CN119056385B - Tributyrin synthesis reaction kettle and tributyrin synthesis reaction method - Google Patents

Tributyrin synthesis reaction kettle and tributyrin synthesis reaction method Download PDF

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Publication number
CN119056385B
CN119056385B CN202411578340.2A CN202411578340A CN119056385B CN 119056385 B CN119056385 B CN 119056385B CN 202411578340 A CN202411578340 A CN 202411578340A CN 119056385 B CN119056385 B CN 119056385B
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Prior art keywords
fixedly connected
rod
tributyrin
stirring
reactor body
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CN202411578340.2A
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CN119056385A (en
Inventor
李金姑
迟维立
王长海
高冬梅
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Shandong Flying Pharmaceutical Ltd By Share Ltd
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Shandong Flying Pharmaceutical Ltd By Share Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/96—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with openwork frames or cages
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/40—Mixers with shaking, oscillating, or vibrating mechanisms with an axially oscillating rotary stirrer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a tributyrin synthesis reaction kettle and a tributyrin synthesis reaction method, which relate to the technical field of synthesis reaction kettles and comprise a reaction kettle body, the reactor body top is provided with the motor, and the output fixedly connected with drive shaft of motor, drive shaft rotate and install in the reactor body, is provided with stirring subassembly in the drive shaft. According to the tributyrin synthesis reaction kettle and the tributyrin synthesis reaction method, the catalyst is uniformly thrown and widely distributed in the reaction kettle body by controlling the reciprocating rotation of the discharge plate, so that the accumulation or the deletion of the catalyst in certain areas is avoided, the efficiency and the consistency of chemical reaction are improved, the chemical reaction rate is accelerated due to the fact that more reactants can be in effective contact with the catalyst, the reaction speed is accelerated due to the uniform distribution of the catalyst, the efficiency of the whole reaction process is improved, and meanwhile, the uniform distribution is also favorable for generating more consistent reaction products, so that the quality and the consistency of the final products are improved.

Description

Tributyrin synthesis reaction kettle and tributyrin synthesis reaction method
Technical Field
The invention relates to the technical field of synthesis reaction kettles, in particular to a tributyrin synthesis reaction kettle and a tributyrin synthesis reaction method.
Background
Tributyrin is an important ester compound and has wide application in various fields of foods, medicines, cosmetics and the like, the synthesis reaction of tributyrin is usually carried out under specific temperature and pressure conditions, an effective catalyst is needed to accelerate the reaction process, and the conventional tributyrin synthesis reaction kettles on the market mainly rely on a traditional stirring and heating system to finish the synthesis process at present;
In the prior art, a fixed stirrer is generally adopted in a tributyrin synthesis reaction kettle, the stirrer is driven by a motor to rotate in the reaction kettle so as to realize the mixing of reactants, meanwhile, the reaction kettle is also provided with a heating device for providing the temperature required by the reaction, and a catalyst is added into the reaction kettle through a manual or automatic feeding system;
However, the tributyrin synthesis reaction kettle of the prior art has the following significant defects:
In the prior art, the catalyst is usually added into a reaction kettle through a simple feeding system, and the distribution of the catalyst in the reaction kettle is often uneven due to the fixed shape and position of a stirrer, so that the situation of partial accumulation or deletion easily occurs, the utilization efficiency of the catalyst is reduced, and the reaction rate and the product quality are possibly influenced;
The stirring efficiency is low, the stirring range of the traditional stirrer in the reaction kettle is limited, the stirring angle is fixed, vortex and dead angle in the mixed solution are difficult to break, uneven distribution of each component in the mixed solution is caused, and the reaction efficiency and the consistency of products are affected.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a tributyrin synthesis reaction kettle and a tributyrin synthesis reaction method, and solves the technical problems mentioned in the background art.
The invention aims at achieving the purposes by adopting the following technical scheme that the tributyrin synthesis reaction kettle comprises a reaction kettle body, wherein a motor is arranged at the top of the reaction kettle body, the output end of the motor is fixedly connected with a driving shaft, the driving shaft is rotatably arranged in the reaction kettle body, and a stirring assembly is arranged on the driving shaft;
The stirring assembly comprises a movable disc arranged on a driving shaft, the bottom of the movable disc is fixedly connected with a fixed frame in a circumferential array manner, a row of stirring rods are arranged on the fixed frame, pushing rods are arranged at the inner ends of the stirring rods, sliding rods are fixedly connected with the bottoms of the pushing rods, the bottoms of the sliding rods are slidably mounted on the fixed frame, first round tables are fixedly connected with the bottoms of the sliding rods, and the first round tables are fixedly mounted at the bottoms of the driving shaft.
