阅读说明：本技术 一种复合多孔热释持香烟用香料及其制备方法 (Composite porous heat-release perfume for cigarettes and preparation method thereof ) 是由 魏敏 叶明樵 董爱君 杨俊鹏 肜霖 李俊升 于 2021-05-28 设计创作，主要内容包括：本发明属于烟用添加剂领域,具体涉及一种复合多孔热释持香烟用香料及其制备方法。本发明采用烟末废料高压加热,然后加入苹果酸高温煅烧,制备烟草多孔材料,再加热浸渍负载相变材料肉豆蔻酸,增强对香料的吸附均匀稳定性,大幅改善对香料快速稳定热释性能,接着浸泡均匀吸附莳萝醛、丁香醛等香料制成复合多孔热释持香烟用香料,使特征辛香香气常温稳定储存,受热快速稳定热释放。将复合多孔香烟用香料的超微粉末加入到三醋酸甘油酯中,在线应用于卷烟工业生产,提供自然、强烈的辛香特征香气,常温稳定性好,燃吸或加热时热释辛香特征明显、持久均匀,协调、丰富烟香,提高卷烟抽吸感官质量。(The invention belongs to the field of tobacco additives, and particularly relates to a composite porous heat-release perfume for cigarettes and a preparation method thereof. According to the invention, tobacco powder waste is heated under high pressure, then malic acid is added for high-temperature calcination to prepare a tobacco porous material, then the tobacco porous material is heated and impregnated with the phase-change material myristic acid, so that the uniform adsorption stability of the spice is enhanced, the rapid and stable heat release performance of the spice is greatly improved, and then the dill aldehyde, syringaldehyde and other spices are uniformly adsorbed by soaking to prepare the spice for the composite porous heat release cigarette, so that the characteristic spicy fragrance is stably stored at normal temperature and is rapidly and stably released by heating. The ultramicro powder of the compound porous perfume for cigarettes is added into glycerol triacetate, is applied to the industrial production of cigarettes on line, provides natural and strong spicy characteristic fragrance, has good stability at normal temperature, has obvious, lasting and uniform heat release spicy characteristic when being burnt or heated, coordinates and enriches the cigarette fragrance, and improves the smoking sensory quality of the cigarettes.)

1. The composite porous heat-release perfume for the cigarettes is characterized in that the perfume for the cigarettes is prepared by adsorbing the perfume by a porous material loaded with a phase-change material;

wherein, the functional group of the phase-change material is one or more than two of hydroxyl, carboxyl, amino and ketone; the perfume contains aldehyde group.

2. The composite porous heat-retaining perfume for cigarettes according to claim 1, wherein the functional group of the phase change material contains a carboxyl group.

3. The composite porous heat-retaining perfume for cigarettes according to claim 2, wherein the phase change material is a fatty acid.

4. The composite porous heat-retaining perfume for cigarettes according to claim 3, wherein the fatty acid is myristic acid.

5. The composite porous heat-releasing cigarette flavor according to claim 1, wherein the flavor contains dill aldehyde and/or syringaldehyde.

6. A preparation method of a composite porous heat-release cigarette flavor is characterized by comprising the following steps:

s1, preparing a porous material;

s2, heating and dipping the porous material S1 and a phase-change material to prepare a porous-phase-change composite material;

s3, adding the ethanol solution of the spice of claim 5 into the porous-phase-change composite material of S2, and performing ultrasonic soaking to obtain the spice for the composite porous heat-release cigarette;

and S4, carrying out low-temperature high-speed shearing, rubbing and crushing on the composite porous heat-release cigarette flavor of S3 to obtain the superfine powder of the composite porous heat-release cigarette flavor.

7. The method for preparing the composite porous heat-release cigarette flavor according to claim 6, wherein in step S1, the waste tobacco material is first pressurized and heated to obtain a tobacco sample, and then malic acid is added to obtain the porous material through high-temperature calcination.

8. The method as claimed in claim 7, wherein in step S1, the pressure heating system is 200-500 MPa, 180-225 ℃ and the temperature is 2-5 h; the high-temperature calcination condition is 800-1000 ℃ and 1-2 h.

