Delta-decalactone catalytic reaction device
By designing a catalytic reaction device of a decanolide that includes a drop funnel, a catalytic reaction assembly and a water bath heating assembly, the cumbersome and inefficient problems in the existing production methods are solved, and efficient and low-cost production of decanolide is achieved.
Patent Information
- Application Number
- CN202421637817.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-11
- Publication Date
- 2025-06-10
- Estimated Expiration
- 2034-07-11
AI Technical Summary
The existing natural decanolide production methods have cumbersome synthesis processes, low yields, long steps and high costs, resulting in low yields.
A catalytic reaction device of decanolide is designed, including a drop funnel, a support frame, a catalytic reaction assembly, agitating assembly, a water bath heating assembly and extraction barrel. By optimizing the reaction conditions and equipment structure, the efficiency of the catalytic reaction is improved.
The catalytic reaction is achieved quickly and stably, which reduces production costs, improves yield and yield, and enhances practicality.
Smart Images
Figure CN222956360U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the field of δ - decanolide production, in particular to a catalytic reaction device for δ - decanolide. Background Technique
[0002] Natural δ - decanolide is widely used in artificial butter, various pastry flavors, some daily chemical flavors and tobacco flavors in daily chemical flavors. The existing production of natural δ - decanolide mainly adopts the following two methods: one is to react cyclohexanedione with n - hexyl bromide, and then oxidize, open - ring, reduce and cyclize to obtain δ - decanolide. The synthesis process of this method is relatively cumbersome and the yield is low; the other is to carry out Dieckmann condensation reaction with diethyl glutarate, and then react with n - heptyl bromide in acetone with anhydrous potassium carbonate, and obtain δ - decanolide through deacidification and oxidation. The cost of this method is reasonable, but the steps are long and the yield is not high.
[0003] Therefore, a catalytic reaction device for δ - decanolide is needed to solve this problem. Content of the Utility Model
[0004] The purpose of the utility model is to provide a catalytic reaction device for δ - decanolide, aiming to solve the problems put forward in the background technique.
[0005] To achieve the above purpose, the utility model provides the following technical solutions:
[0006] A catalytic reaction device for δ - decanolide includes a dropping funnel and a support frame arranged on the dropping funnel. The support frame is connected to a catalytic reaction assembly. The catalytic reaction assembly is embedded with a stirring assembly. A water - bath heating assembly is arranged outside the catalytic reaction assembly. An extraction barrel is arranged on one side of the water - bath heating assembly.
[0007] Preferably, a dropping pipe is arranged below the dropping funnel. The dropping pipe is connected to a soft - pressing hollow ball. The soft - pressing hollow ball is connected to a dropping conical head. The lower end of the support frame is connected to a reaction barrel.
[0008] Preferably, the reaction barrel is provided with a chute. One side of the reaction barrel is connected to a through - pipe. The chute is embedded with a sliding ring.
[0009] Preferably, steel balls are arranged in the chute. The upper part of the steel balls is in contact with the sliding ring. The sliding ring is connected to a hollow gear. A stirring rod is arranged below the hollow gear.
[0010] Preferably, the water - bath heating assembly includes a water - bath barrel. A rotary motor is arranged at the edge of the water - bath barrel. The rotary motor is connected to a rotary shaft. The rotary shaft is provided with a motor gear. The motor gear is embedded with the hollow gear.
[0011] Preferably, a heater is provided on one side of the water bath bucket. The heater is connected to a heating block, and the heating block is installed in the reaction bucket.
[0012] Preferably, a through pipe is provided above the extraction bucket. The through pipe is provided with a rotary valve, and a support table is provided on one side of the extraction bucket.
[0013] Beneficial effects: 0.1 - 0.2 moles of initial ketone, 0.1 g of catalyst, urea, hydrogen peroxide, and acetic acid solution are added to the reaction bucket for catalytic reaction. Water is added to the water bath bucket and the heater is started to keep the water temperature at 60 °C, making the catalytic reaction faster and more stable. The rotating motor drives the hollow gear to slide on the steel balls by using a slip ring, and the sliding is smoother. The hollow gear drives the stirring rod to stir the mixed solution in the reaction bucket for a long time, making the mixture evenly mixed and the reaction faster. When all the hydrogen peroxide in the mixed solution is consumed, the catalytic reaction is completed to obtain a lactone mixed solution. The rotary valve is opened, and the solution is put into the extraction bucket, and toluene is added to the extraction bucket for extraction. Lactone is extracted from the mixture, and the extract is treated with 10% aqueous NaHCO3 solution. The organic layer is separated and dried with MqS04. Toluene is removed by distillation at atmospheric pressure and in vacuo. The residue is purified using GLC, IR, and NMR spectra to obtain the product δ-decalactone. This new type has a low cost, high yield, and strong practicability. Description of the Drawings
[0014] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings described below are only exemplary, and for those of ordinary skill in the art, without creative efforts, other implementation drawings can also be obtained according to the provided drawings.