As a further preference of the technical scheme, the outer wall of the driving shaft is fixedly connected with a plurality of spline rods in a circumferential array, and the movable disc is slidably arranged on the driving shaft on the spline rods.
As a further preference of the technical scheme, the stirring rod is rotatably arranged on the fixed frame, the inner side end of the stirring rod is provided with an adjusting groove, and the pushing rod is slidably arranged on the adjusting groove through the sliding shaft.
As a further preference of the technical scheme, a material guide pipe is rotationally connected on the driving shaft, a second round table is rotationally connected at the bottom of the material guide pipe, the second round table is rotationally installed on the driving shaft, a plurality of baffles are fixedly connected around the side wall of the second round table, and a material discharging plate is rotationally connected between every two adjacent baffles.
As a further preference of the technical scheme, the outer wall of the driving shaft is slidably connected with a shaft seat, the outer wall of the shaft seat is rotationally connected with a control panel, the top of the moving panel is fixedly connected with a connecting rod, the top of the connecting rod is slidably connected with the bottom of the control panel, the top of the control panel is provided with a plurality of linkage rods in a circumferential array, and the other ends of the linkage rods are rotationally connected with the bottom of the discharge plate.
As a further preference of the technical scheme, the bottom of the shaft seat is fixedly connected with a damping spring, the damping spring is sleeved on the driving shaft, the bottom of the damping spring is fixedly connected with a first fixed disc, and the first fixed disc is fixedly installed on the driving shaft.
As a further preference of the technical scheme, the outer wall of the driving shaft is fixedly connected with a second fixed disc, the bottom of the second fixed disc is fixedly connected with a guide rod, the top of the control disc is fixedly connected with an arc-shaped block, and the position of the arc-shaped block corresponds to the position of the guide rod.
As a further preference of the technical scheme, the two sides of the top of the reaction kettle body are fixedly connected with feed boxes, the bottoms of the feed boxes are fixedly connected with conveying pipes, the other ends of the conveying pipes are fixedly connected with the tops of the material guide pipes, and the side walls of the material guide pipes are provided with material discharging grooves.
The invention also discloses a synthesis method of the tributyrin synthesis reaction kettle, which specifically comprises the following steps:
Pumping glycerol in a glycerol storage tank and part of butyric acid in a butyric acid storage tank into a synthesis reaction kettle body under the protection of nitrogen, heating to 60-100 ℃, starting stirring and mixing uniformly, adding p-toluenesulfonic acid serving as a catalyst into a discharge plate in the reaction kettle body through a feed box, a conveying pipe, a material guide pipe and a second round table, uniformly throwing the additive into the reaction kettle body through a control panel and a linkage rod control discharge plate, stirring and mixing the mixed liquid in the reaction kettle body by using a stirring rod, heating the synthesis reaction kettle body to 120-180 ℃, controlling the temperature of a distillation head of a fractionating column to be 100-120 ℃, and then pumping the rest butyric acid into the synthesis reaction kettle body, controlling the temperature to be 120-180 ℃ and reacting for 3-10 hours to obtain a mixture A;
Pumping the mixture A into a synthetic flash tank, heating and flashing by a synthetic flash heater, pumping the product into a condenser, cooling to below 80 ℃, and pumping the product into a rectifying device for rectifying to obtain refined tributyrin.
Compared with the prior art, the method has the following beneficial effects:
by controlling the reciprocating rotation of the discharging plate, the catalyst is uniformly sprayed and widely distributed in the reaction kettle body, the catalyst is prevented from being accumulated or lost in certain areas, and the efficiency and consistency of chemical reaction are improved, because more reactants can be effectively contacted with the catalyst, the chemical reaction rate is accelerated, the reaction speed is accelerated, the efficiency of the whole reaction process is improved, and meanwhile, the uniform distribution is also helpful to produce more consistent reaction products, so that the quality and consistency of the final products are improved.
