A method for preparing a tobacco extract based on catalytic selective oxidation technology

Abstract

The present application relates to a kind of preparation method of tobacco extract based on catalytic selective oxidation technology, selected and set tobacco raw material is placed in sealed reaction vessel;A certain amount of solvent and catalyst are added to the sealed reaction vessel, and oxygen-containing gas is filled into the sealed reaction vessel to a certain pressure;The reaction vessel is heated and continuously stirred for a certain time, and after the reaction is finished, the liquid part is separated to obtain tobacco extract.This technical solution can effectively control the degree of oxidation reaction of target components in tobacco raw material and the selectivity of product by changing the catalytic system, so as to regulate the flavor characteristics of tobacco extract, and realize controllable aroma production.When the tobacco extract is used for tobacco flavoring, the aroma quality and sensory quality of cigarette product can be significantly improved, and the harmony and compatibility of flavor characteristics with tobacco original flavor are excellent, and it can also be applied to the field of producing reconstituted tobacco leaf.

Description

Technical Field

[0001] This invention belongs to the field of tobacco extraction technology, specifically relating to a method for preparing tobacco extract based on catalytic selective oxidation technology. Background Technology

[0002] Tobacco raw materials contain a variety of chemical substances, including lignin, cellulose, starch, terpenes, heterocyclic compounds, alcohols, and aldehydes. These substances undergo oxidation reactions during cigarette production, including conditioning, fermentation, and combustion, to generate various aroma compounds. By using catalytic selective oxidation to directionally convert the chemical components in tobacco raw materials into aroma products with different aroma characteristics, the resulting tobacco extracts can be applied to cigarette production. On the one hand, this significantly improves the aroma quality and sensory characteristics of the product, exhibiting excellent harmony and compatibility between the aroma characteristics and the natural tobacco aroma. On the other hand, by modifying the catalytic system, the aroma characteristics of the tobacco extract can be effectively controlled, achieving controllable aroma production. This tobacco extract can be used in tobacco flavoring and the production of reconstituted tobacco leaves. Summary of the Invention

[0003] The purpose of this invention is to provide a method for preparing tobacco extract based on catalytic selective oxidation technology, so as to effectively control the aroma characteristics of tobacco extract and achieve controllable aroma production.

[0004] To achieve the above objectives, this application employs the following technical solution:

[0005] A method for preparing tobacco extract based on catalytic selective oxidation technology includes the following steps:

[0006] S1. Select the designated tobacco raw material and place it in a sealed reaction container;

[0007] S2. Add the set amount of solvent and catalyst into the sealed reaction vessel and stir until homogeneous;

[0008] S3. Fill the sealed reaction vessel with oxygen-containing gas to the set pressure;

[0009] S4. Heat the reaction vessel and stir continuously for a set time. After the reaction is complete, separate the liquid portion to obtain the tobacco extract.

[0010] Furthermore, the tobacco raw material is one or more of tobacco leaves, tobacco stems, tobacco dust, or tobacco ash.

[0011] Furthermore, the solvent is one or more of water, ethanol, methanol, glycerol, 1,3-propanediol, 1,2-propanediol, and ethyl acetate, and the mass ratio of tobacco raw material to solvent is 1:1-200.

[0012] Furthermore, the catalyst is a metal or a metal oxide, wherein the metal is one or more selected from Fe, Co, Ni, Cu, Zn, Nb, Mo, Ru, Rh, Pd, Ag, Pt, Au, and Re; the metal oxide is one or more selected from Fe2O3, Fe3O4, CoO, Co3O4, MnO2, Mn3O4, NiO, Ni2O3, Ni3O4, Cu2O, CuO, ZnO, Nb2O5, MoO3, RuO2, Rh2O3, AuO, and ReO3; and the mass ratio of tobacco raw material to catalyst is 1:10. -5 -10 -2 .

[0013] Furthermore, when there are two or more catalysts, they are added to step S2 according to the set mass ratio.

