A preparation method and production device of high-purity isolongifolene

Abstract

The present application discloses a method for preparing high-purity isolongifolene and a production device thereof, and relates to the technical field of isolongifolene. The preparation method comprises the following steps: firstly, placing a catalyst in a mixer and raising the temperature in the mixer to 98-100°C; then heating the longifolene to 95-98°C and introducing it into the mixer in at least two batches in sequence for stirring, controlling the total stirring time to be 6-8h, and obtaining high-purity isolongifolene; wherein: the catalyst is obtained by uniformly mixing titanium dioxide, chromium dioxide and vanadium pentoxide acidified with 98% concentrated sulfuric acid with dioctyl phthalate and ammonium metavanadate. The present application has the effect of significantly improving the preparation purity and reducing the difficulty of industrial production.

Description

Technical Field

[0001] The present application relates to the technical field of isolongifolene, and in particular to a preparation method of high-purity isolongifolene and a production device thereof. Background Art

[0002] Isolongifolene is a product obtained by catalytic isomerization of longifolene in heavy turpentine. Like longifolene, it is also a sesquiterpene. It is a new type of raw material in the synthetic fragrance industry. It can be used to synthesize fragrances such as isolongifoleanone, isolongifolenone, isolongifolenol, isolongifolene acetate, and hydroxymethylisolongifolene. It has a woody aroma and is widely used in the modern synthetic fragrance industry.

[0003] In the prior art, the preparation of isolongifolene is mostly carried out by using protonic acid and sulfuric acid as catalysts, and then isomerizing longifolene to obtain it.

[0004] However, since concentrated sulfuric acid is used as a catalyst to isomerize longifolene, the process of obtaining isolongifolene has the problems of high energy consumption, severe equipment corrosion and high production cost, and it is difficult to effectively treat the three wastes, which brings great difficulties to industrial production and needs to be improved. Summary of the invention

[0005] In view of this, the first object of the present application is to provide a method for preparing high-purity isolongifolene, so as to achieve the purpose of improving the preparation purity and reducing the difficulty of industrial production. The specific scheme is as follows:

[0006] A method for preparing high-purity isolongifolene comprises the following steps: firstly, placing a catalyst in a mixer and raising the temperature in the mixer to 98-100° C.; then, heating the longifolene to 95-98° C. and introducing the longifolene into the mixer in sequence in at least two batches for stirring, controlling the total stirring time to be 6-8 hours, and obtaining high-purity isolongifolene;

[0007] The catalyst is obtained by uniformly mixing titanium dioxide, chromium dioxide and vanadium pentoxide acidified with 98% concentrated sulfuric acid, dioctyl phthalate and ammonium metavanadate.

[0008] Preferably: the preparation method of the catalyst comprises the steps of ① placing titanium dioxide, chromium dioxide and vanadium pentoxide in 98% concentrated sulfuric acid for acidification for 1-2 hours, taking out and drying to obtain an acidified blank; ② placing the acidified blank in a reactor at 330-360°C and heating and calcining for 3 hours to obtain a calcined blank; ③ uniformly mixing the calcined blank with dioctyl phthalate and ammonium metavanadate to obtain a catalyst body.

[0009] Preferably, the mass ratio of the titanium dioxide, chromium dioxide and 98% concentrated sulfuric acid is 12-18:10-14:35-42; the mass ratio of the calcined blank, dioctyl phthalate and ammonium metavanadate is 42-48:45-50:1-3.

[0010] Preferably: in step ③, hollow glass microspheres are also included, and the mass ratio of the hollow glass microspheres to the calcined blank is 2-3:7-8.

[0011] Preferably, the mixing mass ratio of the catalyst to the longifolene is 1-20:100.