The stirring range of the stirring rod in the reaction kettle can be adjusted by controlling the up-and-down movement of the moving plate, the fixed frame and the stirring rod, the stirring range of the stirring rod in the reaction kettle can be adjusted, the mixed liquid can be fully stirred at all corners in the reaction kettle, so that the stirring efficiency is improved, the stirring rod can be positioned on the fixed frame to rotate when the fixed frame moves up and down, the stirring angle of the stirring rod is changed, the stirring at multiple angles is favorable for breaking vortex and dead angle in the mixed liquid, the stirring effect is further improved, the components in the mixed liquid are ensured to be distributed more uniformly, the stirring range and the stirring angle are adjusted, the components in the mixed liquid can be ensured to be distributed more uniformly, the quality and the consistency of products are improved, and the stirring device is important for chemical reaction, and the uniform mixing is favorable for accelerating the reaction speed, improving the reaction efficiency and possibly reducing the generation of byproducts.
Drawings
FIG. 1 is a schematic diagram of the overall structure of the present invention;
FIG. 2 is a schematic structural view of the inside of the reaction kettle body in the invention;
FIG. 3 is a schematic view of a stirring assembly according to the present invention;
FIG. 4 is a schematic diagram of the structure of the driving shaft, the spline rod, the moving plate, the fixed frame, the stirring rod, the pushing rod, the sliding rod and the first round table in the invention;
FIG. 5 is a schematic view of the structure of a fixed frame, a stirring rod, an adjusting groove and a pushing rod in the invention;
FIG. 6 is a schematic diagram of the structure of the driving shaft, the discharging plate, the linkage rod, the control panel, the damping spring and the first fixing panel;
FIG. 7 is a schematic diagram of a second round table, a baffle, a discharge plate and a linkage rod according to the present invention;
FIG. 8 is a schematic diagram of the structure of the second fixed disk, the guide rod, the control disk, the arc-shaped block and the first fixed disk in the invention;
FIG. 9 is a schematic diagram of the structure of the feed box, the conveying pipe, the material guiding pipe and the second round table in the invention;
Fig. 10 is a schematic structural view of a control panel and a connecting rod in the present invention.
The device comprises a reaction kettle body, a motor, a driving shaft, a stirring assembly, a 41, a spline rod, a 42, a moving disc, a 43, a fixed frame, a 44, a stirring rod, a 45, an adjusting groove, a 46, a pushing rod, a 47, a sliding rod, a 48, a first round table, a 49, a connecting rod, a 410, a material guiding pipe, a 411, a second round table, a 412, a baffle, a 413, a material discharging plate, a 414, a linkage rod, a 415, a control disc, a 416, a shaft seat, a 417, a damping spring, a 418, a first fixed disc, a 419, an arc-shaped block, a 420, a second fixed disc, a 421, a guide rod, a 422, a material box, a 423, a conveying pipe, a 424 and a material discharging groove.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a technical scheme, which is shown in the drawings 1-10, and comprises a reaction kettle body 1, wherein a motor 2 is arranged at the top of the reaction kettle body 1, the output end of the motor 2 is fixedly connected with a driving shaft 3, the driving shaft 3 is rotatably arranged in the reaction kettle body 1, a stirring assembly 4 is arranged on the driving shaft 3, the stirring assembly 4 comprises a moving disc 42 arranged on the driving shaft 3, the bottom of the moving disc 42 is fixedly connected with a fixed frame 43 in a circumferential array, a row of stirring rods 44 are arranged on the fixed frame 43, a pushing rod 46 is arranged at the inner side end of the stirring rods 44, a sliding rod 47 is fixedly connected with the bottom of the pushing rod 46, the bottom of the sliding rod 47 is slidably arranged on the fixed frame 43, a first round table 48 is fixedly arranged at the bottom of the driving shaft 3, and when the driving shaft 3 is driven to rotate by the motor 2, the moving disc 42 can drive the moving disc 42 to rotate, and the moving disc 42 drives the fixed frame 43 and the stirring rods 44 to rotate, so that mixed liquid in the reaction kettle 1 is mixed;