[0014] Furthermore, when there are two or more catalysts, the first catalyst is added in step S2 first, and after the reaction in step S4 is completed, the second catalyst is added, and steps S2 to S4 are repeated until the reaction of the last catalyst is completed.

[0015] Furthermore, when the catalyst is two or more metals, the order of addition of the catalyst is based on the activity of the metal, with the more active metal added later; when the catalyst is two or more metal oxides, the order of addition of the catalyst is based on the oxidizing power of the metal oxide, with the more active metal added later; when the catalyst is the same metal and its oxide, they are added simultaneously in step S2; when the catalyst is different metals and metal oxides, the metal is added first, followed by the metal oxide.

[0016] Furthermore, the partial pressure of the oxygen-containing gas is 0.01-10.0 MPa, the oxidation reaction temperature is 10-200℃, the stirring speed is 20-1000 rpm, and the reaction time is 0.1-72 h.

[0017] Furthermore, the partial pressure of the oxygen-containing gas is 0.5-5.0 MPa, and the oxidation reaction temperature is 80-200℃.

[0018] The beneficial effects of this invention are:

[0019] 1. This technical solution, by modifying the catalytic system, can effectively control the degree of oxidation reaction of target components in tobacco raw materials and the selectivity of products, thereby regulating the aroma characteristics of tobacco extracts and achieving controllable aroma production. Specifically, because the components of the extract obtained from the same tobacco raw material will not be completely the same when the same metal catalyst or metal oxide catalyst is used for catalytic oxidation, different components can be obtained. Through design, the aroma components of the tobacco extract can be controlled. Furthermore, when two different metals or different metal oxides are used as catalysts, whether both metals are added simultaneously in step S2 or one metal is added first in S2, and after the entire reaction is completed, the second metal is added to the reactants, and steps S2 to S4 are repeated once, the final product is not completely the same as the product obtained when both metals are added simultaneously in step S2. This increases the diversity of aroma components and allows for considerable aroma production control according to actual needs.

[0020] 2. Compared with traditional tobacco extracts, the tobacco extract obtained by this method contains more types and quantities of aroma-producing substances, and the aroma characteristics are well-coordinated and compatible with the natural aroma of tobacco.

[0021] 3. The preparation process is simple. After the catalytic selective oxidation reaction is completed, the tobacco extract product can be obtained by simple separation. Detailed Implementation

[0022] The technical solutions of the present invention will be described in detail below through embodiments. The following embodiments are merely exemplary and can only be used to explain and illustrate the technical solutions of the present invention, and should not be construed as limiting the technical solutions of the present invention.

[0023] In the following embodiments of this application, only a preparation method using one metal oxide as a catalyst is listed. Although the preparation method using a single metal, two or more metals, two or more metal oxides, or sequentially catalyzing the reaction when using two metals or metal oxides is not listed, the use of these catalysts can fully achieve the effects mentioned in the invention, and it should not be considered that the disclosure of this part of the invention is insufficient.

[0024] Example 1:

[0025] Take 10g of tobacco leaves, pulverize them using a ball mill, pass them through a 200-mesh sieve, and place them in a 200ml stainless steel reactor. Add 6.0mg of Co3O4 catalyst and 50g of water. Seal the reactor and fill it with oxygen-containing gas at a partial pressure of 0.5MPa. Maintain a mechanical stirring speed of 300rpm and heat to 80℃ to begin the reaction. The reaction time is 12 hours. After the reaction, centrifuge to obtain the liquid fraction, which is tobacco extract 1. The ratio of tobacco extract to cigarette tobacco by weight is 5:10. 6The amount of flavoring added was used in blank cigarettes, and the sensory evaluation of the added flavoring effect was carried out according to GB5606.4-2005. The scoring results are shown in Table 1.

