Zanthoxylin dissolving and improving process

By employing immersion extraction and solvent-assisted extraction processes, the problem of reduced solubility of zanthoxylum bungeanum in oil-soluble production has been solved, improving extraction efficiency and product quality, reducing environmental pollution, and promoting industrial development.

CN120818404APending Publication Date: 2025-10-21重庆市树上鲜食品(集团)有限公司
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Patent Information

Application Number
CN202511082834.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-08-04
Publication Date
2025-10-21

AI Technical Summary

Technical Problem

In the traditional oil-soluble method for producing Sichuan pepper oil, some of the Sichuan pepper oil molecules dissolve into the vegetable oil or volatile oil and are then carried away by the water vapor generated by the heating of the Sichuan pepper, resulting in reduced solubility, high production costs, and serious environmental pollution.

Method used

The extraction process employs immersion extraction and solvent-assisted extraction. Sichuan pepper is extracted at high temperature and water vapor is collected. After cooling, it is mixed with an organic solvent, allowed to stand and separate into layers, and then heated a second time to improve the solubility of Sichuan pepper oil. Petroleum ether is used as the organic solvent to control oil temperature and solvent evaporation, thereby improving extraction efficiency.

Benefits of technology

It improves the solubility of Sichuan pepper oil, reduces production waste emissions, lowers costs, enhances product quality and market competitiveness, and is beneficial to environmental protection and industrial development.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of zanthoxylum oil processing, and particularly discloses a xanthoxylin dissolving and improving process which comprises the following steps: S1, taking fresh zanthoxylum as a raw material, and sequentially performing impurity removal, cleaning and natural draining; s2, the drained fresh pepper is introduced into vegetable oil at the temperature of 110-130 DEG C to be subjected to extraction; s3, collecting water vapor generated in the step S2, cooling the water vapor to 40-60 DEG C, introducing the cooled water vapor into a mixing tank, and mixing the water vapor with an organic solvent in the mixing tank; s4, standing the mixing tank until obvious layering occurs in the mixing tank, the lower layer is a water layer, the upper layer is a mixing layer, and the water layer and the mixing layer are led out respectively; s5, the mixed layer is subjected to secondary heating to 130-150 DEG C, and the vegetable oil containing the zanthoxylin in the mixed layer is obtained. According to the method, the solubility of zanthoxylin extraction can be improved.
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Description

Technical Field

[0001] The present application relates to the technical field of pepper oil processing, and specifically discloses a pepper oil dissolution and enhancement process. Background Art

[0002] Zanthoxylum bungeanum, also known as 2-hydroxy-4,6-dimethoxyacetophenone, is one of the main active ingredients in Sichuan peppercorns, responsible for their pungent flavor. Zanthoxylum bungeanum imparts a distinctive aroma to products and is widely used in the food and fragrance industries. It also has anesthetic, stimulant, antibacterial, anti-wind and dampness-relieving, insecticidal, and analgesic properties. It also has a direct inhibitory effect on muscle contractions in the uterus, intestines, and bladder caused by certain drugs.

[0003] The molecular structure of zanthoxylum contains multiple oxygen atoms, which gives it a certain polarity. Therefore, zanthoxylum mainly dissolves in organic solvents, while its solubility in water is relatively low. Currently, zanthoxylum is mainly obtained from Sichuan peppercorns through oil dissolution, solvent extraction, and supercritical CO2 extraction. The oil dissolution method involves directly placing Sichuan peppercorns in hot edible vegetable oil, or slowly pouring hot oil into a container containing Sichuan peppercorns to fry them and bring out the aroma, causing the zanthoxylum to dissolve in the oil to form a Sichuan peppercorn oil product. The solvent extraction method involves repeatedly extracting Sichuan peppercorns with organic solvents to obtain Sichuan peppercorn essential oil containing zanthoxylum. The Sichuan peppercorn essential oil is then heated and mixed with edible vegetable oil to produce Sichuan peppercorn oil. The supercritical CO2 extraction method uses liquid CO2 as an extractant to extract zanthoxylum.

