CN116058529A - A kind of low-boiling fuming agent based on azeotropic solvent system and preparation method thereof - Google Patents

Abstract

The invention relates to a cigarette heating technology, and aims to provide a low-boiling-point smoke agent based on an azeotropic solvent system and a preparation method thereof. The fuming agent is formed by mixing glycerol and azeotropic solvent, and the boiling point range of the fuming agent is between 250.3 and 272.5 ℃; in the fuming agent, the mass content of glycerol is 60-90%, and the mass content of azeotropic solvent is 10-40%; the azeotropic solvent is at least one of propyl benzoate, methyl salicylate, ethyl salicylate or isoamyl salicylate. The product of the invention has an azeotropic solvent system, can reduce the boiling point and the fuming temperature of a fuming agent, reduce the formation time of aerosol, and improve the moisture absorption resistance. The added food-grade azeotropic solvent is commonly used as essence and spice, has fragrant and sweet smell, and can also promote the sucking experience of consumers. The preparation method provided by the invention is simple, mild in condition, low in production cost and less in pollution, and can realize large-scale industrial production only by solvent blending.

Description

A kind of low-boiling fuming agent based on azeotropic solvent system and preparation method thereof

technical field

The invention relates to the technology of heating cigarettes, in particular to a low boiling point smoker based on an azeotropic solvent system and a preparation method thereof.

Background technique

In recent years, as consumers pay more and more attention to their own health problems and strengthen tobacco control globally, new types of tobacco, represented by heated cigarettes, develop rapidly and are favored by consumers. Heated cigarettes are the focus of future research and development in the global tobacco industry. Heated cigarettes use a heating source to heat the tobacco core material, and heat its atomized matrix section to 300-400°C, so that the tobacco will produce smoke similar to traditional cigarettes without burning, so as to meet the smoking requirements of consumers . Compared with traditional cigarettes, the harmful chemical substances and biological toxicity in the smoke of heated cigarettes are greatly reduced. While restoring the taste of cigarettes, it reduces the harm to the human body and the environment.

However, there is still a certain gap between the smoking experience of heated cigarettes and traditional cigarettes. Under low temperature conditions, the amount of tobacco smoke is low, and the release of tobacco aroma is not sufficient. In order to make the heating cigarette produce enough amount of smoke when smoking, it is usually necessary to add a certain amount of smoking agent. At present, the smoking agent used in heated cigarettes is mainly glycerol (glycerol), which recondenses and absorbs moisture after heating and vaporizing to form small liquid droplets to form smoke, thereby achieving the effect of smoking. Although glycerol has a good smoking effect, it has strong hygroscopicity, and the inhalation of moisture will reduce the amount of smoke generated, which is not conducive to the storage of cigarettes. In addition, glycerol is easy to ooze out after absorbing water, contaminates cigarette paper, and makes cigarette paper appear macular, which seriously affects the quality stability of heated cigarettes and the smoking experience of consumers.

At present, there are also some research reports on the methods for solving the problem that the smoker in heated cigarettes is extremely hygroscopic. Chinese patent (CN113729269A) discloses a smoke-generating agent for anti-moisture-absorbing cigarettes and its preparation method and application. The inorganic hydrophobic microcapsule shell is used to wrap the smoke-generating agent; Burning plant particles and its preparation method, coating the plant particles loaded with aroma substances and fuming agents with a moisture-proof layer to improve the hygroscopicity of the plant particles; Chinese patent (CN113287781A) uses polylactic acid, polysaccharides and other hydrophobic polymers The porous material containing the fuming agent is coated to solve the problem of water absorption of the fuming agent during storage. In the above-mentioned methods, the fuming agent is coated with a hydrophobic material to reduce the direct contact between the fuming agent, solvent and air, thereby improving the anti-hygroscopicity. However, the modified fuming agent has a high fuming temperature, the preparation process is cumbersome, and the requirement for the coating efficiency of the fuming agent is high. Therefore, it is very important to develop a new type of smoking agent for heating cigarettes, reduce the smoking temperature, ensure a high smoke production, and improve the anti-hygroscopicity.

Contents of the invention

The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide a low-boiling fuming agent based on an azeotropic solvent system and a preparation method thereof, and improve its anti-hygroscopicity while reducing the boiling point of the fuming agent.

In order to solve the problems of the technologies described above, the solution of the present invention is:

A low-boiling fuming agent based on an azeotropic solvent system is provided. The fuming agent is a mixture of glycerol and an azeotropic solvent, and its boiling point ranges from 250.3 to 272.5° C.; The mass content is 60% to 90%, and the mass content of the azeotropic solvent is 10% to 40%; the azeotropic solvent is propyl benzoate, methyl salicylate, ethyl salicylate or isoamyl salicylate at least one of esters.

As a preferred version, the propyl benzoate, methyl salicylate, ethyl salicylate or isoamyl salicylate are food-grade products.

The present invention further provides a method for preparing the aforementioned low-boiling fuming agent, which is characterized in that, comprising:

(1) According to the mass ratio of 60～90:10～40, measure glycerol and azeotropic solvent respectively;

(2) Under the temperature of 35-70 DEG C and the condition of stirring, the smoke-generating agent is obtained after uniformly mixing the glycerol and the azeotropic solvent.