[0012] The second object of the present invention is to provide a production device of high-purity isolongifolene, comprising a mixing and stirring machine composed of a stirring box and a stirring mechanism located in the stirring box;

[0013] The stirring mechanism includes two connecting flanges fixedly connected to the stirring box body and two rotating cylinders respectively inserted into the corresponding connecting flanges and rotatably connected; one end of the rotating cylinder is inserted into the stirring box body, and is rotatably connected to at least three stirring rods distributed with equal arcs and connected to each other in pairs; and a docking arm is rotatably connected between the two paired stirring rods.

[0014] Preferably, the axes of the two rotating cylinders are perpendicular to each other, and the two connecting flanges are respectively fixed on the bottom and the outer peripheral side wall of the mixing box.

[0015] Preferably: a hinged head in the shape of a regular polygon is provided at the corresponding end of the rotating cylinder, and a plurality of hinged columns respectively matching and hinged with the corresponding stirring rods are provided on the outer peripheral side wall of the hinged head; a mating end arm is provided at the end of the stirring rod away from the hinged column, and a mating rotating column for rotatably connecting with the docking arm is provided on the outer side of the mating end arm; both ends of the docking arm are provided with hinged end arms rotatably connected with the corresponding mating rotating column, and the hinged end arm and the docking arm are V-shaped with the opening facing outward.

[0016] Preferably: both ends of the stirring rod are respectively provided with a swing end arm rotatably connected to the hinge column and a V-shaped arm connected to the mating end arm, the opening of the V-shaped arm faces outward, and the V-shaped arm, the stirring rod and the swing end arm form an opening facing inward; the stirring rod is provided with expansion blades on both sides along the length direction, the expansion blades are provided with a plurality of blade teeth distributed at equal intervals along the length direction, and a pushing cavity is formed between the two expansion blades and the stirring rod.

[0017] Preferably, an opening is formed at the upper end of the stirring box body for feeding, and one of the rotating cylinders is connected to a stirring motor, and the stirring motor is fixed on the outer peripheral side wall of the stirring box body.

[0018] It can be seen from the above scheme that the present application provides a preparation method of high-purity isolongifolene and a production device thereof. The preparation method of high-purity isolongifolene is by taking a catalyst obtained by uniformly mixing titanium dioxide, chromium dioxide and vanadium pentoxide acidified with 98% concentrated sulfuric acid with dioctyl phthalate and ammonium metavanadate and mixing and stirring with longifolene, so as to significantly improve the preparation purity in the catalytic isomerization treatment of the catalyst and achieve the purpose of reducing the difficulty of industrial production; the production device of high-purity isolongifolene fully mixes and stirs the catalyst and longifolene as raw materials through a stirring mechanism in a stirring box, and during the mixing and stirring process, the stirring motor drives the matching rotating cylinder to rotate, and the connecting flange plays a role in connecting and fixing with the stirring box and significantly improving the rotation stability of the rotating cylinder, thereby achieving the purpose of reducing the difficulty of industrial production. The rotating cylinder drives a plurality of rotatingly connected stirring rods to perform circumferential rotational motion with the rotating cylinder as the axis and reciprocating swinging motion with the hinged column as the axis; wherein the stirring rod rotates toward one side of the pushing cavity formed by the two expanding blades, thereby achieving the purpose of effectively pushing the material in the pushing cavity to move, and because of the rotational connection of the docking arm, the two matching stirring rods will be symmetrically distributed at both ends of the docking arm, so that the two matching stirring rods will perform rotational motions approaching each other and rotating motions away from each other in the driving movement of the driving cylinder, thereby driving the material in the stirring box to move and mix from the outside to the inside and / or from the inside to the outside while rotating and mixing, thereby significantly improving the catalytic isomerization treatment efficiency of longifolene, so as to achieve the effect of reducing the difficulty of industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying any creative work.

[0020] Figure 1 This is a schematic diagram of the structure of the mixing and stirring machine disclosed in this application;

[0021] Figure 2 This is a schematic diagram of the structure of the stirring mechanism disclosed in this application.