[0004] The main drawback of the solvent extraction method is the problem of residual solvent. Since the organic solvent may not completely evaporate during the heating process, the product aroma is impure. Furthermore, the use of solvents increases product costs and causes a certain degree of atmospheric pollution. Supercritical CO2 extraction, on the other hand, takes a long time, limits the daily processing capacity of fresh peppercorns, and requires expensive, specialized equipment and professional personnel, increasing production costs. Therefore, the oil dissolution method is still the most common method. The main difficulty in the oil dissolution method during production is the difficulty in controlling the oil temperature. Excessively high oil temperatures can cause the aromatic and numbing components in the peppercorns to evaporate and be lost. Especially for fresh peppercorns, some of the zanthoxylum oil dissolved in the vegetable oil or the peppercorn volatile oil is entrained by the water vapor generated by the heat and overflows, resulting in reduced zanthoxylum oil solubility in the vegetable oil. Excessively low oil temperatures can cause the oil to become rancid, preventing the effective components from dissolving fully, resulting in waste and high product costs. Therefore, the inventors have developed a zanthoxylum oil dissolution and enhancement process to address this issue. Summary of the Invention

[0005] The purpose of the present invention is to solve the problem that in the traditional oil-dissolving method for producing pepper oil, part of the pepper oil is dissolved in vegetable oil or volatile oil of pepper and then engulfed by water vapor generated by heating the pepper and overflows, resulting in reduced dissolution of the pepper oil in the vegetable oil.

[0006] In order to achieve the above object, the basic solution of the present invention provides a process for dissolving and improving zanthoxylum bungeanum, comprising the following steps: Step S1, using fresh peppercorns as raw materials, sequentially removing impurities, washing, and naturally draining; Step S2, immersing the drained fresh peppercorns in vegetable oil at 110-130° C. for extraction; Step S3, collecting the water vapor generated in step S2 and cooling it to 40-60°C before passing it into a mixing tank, where the water vapor is mixed with the organic solvent; Step S4, the mixing tank is allowed to stand until distinct stratification occurs in the mixing tank, wherein the lower layer is a water layer and the upper layer is a mixed layer, and the water layer and the mixed layer are respectively discharged; Step S5: reheat the mixed layer to 130-150°C to obtain the vegetable oil containing xinanol in the mixed layer. Furthermore, in the step S2, after the extraction is completed, the peppercorns in the vegetable oil are filtered out and ground until the peppercorn particles have a particle size of 40-60 meshes. In the step S3, the ground peppercorns are mixed with an organic solvent in a mixing tank.

[0007] Furthermore, in step S3, a material rack is placed in the mixing tank, the ground pepper is packaged through a filter bag with filter holes evenly distributed on the surface and placed on the material rack, and an organic solvent is sprayed downward in the mixing tank. The organic solvent contacts the filter bag on the material rack and mixes with the vegetable oil, pepper oil, etc. to form a mixed liquid, which floats on the liquid surface at the bottom of the mixing tank.

[0008] Furthermore, in step S3, the height of the mixed liquid is higher than the height of the material rack.

[0009] Furthermore, the extraction temperature is 110-115°C and the secondary heating temperature is 130-140°C, or the extraction temperature is 115-120°C and the secondary heating temperature is 140-150°C, or the extraction temperature is 120-130°C and the secondary heating temperature is 140-150°C.

[0010] Furthermore, in step S2, the ratio of fresh pepper to vegetable oil is 1:2.

[0011] Furthermore, the organic solvent is petroleum ether.

[0012] The principle and effect of this solution are: The present invention can improve the solubility of extracted zanthoxylum bungeanum, solving the problem in traditional oil-dissolving methods for producing zanthoxylum bungeanum oil, whereby some zanthoxylum bungeanum, after dissolving in vegetable oil or volatile oil of the zanthoxylum bungeanum, is engulfed by water vapor generated by the heating of the zanthoxylum bungeanum and overflows, resulting in reduced zanthoxylum bungeanum solubility in the vegetable oil. The present invention can significantly enhance the market competitiveness of the product, increase the economic benefits of the enterprise, and simultaneously reduce waste emissions during the production process, thereby contributing to environmental protection. The invention is of great significance for improving the quality of zanthoxylum bungeanum oil, enhancing its bioavailability, improving production efficiency, expanding its application areas, promoting industrial development, environmental protection, and scientific research.

[0013] Based on the same inventive concept, the present invention provides a method for processing pepper oil, which includes the above-mentioned pepper oil dissolution and enhancement process. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present application. For those skilled in the art, other drawings can be obtained based on these drawings without creative work.

[0015] Figure 1 A schematic diagram of a zanthoxylum bungeanum dissolution and enhancement process proposed in an embodiment of the present application is shown. DETAILED DESCRIPTION

[0016] In order to further illustrate the technical means and effects adopted by the present invention to achieve the predetermined purpose of the invention, the specific implementation methods, structures, features and effects of the present invention are described in detail below in conjunction with the accompanying drawings and preferred embodiments.

[0017] A process for dissolving and improving Zanthoxylum bungeanum, the flow chart is as follows Figure 1 shown.