In addition, the outer wall of the driving shaft 3 is fixedly connected with a plurality of spline rods 41, the movable disc 42 is slidably arranged on the spline rods 41, the movable disc 42 can be slidably arranged on the spline rods 41 in the vertical direction, the driving shaft 3 can drive the movable disc 42 to synchronously rotate through the spline rods 41, the stirring rod 44 is rotatably arranged on the fixed frame 43, the inner side end of the stirring rod 44 is provided with an adjusting groove 45, the pushing rod 46 is slidably arranged on the adjusting groove 45 through a sliding shaft, when the stirring rod 44 moves up and down, the stirring rod 44 rotates due to the fixed position of the pushing rod 46, and the sliding shaft on the pushing rod 46 slides in the adjusting groove 45, so that the stirring assembly 4 can be more flexibly stirred, and the mixing efficiency and the mixing quality are improved;
At the upper end of the driving shaft 3, a material guiding pipe 410 is designed to be rotatably connected, the bottom of the material guiding pipe 410 is connected with a second round table 411 in a rotating connection way, the second round table 411 is designed to be rotatably installed on the driving shaft 3, a plurality of baffles 412 are fixedly connected to the periphery of the side wall of the second round table 411, the baffles 412 are uniformly distributed on the side wall of the second round table 411 to ensure the uniformity of the functions, and a material discharging plate 413 is rotatably connected between the adjacent baffles 412, so that the material discharging plate 413 can flexibly rotate between the baffles 412, and when the catalyst in the material guiding pipe 410 slides onto the second round table 411, the catalyst on the second round table 411 slides along the guiding function of the baffles 412 and moves onto the material discharging plate 413, and the material discharging plate 413 performs throwing treatment on the catalyst to ensure the uniform distribution of the catalyst;
The outer wall of the driving shaft 3 is in sliding connection with a shaft seat 416, the outer wall of the shaft seat 416 is in rotating connection with a control disc 415, the top of the moving disc 42 is fixedly connected with a connecting rod 49, the top of the connecting rod 49 is in sliding connection with the bottom of the control disc 415 so as to ensure flexible movement of the control disc 415, the top of the control disc 415 is provided with a plurality of linkage rods 414 in a circumferential array, the other ends of the linkage rods 414 are in rotating connection with the bottom of the discharge plate 413, and when the shaft seat 416 slides up and down on the driving shaft 3, the shaft seat 416 and the control disc 415 move up and down to drive the linkage rods 414 to move up and down, so that the linkage rods 414 drive the discharge plate 413 to reciprocate, and the catalyst is thrown out;
The bottom of the shaft seat 416 is fixedly connected with a damping spring 417, the damping spring 417 is sleeved on the driving shaft 3 to ensure that proper resistance is provided in the moving process of the shaft seat 416 and the control panel 415, the bottom of the damping spring 417 is fixedly connected with a first fixed panel 418, the first fixed panel 418 is fixedly arranged on the driving shaft 3, and the shaft seat 416 and the control panel 415 can be driven to move upwards and reset under the elastic acting force of the damping spring 417 so as to ensure the stable operation of the whole system;
The outer wall of the driving shaft 3 is fixedly connected with a second fixed disc 420, the bottom of the second fixed disc 420 is fixedly connected with a guide rod 421, the top of the control disc 415 is fixedly connected with an arc-shaped block 419, the position of the arc-shaped block 419 corresponds to the position of the guide rod 421, and when the driving shaft 3 drives the second fixed disc 420 and the guide rod 421 to synchronously rotate, the guide rod 421 can push the arc-shaped block 419, the shaft seat 416 and the control disc 415 to move downwards in the rotating process so as to realize accurate control of catalyst throwing treatment;
The tank 422 is fixedly connected to the two sides of the top of the reaction kettle body 1, the conveying pipe 423 is fixedly connected to the bottom of the tank 422, the other end of the conveying pipe 423 is fixedly connected to the top of the material guiding pipe 410, so that the catalyst is smoothly conveyed into the material guiding pipe 410 from the tank 422, the material discharging groove 424 is formed in the side wall of the material guiding pipe 410, after the catalyst is put into the tank 422, the catalyst in the tank 422 is put into the material guiding pipe 410 through the conveying pipe 423, and the catalyst in the material guiding pipe 410 is separated through the material discharging groove 424 and is put into the second round table 411, so that the uniform distribution and throwing treatment of the catalyst on the second round table 411 are ensured.
