CN111495289B - Gas-liquid two-phase continuous reaction device and preparation method of sorbol - Google Patents
Gas-liquid two-phase continuous reaction device and preparation method of sorbol Download PDFInfo
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Abstract
The invention relates to a gas-liquid two-phase continuous reaction device and a preparation method of sorbol. The gas-liquid two-phase continuous reaction device comprises a continuous reactor, a liquid tank, a crude product output pipe and a collecting tank, wherein the continuous reactor comprises a degassing pump, a liquid inlet pipe, an air inlet pipe, a post-pump liquid pipe, a pressure stabilizing tank and a liquid outlet pipe; the liquid tank is respectively communicated with the liquid outlet pipe and the liquid inlet pipe, and a liquid discharging valve is arranged between the liquid tank and the liquid inlet pipe; the crude product output pipe is respectively communicated with the side wall of the liquid tank and the collecting tank. The preparation method of the sorbol is a method for preparing the sorbol by using the gas-liquid two-phase continuous reaction device and taking acetaldehyde gas as a raw material and alkali liquor as a catalyst. The gas-liquid two-phase continuous reaction device and the preparation method of the sorbol are used for the continuous production of the sorbol, and can improve the collection rate of acetaldehyde gas and the yield of a sorbol product.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a gas-liquid two-phase continuous reaction device and a preparation method of sorbol.
Background
The pyrenal has green fragrance, fruity fragrance and sweet taste, has fresh melon lasting appeal (essence and spice dictionary 305 of Lingxiang), is used as a food (spice) additive (synthetic edible spice handbook compiled by Ministry of light industry research in Jinan City), and is widely used in food industries such as soft drink, candy, jelly, jam and the like; the antibacterial mildew preventive has the advantages of strong antibacterial activity, no residue, high safety and the like, is used as a natural mildew preventive (CN 107668199A, Maweibin), and is widely applied to grain storage industries such as rice, corn, peanut and the like; is an excellent food additive and mildew preventive.
Sorbal, also known as: trans-2, 4-hexadienal (CAS number: 142-83-6) is generally prepared by aldol condensation of acetaldehyde and crotonaldehyde, wherein crotonaldehyde also comes from aldol condensation between two acetaldehyde molecules (Xushouchhang Chang Shu organic chemistry: 252-253), i.e. three acetaldehyde molecules are subjected to aldol condensation twice in succession to obtain the pyrenal.
At present, the reaction mechanism for preparing the sorbal by taking acetaldehyde as a raw material is as follows: acetaldehyde can interact with two molecules in the presence of a base catalyst, in which the alpha-hydrogen of one aldehyde molecule is added to the carbonyl oxygen atom of another aldehyde molecule, to produce a product which is a beta-hydroxyaldehyde. This reaction is therefore called aldol condensation or aldol condensation.
The reaction sequence of the aldol condensation reaction is: firstly, alkali abstracts a proton on a carbon a in a molecule of acetaldehyde to generate enol anions;
in the second step, the negative ion is used as a nucleophilic reagent to perform nucleophilic addition reaction with another molecule of aldehyde to generate an alkoxy negative ion.
In a third step, the negative alkoxide ion is specific to OH—Stronger bases, which abstract a proton from a water molecule to form a hydroxyaldehyde.
In the fourth step, the beta-hydroxyaldehyde generated from the two aldehydes easily loses one molecule of water when heated, and alpha, beta-unsaturated aldehyde (crotonaldehyde) is generated.
Similar to the reaction process of acetaldehyde into crotonaldehyde, acetaldehyde continues to react with crotonaldehyde to produce sorb aldehyde through aldol condensation.
However, in the current industrial process route for preparing the sorb aldehyde by using the acetaldehyde as the raw material, a closed reaction pot is usually adopted for batch production, and the reaction is carried out under the condition of cooling and controlling the temperature to be about 5 ℃ or slowly heating and reacting under the condition of controlling the temperature to be 85-90 ℃ in the presence of pyridine. However, the yield of the prior preparation method is generally less than 45 percent. Although acetaldehyde is easy to dissolve in water, acetaldehyde is easy to overflow from an aqueous solution (the boiling point of acetaldehyde is 20.8 ℃), the requirement on reaction temperature is strict, volatilization loss is large, and in addition, during batch production, the pyrenal has more side reactions in a reactor, so that the product yield is low, and meanwhile, the production site has large pungent odor and the working environment is severe.
Disclosure of Invention
Based on the above, the present invention aims to provide a gas-liquid two-phase continuous reaction apparatus, which can be used for continuous production of preparing the sorbosol by using acetaldehyde as a raw material, and can improve the collection rate of acetaldehyde gas and the yield of the sorbosol product.
The technical scheme of the invention is as follows:
a gas-liquid two-phase continuous reaction apparatus, comprising:
the continuous reactor comprises a degassing pump, a liquid inlet pipe, an air inlet pipe, a post-pump liquid pipe, a pressure stabilizing tank and a liquid outlet pipe, wherein one end of the degassing pump is connected with the liquid inlet pipe, the other end of the degassing pump is connected with the post-pump liquid pipe, a liquid inlet regulating valve is arranged at the inlet of the liquid inlet pipe, an air inlet regulating valve is arranged at the inlet of the air inlet pipe, the air inlet pipe is communicated with the liquid inlet pipe, the communicating part is positioned between the liquid inlet regulating valve and the degassing pump, the inlet end of the pressure stabilizing tank is communicated with the post-pump liquid pipe, the outlet end of the pressure stabilizing tank is communicated with the liquid;
the top of the liquid tank is communicated with the liquid outlet pipe, the bottom of the liquid tank is communicated with the liquid inlet pipe, and a liquid discharging valve is arranged between the liquid tank and the liquid inlet pipe;
a crude product output pipe, one end of which is communicated with the side wall of the liquid tank; and
and the top of the collecting tank is communicated with the other end of the crude product output pipe.
