Green and efficient caryophyllene hydration device

Abstract

The utility model provides a green and efficient caryophyllene hydration device which comprises a slurry bed reaction tower or a fixed bed reaction tower which is directly connected with the middle part of a rectifying tower; a micro-interface strengthening unit is arranged at the bottom of the slurry bed reaction tower; and micro-interface strengthening units are arranged at the bottom and the top of the solid bed reaction tower. According to the device, the reaction rate can be multiplied, the energy consumption of the reaction is reduced, and the device is environment-friendly and better meets the requirements of green chemistry.

Description

Technical Field

[0001] The utility model relates to the field of chemical engineering and process technology, and in particular to a green and efficient caryophyllene hydration device. Background Art

[0002] Rosin distillation is a crucial process in forestry. It involves separating purified rosin liquid using steam or other methods to obtain rosin and turpentine. Rosin primarily consists of rosin and turpentine, which have different boiling points and can therefore be separated through distillation. During distillation, heating liquefies the rosin, causing the turpentine (lower boiling point) to evaporate first, while the rosin (higher boiling point) remains as a residue. Heavy turpentine can be used as a raw material for the production of caryophyllene alcohol.

[0003] Caryophyllene alcohol is naturally present in the high-boiling-point fraction of Asian mint oil or peppermint oil. It has a unique aroma and can be used to formulate various spices, cosmetics, and as a food additive. Caryophyllene alcohol also exhibits antibacterial and anti-inflammatory biological activities and can be used to synthesize new antiasthmatic and antitussive drugs with long-lasting antiasthmatic effects and low toxicity. Therefore, the preparation process of caryophyllene alcohol has attracted widespread attention. Current preparation methods use caryophyllene as a raw material and perform a hydration reaction under acid catalysis, such as using sulfuric acid, chloroacetic acid, p-toluenesulfonic acid, macroporous strongly acidic cation exchange resins, molecular sieves, etc. as catalysts in various solvents, but these methods have not yielded satisfactory results (see: Cao Yurong et al., Journal of Chemistry in Universities, Vol. 20, No. 7, pp. 1086-1087, 1999). Other methods also involve reacting caryophyllene with optically active D- and L-camphorsulfonic acids, respectively, to obtain optically active caryophyllene alcohol, or by isolating caryophyllene from isolongifolene residues to obtain high-purity caryophyllene alcohol. The above preparation methods all have defects that are difficult to solve: the preparation conditions are difficult to carry out industrial production, and the reaction rate of the device is low.

[0004] In view of this, the present utility model is proposed. Utility Model Content

[0005] The purpose of the utility model is to provide a green and efficient caryophyllene hydration device, which utilizes a micro-interface strengthening device to effectively improve the mass transfer rate of the strengthened interface and greatly improve the reaction rate.

[0006] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are adopted:

[0007] The utility model provides a green and efficient caryophyllene hydration device, comprising a slurry bed reaction tower or a fixed bed reaction tower, wherein the slurry bed reaction tower or the fixed bed reaction tower is directly connected to the middle part of a distillation tower, and a micro-interface strengthening unit is arranged at the bottom of the slurry bed reaction tower / solid bed reaction tower.

[0008] In the present invention, a micro-interface strengthening unit is provided to increase the reaction rate. In a slurry bed reaction tower, only a single micro-interface strengthening unit is provided at the bottom of the reaction tower. The reason for this is that, in the design of the slurry bed reaction tower, the reaction materials are mixed in the pipeline and then enter the middle of the slurry bed reaction tower. The filter can filter out the catalyst and re-enter the slurry bed reaction tower from the middle. The catalyst and the reaction materials can be mixed in advance in the middle of the reaction tower and then enter the micro-interface strengthening unit for reaction, thereby ensuring a more complete reaction.

[0009] In a solid-state bed reaction tower, the catalyst can be fixed in the fixed bed reaction tower and does not need to be recovered. Therefore, the reactants need to be crushed separately through a micro-interface strengthening unit and then react with the catalyst fixed in the fixed bed reaction tower.

[0010] In the present invention, the slurry bed reaction tower or the solid bed reaction tower has slightly different design concepts due to the different catalyst recovery designs, but the technical effects achieved are basically the same.

[0011] Preferably, as a further specific embodiment, the inlet in the middle of the slurry bed reaction tower is directly connected to the filter, and the bottom outlet of the filter is directly connected to the vacuum distillation tower; a condenser is provided at the top of the vacuum distillation tower, and a reboiler is provided at the bottom of the vacuum distillation tower, and the condenser is directly connected to the recrystallization tower.