In the embodiment of the invention, the catalyst such as the toluene sulfonic acid is added into the feed box 422, the catalyst in the feed box 422 is conveyed to the material guide pipe 410 through the conveying pipe 423, the material guide pipe 410 further feeds the catalyst onto the second round table 411 through the material discharge groove 424, and then the catalyst on the second round table 411 slides down and moves onto the material discharge plate 413, and finally feeds into the reaction kettle body 1 through the material discharge plate 413;
By starting the motor 2, the driving shaft 3 starts to rotate synchronously, the spline rod 41 is driven to rotate synchronously by the rotation of the driving shaft 3, the movable disc 42 is driven to rotate synchronously by the spline rod 41, the fixed frame 43 rotates synchronously by the rotation of the movable disc 42, the fixed frame 43 further drives a row of stirring rods 44 to rotate, and the rotating stirring rods 44 stir the mixed liquid in the reaction kettle body 1;
Meanwhile, the driving shaft 3 can drive the second fixed disc 420 to synchronously rotate in the rotating process, the rotation of the second fixed disc 420 can drive the guide rod 421 to synchronously rotate, when the guide rod 421 moves to the position of the movable arc block 419, the guide rod 421 can push the arc block 419 to move downwards in the rotating process, through the movement of the arc block 419, the shaft seat 416 and the control disc 415 also move downwards, and compress the damping spring 417, the downward movement of the control disc 415 can drive the linkage rod 414 to move downwards, and then the linkage rod 414 drives the discharge plate 413 to move downwards, when the guide rod 421 slides from the arc block 419 to be out of contact, under the elastic acting force of the damping spring 417, the control disc 415, the shaft seat 416 and the arc block 419 can move upwards, so that the control disc 415 can drive the linkage rod 414 to move upwards, and then drive the discharge plate 413 to move upwards, and the reciprocating rotation of the discharge plate enables the catalyst to be uniformly and widely distributed in the reaction kettle body 1, so that the accumulation or the lack of the catalyst in certain areas is avoided, the uniform distribution is favorable for improving the efficiency and the consistency of chemical reaction, and the uniform distribution is favorable for improving the reaction efficiency and the uniform reaction rate, and the uniform reaction mass, and the uniform reaction rate are also favorable for the reaction and the uniform reaction rate;
In addition, the drive shaft 3 drives the movable disc 42 through the spline rod 41 to synchronously rotate when rotating, so that the movable disc 42 drives the fixed frame 43 and the stirring rod 44 to synchronously rotate, and therefore, the stirring rod 44 can be used for carrying out mixing treatment on the mixed liquid in the reaction kettle body 1, when the control disc 415 moves up and down, the connecting rod 49 can be driven to move up and down, and then the connecting rod 49 drives the movable disc 42 to move up and down on the spline rod 41, the movable disc 42 can drive the fixed frame 43 and the stirring rod 44 to move up and down, and therefore, the stirring range of the stirring rod 44 in the reaction kettle body 1 is changed, the stirring range of the stirring rod 44 in the reaction kettle body 1 can be adjusted by controlling the movable disc 42, the fixed frame 43 and the stirring rod 44, and the stirring rod 44 can be adjusted, the stirring efficiency can be improved, the stirring angle can be improved, the stirring effect can be improved, the uniform stirring effect can be improved, and the stirring quality can be further improved, and the uniform stirring effect can be improved, and the mixing effect can be further improved.