[0026] Example 2:

[0027] Take 10g of tobacco leaves, pulverize them using a ball mill, pass them through a 200-mesh sieve, and place them in a 200ml stainless steel reactor. Add 3.0mg of MnO2 catalyst and 100g of ethanol to the reactor. Seal the reactor and fill it with oxygen-containing gas at a partial pressure of 1.5MPa. Maintain a mechanical stirring speed of 500rpm and heat to 120℃ to begin the reaction. The reaction time is 8 hours. After the reaction is complete, filter to obtain the liquid portion, which is tobacco extract 2. The ratio of tobacco extract to cigarette tobacco by weight is 9:10. 6 The amount of flavoring added was used in blank cigarettes, and the effect of the added flavoring was evaluated by sensory evaluation according to GB5606.4-2005. The scoring results are shown in Table 1.

[0028] Example 3:

[0029] Take 10g of tobacco leaves, pulverize them using a ball mill, pass them through a 200-mesh sieve, and place them in a 500ml stainless steel reactor. Add 2.0mg of Mn3O4 catalyst and 200g of 1,2-propanediol. Seal the reactor and fill it with oxygen-containing gas at a partial pressure of 2.0MPa. Maintain a mechanical stirring speed of 800rpm and heat to 160℃ to begin the reaction. The reaction time is 3 hours. After the reaction is complete, filter to obtain the liquid portion, which is tobacco extract 3. The ratio of tobacco extract to cigarette tobacco by weight is 15:10. 6 The amount of flavoring added was used in blank cigarettes, and the sensory evaluation of the added flavoring effect was carried out according to GB5606.4-2005. The scoring results are shown in Table 1.

[0030] Example 4:

[0031] Take 10g of tobacco stems, grind them using a ball mill, pass them through a 200-mesh sieve, and place them in a 1000ml stainless steel reactor. Add 50mg of AuO catalyst and 500g of ethanol to the reactor. Seal the reactor and fill it with oxygen-containing gas at a partial pressure of 2.5MPa. Maintain a mechanical stirring speed of 600rpm and heat to 150℃ to begin the reaction. The reaction time is 5 hours. After the reaction is complete, filter to obtain the liquid portion, which is tobacco extract 4. The ratio of tobacco extract to cigarette tobacco by weight is 5:10. 5 The amount of flavoring added was used in blank cigarettes, and the sensory evaluation of the added flavoring effect was carried out according to GB5606.4-2005. The scoring results are shown in Table 1.

[0032] Example 5:

[0033] Take 10g of tobacco powder, grind it using a ball mill, pass it through a 200-mesh sieve, and place it in a 2000ml stainless steel reactor. Add 100mg of Pt catalyst and 1000g of glycerol to the reactor. Seal the reactor and fill it with oxygen-containing gas at a partial pressure of 3.0MPa. Maintain a mechanical stirring speed of 700rpm and heat to 130℃ to begin the reaction. The reaction time is 6 hours. After the reaction is complete, filter to obtain the liquid portion, which is tobacco extract 5. The ratio of tobacco extract to cigarette tobacco by weight is 8:10. 5 The amount of flavoring added was used in blank cigarettes, and the sensory evaluation of the added flavoring effect was carried out according to GB5606.4-2005. The scoring results are shown in Table 1.

[0034] Example 6:

[0035] Take 10g of tobacco dust, pulverize it using a ball mill, pass it through a 200-mesh sieve, and place it in a 500ml stainless steel reactor. Add 80mg of Fe3O4 catalyst and 300g of ethyl acetate. Seal the reactor and fill it with oxygen-containing gas at a partial pressure of 3.5MPa. Maintain a mechanical stirring speed of 400rpm and heat to 110℃ to begin the reaction. The reaction time is 10 hours. After the reaction is complete, filter to obtain the liquid fraction, which is tobacco extract 6. The ratio of tobacco extract to cigarette tobacco by weight is 13:10. 6 The amount of flavoring added was used in blank cigarettes, and the sensory evaluation of the added flavoring effect was carried out according to GB5606.4-2005. The scoring results are shown in Table 1.