The gas-liquid two-phase continuous reaction device is suitable for continuous production of preparing the aldehyde from acetaldehyde serving as a raw material, wherein the acetaldehyde gas enters a continuous reactor through a gas inlet pipe, alkali liquor serving as a catalyst is originally stored in a liquid tank and enters the continuous reactor through a liquid inlet pipe, and during production, negative pressure is formed in front of a degassing pump by operating a liquid inlet regulating valve, a liquid outlet regulating valve and a gas inlet regulating valve, and positive pressure is formed behind a degassing pump, so that the acetaldehyde gas can be continuously sucked into the continuous reactor in a negative pressure mode through reaction, and the acetaldehyde gas is conveniently collected; the working principle of the degassing pump is that high-pressure gas and high-boiling-point organic matters are fully mixed in the pump when the pump rotates, so that a small amount of low-boiling-point solvent remained in the high-boiling-point organic matters is blown off conveniently; according to the invention, when the pump runs, the high vacuum degree in front of the pump is realized by adjusting the feeding and discharging valve, the function of air suction is realized, the low-boiling-point gas acetaldehyde is continuously sucked into the alkali liquor, and the effect of promoting gas-liquid two-phase mixed mass transfer is achieved; the liquid tank is used for storing alkali liquor on one hand and receiving crude products (crude oil) generated by the reaction and the alkali liquor flowing into the liquid tank from the top of the liquid tank together, the crude products and the alkali liquor can be automatically layered in the liquid tank, the crude products are arranged on the upper layer and can enter the collecting tank through the crude product output pipe, and the alkali liquor on the lower layer enters the continuous reactor again through the liquid inlet pipe. The continuous production of the sorbosol is realized by recycling the alkali liquor, continuously supplying acetaldehyde gas into the gas inlet pipe and continuously and periodically discharging the crude product from the collecting tank, so that the yield of the sorbosol product can be improved; of course, the gas-liquid two-phase continuous reaction device can also be applied to the continuous production of other gas-liquid two-phase reactions.
Preferably, the liquid tank comprises a tank body and a separation inclined plate, the separation inclined plate is fixed on the inner wall of the tank body and divides the inner cavity of the tank body into an upper cavity and a lower cavity, the crude product output pipe is communicated with the lower cavity, and a mixture input port is defined by the bottom end of the separation inclined plate and the inner wall of the tank body; the gas-liquid two-phase continuous reaction device further comprises a liquid return pipe, one end of the liquid return pipe is communicated with the liquid outlet pipe, and the other end of the liquid return pipe extends into the tank body and is communicated with the upper cavity. Through the setting of separation swash plate in the fluid reservoir, divide into upper and lower two parts with the fluid reservoir, follow the last down natural flow of following after lye and the crude (the following mixture of lye and crude is called for short the mixed liquid) get into the fluid reservoir from the top, can slow down mixed liquid ejection of compact speed and the stirring effect to the partial mixed liquid of fluid reservoir, the crude of being convenient for is separated and is assembled under the separation swash plate in the mixed liquid to discharge the collection tank through crude output tube, bottom lye then gets back to the continuous reactor well cycle through the tapping valve, the drainage tube, feed liquor pipe and uses.
Preferably, the elevation angle of the separation inclined plate is 50-70 degrees, one end of the liquid return pipe extending into the tank body is close to the bottom end of the separation inclined plate, and the communication position of the crude product output pipe and the side wall of the liquid tank is located at the upper half part of the tank body. Through the setting of the elevation angle of the separation inclined plate, the setting of the specific relative position between the liquid return pipe and the separation inclined plate and the setting of the position of the crude product output pipe, the stirring of the original alkali liquor of the lower part when the mixed liquid enters from the top of the liquid tank is further minimized, the layering efficiency of the crude product and the alkali liquor is promoted, the crude product is more efficiently gathered below the separation inclined plate, and the crude product is convenient to output.
Preferably, the gas-liquid two-phase continuous reaction device is characterized by further comprising a gas introducing pipe, a first gas overflow pipe and a second gas overflow pipe, wherein the gas introducing pipe is communicated with a gas inlet pipe of the continuous reactor; one end of the first air overflow pipe is communicated with the top of the liquid tank, and the other end of the first air overflow pipe is communicated with the air entraining pipe; one end of the second air overflow pipe is communicated with the top of the collecting tank, and the other end of the second air overflow pipe is communicated with the air entraining pipe. Acetaldehyde gas can enter the air inlet pipe through an air inlet pipe, for example, the air inlet pipe can be communicated with an air overflow pipe of a benzaldehyde production device, namely, the acetaldehyde gas is derived from acetaldehyde which is a byproduct of benzaldehyde production; because acetaldehyde is volatile, acetaldehyde gas in the liquid tank and the collecting tank (which is not reacted in the continuous reactor and is brought out with alkali liquor and has part overflowing from the alkali liquor and an oil layer in the tank body) and acetaldehyde in the air entraining pipe can be sucked into the air inlet pipe through the first air overflow pipe and the second air overflow pipe, and then enter the continuous reactor to continuously perform aldol condensation reaction to generate the pyrenal, so that the utilization rate of the acetaldehyde and the yield of the pyrenal are improved.
Furthermore, a vacuum meter is arranged on the liquid inlet pipe, a gas flowmeter is arranged on the gas inlet pipe, and a pressure gauge is arranged on the pressure stabilizing tank. Through the arrangement of the vacuum meter, the gas flowmeter and the pressure meter, the pressure of the pipeline and the flow of gas entering the pipeline can be more accurately controlled so as to realize the control of production.
The invention also provides a method for preparing the sorbosol by using the gas-liquid two-phase continuous reaction device, which comprises the following steps:
(1) placing prepared alkali liquor in a liquor tank, wherein the alkali liquor comprises 0.5-15 wt% of NaOH solution and 2.5-20 wt% of Na2CO3Solution composition;
(2) setting the liquid inlet regulating valve, the liquid outlet regulating valve and the liquid discharge valve in a fully open state, setting the gas inlet regulating valve in a fully closed state, and starting the degassing pump to enable the alkali liquor to circularly flow between the continuous reactor and the liquid tank;
(3) slowly closing the liquid inlet regulating valve until the liquid inlet regulating valve reaches negative pressure before the degassing pump, and slowly closing the liquid outlet regulating valve until the liquid outlet regulating valve reaches positive pressure after the degassing pump;
(4) slowly opening an air inlet regulating valve to input acetaldehyde gas, so that aldol condensation reaction occurs in the continuous reactor;
(5) collecting the crude product from the collection tank.
The preparation method of the sorbol utilizes the gas-liquid two-phase continuous reaction device, takes the specific alkali liquor as the catalyst, and reasonably adjusts the liquid inlet adjusting valve and the liquid outlet adjusting valve, so that the continuous reactor is in a stable pressure building state (namely the pressure is maintained near a certain stable value) in the production process, acetaldehyde gas is continuously sucked into the alkali liquor through the air inlet pipe in a negative pressure manner, and aldol condensation reaction is continuously carried out in the continuous reactor to generate the sorbol; the preparation reaction equation of the invention is as follows:
compared with the existing preparation method of the sorbic aldehyde, the preparation method has the following advantages:
(1) according to the invention, acetaldehyde gas is continuously sucked into the continuous reactor in a negative pressure manner, so that the acetaldehyde collection rate is effectively improved;
(2) the invention adopts the gas-liquid two-phase continuous reactor to replace the original intermittent reaction kettle, avoids the phenomenon of serious leakage, leakage and leakage of the original process, greatly reduces the concentration of pungent odor in production places, greatly improves the working environment, and effectively improves the utilization rate of acetaldehyde gas and the product yield;
(3) the invention has mild reaction conditions, avoids the problem that the original process needs refrigeration and temperature control (about 5 ℃) or uses organic solvent, reduces the production cost and improves the production efficiency.