[0022] Explanation of the reference numerals: 1. Mixing mixer; 11. Mixing box; 2. Mixing mechanism; 21. Mixing motor; 22. Rotating cylinder; 23. Connecting flange; 24. Articulated head; 241. Articulated column; 25. Mixing rod; 251. Swinging end arm; 252. Expanding blade; 253. Blade teeth; 254. V-shaped arm; 255. Matching end arm; 256. Matching rotating column; 257. Pushing cavity; 26. Docking arm; 261. Articulated end arm. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0024] The following will specifically analyze the preparation method and production device of high-purity isolongifolene of the present application.

[0025] A method for preparing high-purity isolongifolene comprises the following steps: firstly, placing a catalyst in a mixing and blending machine, and raising the temperature in the mixing and blending machine to 98-100° C.; then, heating the longifolene to 95-98° C., and then introducing the longifolene into the mixing and blending machine in at least two batches in sequence for stirring, controlling the overall mixing mass ratio of the catalyst to the longifolene to be 1-20:100, and controlling the total stirring time to be 6-8 hours, to obtain high-purity isolongifolene;

[0026] Wherein: the catalyst is obtained by uniformly mixing titanium dioxide, chromium dioxide and vanadium pentoxide acidified with 98% concentrated sulfuric acid with dioctyl phthalate and ammonium metavanadate. And the preparation method of the catalyst comprises the steps of ① placing titanium dioxide, chromium dioxide and vanadium pentoxide in 98% concentrated sulfuric acid for acidification for 1-2h, and the mass ratio of titanium dioxide, chromium dioxide and 98% concentrated sulfuric acid is 12-18:10-14:35-42, taking out and drying after the acidification is completed to obtain the acidified blank; ② placing the acidified blank in a reactor at 330-360℃ and heating and calcining for 3h to obtain the calcined blank; ③ uniformly mixing the calcined blank with dioctyl phthalate and ammonium metavanadate, and the mass ratio of the calcined blank with dioctyl phthalate and ammonium metavanadate is 42-48:45-50:1-3 to obtain the catalyst body.

[0027] like Figure 1As shown, a high-purity isolongifolene production device includes a mixing mixer 1 consisting of a mixing box 11 and a mixing mechanism 2 located in the mixing box 11. A mixing motor 21 for driving the mixing mechanism 2 to produce high-purity isolongifolene is fixedly mounted on the side wall of the mixing box 11.

[0028] like Figure 2 As shown, the stirring mechanism 2 includes two connecting flanges 23 connected and fixed to the stirring box 11 and two rotating cylinders 22 respectively inserted in the corresponding connecting flanges 23 and rotatably connected. One end of the two rotating cylinders 22 is inserted into the stirring box 11, and at least three stirring rods 25 with equal arc distribution and paired with each other are rotatably connected. Among them, a docking arm 26 is rotatably connected between the two paired stirring rods 25. It should be noted that the stirring motor 21 is connected and fixed to one of the rotating cylinders 22 inserted on the outer peripheral side wall of the stirring box 11, so that the stirring motor 21 drives the corresponding rotating cylinder 22 to rotate, so as to achieve the purpose of driving a combination of multiple stirring rods 25 matched in pairs to achieve efficient production of high-purity isolongifolene. At the same time, an opening is formed at the upper end of the stirring box 11 for feeding, thereby reducing the difficulty of feeding.

[0029] It should be mentioned that the axes of the two rotating cylinders 22 are perpendicular to each other, and the two connecting flanges 23 are respectively fixed on the bottom and the outer peripheral side wall of the stirring box 11, so that a downward angle is formed between the two paired stirring rods 25, so that during the rotation of the stirring rods 25, the material can be stirred from the lower side of one end to the upper side of the other end and from the upper side of the corresponding end to the lower side of the other end, thereby achieving the purpose of improving the preparation purity and reducing the difficulty of industrial production.