[0036] Table 1. Effects of tobacco extracts based on catalytic selective oxidation technology on blank Golden Leaf (Da Jin Yuan) cigarettes.

[0037]

[0038]

[0039] Table 1 shows the sensory evaluation results of adding the tobacco extract obtained after the catalytic selective oxidation reaction of tobacco raw materials to blank Golden Leaf (Da Jin Yuan) cigarettes in different embodiments. The blank Golden Leaf (Da Jin Yuan) cigarettes are blank cigarettes without added flavorings or sugars.

[0040] As shown in Table 1, compared with the blank sample without added flavoring, the six groups of cigarette samples with the tobacco extract described in the examples generally showed improvements in multiple indicators, including aroma quality, aroma quantity, off-flavors, permeability, strength, concentration, smoothness, irritation, dryness, sweetness, and aftertaste. Furthermore, due to the different catalytic conditions of the selective oxidation reaction of tobacco raw materials, the types of oxidation reactions and product selectivity varied, resulting in differences in the degree of improvement in the above indicators.

[0041] The above descriptions are merely some specific embodiments of the present invention, but the scope of protection of the present invention is not limited thereto, nor does the order of the embodiments limit the present invention in any way. Any changes or substitutions made by those skilled in the art within the scope of the technology reported in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention is not limited to the above embodiments, and should be determined by the scope of the claims.

Claims

1. A method for preparing tobacco extract based on catalytic selective oxidation technology, characterized in that, Includes the following steps: S1. Select the designated tobacco raw material and place it in a sealed reaction container; S2. Add the set amount of solvent and catalyst into the sealed reaction vessel and stir until homogeneous; S3. Fill the sealed reaction vessel with oxygen-containing gas to the set pressure; S4. Heat the reaction vessel and stir continuously for a set time. After the reaction is complete, separate the liquid portion to obtain the tobacco extract. The catalyst is a metal or a metal oxide, wherein the metal is one or more selected from Fe, Co, Ni, Cu, Zn, Nb, Mo, Ru, Rh, Pd, Ag, Pt, Au, and Re; the metal oxide is one or more selected from Fe2O3, Fe3O4, CoO, Co3O4, MnO2, Mn3O4, NiO, Ni2O3, Ni3O4, Cu2O, CuO, ZnO, Nb2O5, MoO3, RuO2, Rh2O3, AuO, and ReO3; the mass ratio of tobacco raw material to catalyst is 1:

10. -5 -10 -2 ; When there are two or more catalysts, the order of addition of the catalysts is based on the activity of the metals, with the more active ones added later; when the catalyst is a metal oxide, the one with the stronger oxidizing power is added later; when the catalyst is the same metal and metal oxide, they are added simultaneously in step S2. When there are two or more catalysts, the first catalyst is added in step S2 first. After the reaction in step S4 is completed, the second catalyst is added, and steps S2 to S4 are repeated until the reaction of the last catalyst is completed. The partial pressure of the oxygen-containing gas is 0.5-5.0 MPa, and the oxidation reaction temperature is 80-200 °C. o C; The stirring speed is 20-1000 rpm; the reaction time is 0.1-72 h.

2. The method for preparing tobacco extract based on catalytic selective oxidation technology according to claim 1, characterized in that, The tobacco raw materials are one or more of tobacco leaves, tobacco stems, and tobacco dust.

3. The method for preparing tobacco extract based on catalytic selective oxidation technology according to claim 1, characterized in that, The solvent is one or more of water, ethanol, methanol, glycerol, 1,3-propanediol, 1,2-propanediol, and ethyl acetate, and the mass ratio of tobacco raw material to solvent is 1:1-200.

4. The method for preparing tobacco extract based on catalytic selective oxidation technology according to claim 1, characterized in that, When there are two or more catalysts, they are added to step S2 according to the set mass ratio.

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