Further, after the crude product is collected, a water washing procedure and a separation procedure are carried out to obtain a finished product of the pyrenal and a byproduct of the crotonaldehyde, and then the byproduct of the crotonaldehyde is continuously put into the liquid inlet pipe. The water washing process may specifically include: washing, neutralizing and standing the crude product, and then removing moisture, wherein the separation process specifically comprises the step of carrying out reduced pressure fractionation on the crude product after moisture removal to obtain a finished product of the pyrenal and a byproduct of crotonaldehyde. The separated crotonaldehyde is continuously introduced into the continuous reactor, so that the recycling is realized, and the yield of the sorbal is further improved.
Preferably, the acetaldehyde gas is derived from: the acetaldehyde gas is a byproduct generated in the process of producing natural benzaldehyde by taking natural cinnamon oil or natural cinnamaldehyde as a raw material to perform an aldol condensation reaction. Because the acetaldehyde gas is the acetaldehyde gas of an all-natural carbon source, the prepared sorbic aldehyde is natural sorbic aldehyde. Specifically, the natural cinnamon oil can be obtained by selecting cinnamon bark, branches and leaves and other parts and adopting various physical methods (mainly a water vapor method), wherein the weight content of cinnamaldehyde is more than or equal to 70%; the natural cinnamaldehyde can be cinnamaldehyde obtained by physically separating (usually adopting high vacuum falling film fractionation) and purifying natural cinnamon oil, wherein the weight content of cinnamaldehyde is more than or equal to 90%.
With the improvement of living standard, people have higher requirements on food safety, and tend to use safer and healthier natural additives and natural mildewcides. The idea that natural products are healthier than chemical compounds is reflected in food laws and regulations, and natural sorbosol becomes an urgent need of industries such as domestic food additives, grain storage mildewproof agents and the like. Natural sorbellal is a naturally-occurring small-molecular volatile substance and exists in a small amount in plants such as kiwi fruits, olives, tomatoes, tea leaves and the like; it is also present in small amount in parched peanut, caviar, and naturally oxidized salmon oil. Because the content of the natural aldehyde is extremely low in natural resources, the high-purity natural aldehyde can not be directly extracted so far, and the market demand can not be met.
According to the current international general rule, the sorb prepared by using an all-natural carbon source as a raw material can be regarded as a natural sorb equivalent for use. In order to prepare natural sorbellal equivalents, the search for all natural carbon sources is an urgent task, and the search for natural acetaldehyde, crotonaldehyde and the like is a main direction. Natural acetaldehyde is produced in the natural fermentation process of alcohols, but the content is low and the components are complex. Crotonaldehyde is also present in small amounts in nature and is complex in composition.
At present, in the process of producing natural benzaldehyde by taking natural cinnamaldehyde as a raw material in China, acetaldehyde gas is generated at the same time, and the reaction formula is as follows:
in this process, the acetaldehyde, except for the two "H" s, is derived from the "H" s involved in the "retro-aldol condensation" reaction (the reaction of acetaldehyde with benzaldehyde to form cinnamaldehyde and water is an "aldol condensation" reaction; the reverse of which is known in the industry as the "retro-aldol condensation" reaction)2The remainder C, H, O, other than O ", was derived from natural cinnamaldehyde, corresponding to 95.45% (42/44 = 95.45%) supplied by natural cinnamaldehyde, and was entirely within the category of all natural carbon sources.
Although the natural benzaldehyde is produced in the process of producing natural benzaldehyde along with the production of natural acetaldehyde gas by-products, the yield of acetaldehyde gas is low, namely about 76kg per day (at present, 5 plants for producing natural benzaldehyde in China have the total yield of about 250 tons every year, the annual yield of a single plant is only about 50 tons, the yield of natural benzaldehyde in each plant is about 200 kg/day, the theoretical yield of the by-product natural acetaldehyde is 83 kg/day, and about 8 percent of the by-product natural acetaldehyde and cinnamaldehyde are deducted), and the natural benzaldehyde is extremely easy to volatilize, so that the natural benzaldehyde is difficult to recover, and no successful recovery and utilization cases exist so far.
According to the invention, by selecting the acetaldehyde gas as a by-product in the process of producing natural benzaldehyde through the preferred embodiment, the all-natural carbon source raw material for preparing the sorbic aldehyde is ensured, the obtained sorbic aldehyde is the natural sorbic aldehyde, the natural degree of the sorbic aldehyde is high, the sorbic aldehyde not only belongs to the category of all-natural carbon sources, but also has the natural source of more than 95%; but also realizes the recycling of byproducts in the production process of natural benzaldehyde, and is green and environment-friendly.
Preferably, in the step (3), the feed liquid regulating valve is slowly closed until the gauge pressure before the degassing pump is (-0.035 +/-0.025) MPa, and after the vacuum before the degassing pump is stabilized, the feed liquid regulating valve is continuously and slowly closed until the gauge pressure in the pressure stabilizing tank is (0.40 +/-0.20) MPa; and (4) after the vacuum before the degassing pump and the pressure in the pressure stabilizing tank are stable, slowly opening the gas inlet regulating valve in the step (4) until the input flow of the acetaldehyde gas is 20-60L/min. In the process of preparing the natural sorbal by using the byproduct natural acetaldehyde gas in the process of producing the natural benzaldehyde as the raw material, because the yield of the acetaldehyde gas is low and the acetaldehyde gas is difficult to recover, if the preferable specific settings of the vacuum before the pump and the pressure after the pump are carried out and the input flow rate of the acetaldehyde gas is limited, the utilization rate of the acetaldehyde gas can be further effectively ensured and the yield of the natural sorbal can be improved.
Preferably, the gas-liquid two-phase continuous reaction device comprises a plurality of continuous reactors used in series or in parallel, and/or the continuous reactors comprise a plurality of degassing pumps used in series or in parallel. The production efficiency can be greatly improved by using a plurality of continuous reactors in series or in parallel or using a plurality of degassing pumps in series or in parallel in the continuous reactors, or by using a plurality of continuous reactors in series or in parallel and simultaneously using a plurality of degassing pumps in series or in parallel in each continuous reactor.