[0015] Figure 1 Schematic diagram of the overall structure of the present invention;
[0016] Figure 2 Structural diagram of the catalytic reaction component of the present invention;
[0017] Figure 3 Schematic diagram of the stirring component structure of the present invention;
[0018] Figure 4 Schematic diagram of the multi-water bath heating component structure of the present invention;
[0019] Figure 5 Schematic diagram of the extraction bucket structure of the present invention.
[0020] Legend Explanation:
[0021] 1. Dropping funnel; 2. Support frame; 3. Catalytic reaction component; 4. Stirring component; 5. Water bath heating component; 6. Extraction barrel; 11. Dropping tube; 12. Soft pressing hollow ball; 13. Dropping conical head; 21. Reaction barrel; 22. Connecting pipe; 31. Chute; 32. Slip ring; 33. Steel ball; 34. Stirring rod; 35. Hollow gear; 51. Water bath barrel; 52. Rotating motor; 53. Rotating shaft; 54. Motor gear; 511. Heater; 512. Heating block; 61. Rotating valve; 63. Support table. Detailed implementation mode
[0022] The following will further describe the present utility model in detail with reference to the drawings and embodiments. Obviously, the described embodiments are only a part of the embodiments of the utility model, rather than all embodiments. Without conflict, the embodiments in the present application and the features in the embodiments can be combined with each other. Based on the embodiments in the utility model, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the utility model.
[0023] It should be noted that if there are directional indications (such as up, down, left, right, front, back...) involved in the embodiments of the utility model, the directional indications are only used to explain the relative position relationship and movement conditions between components in a specific posture (as shown in the drawings). If the specific posture changes, the directional indications will also change accordingly.
[0024] In addition, "a plurality" means two or more. In addition, the technical solutions between the various embodiments can be combined with each other, but it must be based on the fact that those of ordinary skill in the art can use them. When the combination of technical solutions conflicts with each other or cannot be realized, it should be considered that such a combination of technical solutions does not exist and is not within the protection scope required by the utility model.
[0025] Please refer to the attached drawings of the specification Figures 1-4 A catalytic reaction device for δ-decalactone, comprising a dropping funnel 1 and a support frame 2 provided on the dropping funnel 1. The support frame 2 is connected to a catalytic reaction component 3. The catalytic reaction component 3 is fitted with a stirring component 4. A water bath heating component 5 is provided outside the catalytic reaction component 3. An extraction barrel 6 is provided on one side of the water bath heating component 5.
[0026] Further, a dropping tube 11 is provided below the dropping funnel 1. The dropping tube 11 is connected to a soft pressing hollow ball 12, and the soft pressing hollow ball 12 is connected to a dropping conical head 13. The lower end of the support frame 2 is connected to a reaction barrel 21. 0.1 - 0.2 moles of the initial ketone and 0.1 g of the catalyst are added to the reaction barrel 21 and stirred and mixed. Then, urea, hydrogen peroxide, and acetic acid solution are added to the dropping funnel 1. The mixed solution is extruded from the dropping tube 11 into the dropping conical head 13 by squeezing the soft pressing hollow ball 12 and dripped into the reaction barrel 21 from the dropping conical head 13. After the addition is completed, the catalytic reaction starts.
[0027] Further, the reaction barrel 21 is provided with a chute 31. One side of the reaction barrel 21 is connected to a through - tube 22, and the chute 31 is fitted with a sliding ring 32.
[0028] Further, steel balls 33 are provided in the chute 31. The upper part of the steel balls 33 is in contact with the sliding ring 32. The sliding ring 32 is connected to a hollow gear 35, and a stirring rod 34 is provided below the hollow gear 35.
[0029] Further, the water - bath heating assembly 5 includes a water - bath barrel 51. A rotary motor 52 is provided at the edge of the water - bath barrel 51. The rotary motor 52 is connected to a rotary shaft 53. The rotary shaft 53 is provided with a motor gear 54. The motor gear 54 is fitted with the hollow gear 35. The rotary motor 52 drives the rotary shaft 53 to rotate. The rotary shaft 53 drives the hollow gear 35 to rotate through the motor gear 54. When the hollow gear 35 rotates, the sliding ring 32 slides on the steel balls 33, and the sliding is smoother. The hollow gear 35 drives the stirring rod 34 to stir the mixed solution in the reaction barrel 21 for a long time until all the hydrogen peroxide in the mixed solution is consumed and the catalytic reaction is completed to obtain a lactone mixed solution.
[0030] Further, a heater 511 is provided on one side of the water - bath barrel 51. The heater 511 is connected to a heating block 512. The heating block 512 is installed in the reaction barrel 21. Water is added to the water - bath barrel 51 and the heater 511 is started to heat the water in the water - bath barrel 51 by using the heating block 512 until the water temperature remains at 60 degrees Celsius.