[0012] Preferably, as a further specific embodiment, the solid-state reaction tower is directly connected to the middle inlet of the vacuum distillation tower, a condenser is provided at the top of the vacuum distillation tower, and a reboiler is provided at the bottom of the vacuum distillation tower; the condenser is directly connected to the recrystallization tower.

[0013] Preferably, as a further specific embodiment, the top outlet of the distillation tower is connected to a condenser, and the bottom inlet of the condenser is reconnected to the distillation tower; a reboiler is provided at the bottom outlet of the distillation tower.

[0014] Since the slurry bed reactor needs to recover the catalyst, the mixture and catalyst after the reaction need to be directly connected to the filter. The filter recovers the catalyst through filtration and returns it to the slurry bed reactor, realizing the recycling of the catalyst. The reboiler at the bottom of the distillation tower can provide energy for the distillation tower, and the condenser can condense the product.

[0015] The solid-state bed reaction tower does not require catalyst recovery, and the product after the reaction is completed directly enters the vacuum distillation tower for impurity separation.

[0016] Preferably, as a further specific embodiment, the bottom outlet of the recrystallization tower is connected to an external circulation pipeline, and the inlet of the circulation pipeline is connected to the top of the recrystallization tower; a delivery pump and a condenser are provided on the circulation line, and a material outlet is provided on the condenser.

[0017] In the present invention, multiple recrystallizations of the product can be achieved by setting a circulation pipeline outside the recrystallization tower, which is beneficial to improving the purity of the product; at the same time, the delivery pump can provide power for the product circulation, and the condenser can condense the product, which is more convenient for the delivery pump to transport. In addition, the product after multiple recrystallizations is condensed and flows out of the condenser for easier collection.

[0018] Preferably, as a further specific embodiment, a recrystallization solvent inlet is provided at 1 / 3 of the distance from the bottom of the recrystallization tower.

[0019] This arrangement allows the recrystallization reagent to contact the raw material from bottom to top against gravity, thus ensuring that the raw material can be fully recrystallized and further ensuring the purity of the product. At the same time, it can also maintain a certain distance from other inlets or outlets to prevent material backflow and contamination of the pipeline.

[0020] Preferably, as a further specific embodiment, a raw material inlet is provided at 1 / 3 of the distance from the bottom of the distillation tower.

[0021] This setting method can also ensure the reaction of raw materials from bottom to top, which is beneficial to improving the conversion rate of raw materials. At the same time, it can also maintain a certain distance from other inlets or outlets to prevent material backflow and contamination of the pipeline.

[0022] Compared with the prior art, the beneficial effects of the present invention are:

[0023] The reaction device has been designed to increase the reaction rate exponentially while reducing the energy consumption of the reaction. It is environmentally friendly and more in line with the requirements of green chemistry. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Various other advantages and benefits will become apparent to those skilled in the art upon reading the detailed description of the preferred embodiment below. The accompanying drawings are for illustration purposes only and are not to be considered as limiting the present invention. The same reference symbols are used throughout the accompanying drawings to represent the same components. In the accompanying drawings:

[0025] Figure 1:Schematic diagram of solid-state bed micro-interface enhanced reaction device;

[0026] Figure 2 : Schematic diagram of slurry bed micro-interface enhanced reaction device.

[0027] 1-rosin inlet, 2-distillation tower, 3-reboiler, 4-micro interface enhanced reactor, 5-heavy turpentine inlet, 6-fixed bed, 7-condenser, 8-fixed bed reaction tower, 9-vacuum distillation tower,

[0028] 10-recrystallization solvent inlet, 11-recrystallization tower, 12-condenser, 13-micro interface strengthening unit,

[0029] 14-circulation pump, 15-reboiler;

[0030] 1'-rosin inlet, 2'-distillation tower, 3'-reboiler, 6'-solid acid catalyst inlet pipeline,

[0031] 7'-condenser, 8'-slurry bed reaction tower, 9'-filter, 10'-vacuum distillation tower,

[0032] 11'-recrystallization solvent inlet, 12'-recrystallization tower, 13'-condenser, 14'-circulation pump,