For a better understanding and practice, the invention is described in detail below with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic configuration diagram of a gas-liquid two-phase continuous reaction apparatus according to example 1 of the present invention;
wherein:
1-a continuous reactor, 11-a degassing pump, 12-a liquid inlet pipe, 121-a liquid inlet regulating valve, 122-a vacuum gauge, 13-an air inlet pipe, 131-an air inlet regulating valve, 132-a gas flowmeter, 14-a post-pump liquid pipe, 15-a pressure stabilizing tank, 151-a pressure gauge, 16-a liquid outlet pipe, 161-a liquid outlet regulating valve, 2-a liquid tank, 21-a tank body, 22-a separation inclined plate, 23-an upper cavity, 24-a lower cavity, 25-a mixed liquid inlet, 3-a crude product outlet pipe, 31-an oil drain valve, 4-a collection tank, 41-a crude product discharge pipe, 411-a crude product discharge valve, 5-an air guide pipe, 6-a first gas overflow pipe, 7-a second gas overflow pipe, 8-a liquid guide pipe, 81-a liquid drain valve and 9-a liquid return pipe, θ: the elevation angle of the inclined separating plate.
Detailed Description
The following specific examples of the present invention are given to further clarify the invention, but it should be understood that they are not intended to limit the invention thereto. Further, in the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be configured in a specific orientation, and operate, and thus, should not be construed as limiting the present invention. In addition, when an element is referred to as being "secured" to another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "in communication" with another element, it can be directly in communication with the other element or intervening elements may also be present.
Example 1
The gas-liquid two-phase continuous reaction device of the embodiment, as shown in fig. 1, comprises a continuous reactor 1, a liquid tank 2, a crude product output pipe 3 and a collection tank 4; the continuous reactor 1 comprises a degassing pump 11, a liquid inlet pipe 12, an air inlet pipe 13, a post-pump liquid pipe 14, a pressure stabilizing tank 15 and a liquid outlet pipe 16, one end of the degassing pump 11 is connected with the liquid inlet pipe 12, the other end of the degassing pump is connected with the post-pump liquid pipe 14, a liquid inlet regulating valve 121 is arranged at the inlet of the liquid inlet pipe 12, an air inlet regulating valve 131 is arranged at the inlet of the air inlet pipe 13, the air inlet pipe 13 is communicated with the liquid inlet pipe 12, the communication position is positioned between the liquid inlet regulating valve 121 and the degassing pump 11, the inlet end of the pressure stabilizing tank 15 is communicated with the post-pump liquid pipe 14; the top of the liquid tank 2 is communicated with a liquid outlet pipe 16, the bottom of the liquid tank is communicated with a liquid inlet pipe 12, a liquid discharging valve 81 is arranged between the liquid tank 2 and the liquid inlet pipe 12, and the liquid tank 2 can be communicated with the liquid inlet pipe through a liquid guiding pipe 8; one end of the crude product output pipe 3 is communicated with the side wall of the liquid tank 2, and the other end is communicated with the top of the collecting tank 4.
The gas-liquid two-phase continuous reaction device of the embodiment is suitable for continuous production of preparing the aldehyde from acetaldehyde as a raw material, wherein acetaldehyde gas can enter the continuous reactor 1 through the gas inlet pipe 13, alkali liquor as a catalyst is originally stored in the liquid tank 2 and enters the continuous reactor 1 through the liquid inlet pipe 12, and during production, negative pressure is formed in front of the degassing pump 11 by operating the liquid inlet regulating valve 121, the liquid outlet regulating valve 161 and the gas inlet regulating valve 131, and positive pressure is formed behind the degassing pump 11, so that the acetaldehyde gas can be continuously sucked into the continuous reactor 1 in a negative pressure manner through reaction, and the acetaldehyde gas can be conveniently collected; the working principle of the degassing pump is that high-pressure gas and high-boiling-point organic matters are fully mixed in the pump when the pump rotates, so that a small amount of low-boiling-point solvent remained in the high-boiling-point organic matters is blown off conveniently; according to the invention, when the pump operates, the liquid inlet regulating valve 121 and the liquid outlet regulating valve 161 are regulated to realize high vacuum degree before the pump, the function of air suction is realized, low-boiling point gas acetaldehyde is continuously sucked into the alkali liquor to achieve the effect of promoting gas-liquid two-phase mixed mass transfer, and in other embodiments, the external low-boiling point gas can be introduced into the pump to carry out two-phase reaction; the liquid tank 2 is used for storing alkali liquor on one hand and receiving crude products (crude oil) generated by reaction in the continuous reactor 1 and the alkali liquor jointly entering from the top of the liquid tank 2 on the other hand, the crude products and the alkali liquor can be automatically layered in the liquid tank 2, the crude products are arranged on the upper layer, then the crude products can enter the collecting tank 4 through the crude product output pipe 3, and the alkali liquor on the lower layer enters the continuous reactor again through the liquid guide pipe 8 and the liquid inlet pipe 12. The continuous production of the sorbosol is realized by recycling the alkali liquor, continuously supplying acetaldehyde gas into the gas inlet pipe and continuously and periodically discharging the crude product from the collecting tank, so that the yield of the sorbosol product can be improved; of course, the gas-liquid two-phase continuous reaction device can also be applied to the continuous production of other gas-liquid two-phase reactions, and the following description of the use of the gas-liquid two-phase continuous reaction device takes the preparation of the sorbosol as an example, but is not limited to the continuous production and use of the sorbosol.
In a preferred embodiment, the liquid tank 2 may include a tank 21 and a separation sloping plate 22, the separation sloping plate 22 is fixed on the inner wall of the tank 21, the inner cavity of the tank 21 is divided into an upper cavity 23 and a lower cavity 24, the crude product output pipe 3 is communicated with the lower cavity 24, and a mixed liquid input port 25 is defined by the bottom end of the separation sloping plate 22 and the inner wall of the tank 21 (hereinafter, the mixture of the alkali liquor and the crude product is simply referred to as mixed liquid); the gas-liquid two-phase continuous reaction device also comprises a liquid return pipe 9, one end of the liquid return pipe 9 is communicated with the liquid outlet pipe 16, and the other end of the liquid return pipe 9 extends into the tank body 21 and is communicated with the upper cavity 23. Through the setting of separation swash plate 22 in the fluid reservoir 2, divide into fluid reservoir 2 upper and lower two parts, in the continuous production process who uses acetaldehyde as raw materials preparation mountain pear aldehyde, mix the liquid from the top get into behind the fluid reservoir 2 from last down natural flow, can slow down mixed liquid ejection of compact speed and to the stirring effect of part alkali lye under the fluid reservoir 2, be convenient for crude and alkali lye separation and collect the upper strata in separation swash plate 22 below, and discharge collection tank 4 through crude output tube 3, lower floor's alkali lye is then through bleeder valve 81, the liquid-guiding pipe 8, liquid inlet pipe 12 gets back to continuous reactor 1 mesocycle and uses. In the concrete embodiment, can set up a fuel outlet valve 31 on the crude output tube 3, be the closure state during the beginning, open the fuel outlet valve after reacting a period and emit the crude to holding tank 4, holding tank 4 can also be including the crude bleeder line 41 that is located its bottom, is provided with crude bleeder valve 411 on the crude bleeder line 41, in time emits the crude in holding tank 4 through opening crude bleeder valve 411. In a further preferred embodiment, the elevation angle theta of the separation inclined plate 22 is 50-70 degrees, one end of the liquid return pipe 9 extending into the tank body 21 is close to the bottom end of the separation inclined plate 22, and the position where the crude product output pipe 3 is communicated with the side wall 2 of the liquid tank is positioned at the upper half part of the tank body 21. Through the arrangement of the elevation angle of the separation inclined plate 22, the arrangement of the specific relative position between the liquid return pipe 9 and the separation inclined plate 22 and the arrangement of the position of the crude product output pipe 3, the stirring of the lower part of original alkali liquor reaches the minimum when the mixed liquid enters from the top of the liquid tank 2, the layering efficiency of the crude product and the alkali liquor is promoted, the crude product is more efficiently gathered below the separation inclined plate, the crude product on the upper layer is convenient to output, and the alkali liquor on the lower layer flows back to the continuous reactor 1 through the liquid guide pipe 8 and the liquid inlet pipe 12 for recycling. In a specific embodiment, the liquid tank 2 is a vertical tank with a volume of 2500L, the outlet of the lye return pipe 9 is inserted into the position of half height of the liquid tank, the separating inclined plate 22 is in an ellipse shape with a cut section, the separating inclined plate is welded and fixed with the inner wall of the tank body 21 in a sealing way, the length of the mixture input port 25 on the major axis of the ellipse accounts for about 1/10 of the total length of the major axis, and the elevation angle of the separating inclined plate is about 60 degrees.