[0030] like Figure 2As shown, a hinged head 24 in the shape of a regular polygon is provided at the corresponding end of the rotating cylinder 22. A plurality of hinged columns 241 are provided on the outer peripheral side wall of the hinged head 24, which are matched with and hinged to the corresponding stirring rods 25. At the same time, a matching end arm 255 is provided at the end of the stirring rod 25 away from the hinged column 241, and a matching rotating column 256 for rotationally connecting with the docking arm 26 is provided on the outer side of the matching end arm 255, so that the stirring rod 25 forms a stable rotation connection structure with the hinged head 24 and the docking arm 26. Among them, hinged end arms 261 rotationally connected with the corresponding matching rotating column 256 are provided at both ends of the docking arm 26, and the hinged end arm 261 and the docking arm 26 are V-shaped and open outward. At the same time, a swinging end arm 251 rotationally connected with the hinged column 241 and a V-shaped arm 254 connected with the matching end arm 255 are provided at both ends of the stirring rod 25. The opening of the V-shaped arm 254 faces outward, and the V-shaped arm 254, the stirring rod 25 and the swing end arm 251 form an opening facing inward, so as to achieve the purpose of improving the rotational connection stability between the stirring rod 25 and the hinged head 24 and the docking arm 26, while expanding the stirring range of the stirring mechanism 2 and improving the mixing efficiency and effect of the materials, so that the production device of high-purity isolongifolene has the effect of significantly improving the preparation purity and reducing the difficulty of industrial production.

[0031] It should be noted that, in order to further enhance the mixing and stirring effect of the stirring mechanism 2 on the material, expansion blades 252 are provided on both sides of the stirring rod 25 along the length direction. A plurality of blade teeth 253 with equal spacing are provided on the expansion blades 252 along the length direction, and a pushing cavity 257 is formed between the two expansion blades 252 and the stirring rod 25. When the stirring mechanism 2 is running and the stirring rod 25 is rotated, the rotation direction of the stirring rod 25 is consistent with the direction of the pushing cavity 257 formed between the two expansion blades 252 and the stirring rod 25, so that the stirring rod 25 pushes the mixed material in the pushing cavity 257 for efficient mixing and stirring, and in the movement and isomerization of the mixed material, part of the mixed material retained in the pushing cavity 257 is caused to overflow through the expansion blades 252 and the blade teeth 253 under the pressure of the front end material entering the pushing cavity 257, thereby forming a multi-striped discharging and dispersion mixing effect, so that the production device of the high-purity isolongifolene has the effect of significantly improving the preparation purity and reducing the difficulty of industrial production.

[0032] According to detection, the isomerization yield of isolongifolene obtained by the preparation method of high-purity isolongifolene and the production device thereof is greater than 95%.

[0033] Embodiment 1

[0034] A method for preparing high-purity isolongifolene comprises the following steps: firstly, placing a catalyst in a mixing and blending machine, and raising the temperature in the mixing and blending machine to 98° C.; then, heating the longifolene to 95° C., and then introducing the longifolene into the mixing and blending machine in at least two batches in sequence for stirring, controlling the overall mixing mass ratio of the catalyst to the longifolene to be 1:100, and controlling the total stirring time to be 6 hours, to obtain high-purity isolongifolene;

[0035] Wherein: the catalyst is obtained by uniformly mixing titanium dioxide, chromium dioxide and vanadium pentoxide treated by 98% concentrated sulfuric acid with dioctyl phthalate and ammonium metavanadate. And the preparation method of the catalyst includes the steps of ① placing titanium dioxide, chromium dioxide and vanadium pentoxide in 98% concentrated sulfuric acid for acidification for 1 hour, and the mass ratio of titanium dioxide, chromium dioxide and 98% concentrated sulfuric acid is 15:10:35, taking out and drying after the acidification is completed to obtain the acidification blank; ② placing the acidification blank in a reactor at 330°C and heating and calcining for 3 hours to obtain the calcination blank; ③ uniformly mixing the calcination blank with dioctyl phthalate and ammonium metavanadate, and the mass ratio of the calcination blank with dioctyl phthalate and ammonium metavanadate is 45:45:1 to obtain the catalyst body.