The invention also discloses a synthesis method of the tributyrin synthesis reaction kettle, which specifically comprises the following steps:
Pumping glycerol in a glycerol storage tank and part of butyric acid in a butyric acid storage tank into a synthesis reaction kettle body 1 under the protection of nitrogen, heating to 60-100 ℃, starting stirring and mixing uniformly, adding p-toluenesulfonic acid serving as a catalyst into a discharge plate 413 in the reaction kettle body 1 through a feed box 422, a conveying pipe 423, a material guide pipe 410 and a second round table 411, uniformly spraying the additive into the reaction kettle body 1 by controlling the discharge plate 413 through a control panel 415 and a linkage rod 414, stirring and mixing the mixed liquid in the reaction kettle body 1 by utilizing a stirring rod 44, heating the synthesis reaction kettle body 1 to 120-180 ℃, controlling the temperature of a distillation head of a fractionating column to be 100-120 ℃, then pumping the rest butyric acid into the synthesis reaction kettle body 1, controlling the temperature to be 120-180 ℃, and reacting for 3-10 hours to obtain a mixture A;
Pumping the mixture A into a synthetic flash tank, heating and flashing by a synthetic flash heater, pumping the product into a condenser, cooling to below 80 ℃, and pumping the product into a rectifying device for rectifying to obtain refined tributyrin.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (3)

1.一种三丁酸甘油酯合成反应釜，包括反应釜本体（1），其特征在于：反应釜本体（1）顶部设置有电机（2），电机（2）的输出端固定连接有驱动轴（3），驱动轴（3）转动安装在反应釜本体（1）内，驱动轴（3）上设置有搅拌组件（4）；1. A tributyrin synthesis reactor, comprising a reactor body (1), characterized in that: a motor (2) is arranged on the top of the reactor body (1), a drive shaft (3) is fixedly connected to the output end of the motor (2), the drive shaft (3) is rotatably mounted in the reactor body (1), and a stirring assembly (4) is arranged on the drive shaft (3); 搅拌组件（4）包括设置在驱动轴（3）上的移动盘（42），移动盘（42）底部呈圆周阵列固定连接有固定框（43），固定框（43）上设置有一排搅拌杆（44），搅拌杆（44）内侧端设置有推动杆（46），推动杆（46）底部固定连接有滑杆（47），滑杆（47）底部滑动安装在固定框（43）上，滑杆（47）底部固定连接有第一圆台（48），第一圆台（48）固定安装在驱动轴（3）底部；The stirring assembly (4) comprises a movable disk (42) arranged on the driving shaft (3); the bottom of the movable disk (42) is fixedly connected to a fixed frame (43) in a circumferential array; a row of stirring rods (44) is arranged on the fixed frame (43); a pushing rod (46) is arranged at the inner end of the stirring rod (44); a sliding rod (47) is fixedly connected to the bottom of the pushing rod (46); the bottom of the sliding rod (47) is slidably mounted on the fixed frame (43); the bottom of the sliding rod (47) is fixedly connected to a first truncated platform (48); and the first truncated platform (48) is fixedly mounted on the bottom of the driving shaft (3); 驱动轴（3）外壁固定连接有若干花键杆（41），且移动盘（42）滑动安装在花键杆（41）上驱动轴（3）；A plurality of spline rods (41) are fixedly connected to the outer wall of the driving shaft (3), and a moving plate (42) is slidably mounted on the spline rods (41) to drive the shaft (3); 搅拌杆（44）转动安装在固定框（43）上，搅拌杆（44）内侧端开设有调节槽（45），且推动杆（46）通过滑轴滑动安装在调节槽（45）上；The stirring rod (44) is rotatably mounted on the fixed frame (43); an adjustment groove (45) is provided at the inner end of the stirring rod (44); and a push rod (46) is slidably mounted on the adjustment groove (45) via a sliding shaft; 驱动轴（3）上转动连接有导料管（410），导料管（410）底部转动连接有第二圆台（411），且第二圆台（411）转动安装在驱动轴（3）上，第二圆台（411）侧壁四周固定连接有若干挡板（412），相邻挡板（412）之间转动连接有排料板（413）；A material guide tube (410) is rotatably connected to the driving shaft (3); a second truncated platform (411) is rotatably connected to the bottom of the material guide tube (410); the second truncated platform (411) is rotatably mounted on the driving shaft (3); a plurality of baffles (412) are fixedly connected to the side walls of the second truncated platform (411); and a material discharge plate (413) is rotatably connected between adjacent baffles (412); 驱动轴（3）外壁滑动连接有轴座（416），且轴座（416）外壁转动连接有控制盘（415），且移动盘（42）顶部固定连接有连接杆（49），连接杆（49）顶部与控制盘（415）底部滑动连接，控制盘（415）顶部呈圆周阵列设置有若干连动杆（414），连动杆（414）另一端与排料板（413）底部转动连接；The