In a specific embodiment, the surge tank can be a vertical tank, the volume of the surge tank is about 40L, the diameters of the inlet pipe and the outlet pipe of the surge tank (namely the diameters of the liquid pipe and the liquid outlet pipe after the pump) are consistent with the diameter of the outlet of the degassing pump, the diameter of the tank body is not less than 2 times of the diameters of the inlet pipe and the outlet pipe, and two pairs of sight glasses are arranged above and below the tank body to facilitate the observation of the emulsified state of the liquid. In a preferred embodiment, the degassing pump can be modified by expanding the volume, for example, expanding the volume by 4-5 times (i.e. increasing the number of the blades of the blade-shaped rotor from 1 to 4-5), so that the gas suction efficiency of the degassing pump can be improved, the stirring time in the pump can be prolonged, and the gas-liquid mixing effect can be promoted.
In a preferred embodiment, the gas-liquid two-phase continuous reaction device further comprises a gas introducing pipe 5, a first gas overflow pipe 6 and a second gas overflow pipe 7, wherein the gas introducing pipe 5 is communicated with a gas inlet pipe 13 of the continuous reactor 1; one end of the first gas overflow pipe 6 is communicated with the top of the liquid tank 2, and the other end is communicated with the gas guide pipe 5; one end of the second gas overflow pipe 7 is communicated with the top of the collecting tank 4, and the other end is communicated with the gas guide pipe 5. Acetaldehyde gas may enter the inlet duct 13 through the bleed air duct 5, for example in one particular embodiment the bleed air duct 5 is in communication with an overflow duct of a benzaldehyde production plant, i.e. acetaldehyde gas is derived from acetaldehyde, a by-product of the benzaldehyde production; because acetaldehyde is volatile, acetaldehyde gas in the liquid tank 2 and the collecting tank 4 and acetaldehyde in the air guide pipe 5 can be sucked into the air inlet pipe 13 through the first air overflow pipe 6 and the second air overflow pipe 7, and then enter the continuous reactor 1 to continuously perform aldol condensation reaction to generate the sorbal, so that the utilization rate of acetaldehyde and the yield of the sorbal are improved.
In one embodiment, the liquid inlet pipe 12 is provided with a vacuum gauge 122, the gas inlet pipe 13 is provided with a gas flow meter 132, and the surge tank 15 is provided with a pressure gauge 151. By the arrangement of the vacuum gauge 122, the gas flow meter 132 and the pressure gauge 151, the pressure of the pipeline and the flow rate of the gas entering the pipeline can be more accurately controlled so as to realize the control of the production.
Example 2
The embodiment of the invention provides a method for preparing sorb aldehyde, which uses the gas-liquid two-phase continuous reaction device and comprises the following steps:
(1) placing an alkali liquor in the liquid tank 2, wherein the alkali liquor comprises 0.5 weight percent of NaOH solution and 2.5 weight percent of Na2CO3Solution composition;
(2) setting the liquid inlet regulating valve 121, the liquid outlet regulating valve 161 and the liquid discharging valve 81 in a fully open state, setting the gas inlet regulating valve 131 in a fully closed state, and starting the degassing pump 11 to enable the alkali liquor to circularly flow between the continuous reactor 1 and the liquid tank 2;
(3) slowly closing the liquid inlet regulating valve 121 until the front of the degassing pump 11 reaches negative pressure, and slowly closing the liquid outlet regulating valve 161 until the rear of the degassing pump 11 reaches positive pressure;
(4) slowly opening the gas inlet regulating valve 131 to input acetaldehyde gas, so that aldol condensation reaction occurs in the continuous reactor 1;
(5) the crude product is collected from the collection tank 4.
In the preparation method of the sorbol, the gas-liquid two-phase continuous reaction device provided by the embodiment of the invention is utilized, the specially prepared alkali liquor is used as a catalyst, and the liquid inlet regulating valve and the liquid outlet regulating valve are reasonably regulated, so that the continuous reactor is in a stable pressure building state (namely a vacuum meter and a pressure gauge are maintained near a certain stable value) in the production process, acetaldehyde gas is continuously sucked into the alkali liquor through the air inlet pipe under negative pressure, and the aldol condensation reaction is continuously carried out in the continuous reactor, thereby realizing the continuous production of the sorbol, and effectively improving the collection rate of the acetaldehyde and the yield of the sorbol. The reaction equation for preparing the sorbosol in this example is as follows:
compared with the existing preparation method of the sorbic aldehyde, the preparation method has the following advantages:
(1) according to the invention, acetaldehyde gas is continuously sucked into the continuous reactor in a negative pressure manner, so that the acetaldehyde collection rate is effectively improved;
(2) the invention adopts the gas-liquid two-phase continuous reactor to replace the original intermittent reaction kettle, avoids the phenomenon of serious leakage, leakage and leakage of the original process, greatly reduces the concentration of pungent odor in production places, greatly improves the working environment, and effectively improves the utilization rate of acetaldehyde gas and the product yield;
(3) the invention has mild reaction conditions, avoids the problem that the original process needs refrigeration and temperature control (about 5 ℃) or uses organic solvent, reduces the production cost and improves the production efficiency.