As a preferred solution, when mixing, the temperature is controlled to be 35-70°C.

As a preferred solution, the stirring is carried out in a magnetic manner, and the rotation speed during stirring is 50-200 rpm.

The present invention also provides an application method of the aforementioned low-boiling fuming agent, which is to spray the fuming agent on the dried tobacco leaf raw material, and control the mass content of the fuming agent to be 20% of the tobacco leaf raw material; then the tobacco leaf raw material It is dried at a low temperature of 40-70° C., and then prepared into heated cigarettes through a cigarette rolling machine.

Description of invention principle:

Propyl benzoate, methyl salicylate, ethyl salicylate and isoamyl salicylate are widely used in daily necessities, food and other fields, and are important fine chemicals. Because of its strong aroma, it is often used as a fixative for daily flavors and food flavors and fragrances. In the tobacco processing industry, methyl salicylate can also be used as one of the essence components (patent CN111269753A). However, there is currently no documented use of such products as smoker components.

Propyl benzoate, methyl salicylate, ethyl salicylate or isoamyl salicylate and glycerol can form an azeotropic solvent system in a specific ratio. For example, after propyl benzoate, methyl salicylate, ethyl salicylate and isoamyl salicylate form an azeotropic solvent system with glycerin, their azeotropic points are 228.8, 221.4, 230.5 and 267°C respectively (Anal. Chem. 1947, 19, 508-600). The azeotropic solvent system has a lower boiling point than that of pure glycerol (290.0°C).

The principle can be explained as food-grade propyl benzoate, methyl salicylate, ethyl salicylate or isoamyl salicylate and other solvents form an azeotropic solvent system with glycerol, compared with pure glycerol Has a lower boiling point. Therefore, adding this type of azeotropic solvent to glycerol can reduce the boiling point and fuming temperature of the fuming agent, and shorten the formation time of the aerosol. In addition, the hydroxyl group in glycerol is easy to form intermolecular hydrogen bonds with water molecules in the air, which is extremely hygroscopic. Propyl benzoate, methyl salicylate, ethyl salicylate, or isopentyl salicylate are relatively less hygroscopic than pure glycerol rich in hydroxyl groups, so adding this The azeotrope-like solvent can also reduce the hygroscopicity of the fuming agent and improve its anti-moisture absorption effect. To sum up, adding this type of azeotropic solvent to glycerol can reduce the boiling point of the fuming agent and improve its anti-hygroscopicity.

Compared with prior art, the beneficial effect of the present invention is:

1. Add food-grade azeotropic solvent to glycerol, which can form an azeotropic solvent system with glycerol, reduce the boiling point and fuming temperature of the fuming agent, reduce the formation time of aerosol, and improve its anti-moisture absorption at the same time sex.

2. The added food-grade azeotropic solvent is often used as flavor and fragrance, which has a sweet smell and can also enhance consumers' smoking experience.

3. The preparation method of the fuming agent is simple, the conditions are mild, and only solvent blending is required, the production cost is low, the pollution is less, and large-scale industrial production can be realized.

Detailed ways

Below in conjunction with specific embodiment the present invention is described in further detail:

The raw materials used in the present invention are described as follows: Food grade glycerol (purity ≥ 99%) is purchased from Xi'an Musen Biological Engineering Co., Ltd; food grade propyl benzoate (purity ≥ 99%), methyl salicylate ( Purity ≥ 99%), ethyl salicylate (purity ≥ 99%) and isoamyl salicylate (purity ≥ 99%) were purchased from Hubei Chengfeng Chemical Co., Ltd.; potassium carbonate (purity ≥ 99%) was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.

The following examples can enable those skilled in the art to understand the present invention more comprehensively, but do not limit the present invention in any way.

1, the present invention is based on the low-boiling fuming agent of azeotropic solvent system, and its preparation method comprises the following steps:

(1) According to the mass ratio of 60～90︰10～40, measure glycerol and azeotropic solvent respectively; the azeotropic solvent can be selected from propyl benzoate, methyl salicylate, ethyl salicylate or salicylic acid At least one of the isoamyl esters is a food-grade product.

(2) Mix the glycerol and the azeotropic solvent uniformly at a temperature of 35-70° C. and under stirring conditions; during mixing, magnetic stirring may be used, and the rotational speed during stirring is 50-200 rpm.

After uniform mixing, the fuming agent is obtained, and the boiling point of the fuming agent is in the range of 250.3-272.5°C.

2. In Examples 1-7, referring to the above-mentioned method, the fuming agents based on solvent azeotropy were respectively prepared. The preparation parameters and boiling points of the fuming agents in each embodiment are shown in Table 1.

Table 1

3. The application method of the fuming agent in the present invention is as follows:

The smoking agent is sprayed on the dried tobacco leaf raw material, and the mass content of the smoking agent is controlled to be 20% of the tobacco leaf raw material; then the tobacco leaf raw material is dried at a low temperature of 40-70 DEG C, and then prepared into heated cigarettes by a cigarette rolling machine.

