaction unit 2 after reaching 140-200 ℃, the temperature of the gas-liquid separation reaction unit 2 is 130-210 ℃, the reaction residence time is 5-10 min, the feed liquid flowing out of the gas-liquid separation reaction unit 2 flows into the cooling unit 3, the temperature of the temperature area of the cooling unit 3 is 50-60 ℃, the residence time is 20-30 s, the reaction feed liquid flows into the back pressure valve 5 after cooling by the cooling unit 3, the back pressure valve 5 is set to be 5-10 bar, finally the feed liquid flowing out of the back pressure valve 5 flows into the collector 6, and the feed liquid in the collector 6 is subjected to liquid chromatography analysis and is compared with the cardanol standard, and the result is shown in the table 1.
Comparative examples 1 to 3
The cardanol continuous flow synthesis device of this comparative example was the same as in example 1; in the cardanol synthesis process of this comparative example, the temperature of the gas-liquid separation reaction unit 2 was 140 ℃, and the total cardanol content in the synthesized product was as shown in table 1, except that the same was made in example 1.
Comparative example 4
The cardanol synthesizing device used in comparative example 4 was a conventional tubular reactor in which the gas-liquid separation reaction unit 2 in example 1 was replaced with a reaction unit; in the cardanol synthesis process of comparative example 4, the residence time of cashew nut shell oil in the reaction unit was 7 to 13min, and the total cardanol content in the synthesized product was as shown in table 1, except that the reaction time was the same as in example 1.
TABLE 1
As is clear from the above table, examples 1 to 4 used the gas permeable jacketed pipe reactor, and the produced products had cardanol contents of 78.92 to 84.64%. From examples 1 to 4, it is understood that the temperature of the gas-liquid separation reaction unit is 180 to 200 ℃, the pressure of the back pressure valve is 9bar, and the total phenol content of the synthesized product is higher when the residence time of the feed liquid in the gas-liquid separation reaction unit is 7 to 9min.
When the temperature of the gas-liquid separation reaction unit is 180 ℃, the pressure of the back pressure valve is 9bar, and the retention time of the feed liquid in the gas-liquid separation reaction unit is 7min, the content of the cardanol total phenol is the highest and is 84.64%.
From comparative examples 1 to 3 and example 1, it is understood that when the residence time of the feed liquid in the gas-liquid separation reaction unit is too short, the back pressure valve pressure is too low, or the temperature of the gas-liquid separation reaction unit is too low, the total cardanol content in the synthesized product is significantly reduced.
As can be seen from comparing example 1 with comparative example 4, the total phenol content of the product obtained in example 1 was 23.3% higher than that of the product obtained in comparative example 4 when the reaction conditions were the same.
The above examples are preferred embodiments of the present utility model, but the embodiments of the present utility model are not limited by the above examples, and any other modifications, substitutions, and combinations are equivalent without departing from the spirit and principles of the present utility model.
Claims (10)
1. The cardanol continuous flow synthesis device is characterized by comprising a temperature raising unit, a gas-liquid separation reaction unit and a cooling unit which are sequentially connected in series;
wherein, the temperature raising unit and the temperature lowering unit are continuous reactors; the gas-liquid separation reaction unit comprises a heating inner pipe, a reaction pipe and a gas collecting pipe, wherein the heating inner pipe, the reaction pipe and the gas collecting pipe are coaxially fixed in sequence from the center to the outside to form a sleeve, an annular gap between the outer wall surface of the heating inner pipe and the wall surface of the reaction pipe forms a micro-channel reaction zone, the micro-channel reaction zone is provided with a feed inlet and a discharge outlet, the wall surface of the reaction pipe adjacent to the gas collecting pipe in the micro-channel reaction zone is a gas selective permeable membrane, and the heating inner pipe is provided with a heat conducting medium inlet and a heat conducting medium outlet;
wherein the temperature raising unit is used for preheating the reaction feed liquid; the gas-liquid separation reaction unit is used for decarboxylation reaction of the reaction feed liquid; the cooling unit is used for cooling the product obtained by the decarboxylation reaction.
2. The continuous flow cardanol synthesis device of claim 1, wherein the temperature raising unit is one or more of a microreactor, a tubular reactor and a static mixer.
3. The continuous flow cardanol synthesizer according to claim 2, wherein the temperature raising unit is a microreactor.
4. The continuous flow cardanol synthesizing device of claim 1, wherein the cooling unit is a micro-reactor and/or a tubular reactor.
5. The continuous flow cardanol synthesizer of claim 4, wherein the cooling unit is a microreactor.
6. The continuous flow cardanol synthesizer of claim 1, wherein the heat conducting medium is heat conducting oil.
7. The continuous flow cardanol synthesizer according to claim 1, wherein said temperature raising unit and said temperature lowering unit independently further comprise a heat exchanger;
the heat exchange medium of the heat exchanger is heat conduction oil.
8. The continuous flow cardanol synthesizer according to claim 1, further comprising a feed pump upstream of said temperature raising unit;
wherein, the feed pump is a plunger pump, a diaphragm pump or a syringe pump.
9. The cardanol continuous flow synthesizer of claim 8, wherein the cooling unit further comprises a pressure controller and a collection unit;
wherein the collection unit is disposed downstream of the pressure controller;
wherein the collecting unit is a collector;
wherein the pressure controller is a back pressure valve.
10. The continuous flow cardanol synthesizer according to claim 9, wherein the continuous flow synthesizer is connected in series in the following order: the device comprises a feeding pump, a temperature raising unit, a gas-liquid separation reaction unit, a cooling unit, a pressure controller and a collecting unit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320242806.6U CN219580555U (en) | 2023-02-16 | 2023-02-16 | Anacardol continuous flow synthesizer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320242806.6U CN219580555U (en) | 2023-02-16 | 2023-02-16 | Anacardol continuous flow synthesizer |
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| Publication Number | Publication Date |
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| CN219580555U true CN219580555U (en) | 2023-08-25 |
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| CN202320242806.6U Active CN219580555U (en) | 2023-02-16 | 2023-02-16 | Anacardol continuous flow synthesizer |
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