Example 3
The embodiment of the invention provides a method for preparing sorb aldehyde, which uses the gas-liquid two-phase continuous reaction device and comprises the following steps:
(1) placing an alkali liquor in the liquid tank 2, wherein the alkali liquor consists of 15 weight percent of NaOH solution and 20 weight percent of Na2CO3Solution composition;
(2) setting the liquid inlet regulating valve 121, the liquid outlet regulating valve 161 and the liquid discharging valve 81 in a fully open state, setting the gas inlet regulating valve 131 in a fully closed state, and starting the degassing pump 11 to enable the alkali liquor to circularly flow between the continuous reactor 1 and the liquid tank 2;
(3) slowly closing the liquid inlet regulating valve 121 until the front of the degassing pump 11 reaches negative pressure, and slowly closing the liquid outlet regulating valve 161 until the rear of the degassing pump 11 reaches positive pressure;
(4) slowly opening the gas inlet regulating valve 131 to input acetaldehyde gas, so that aldol condensation reaction occurs in the continuous reactor 1;
(5) collecting the crude product from the collection tank 4;
(6) a water washing procedure: washing, neutralizing and standing the crude product, and then removing water;
(7) a separation process: and (3) carrying out reduced pressure fractionation on the crude product after the moisture is removed to obtain a finished product of the pyrenal and a byproduct of the crotonaldehyde, and continuously introducing the byproduct of the crotonaldehyde into the liquid inlet pipe.
The preparation method of the sorbosol in this embodiment realizes obtaining the finished product of the sorbosol from the crude product on the basis of the embodiment 2, and simultaneously realizes recycling of the crotonaldehyde, which is a byproduct, and further improves the yield of the sorbosol.
Example 4
With the improvement of living standard, people have higher requirements on food safety, and tend to use safer and healthier natural additives and natural mildewcides. The idea that natural products are healthier than chemical compounds is reflected in food laws and regulations, and natural sorbosol becomes an urgent need of industries such as domestic food additives, grain storage mildewproof agents and the like. Natural sorbellal is a naturally-occurring small-molecular volatile substance and exists in a small amount in plants such as kiwi fruits, olives, tomatoes, tea leaves and the like; it is also present in small amount in parched peanut, caviar, and naturally oxidized salmon oil. Because the content of the natural aldehyde is extremely low in natural resources, the high-purity natural aldehyde can not be directly extracted so far, and the market demand can not be met.
According to the current international general rule, the sorb prepared by using an all-natural carbon source as a raw material can be regarded as a natural sorb equivalent for use. In order to prepare natural sorbellal equivalents, the search for all natural carbon sources is an urgent task, and the search for natural acetaldehyde is the main direction. Natural acetaldehyde is produced in the natural fermentation process of alcohols, but the content is low and the components are complex.
At present, in the process of producing natural benzaldehyde by taking natural cinnamaldehyde as a raw material in China, acetaldehyde gas is generated at the same time, and the reaction formula is as follows:
in this process, the acetaldehyde, except for the two "H" s, is derived from the "H" s involved in the "retro-aldol condensation" reaction (the reaction of acetaldehyde with benzaldehyde to form cinnamaldehyde and water is an "aldol condensation" reaction; the reverse of which is known in the industry as the "retro-aldol condensation" reaction)2The remainder C, H, O, other than O ", was derived from natural cinnamaldehyde, corresponding to 95.45% (42/44 = 95.45%) supplied by natural cinnamaldehyde, and was entirely within the category of all natural carbon sources.
Although the natural benzaldehyde is produced in the process of producing natural benzaldehyde along with the production of natural acetaldehyde gas by-products, the yield of acetaldehyde gas is low, namely about 76kg per day (at present, 5 plants for producing natural benzaldehyde in China exist, the total yield in China is about 250 tons every year, the annual yield of a single plant is only about 50 tons, the yield of natural benzaldehyde in each plant is about 200 kg/day, the theoretical yield of the by-product natural acetaldehyde is 83 kg/day, about 8 percent of the by-product natural acetaldehyde and cinnamaldehyde are deducted to generate the phenylpentadienal by-products), and the acetaldehyde gas is extremely easy to volatilize, so that the natural benzaldehyde is difficult to recover, and no successful recovery and utilization case exists.
The embodiment of the invention provides a preparation method of natural sorbol, which uses the gas-liquid two-phase continuous reaction device and comprises the following steps:
(1) NaOH with the mass concentration of 12 percent and Na with the mass concentration of 4 percent are prepared2CO3Respectively absorbing 750kg of the solution and the solution into a liquid tank to obtain 1500kg of NaOH solution with the mass concentration of 6% and Na2CO3 solution with the mass concentration of 2% as alkali liquid catalysts;
(2) the alkali liquor discharging valve, the liquid inlet regulating valve and the liquid outlet regulating valve are sequentially and fully opened, at the moment, the air inlet regulating valve is regulated to be in a fully closed state, the alkali liquor automatically flows into the pressure stabilizing tank from the liquid tank (observed through a sight glass on the pressure stabilizing tank), and the degassing pump is started, so that the alkali liquor circularly flows between the continuous reactor 1 and the liquid tank 2;
(3) gas-liquid two-phase continuous reaction: firstly, the liquid inlet regulating valve is slowly closed to the state that the pointer of the vacuum meter is stabilized at-0.035 +/-0.001 MPa, secondly, slowly closing the liquid outlet regulating valve until the pointer of the pressure gauge is stabilized at 0.40 +/-0.02 MPa, forming negative pressure before the degassing pump and positive pressure after the degassing pump, wherein the flow of the alkaline liquor of the degassing pump is about 40L/min, finally slowly opening the gas inlet regulating valve to introduce natural acetaldehyde gas, wherein the flow of the natural acetaldehyde gas is 40L/min, during the dynamic stirring and mixing process in the continuous reactor, the natural acetaldehyde gas first develops into a gas film, secondly, breaking the air film into large bubbles, breaking the large bubbles into small bubbles again until the small bubbles are broken into micro bubbles with the diameter of 5-20nm, gradually forming emulsion with alkali liquor, greatly increasing the contact area of gas and liquid, observing that the pressure stabilizing tank is in an emulsion state, having good mixing effect, and realizing continuous aldol condensation reaction of gas and liquid phases; wherein the natural acetaldehyde gas is derived from: in the process of producing natural benzaldehyde by taking natural cinnamon oil or natural cinnamaldehyde as a raw material to carry out an aldol condensation reaction, the generated byproduct acetaldehyde gas, namely the air inlet pipe 13 is communicated with an air overflow pipe of a natural benzaldehyde production device, and if the gas-liquid two-phase continuous reactor further comprises an air introducing pipe 5, the air introducing pipe 5 is directly communicated with the air overflow pipe of the natural benzaldehyde production device;
(4) collecting the crude product from the collection tank.