[0018] Example 1: Step S1, raw material processing, using fresh pepper as raw material, sequentially undergoing impurity removal, cleaning and natural draining, preferably without any wet watermarks attached to the surface of the pepper, so as to retain the delicious taste of the pepper and retain the natural ingredients and physiologically active substances in the pepper to the greatest extent.

[0019] Step S2, extraction, pouring 100 kg of vegetable oil into an extraction tank while draining 50 kg of fresh peppercorns, and heating the vegetable oil to 110-115° C., and introducing the fresh peppercorns into the vegetable oil at 110-115° C. for extraction, continuously stirring with a low-speed stirrer during the extraction process, and the extraction time is 20-30 minutes. After the extraction is completed, filtering the peppercorns from the vegetable oil and grinding them until the peppercorn particles have a particle size of 40-60 meshes.

[0020] Step S3, solvent-assisted extraction, collecting water vapor generated during the extraction process of fresh pepper, transporting the water vapor in the form of a pipeline, cooling the water vapor temperature to 40-50° C. during the transportation process, and then passing it into a mixing tank, a material rack is placed in the mixing tank, the ground pepper is packaged through a filter bag with filter holes evenly distributed on the surface and placed on the material rack, petroleum ether is sprayed downward in the mixing tank, the petroleum ether contacts the filter bag on the material rack and is mixed with vegetable oil, zanthoxylum bungeanum, etc. to form a mixed liquid, which floats on the liquid surface at the bottom of the mixing tank, and the height of the mixed liquid is higher than the height of the material rack, so as to fully extract the ground pepper.

[0021] Step S4, standing and stratifying, standing the mixing tank until the mixed layer formed by the water layer and the mixed liquid in the mixing tank shows obvious stratification, passing the water layer into the water treatment tank, and passing the mixed layer into the heating tank.

[0022] Step S5, secondary heating, heating the heating tank to 130-140°C, so that the residual water vapor evaporates, and the petroleum ether with a boiling point of 60-70°C also evaporates, and the residue in the heating tank is the vegetable oil containing zanthoxylum bungeanum.

[0023] Example 2: Step S1, raw material processing, using fresh pepper as raw material, sequentially undergoing impurity removal, cleaning and natural draining, preferably without any wet watermarks attached to the surface of the pepper, so as to retain the delicious taste of the pepper and retain the natural ingredients and physiologically active substances in the pepper to the greatest extent.

[0024] Step S2, extraction, pouring 100 kg of vegetable oil into an extraction tank while draining 50 kg of fresh peppercorns, and heating the vegetable oil to 115-120° C., and introducing the fresh peppercorns into the vegetable oil at 115-120° C. for extraction, continuously stirring with a low-speed stirrer during the extraction process, and the extraction time is 20-30 minutes. After the extraction is completed, filtering out the peppercorns in the vegetable oil and grinding them until the peppercorn particles have a particle size of 40-60 meshes.

[0025] Step S3, solvent-assisted extraction, collecting water vapor generated during the extraction process of fresh pepper, transporting the water vapor in the form of a pipeline, cooling the water vapor temperature to 50-60° C. during the transportation process, and then passing it into a mixing tank, a material rack is placed in the mixing tank, the ground pepper is packaged through a filter bag with filter holes evenly distributed on the surface and placed on the material rack, petroleum ether is sprayed downward in the mixing tank, the petroleum ether contacts the filter bag on the material rack and is mixed with vegetable oil, zanthoxylum bungeanum, etc. to form a mixed liquid, which floats on the liquid surface at the bottom of the mixing tank, and the height of the mixed liquid is higher than the height of the material rack, so as to fully extract the ground pepper.

[0026] Step S4, standing and stratifying, standing the mixing tank until the mixed layer formed by the water layer and the mixed liquid in the mixing tank shows obvious stratification, passing the water layer into the water treatment tank, and passing the mixed layer into the heating tank.

[0027] Step S5, secondary heating, heating the heating tank to 140-150°C, so that the residual water vapor evaporates, and the petroleum ether with a boiling point of 60-70°C also evaporates, and the residue in the heating tank is the vegetable oil containing zanthoxylum bungeanum.

[0028] Example 3: Step S1, raw material processing, using fresh pepper as raw material, sequentially undergoing impurity removal, cleaning and natural draining, preferably without any wet watermarks attached to the surface of the pepper, so as to retain the delicious taste of the pepper and retain the natural ingredients and physiologically active substances in the pepper to the greatest extent.

[0029] Step S2, extraction, pouring 100 kg of vegetable oil into an extraction tank while draining 50 kg of fresh peppercorns, and heating the vegetable oil to 120-130° C., and introducing the fresh peppercorns into the vegetable oil at 120-130° C. for extraction, continuously stirring with a low-speed stirrer during the extraction process, and the extraction time is 20-30 minutes. After the extraction is completed, filtering out the peppercorns in the vegetable oil and grinding them until the peppercorn particles have a particle size of 40-60 meshes.