[0036] like Figure 1 As shown, a high-purity isolongifolene production device includes a mixing mixer 1 consisting of a mixing box 11 and a mixing mechanism 2 located in the mixing box 11. A mixing motor 21 for driving the mixing mechanism 2 to produce high-purity isolongifolene is fixedly mounted on the side wall of the mixing box 11.

[0037] like Figure 2 As shown, the stirring mechanism 2 includes two connecting flanges 23 connected and fixed to the stirring box 11 and two rotating cylinders 22 respectively inserted in the corresponding connecting flanges 23 and rotatably connected. One end of the two rotating cylinders 22 is inserted into the stirring box 11, and at least three stirring rods 25 with equal arc distribution and paired with each other are rotatably connected. Among them, a docking arm 26 is rotatably connected between the two paired stirring rods 25. It should be noted that the stirring motor 21 is connected and fixed to one of the rotating cylinders 22 inserted on the outer peripheral side wall of the stirring box 11, so that the stirring motor 21 drives the corresponding rotating cylinder 22 to rotate, so as to achieve the purpose of driving a combination of multiple stirring rods 25 matched in pairs to achieve efficient production of high-purity isolongifolene. At the same time, an opening is formed at the upper end of the stirring box 11 for feeding, thereby reducing the difficulty of feeding.

[0038] It should be mentioned that the axes of the two rotating cylinders 22 are perpendicular to each other, and the two connecting flanges 23 are respectively fixed on the bottom and the outer peripheral side wall of the stirring box 11, so that a downward angle is formed between the two paired stirring rods 25, so that during the rotation of the stirring rods 25, the material can be stirred from the lower side of one end to the upper side of the other end and from the upper side of the corresponding end to the lower side of the other end, thereby achieving the purpose of improving the preparation purity and reducing the difficulty of industrial production.

[0039] like Figure 2 As shown, a hinged head 24 in the shape of a regular polygon is provided at the corresponding end of the rotating cylinder 22. A plurality of hinged columns 241 are provided on the outer peripheral side wall of the hinged head 24, which are matched with and hinged to the corresponding stirring rods 25. At the same time, a matching end arm 255 is provided at the end of the stirring rod 25 away from the hinged column 241, and a matching rotating column 256 for rotationally connecting with the docking arm 26 is provided on the outer side of the matching end arm 255, so that the stirring rod 25 forms a stable rotation connection structure with the hinged head 24 and the docking arm 26. Among them, hinged end arms 261 rotationally connected with the corresponding matching rotating column 256 are provided at both ends of the docking arm 26, and the hinged end arm 261 and the docking arm 26 are V-shaped and open outward. At the same time, a swinging end arm 251 rotationally connected with the hinged column 241 and a V-shaped arm 254 connected with the matching end arm 255 are provided at both ends of the stirring rod 25. The opening of the V-shaped arm 254 faces outward, and the V-shaped arm 254, the stirring rod 25 and the swing end arm 251 form an opening facing inward, so as to achieve the purpose of improving the rotational connection stability between the stirring rod 25 and the hinged head 24 and the docking arm 26, while expanding the stirring range of the stirring mechanism 2 and improving the mixing efficiency and effect of the materials, so that the production device of high-purity isolongifolene has the effect of significantly improving the preparation purity and reducing the difficulty of industrial production.