13.6kg of crude product is collected at 1 st shift (8 hours), the content of the sorbosol is 86.1 percent, and the yield is 36.2 percent (the acetaldehyde gas generated by the natural benzaldehyde in 8 hours per shift deducts 8 percent of consumption of the acetaldehyde gas in side reaction with the cinnamaldehyde, 25.3kg of acetaldehyde is actually generated in each shift, 18.4kg of the natural sorbosol can be generated theoretically, the yield is 18.4/25.3=72.7 percent theoretically, and the actual yield% = calculated mass of the sorbosol/total mass of the acetaldehyde); collecting 18.8kg of crude products in class 2, wherein the content of the sorbosol is 81.2 percent, and the yield is 60.3 percent; collecting 18.9kg of crude products in class 3, wherein the content of the sorbosol is 81.1 percent, and the yield is 60.5 percent (actual number is divided by theoretical number); 18.9kg of crude products are collected in the 4 th shift, the content of the sorbosol is 80.9 percent, and the yield is 60.4 percent. The 1 st shift adopts new alkali liquor, partial products can be dissolved in the alkali liquor (or the oil-water separation effect is poor), and the yield is lower and is only 36.2 percent; and in the 2 nd to 4 th shifts, the yield is basically kept to be more than 60 percent.
On the basis of the preparation method of the sorbic aldehyde, the preparation method further utilizes natural cinnamon oil or natural cinnamaldehyde as a raw material to carry out aldol condensation reaction to produce a byproduct generated by natural benzaldehyde, wherein the byproduct is natural acetaldehyde, and compared with the existing preparation method of the sorbic aldehyde, the preparation method of the natural sorbic aldehyde has the following advantages:
(1) acetaldehyde gas is continuously sucked into alkali liquor under negative pressure, so that the problem that natural acetaldehyde gas is difficult to collect from a natural benzaldehyde production device is effectively solved, high-efficiency recovery is realized, and the problem that the acetaldehyde gas leaks into the atmosphere to pollute the environment is avoided; meanwhile, the production cost is reduced, the collection rate and the production efficiency of acetaldehyde gas are improved, and a green production process for efficiently preparing the natural pyrenal is realized;
(2) the gas-liquid two-phase continuous reactor is adopted to replace the original intermittent reaction kettle, so that the phenomenon of serious leakage caused by leakage in the original process is avoided, the degree of pungent odor in production places is greatly reduced, and the working environment is greatly improved;
(3) the natural sorbosol is prepared by carrying out aldol condensation reaction in a gas-liquid two-phase continuous reaction mode, the condition is mild, the problem that the original process needs refrigeration temperature control (about 5 ℃) or organic solvent is solved, the process is simple, the operation is simple and convenient, the production cost is reduced, the product yield is obviously improved, and the yield is improved from 45 percent of the original process to more than 55 percent of the existing process;
(4) the alkali liquor catalyst is recycled, the catalyst is supplemented in real time, the method is environment-friendly, green and pollution-free, the product is simple and convenient to separate, the natural degree of the sorbosol is high, the sorbosol belongs to the category of all-natural carbon sources, and the natural source reaches more than 95%.
In a preferred embodiment, a condenser can be added before an air overflow pipe of a device for producing natural benzaldehyde, acetaldehyde gas is further cooled, a small amount of benzaldehyde gas brought out by the acetaldehyde gas is cooled and separated, a small amount of benzaldehyde gas can be prevented from being mixed (the boiling point is 177 ℃, the boiling point of the benzaldehyde is 173 ℃), and the difficulty of finally purifying a crude product to obtain a finished product of natural benzaldehyde is reduced. In another preferred embodiment, a plurality of continuous reactors can be arranged in series or in parallel in the gas-liquid two-phase continuous reaction device, and/or a plurality of degassing pumps can be arranged in series or in parallel in the continuous reactors, so that the production efficiency can be greatly improved.
Example 5
Continuing to use the alkali liquor in the embodiment 4, continuously and slowly adjusting the liquid inlet adjusting valve to a state that the pointer of the vacuum gauge is stabilized at-0.045 +0.005MPa, and keeping the other conditions consistent with the conditions in the embodiment 4: collecting 18.2kg of crude products in the 5 th shift, wherein the content of the sorbellal is 77.1 percent, and the yield is 55.4 percent; collecting 18.2kg of crude products in the 6 th shift, wherein the content of the sorbellal is 77.3 percent, and the yield is 55.5 percent; 18.1kg of crude products are collected in the 7 th shift, the content of the sorbic aldehyde is 77.4 percent, and the yield is 55.3 percent. The average yield of the products in the 5 th to 7 th shifts is about 55.4 percent.
Example 6
Continuing to use the alkali liquor in example 5, and continuing to slowly adjust the liquid inlet adjusting valve to stabilize the pointer of the vacuum gauge at-0.025 +0.005MPa, wherein other conditions are consistent with those in example 4: collecting 18.1kg of crude products in class 8, wherein the content of the sorbellal is 77.3 percent, and the yield is 55.2 percent; collecting 18.1kg of crude products in the 9 th shift, wherein the content of the sorbosol is 77.3 percent, and the yield is 55.2 percent; 18.2kg of crude products are collected in the 10 th shift, the content of the sorbic aldehyde is 77.2 percent, and the yield is 55.5 percent. The average yield is about 55.3 percent in the 8 th to 10 th shifts.
Example 7
And continuing to use the alkali liquor in the example 6, and continuously and slowly adjusting the liquid outlet adjusting valve until the pointer of the pressure gauge is stabilized at 0.50+0.02MPa, wherein other conditions are consistent with those in the example 4: collecting 16.8kg of crude products in the 11 th shift, wherein the content of the sorbellal is 82.9 percent, and the yield is 55.0 percent; collecting 16.8kg of crude products in the 12 th shift, wherein the content of the sorbellal is 82.6 percent, and the yield is 54.8 percent; 16.9kg of crude products are collected in the 13 th shift, the content of the sorbellal is 82.7 percent, and the yield is 55.2 percent. In the 11 th to 13 th shifts, the yield of the crude product is lower, but the content of the sorbosol is increased, and the total average yield is about 55.0 percent.
Example 8
And continuing to use the alkali liquor in the embodiment 7, and continuing to slowly adjust the liquid outlet adjusting valve until the pointer of the pressure gauge is stabilized at 0.30+0.02MPa, wherein other conditions are consistent with those in the embodiment 4: 17.9kg of crude products are collected in the 14 th shift, the content of the sorbosol is 77.1 percent, and the yield is 54.5 percent; 17.8kg of crude products are collected in the 15 th shift, the content of the sorbosol is 77.0 percent, and the yield is 54.1 percent; 17.9kg of crude products are collected in the 16 th shift, the content of the sorbosol is 77.2 percent, and the yield is 54.6 percent. The average yield of the products in the 14 th to 16 th shifts is about 54.4 percent.