[0033] 15'-reboiler, 16'-condenser. DETAILED DESCRIPTION

[0034] The technical solution of the present invention will be clearly and completely described below in conjunction with the accompanying drawings and specific embodiments, but those skilled in the art will understand that the embodiments described below are part of the embodiments of the present invention, rather than all of the embodiments, and are only used to illustrate the present invention, and should not be regarded as limiting the scope of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative work are within the scope of protection of the present invention. If specific conditions are not specified in the embodiments, they are carried out according to conventional conditions or the conditions recommended by the manufacturer. If the manufacturer is not specified for the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0035] In the description of this utility model, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicating positions or relationships, are based on the positions or relationships shown in the accompanying drawings and are intended solely to facilitate the description of this utility model and simplify the description. They do not indicate or imply that the devices or components referred to must have a specific orientation, be constructed, or operate in a specific orientation. Therefore, they should not be construed as limitations on this utility model. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0036] In the description of this utility model, it should be noted that, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "connected" should be understood in a broad sense. For example, they can refer to fixed connections, detachable connections, or integral connections; mechanical connections, electrical connections; direct connections, indirect connections through an intermediate medium, and internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in this utility model based on the specific circumstances.

[0037] In order to more clearly illustrate the technical solution of the present invention, it is described below in the form of specific embodiments.

[0038] Example

[0039] Reference Figure 1 , Figure 1 It is a schematic diagram of a solid-state bed micro-interface enhanced reaction device. The top of the rectifying tower 2 is provided with an outlet in parallel with a condenser 7, and the condenser 7 is provided with an outlet. The turpentine obtained by the reaction of the rosin flows out from the condenser 7. The bottom of the rectifying tower 2 is provided with a rosin inlet 1, and the bottom of the rectifying tower 2 is connected in parallel with a reboiler 3 to achieve reheating of the rectifying tower 2. The raw material rosin is passed into the rectifying tower 2 from the rosin inlet 1 for rectification. The rosin inlet is arranged at 1 / 3 of the distance from the bottom of the rectifying tower 2. The rectification obtains two components, turpentine and heavy turpentine. The turpentine passes through the condenser 7 from the top outlet of the rectifying tower 2. The reboiler 3 can supply energy for the rectifying tower 2, so that the raw material inside the rectifying tower 2 can be continuously vaporized, and the catalyst is placed in the fixed bed 6.

[0040] After rosin is distilled in the distillation tower 2, heavy turpentine is obtained. The heavy turpentine enters the fixed bed reaction tower 8 from the heavy turpentine inlet 5. The bottom of the fixed bed reaction tower 8 is provided with a micro-interface strengthening unit 4. During the reaction, water enters the fixed bed reaction tower 8 from the micro-interface strengthening unit 4 to react; the solid acid catalyst enters the fixed bed 6 for fixation, and the heavy turpentine, water and solid acid catalyst enter the fixed bed reaction tower 8. After sufficient reaction in the fixed bed reaction tower 8, they enter the vacuum distillation tower 9 for vacuum distillation. A condenser 13 is provided at the top of the vacuum distillation tower 9. The condenser 13 is connected in parallel with the vacuum distillation tower 9. The condenser 13 condenses the raw materials after vacuum distillation, so that the raw materials after vacuum distillation enter the recrystallization tower 11 for recrystallization; a reboiler 15 is provided at the bottom of the vacuum distillation tower 9. The reboiler can provide energy for the vacuum distillation tower 9.

[0041] The recrystallization tower 11 is provided with an external circulation pipeline, which is equipped with a condenser 12 and a circulation pump 14. The condenser 12 can condense the raw materials after recrystallization, and the circulation pump 14 provides power for the circulation of the materials. A recrystallization solvent inlet 10 is provided at 1 / 3 of the distance from the bottom of the recrystallization tower 11. After the recrystallization solvent enters the recrystallization tower 11, it is recrystallized with the raw materials after vacuum distillation. The provision of the external circulation pipeline enables the raw materials to be recrystallized multiple times to ensure the purity of the materials. The caryophyllene alcohol obtained by refining flows out of the condenser 12.