[0030] Step S3, solvent-assisted extraction, collecting water vapor generated during the extraction process of fresh pepper, transporting the water vapor in the form of a pipeline, cooling the water vapor temperature to 50-60° C. during the transportation process, and then passing it into a mixing tank, a material rack is placed in the mixing tank, the ground pepper is packaged through a filter bag with filter holes evenly distributed on the surface and placed on the material rack, petroleum ether is sprayed downward in the mixing tank, the petroleum ether contacts the filter bag on the material rack and is mixed with vegetable oil, zanthoxylum bungeanum, etc. to form a mixed liquid, which floats on the liquid surface at the bottom of the mixing tank, and the height of the mixed liquid is higher than the height of the material rack, so as to fully extract the ground pepper.

[0031] Step S4, standing and stratifying, standing the mixing tank until the mixed layer formed by the water layer and the mixed liquid in the mixing tank shows obvious stratification, passing the water layer into the water treatment tank, and passing the mixed layer into the heating tank.

[0032] Step S5, secondary heating, heating the heating tank to 140-150°C, so that the residual water vapor evaporates, and the petroleum ether with a boiling point of 60-70°C also evaporates, and the residue in the heating tank is the vegetable oil containing zanthoxylum bungeanum.

[0033] Comparative Example 1: Step S1, raw material processing, using fresh pepper as raw material, sequentially undergoing impurity removal, cleaning and natural draining, preferably without any wet watermarks attached to the surface of the pepper, so as to retain the delicious taste of the pepper and retain the natural ingredients and physiologically active substances in the pepper to the greatest extent.

[0034] Step S2, extraction, pouring 100 kg of vegetable oil into an extraction tank while draining 50 kg of fresh peppercorns, and heating the vegetable oil to 110-115° C., and introducing the fresh peppercorns into the vegetable oil at 110-115° C. for extraction, continuously stirring with a low-speed stirrer during the extraction process, and the extraction time is 20-30 minutes. After the extraction is completed, filtering the peppercorns from the vegetable oil and grinding them until the peppercorn particles have a particle size of 40-60 meshes.

[0035] Step S3, solvent-assisted extraction, a material rack is placed in the mixing tank, the ground pepper is encapsulated through a filter bag with filter holes evenly distributed on the surface and placed on the material rack, petroleum ether is sprayed downward in the mixing tank, the petroleum ether contacts the filter bag on the material rack and mixes with vegetable oil, zanthoxylum bungeanum, etc. to form a mixed liquid, which floats on the liquid surface at the bottom of the mixing tank. The height of the mixed liquid is higher than the height of the material rack, so that the ground pepper is fully extracted.

[0036] Step S4, secondary heating, heating the heating tank to 130-150° C., petroleum ether with a boiling point of 60-70° C. evaporates, and the residue in the heating tank is vegetable oil containing zanthoxylum bungeanum.

[0037] Comparative Example 2: Step S1, raw material processing, using fresh pepper as raw material, sequentially undergoing impurity removal, cleaning and natural draining, preferably without any wet watermarks attached to the surface of the pepper, so as to retain the delicious taste of the pepper and retain the natural ingredients and physiologically active substances in the pepper to the greatest extent.

[0038] Step S2, extraction, pouring 100 kg of vegetable oil into an extraction tank while draining 50 kg of fresh peppercorns, and heating the vegetable oil to 115-130° C., and introducing the fresh peppercorns into the vegetable oil at 115-130° C. for extraction, continuously stirring with a low-speed stirrer during the extraction process, and the extraction time is 20-30 minutes. After the extraction is completed, filtering out the peppercorns from the vegetable oil and grinding them until the peppercorn particles have a particle size of 40-60 meshes.

[0039] Step S3, solvent-assisted extraction, a material rack is placed in the mixing tank, the ground pepper is encapsulated through a filter bag with filter holes evenly distributed on the surface and placed on the material rack, petroleum ether is sprayed downward in the mixing tank, the petroleum ether contacts the filter bag on the material rack and mixes with vegetable oil, zanthoxylum bungeanum, etc. to form a mixed liquid, which floats on the liquid surface at the bottom of the mixing tank. The height of the mixed liquid is higher than the height of the material rack, so that the ground pepper is fully extracted.

[0040] Step S4, secondary heating, heating the heating tank to 150-170° C., petroleum ether with a boiling point of 60-70° C. evaporates, and the residue in the heating tank is vegetable oil containing zanthoxylum bungeanum.