From the repeated use of the alkali liquor in the above examples 4-8, the yield of the natural sorbal is generally over 55%, and compared with the conventional batch reaction kettle, the yield is improved by about 10% (55% -45% = 10%). The best effect is obtained from the 2 nd to 4 th shifts in the example 4, and the yield of the natural sorbosol reaches more than 60 percent, so the process conditions of the example 4 are optimized.
Under the process conditions of the embodiment 4, the alkali liquor is replaced by using 6% of LiOH solution, 8% of NaOH solution and 10% of KOH solution respectively to carry out a comparative test, and the yield result of the pyrialdehyde is about 50% generally; the carbonate and bicarbonate are used to replace the original alkali liquor, the oil content is slowly separated automatically, and the yield is generally lower than 50%.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (10)
1. A gas-liquid two-phase continuous reaction apparatus, comprising:
the continuous reactor comprises a degassing pump, a liquid inlet pipe, an air inlet pipe, a post-pump liquid pipe, a pressure stabilizing tank and a liquid outlet pipe, wherein one end of the degassing pump is connected with the liquid inlet pipe, the other end of the degassing pump is connected with the post-pump liquid pipe, negative pressure is formed in front of the degassing pump by operating a liquid inlet regulating valve, a liquid outlet regulating valve and an air inlet regulating valve during production, positive pressure is formed behind the degassing pump, high-pressure gas and high-boiling-point organic matters are fully mixed in the pump when the pump rotates, and a small amount of low-boiling-point solvent remained in the high-boiling-point organic matters is; a liquid inlet regulating valve is arranged at the inlet of the liquid inlet pipe, an air inlet regulating valve is arranged at the inlet of the air inlet pipe, the air inlet pipe is communicated with the liquid inlet pipe, the communicated part is positioned between the liquid inlet regulating valve and the degassing pump, the inlet end of the pressure stabilizing tank is communicated with the liquid pipe behind the pump, the outlet end of the pressure stabilizing tank is communicated with the liquid outlet pipe, and a liquid outlet regulating valve is arranged on the liquid outlet pipe;
the top of the liquid tank is communicated with the liquid outlet pipe, the bottom of the liquid tank is communicated with the liquid inlet pipe, and a liquid discharging valve is arranged between the liquid tank and the liquid inlet pipe; the liquid tank comprises a tank body and a separation inclined plate, the separation inclined plate is fixed on the inner wall of the tank body and divides an inner cavity of the tank body into an upper cavity and a lower cavity, and a mixed liquid input port is defined by the bottom end of the separation inclined plate and the inner wall of the tank body;
one end of the crude product output pipe is communicated with the side wall of the liquid tank, and the crude product output pipe is communicated with the lower cavity; and
and the top of the collecting tank is communicated with the other end of the crude product output pipe.
2. The gas-liquid two-phase continuous reaction device according to claim 1, characterized in that: the gas-liquid two-phase continuous reaction device further comprises a liquid return pipe, one end of the liquid return pipe is communicated with the liquid outlet pipe, and the other end of the liquid return pipe extends into the tank body and is communicated with the upper cavity.
3. The gas-liquid two-phase continuous reaction device according to claim 2, characterized in that: the elevation angle of the separation inclined plate is 50-70 degrees, one end of the liquid return pipe extending into the tank body is close to the bottom end of the separation inclined plate, and the communication position of the crude product output pipe and the side wall of the liquid tank is located at the upper half part of the tank body.
4. The gas-liquid two-phase continuous reaction device according to claim 1, further comprising a gas-introducing pipe, a first gas overflow pipe and a second gas overflow pipe, wherein the gas-introducing pipe is communicated with the gas inlet pipe of the continuous reactor; one end of the first air overflow pipe is communicated with the top of the liquid tank, and the other end of the first air overflow pipe is communicated with the air entraining pipe; one end of the second air overflow pipe is communicated with the top of the collecting tank, and the other end of the second air overflow pipe is communicated with the air entraining pipe.
5. The gas-liquid two-phase continuous reaction device according to claim 1, wherein a vacuum gauge is disposed on the liquid inlet pipe, a gas flowmeter is disposed on the gas inlet pipe, and a pressure gauge is disposed on the pressure-stabilizing tank.
6. The method for preparing the sorbosol by using the gas-liquid two-phase continuous reaction device according to any one of claims 1 to 5, which is characterized by comprising the following steps:
(1) placing prepared alkali liquor in a liquor tank, wherein the alkali liquor comprises 0.5-15 wt% of NaOH solution and 2.5-20 wt% of Na2CO3Solution composition;
(2) setting the liquid inlet regulating valve, the liquid outlet regulating valve and the liquid discharge valve in a fully open state, setting the gas inlet regulating valve in a fully closed state, and starting the degassing pump to enable the alkali liquor to circularly flow between the continuous reactor and the liquid tank;
(3) slowly closing the liquid inlet regulating valve until the liquid inlet regulating valve reaches negative pressure before the degassing pump, and slowly closing the liquid outlet regulating valve until the liquid outlet regulating valve reaches positive pressure after the degassing pump;
(4) slowly opening an air inlet regulating valve to input acetaldehyde gas, so that aldol condensation reaction occurs in the continuous reactor;
(5) collecting the crude product from the collection tank.
7. The method for preparing the sorbosol according to claim 6, wherein the crude product is collected and then subjected to a water washing process and a separation process to obtain a final product of the sorbosol and a byproduct of the crotonaldehyde, and then the byproduct of the crotonaldehyde is continuously fed into the liquid inlet pipe.
8. The method of claim 6, wherein the acetaldehyde gas is derived from: the acetaldehyde gas is a byproduct generated in the process of producing natural benzaldehyde by taking natural cinnamon oil or natural cinnamaldehyde as a raw material to perform an aldol condensation reaction.
9. The method for preparing the sorbosol according to claim 8, wherein in the step (3), the feed liquid regulating valve is slowly closed until the gauge pressure before the degassing pump is (-0.035 ± 0.025) MPa, after the vacuum before the degassing pump is stabilized, the discharge liquid regulating valve is continuously and slowly closed until the gauge pressure in the pressure stabilizing tank is (0.40 ± 0.20) MPa; and (4) after the vacuum before the degassing pump and the pressure in the pressure stabilizing tank are stable, slowly opening the gas inlet regulating valve in the step (4) until the input flow of the acetaldehyde gas is 20-60L/min.
10. The method for preparing the sorbanal according to claim 6, wherein the gas-liquid two-phase continuous reaction device comprises a plurality of continuous reactors connected in series or in parallel, and/or the continuous reactors comprise a plurality of degassing pumps connected in series or in parallel.
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