[0040] It should be noted that, in order to further enhance the mixing and stirring effect of the stirring mechanism 2 on the material, expansion blades 252 are provided on both sides of the stirring rod 25 along the length direction. A plurality of blade teeth 253 with equal spacing are provided on the expansion blades 252 along the length direction, and a pushing cavity 257 is formed between the two expansion blades 252 and the stirring rod 25. When the stirring mechanism 2 is running and the stirring rod 25 is rotated, the rotation direction of the stirring rod 25 is consistent with the direction of the pushing cavity 257 formed between the two expansion blades 252 and the stirring rod 25, so that the stirring rod 25 pushes the mixed material in the pushing cavity 257 for efficient mixing and stirring, and in the movement and isomerization of the mixed material, part of the mixed material retained in the pushing cavity 257 is caused to overflow through the expansion blades 252 and the blade teeth 253 under the pressure of the front end material entering the pushing cavity 257, thereby forming a multi-striped discharging and dispersion mixing effect, so that the production device of the high-purity isolongifolene has the effect of significantly improving the preparation purity and reducing the difficulty of industrial production.

[0041] After testing, the isomerization yield of isolongifolene was 95.6%.

[0042] Embodiment 2

[0043] The difference between Example 2 and Example 1 is that the method for preparing high-purity isolongifolene in Example 2 comprises the following steps: first, placing a catalyst in a mixer and raising the temperature in the mixer to 99° C.; then heating the longifolene to 96° C. and introducing the longifolene into the mixer in sequence in at least two batches for stirring, controlling the overall mixing mass ratio of the catalyst to the longifolene to be 1:10, and controlling the total stirring time to be 7 hours, to obtain high-purity isolongifolene;

[0044] Wherein: the catalyst is obtained by uniformly mixing titanium dioxide, chromium dioxide and vanadium pentoxide treated by 98% concentrated sulfuric acid with dioctyl phthalate and ammonium metavanadate. And the preparation method of the catalyst includes the steps of ① placing titanium dioxide, chromium dioxide and vanadium pentoxide in 98% concentrated sulfuric acid for acid treatment for 1.5 hours, and the mass ratio of titanium dioxide, chromium dioxide and 98% concentrated sulfuric acid is 12:12:39, taking out and drying after the acid treatment is completed to obtain the acid treatment blank; ② placing the acid treatment blank in a reactor at 345℃ and heating and calcining for 3 hours to obtain the calcined blank; ③ uniformly mixing the calcined blank with dioctyl phthalate and ammonium metavanadate, and the mass ratio of the calcined blank with dioctyl phthalate and ammonium metavanadate is 42:47:2 to obtain the catalyst body.

[0045] After testing, the isomerization yield of isolongifolene obtained was 96.2%.

[0046] Embodiment 3

[0047] The difference between Example 3 and Example 1 is that the method for preparing high-purity isolongifolene in Example 3 comprises the following steps: first, placing a catalyst in a mixer and raising the temperature in the mixer to 100° C.; then heating the longifolene to 98° C. and introducing the longifolene into the mixer in sequence in at least two batches for stirring, controlling the overall mixing mass ratio of the catalyst to the longifolene to be 1:5, and controlling the total stirring time to be 8 hours, to obtain high-purity isolongifolene;

[0048] Wherein: the catalyst is obtained by uniformly mixing titanium dioxide, chromium dioxide and vanadium pentoxide acidified with 98% concentrated sulfuric acid with dioctyl phthalate and ammonium metavanadate. And the preparation method of the catalyst comprises the steps of ① placing titanium dioxide, chromium dioxide and vanadium pentoxide in 98% concentrated sulfuric acid for acidification for 2 hours, and the mass ratio of titanium dioxide, chromium dioxide and 98% concentrated sulfuric acid is 18:14:35, taking out and drying after the acidification is completed to obtain the acidification blank; ② placing the acidification blank in a reactor at 360°C for heating and calcining for 3 hours to obtain the calcination blank; ③ uniformly mixing the calcination blank with dioctyl phthalate and ammonium metavanadate, and the mass ratio of the calcination blank with dioctyl phthalate and ammonium metavanadate is 48:50:3 to obtain the catalyst body.

[0049] After testing, the isomerization yield of isolongifolene was 95.8%.

[0050] Embodiment 4

[0051] The difference between Example 4 and Example 1 is that in step ③ of Example 4, hollow glass microspheres are further included, and the mass ratio of the hollow glass microspheres to the calcined blank is 1:4.