[0041] The data of comparative examples 1, 2, 3 and comparative examples 1 and 2 are as follows: Sample No. Zanthoxylum bungeanum concentration in extract (mg / ml) Zanthoxylum bungeanum concentration after secondary heating (mg / ml) Overall dissolved content of Zanthoxylum bungeanum (%) Example 1 42.24 123.26 62.23 Example 2 41.17 120.18 61.87 Example 3 42.57 119.58 91.95 Comparative Example 1 43.35 86.65 54.56 Comparative Example 2 41.96 88.36 55.02 According to the comparative analysis of the table, the concentration of zanthoxylum bungeanum in Example 2 and Example 3 is slightly reduced after the secondary heating. The possible reason is that the secondary heating temperature is higher than that of Example 1, and some zanthoxylum bungeanum may have decomposed. However, compared with Comparative Examples 1 and 2, the solubility of the zanthoxylum bungeanum extracted in Examples 1, 2 and 3 is improved, which can significantly improve the market competitiveness of the product and increase the economic benefits of the enterprise. At the same time, it reduces waste emissions in the production process, which is beneficial to environmental protection. It is of great significance for improving the quality of pepper oil products, enhancing bioavailability, improving production efficiency, expanding application areas, promoting industrial development, environmental protection and scientific research.

[0042] Based on the same inventive concept, Example 4 provides a method for processing pepper oil, which includes the pepper oil dissolution and enhancement process of Examples 1, 2, and 3, and uses the extract obtained in steps S2 and S5 of Examples 1, 2, and 3 and the secondary heated vegetable oil as raw materials to produce pepper oil.

[0043] The above description is merely a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Although the present invention has been disclosed as a preferred embodiment as above, it is not intended to limit the present invention. Any person skilled in the art can make some changes or modifications to equivalent embodiments using the technical contents disclosed above without departing from the scope of the technical solution of the present invention. However, any indirect modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. A process for dissolving and improving zanthoxylum bungeanum, characterized in that: The following steps are involved: Step S1, using fresh peppercorns as raw materials, sequentially removing impurities, washing, and naturally draining; Step S2, immersing the drained fresh peppercorns in vegetable oil at 110-130° C. for extraction; Step S3, collecting the water vapor generated in step S2 and cooling it to 40-60°C before passing it into a mixing tank, where the water vapor is mixed with the organic solvent; Step S4, the mixing tank is allowed to stand until distinct stratification occurs in the mixing tank, wherein the lower layer is a water layer and the upper layer is a mixed layer, and the water layer and the mixed layer are respectively discharged; Step S5, secondary heating, heating the heating tank to 130-140°C, so that the residual water vapor evaporates, and the petroleum ether with a boiling point of 60-70°C also evaporates, and the residue in the heating tank is the vegetable oil containing zanthoxylum bungeanum.

2. A process for dissolving and improving zanthoxylum bungeanum according to claim 1, characterized in that: In the step S2, after the extraction is completed, the peppercorns in the vegetable oil are filtered out and ground until the peppercorn particles have a particle size of 40-60 mesh. In the step S3, the ground peppercorns are mixed with an organic solvent in a mixing tank.

3. A process for dissolving and improving zanthoxylum bungeanum according to claim 2, characterized in that: In step S3, a material rack is placed in the mixing tank, the ground pepper is packaged through a filter bag with filter holes evenly distributed on the surface and placed on the material rack, and an organic solvent is sprayed downward in the mixing tank. The organic solvent contacts the filter bag on the material rack and mixes with the vegetable oil, pepper oil, etc. to form a mixed liquid, which floats on the liquid surface at the bottom of the mixing tank.

4. A process for dissolving and improving zanthoxylum bungeanum according to claim 3, characterized in that: In step S3, the height of the mixed liquid is higher than the height of the material rack.

5. A process for dissolving and improving zanthoxylum bungeanum according to claim 1, characterized in that: The extraction temperature is 110-115°C, and the secondary heating temperature is 130-140°C, or the extraction temperature is 115-120°C, and the secondary heating temperature is 140-150°C, or the extraction temperature is 120-130°C, and the secondary heating temperature is 140-150°C.

6. A process for dissolving and improving zanthoxylum bungeanum according to claim 1, characterized in that: In step S2, the ratio of fresh pepper to vegetable oil is 1:

2.

7. A process for dissolving and improving zanthoxylum bungeanum according to claim 1, characterized in that: The organic solvent is petroleum ether.

8. A method for processing pepper oil, characterized in that: The processing method comprises the zanthoxylum bungeanum dissolving and enhancing process according to any one of claims 1 to 7.