outer wall of the driving shaft (3) is slidably connected to a shaft seat (416), and the outer wall of the shaft seat (416) is rotatably connected to a control disk (415), and the top of the movable disk (42) is fixedly connected to a connecting rod (49), the top of the connecting rod (49) is slidably connected to the bottom of the control disk (415), and a plurality of linkage rods (414) are arranged in a circular array on the top of the control disk (415), and the other end of the linkage rod (414) is rotatably connected to the bottom of the discharge plate (413); 轴座（416）底部固定连接有阻尼弹簧（417），阻尼弹簧（417）套设在驱动轴（3）上，且阻尼弹簧（417）底部固定连接有第一固定盘（418），且第一固定盘（418）固定安装在驱动轴（3）上；A damping spring (417) is fixedly connected to the bottom of the shaft seat (416), the damping spring (417) is sleeved on the drive shaft (3), and a first fixed plate (418) is fixedly connected to the bottom of the damping spring (417), and the first fixed plate (418) is fixedly mounted on the drive shaft (3); 驱动轴（3）外壁固定连接有第二固定盘（420），第二固定盘（420）底部固定连接有导向杆（421），控制盘（415）顶部固定连接有弧形块（419），且弧形块（419）的位置与导向杆（421）的位置相互对应。A second fixed disk (420) is fixedly connected to the outer wall of the driving shaft (3), a guide rod (421) is fixedly connected to the bottom of the second fixed disk (420), and an arc block (419) is fixedly connected to the top of the control disk (415), and the position of the arc block (419) corresponds to the position of the guide rod (421). 2.根据权利要求1所述的一种三丁酸甘油酯合成反应釜，其特征在于：反应釜本体（1）顶部两侧固定连接有料箱（422），料箱（422）底部固定连接有输送管（423），输送管（423）另一端与导料管（410）顶部固定连接，导料管（410）侧壁开设有排料槽（424）。2. A tributyrin synthesis reactor according to claim 1, characterized in that: a material box (422) is fixedly connected to both sides of the top of the reactor body (1), a conveying pipe (423) is fixedly connected to the bottom of the material box (422), the other end of the conveying pipe (423) is fixedly connected to the top of the material guide pipe (410), and a discharge groove (424) is opened on the side wall of the material guide pipe (410). 3.如权利要求2任一项所述的一种三丁酸甘油酯合成反应釜的合成方法，其特征在于：具体包括以下步骤：3. The method for synthesizing a tributyrin synthesis reactor according to any one of claim 2, characterized in that it specifically comprises the following steps: 步骤一、在氮气保护下，将甘油储罐中的甘油及丁酸储罐中的部分丁酸泵入到合成反应釜本体（1）升温至60-100℃，并开启搅拌混合均匀后，通过料箱（422）、输送管（423）、导料管（410）、第二圆台（411）将对甲基苯磺酸作为催化剂添加到反应釜本体（1）中的排料板（413）中，然后将通过控制盘（415）、连动杆（414）控制排料板（413）对添加剂均匀的抛洒在反应釜本体（1）内，并利用搅拌杆（44）对反应釜本体（1）内混合液进行搅拌混合处理，然后将合成反应釜本体（1）温度升温至120-180℃，控制分馏柱的蒸馏头温度在100-120℃反应，然后将剩余的丁酸泵入到合成反应釜本体（1）中，并控制温度在120-180℃，反应3-10h，得到混合物A；Step 1: Under nitrogen protection, pump glycerol in the glycerol storage tank and part of the butyric acid in the butyric acid storage tank into the synthesis reactor body (1), heat it to 60-100°C, start stirring and mix it evenly, add p-toluenesulfonic acid as a catalyst to the discharge plate (413) in the reactor body (1) through the material box (422), the conveying pipe (423), the guide pipe (410), and the second round table (411), and then control the control panel (415) and the connecting rod (414) to control the reaction of the reactor body (1). The discharge plate (413) evenly sprinkles the additive into the reactor body (1), and the stirring rod (44) is used to stir and mix the mixed liquid in the reactor body (1), then the temperature of the synthesis reactor body (1) is raised to 120-180° C., the temperature of the distillation head of the fractionation column is controlled at 100-120° C., and then the remaining butyric acid is pumped into the synthesis reactor body (1), and the temperature is controlled at 120-180° C., and the reaction is carried out for 3-10 hours to obtain a mixture A; 步骤二、将混合物A泵入到合成闪蒸罐中并通过合成闪蒸加热器加热闪蒸，然后，将产物泵入到冷凝器中降温至80℃以下，并泵入到精馏装置精馏得到精制的三丁酸甘油酯。Step 2: Pump mixture A into a synthesis flash tank and heat it through a synthesis flash heater for flash evaporation. Then, pump the product into a condenser to cool it to below 80° C. and pump it into a distillation device for distillation to obtain refined tributyrin.
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