[0052] After testing, the isomerization yield of isolongifolene obtained was 96.4%.

[0053] Embodiment 5

[0054] The difference between Example 5 and Example 1 is that in step ③ of Example 5, hollow glass microspheres are further included, and the mass ratio of the hollow glass microspheres to the calcined blank is 1:3.

[0055] After testing, the isomerization yield of isolongifolene obtained was 96.6%.

[0056] Embodiment 6

[0057] The difference between Example 6 and Example 1 is that in step ③ of Example 6, hollow glass microspheres are further included, and the mass ratio of the hollow glass microspheres to the calcined blank is 3:7.

[0058] After detection, the isomerization yield of isolongifolene obtained was 96.9%.

[0059] In summary, the present application provides a method for preparing high-purity isolongifolene and a production device thereof. The method for preparing high-purity isolongifolene comprises mixing and stirring a catalyst obtained by uniformly mixing titanium dioxide, chromium dioxide and vanadium pentoxide acidified with 98% concentrated sulfuric acid with dioctyl phthalate and ammonium metavanadate, so as to significantly improve the preparation purity in the catalytic isomerization treatment of the catalyst and achieve the purpose of reducing the difficulty of industrial production; the production device for high-purity isolongifolene fully mixes and stirs the catalyst and longifolene as raw materials through a stirring mechanism 2 in a stirring box 11, and during the mixing and stirring process, a stirring motor 21 drives a matching rotating cylinder 22 to rotate, and a connecting flange 23 plays a role in being connected and fixed to the stirring box 11 and significantly improving the rotation stability of the rotating cylinder 22, so that under the drive of the rotating cylinder 22 The plurality of stirring rods 25 connected in rotation are driven to perform circumferential rotational motion with the rotating cylinder 22 as the axis and reciprocating swinging motion with the hinged column 241 as the axis; wherein, the stirring rod 25 rotates toward one side of the pushing cavity 257 formed by the two expanding blades 252, so as to achieve the purpose of effectively pushing the material in the pushing cavity 257 to move, and because of the rotational connection of the docking arm 26, the two matching stirring rods 25 will be symmetrically distributed at both ends of the docking arm 26, so that the two matching stirring rods 25 will make rotational motions approaching each other and rotating motions away from each other in the driving movement of the driving cylinder, thereby driving the material in the stirring box 11 to move and mix from the outside to the inside and / or from the inside to the outside while rotating and mixing, thereby significantly improving the catalytic isomerization treatment efficiency of longifolene, so as to achieve the effect of reducing the difficulty of industrial production.

[0060] The "first", "second", "third", "fourth", etc. (if any) referred to in this application are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the data used in this way can be interchangeable where appropriate, so that the embodiments described herein can be implemented in an order other than that illustrated or described herein. In addition, the terms "including" and "having" and any of their variations are intended to cover non-exclusive inclusions, for example, a process, method or device that includes a series of steps or units is not necessarily limited to those steps or units that are clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods or devices.

[0061] It should be noted that the descriptions involving "first", "second", etc. in this application are only for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In addition, the technical solutions between the various embodiments can be combined with each other, but they must be based on the ability of ordinary technicians in this field to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such combination of technical solutions does not exist and is not within the scope of protection required by this application.

[0062] Specific examples are used herein to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only used to help understand the method of the present application and its core idea. At the same time, for those skilled in the art, according to the idea of ​​the present application, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as a limitation on the present application.