[0042] Reference Figure 2 , Figure 2 It is a schematic diagram of a slurry bed micro-interface enhanced reaction device. The top of the distillation tower 2' is provided with an outlet in parallel with a condenser 7', and the condenser 7' is provided with an outlet. The turpentine obtained by the reaction of the rosin flows out from the condenser 7'. The bottom of the distillation tower 2' is provided with a rosin inlet 1', which is arranged at 1 / 3 of the distance from the bottom of the distillation tower 2'. The bottom of the distillation tower 2' is connected in parallel with a reboiler 3' to achieve reheating of the distillation tower 2'. The raw material rosin is passed into the distillation tower 2' from the rosin inlet 1' for distillation. The distillation obtains two components, turpentine and heavy turpentine. The turpentine is exported from the top of the distillation tower 2' through the condenser 7'. The reboiler 3' can supply energy for the distillation tower 2', so that the raw material inside the distillation tower 2' can be continuously vaporized.

[0043] After rosin is rectified in a distillation tower 2', it is converted into heavy turpentine. The heavy turpentine enters a slurry bed reactor 8' through a heavy turpentine inlet 5'. A micro-interface strengthening unit 4' is provided at the bottom of the slurry bed reactor 8'. During the reaction, water enters the slurry bed reactor 8' from the micro-interface strengthening unit 4' to react. The heavy turpentine rectified in the distillation tower 2' and the solid acid are mixed in the inlet pipelines and then enter the slurry bed reactor 8' through the heavy turpentine inlet 5'. At this time, the water, heavy turpentine, and solid acid catalyst react in the slurry bed reactor 8'. After the reaction is completed, the solid acid catalyst enters a filter 9' along with the product for filtration and recovery. The catalyst is filtered through the filter 9' and returned to the slurry bed reactor 8', thereby achieving catalyst reuse. The product passes through the filter 9' and enters a vacuum distillation tower 10' for vacuum distillation.

[0044] A condenser 16' is provided at the top of the vacuum distillation tower 10' to cool the product after vacuum distillation before entering the recrystallization tower 11'. A reboiler 15' is provided at the bottom of the vacuum distillation tower 10' to provide energy for the vacuum distillation tower 10'.

[0045] The product after vacuum distillation enters a recrystallization tower 12', which has an external circulation pipeline. The circulation pipeline is provided with a condenser 13' and a circulation pump 14'. The condenser 13' can condense the raw material after recrystallization, and the circulation pump 14' provides power for the circulation of the material. A recrystallization solvent inlet 11' is provided at 1 / 3 of the bottom of the recrystallization tower 12'. After the recrystallization solvent enters the recrystallization tower 12', it is recrystallized with the raw material after vacuum distillation. The provision of the external circulation pipeline enables the raw material to be recrystallized multiple times to ensure the purity of the material. The caryophyllene alcohol obtained by refining flows out from the condenser 13'.

[0046] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the above embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A green and efficient caryophyllene hydration device, characterized in that: It comprises a slurry bed reaction tower or a fixed bed reaction tower, which is directly connected to the middle of a distillation tower. A micro-interface strengthening unit is provided at the bottom of the slurry bed reaction tower / solid bed reaction tower.

2. The green and efficient caryophyllene hydration device according to claim 1, characterized in that: The inlet in the middle of the slurry bed reaction tower is directly connected to the filter, and the bottom outlet of the filter is directly connected to the vacuum distillation tower; a condenser is provided at the top of the vacuum distillation tower, and a reboiler is provided at the bottom of the vacuum distillation tower, and the condenser is directly connected to the recrystallization tower.

3. The green and efficient caryophyllene hydration device according to claim 1, characterized in that: The solid-state bed reaction tower is directly connected to the middle inlet of the vacuum distillation tower. A condenser is provided at the top of the vacuum distillation tower, and a reboiler is provided at the bottom of the vacuum distillation tower. The condenser is directly connected to the recrystallization tower.

4. The green and efficient caryophyllene hydration device according to claim 1, characterized in that: The top outlet of the distillation tower is connected to a condenser, and the bottom inlet of the condenser is reconnected to the distillation tower; a reboiler is provided at the bottom outlet of the distillation tower.

5. The green and efficient caryophyllene hydration device according to any one of claims 2-3, characterized in that: The bottom outlet of the recrystallization tower is connected to a circulation pipeline, the inlet of the circulation pipeline is connected to the top of the recrystallization tower; a delivery pump and a condenser are provided on the circulation pipeline, and a material outlet is provided on the condenser.

6. The green and efficient caryophyllene hydration device according to claim 5, characterized in that: A recrystallization solvent inlet is provided at 1 / 3 of the bottom of the recrystallization tower.

7. The green and efficient caryophyllene hydration device according to claim 1, characterized in that: A raw material inlet is provided at 1 / 3 of the distance from the bottom of the distillation tower.

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