[0031] Further, a through - tube 22 is provided above the extraction barrel 6. The through - tube 22 is provided with a rotary valve 61. A support table 63 is provided on one side of the extraction barrel 6. After the catalytic reaction is completed to obtain a lactone mixed solution, the rotary valve 61 is opened, and the solution is put into the extraction barrel 6, and toluene is added to the extraction barrel 6 for extraction.
[0032] First, add 0.1 - 0.2 moles of the initial ketone and 0.1 g of the catalyst to the reaction barrel 21 and stir to mix. Then, add urea, hydrogen peroxide, and acetic acid solution to the dropping funnel 1. Squeeze the mixed solution from the dropping tube 11 into the dropping conical head 13 by squeezing the soft pressing hollow ball 12, and drip it into the reaction barrel 21 from the dropping conical head 13. After the addition is completed, start the catalytic reaction. Add water to the water bath barrel 51 and start the heater 511 to heat the water in the water bath barrel 51 using the heating block 512 until the water temperature remains at 60 degrees Celsius. Subsequently, start the rotating motor 52. The rotating motor 52 drives the rotating shaft 53 to rotate. The rotating shaft 53 drives the hollow gear 35 to rotate through the motor gear 54. When the hollow gear 35 rotates, it slides on the steel balls 33 using the slip ring 32, making the sliding smoother. The hollow gear 35 drives the stirring rod 34 to stir the mixed solution in the reaction barrel 21 for a long time until all the hydrogen peroxide in the mixed solution is consumed. After the catalytic reaction is completed, obtain the lactone mixed solution. Open the rotary valve 61, put the solution into the extraction barrel 6, and add toluene to the extraction barrel 6 for extraction. Extract the lactone from the mixture, and treat the extract with 10% aqueous NaHCO3 solution. Separate the organic layer and dry it with MqS04. Distill off toluene under atmospheric pressure and in vacuo. Purify the residue using GLC, IR, and NMR spectra to obtain the product δ-decalactone. This new type has a lower cost, a high yield, and strong practicability.
[0033] The above are only the preferred embodiments of the present utility model and are not intended to limit the present utility model. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present utility model shall be included within the protection scope of the present utility model.
[0034] For those skilled in the art, it is obvious that the present utility model is not limited to the details of the above-described exemplary embodiments, and can be implemented in other specific forms without departing from the spirit or basic characteristics of the present utility model. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present utility model is defined by the appended claims rather than the above description. Therefore, it is intended to embrace all changes falling within the meaning and scope of the equivalent elements of the claims within the present utility model. Any reference signs in the claims should not be regarded as limiting the claimed rights.
[0035] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. A butyl-decanoic acid catalytic reaction device, comprising a dropping funnel (1) and a support frame (2) arranged on the dropping funnel (1), the support frame (2) is connected to a catalytic reaction component (3), the catalytic reaction component (3) is embedded with a stirring component (4), a water bath heating component (5) is arranged on the outside of the catalytic reaction component (3), and an extraction barrel (6) is arranged on one side of the water bath heating component (5).
2. A butyl-decanoic acid catalytic reaction device according to claim 1, characterized in that: A dripping tube (11) is provided below the dripping funnel (1), the dripping tube (11) is connected to a soft press hollow ball (12), the soft press hollow ball (12) is connected to a dripping cone head (13), and the lower end of the support frame (2) is connected to a reaction barrel (21).
3. A butyl-decanoic acid catalytic reaction device according to claim 2, characterized in that: The reaction barrel (21) is provided with a slide groove (31), one side of the reaction barrel (21) is connected to a through pipe (22), and the slide groove (31) is engaged with a slip ring (32).
4. A butyl-decanoic acid catalytic reaction device according to claim 3, characterized in that: A steel ball (33) is arranged in the slide groove (31), the upper part of the steel ball (33) is in contact with the sliding ring (32), the sliding ring (32) is connected to the hollow gear (35), and a stirring rod (34) is arranged below the hollow gear (35).
5. A butyl-decanoic acid catalytic reaction device according to claim 1, characterized in that: The water bath heating component (5) comprises a water bath barrel (51), a rotating motor (52) is provided at the edge of the water bath barrel (51), the rotating motor (52) is connected to a rotating shaft (53), the rotating shaft (53) is provided with a motor gear (54), and the motor gear (54) is engaged with a hollow gear (35).
6. A butyl-decanoic acid catalytic reaction device according to claim 5, characterized in that: A heater (511) is provided on one side of the water bath barrel (51), and the heater (511) is connected to a heating block (512), and the heating block (512) is installed in the reaction barrel (21).
7. A butyl-decanoic acid catalytic reaction device according to claim 1, characterized in that: A through pipe (22) is provided above the extraction barrel (6), and a rotary valve (61) is provided on the through pipe (22). A support table (63) is provided on one side of the extraction barrel (6).