Claims

1. A production device for high-purity isolongifolene, Features: A mixing and stirring machine (1) comprising a stirring box (11) and a stirring mechanism (2) located in the stirring box (11); The stirring mechanism (2) comprises two connecting flanges (23) connected and fixed to the stirring box (11) and two rotating cylinders (22) respectively inserted into the corresponding connecting flanges (23) and rotatably connected; one end of the rotating cylinder (22) is inserted into the stirring box (11) and is rotatably connected to at least three stirring rods (25) distributed at equal arcs and connected to each other in pairs; and a docking arm (26) is rotatably connected between the two paired stirring rods (25); the two rotating cylinders The axes of the two connecting flanges (23) are perpendicular to each other, and the two connecting flanges (23) are respectively fixed on the bottom and the outer peripheral side wall of the stirring box body (11); a corresponding end of the rotating cylinder (22) is provided with a hinged head (24) in the shape of a regular polygon, and a plurality of hinged columns (241) are provided on the outer peripheral side wall of the hinged head (24) and are respectively matched with and hinged to the corresponding stirring rods (25); a matching end arm (255) is provided at one end of the stirring rod (25) away from the hinged column (241) The outer side of the mating end arm (255) is provided with a mating rotating column (256) for rotatably connecting with the docking arm (26); both ends of the docking arm (26) are provided with hinged end arms (261) rotatably connected with the corresponding mating rotating column (256), and the hinged end arm (261) and the docking arm (26) are V-shaped and open outward; the two ends of the stirring rod (25) are respectively provided with a swinging end arm (251) rotatably connected with the hinge column (241) and a swinging end arm (251) rotatably connected with the mating end arm (26). A V-shaped arm (254) is connected to the stirring rod (255), the opening of the V-shaped arm (254) faces outward, and the V-shaped arm (254), the stirring rod (25) and the swing end arm (251) form an opening facing inward; both sides of the stirring rod (25) along the length direction are provided with expansion blades (252), and the expansion blades (252) are provided with a plurality of blade teeth (253) distributed at equal intervals along the length direction, and a pushing cavity (257) is formed between the two expansion blades (252) and the stirring rod (25).

2. A production device for high-purity isolongifolene according to claim 1, Features: An opening is formed at the upper end of the stirring box (11) for feeding materials, and one of the rotating cylinders (22) is connected to a stirring motor (21), and the stirring motor (21) is fixed on the outer peripheral side wall of the stirring box (11).

3. A method for preparing high-purity isolongifolene, using the production device for high-purity isolongifolene according to any one of claims 1 to 2, It is characterized in that The method comprises the following steps: firstly, placing a catalyst into a mixing and stirring machine (1), and raising the temperature in the mixing and stirring machine (1) to 98-100° C.; then, heating longifolene to 95-98° C., and then introducing the longifolene into the mixing and stirring machine (1) in at least two batches in sequence for stirring, and controlling the total stirring time to be 6-8 hours, so as to obtain high-purity isolongifolene; Wherein: the catalyst is obtained by uniformly mixing titanium dioxide, chromium dioxide and vanadium pentoxide acidified with 98% concentrated sulfuric acid, dioctyl phthalate and ammonium metavanadate.

4. The method for preparing high-purity isolongifolene according to claim 3, Features: The preparation method of the catalyst comprises the steps of: ① placing titanium dioxide, chromium dioxide and vanadium pentoxide in 98% concentrated sulfuric acid for acid treatment for 1-2 hours, taking out and drying to obtain an acid-treated blank; ② placing the acid-treated blank in a reactor at 330-360° C. for heating and calcining for 3 hours to obtain a calcined blank; and ③ uniformly mixing the calcined blank with dioctyl phthalate and ammonium metavanadate to obtain a catalyst body.

5. A method for preparing high-purity isolongifolene according to claim 4, Features: The mass ratio of titanium dioxide, chromium dioxide and 98% concentrated sulfuric acid is 12-18:10-14:35-42; the mass ratio of the calcined blank, dioctyl phthalate and ammonium metavanadate is 42-48:45-50:1-3.

6. The method for preparing high-purity isolongifolene according to claim 5, Features: In step ③, hollow glass microspheres are also included, and the mass ratio of the hollow glass microspheres to the calcined blank is 2-3:7-8.

7. The method for preparing high-purity isolongifolene according to claim 3, Features: The mixing mass ratio of the catalyst to the longifolene is 1-20:100.

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