4. The situation of comparative examples:

(1) Comparative example 1: pure glycerol was used as the smoke-generating agent, and its boiling point was 292.0°C.

(2) Comparative Example 2: The smoking agent was prepared according to the records in the public literature (J.Phys.Conf.Ser.2021, 1802, 022025; Chinese Journal of Tobacco, 2021, 27, 1-9), wherein the mass of glycerol The proportion is 90%, the mass proportion of propylene glycol is 10%, and its boiling point is 260°C.

5. Comparative test and analysis conclusion:

(1) Test object

Referring to the contents of the aforementioned application methods, the smoking agent products in Examples 1-8 and Comparative Examples 1-2 were used in the cigarette manufacturing process respectively; in the finally obtained cigarette products containing smoking agent, the smoking agent accounted for The mass content of raw materials is 20%. Each cigarette product is defined as Examples 9-16 and Comparative Examples 3-4 in order, respectively corresponding to Examples 1-8 and Comparative Examples 1-2, and they are jointly used as test objects.

(2) Comparative test

Carry out hygroscopicity test for the smoking agent and cigarette products described in Examples 1-16 and Comparative Examples 1-4:

(2.1) Put the saturated potassium carbonate solution into an airtight container, and control the relative humidity to be 60±2%.

(2.2) Place 0.5 g of the sample in an open constant weight weighing bottle, and then place it in the above-mentioned airtight container containing saturated potassium carbonate solution.

(2.3) After standing at a constant temperature of 25±1°C for 5 days, record the mass of the sample.

(2.4) Calculate the moisture absorption rate of the sample based on the mass change before and after the sample is placed. Each sample is tested 3 times in parallel, and the average value is taken.

Table 2 shows the moisture absorption rate data of the samples in each example and comparative example.

Table 2

Smoker Moisture absorption rate (%) Smoking material containing fuming agent Moisture absorption rate (%) Example 1 28.2 Example 9 12.8 Example 2 29.3 Example 10 13.3 Example 3 29.1 Example 11 13.0 Example 4 28.8 Example 12 13.2 Example 5 33.5 Example 13 14.9 Example 6 37.1 Example 14 16.1 Example 7 36.5 Example 15 15.9 Example 8 34.2 Example 16 15.3 Comparative example 1 42.1 Comparative example 3 19.2 Comparative example 2 40.3 Comparative example 4 18.2

(3) Analysis and conclusion

From the data in Table 1, Table 2 and comparative examples, it can be known that adding propyl benzoate, methyl salicylate, ethyl salicylate or isoamyl salicylate to glycerol can reduce the boiling point of the smoke-generating agent , Improve its anti-hygroscopicity, and then reduce the moisture absorption rate of cigarette products. The application data of each embodiment of the present invention shows that the anti-hygroscopic effect is better than that of each comparative example.

From Examples 1, 5 and 6, it can be seen that with the increase of the content of the azeotropic solvent, the moisture absorption rate of the smoke-generating agent decreases, and the moisture-proof property improves. From Examples 1 to 4 and 9 to 12, it can be seen that when methyl salicylate is added to glycerin, it has a lower boiling point compared to other azeotropic solvents, but the anti-moisture performance of the smoking agent and cigarette products is similar. big.

Finally, it should be noted that what is listed above are only specific embodiments of the present invention. Obviously, the present invention is not limited to the above embodiments, and many modifications are possible. All deformations that can be directly derived or associated by those skilled in the art from the content disclosed in the present invention should be considered as the protection scope of the present invention.

Claims (6)

1. The low-boiling-point fuming agent based on the azeotropic solvent system is characterized in that the fuming agent is formed by mixing glycerol and an azeotropic solvent, and the boiling point range of the fuming agent is between 250.3 and 272.5 ℃; in the fuming agent, the mass content of glycerol is 60-90%, and the mass content of azeotropic solvent is 10-40%; the azeotropic solvent is at least one of propyl benzoate, methyl salicylate, ethyl salicylate or isoamyl salicylate.

2. The method of claim 1, wherein the propyl benzoate, methyl salicylate, ethyl salicylate, or isoamyl salicylate is a food grade product.

3. A method of preparing a low boiling point smoking agent based on an azeotropic solvent system as defined in claim 1, comprising:

(1) Respectively weighing glycerol and azeotropic solvent according to the mass ratio of 60-90:10-40;

(2) And uniformly mixing glycerol with the azeotropic solvent under the condition of stirring at the temperature of 35-70 ℃ to obtain the fuming agent.

4. The method according to claim 1, wherein the temperature is controlled to be 35-70 ℃ when the mixing is performed.

5. The method according to claim 1, wherein the stirring is performed magnetically at a rotational speed of 50 to 200rpm.

6. The method for applying the low-boiling-point smoke agent based on the azeotropic solvent system as set forth in claim 1, wherein the smoke agent is sprayed on the dried tobacco leaf raw material, and the mass content of the smoke agent is controlled to be 20% of the tobacco leaf raw material; then the tobacco leaf raw material is dried at a low temperature of 40-70 ℃ and then the heated cigarette is prepared by a cigarette making machine.