9. The method for preparing the composite porous heat-release cigarette flavor according to claim 6, wherein the phase change material is first heated and melted before step S2.

10. The preparation method of the composite porous heat-release perfume for the cigarette as claimed in claim 6, wherein in step S2, the heating temperature is 80-95 ℃; the dipping time is 0.5-1.5 h.

Technical Field

The invention belongs to the field of tobacco additives, and particularly relates to a composite porous heat-release perfume for cigarettes and a preparation method thereof.

Background

Both traditional and novel tobaccos have the requirements of flavor compensation and aroma enhancement and fragrance retention. The flavoring substance is used as tobacco additive, and has effects of flavoring, increasing sweetness, improving taste, relieving irritation, and improving tobacco quality. At present, most of cigarette flavor substances have the characteristics of low boiling point and volatility, the flavor of the cigarette flavor substances is gradually lightened under the influence of external factors or combustion heating, the quality of the cigarette flavor substances is reduced, the application range of the cigarette flavor substances is limited to a certain extent, and the release rate of the tobacco flavor substances can be effectively stabilized and delayed by a stable slow release technology, so that the flavor is lasting and stable. At present, the stable slow release technology of the inclusion compound is more applied to slow release of the tobacco flavor. Common inclusion compounds are inclusion complexes and microcapsules, which maintain the stability of the inclusion subject and slowly release the inclusion subject upon heating. Some slow release materials for adsorbing spices, such as porous material active carbon and the like, have strong capacities of adsorbing and retaining essences, but when smoke passes through, only a small amount of essences enter main stream smoke, so that the slow release capacity of the active carbon slow release spices is weak when the cigarette is burnt and heated, and characteristic aroma is difficult to release; the microcapsule perfuming technology has large influence of temperature and pressure on microcapsules and uneven fragrance release; the ion exchange resin perfuming technology has stable property, good fragrance retention property and good slow release performance, but has narrow range of applicable perfume and high cost.

Zhang Xin et al propose a preparation method of a light-controlled slow-release rod-shaped silica nano perfume (invention patent, acceptance number CN 201810358478. X). Nano mesoporous silica is adopted to carry out perfume entrapment and prepare a photoresponse slow-release nano perfume for wallpaper fragrance enhancement, and the light-controlled slow-release rod-shaped silica nano perfume has a fragrance-holding slow-release effect at normal temperature, but thermogravimetric experiments show that the heat release performance is not strong. The prior clathrate compound slow-release material has the defects and problems of complex material components and process, higher cost of raw materials and processing, unobvious characteristic of heat-releasing fragrance effect, insufficient stability and durability, and the like.

Disclosure of Invention

The composite porous heat-release cigarette spice has the characteristics of stable storage of spicy fragrance at normal temperature, quick and stable heat release when being heated, can provide natural and strong spicy fragrance when being applied to cigarettes, has good stability at normal temperature, has obvious, lasting and uniform heat release characteristics when being burnt or heated, and improves the smoking sensory quality of the cigarettes.

The invention is realized by the following technical scheme:

the composite porous heat-release perfume for the cigarettes is characterized in that the perfume for the cigarettes is prepared by adsorbing the perfume by a porous material loaded with a phase-change material;

wherein, the functional group of the phase-change material is one or more than two of hydroxyl, carboxyl, amino and ketone; the perfume contains aldehyde groups.

The invention has the following excellent technical scheme: the functional group of the phase change material contains a carboxyl group.

The invention has the following excellent technical scheme: the phase change material is a fatty acid.

The invention has the following excellent technical scheme: the fatty acid is myristic acid.

The invention has the following excellent technical scheme: the perfume contains dill aldehyde and/or syringaldehyde.

The invention also provides a preparation method of the composite porous heat-release perfume for the cigarettes, which comprises the following steps:

s1, preparing a porous material;

s2, heating and dipping the porous material S1 and a phase-change material to prepare a porous-phase-change composite material;

s3, adding the ethanol solution of the spice of claim 5 into the porous-phase-change composite material of S2, and performing ultrasonic soaking to obtain the spice for the composite porous heat-release cigarette;

and S4, carrying out low-temperature high-speed shearing, rubbing and crushing on the composite porous heat-release cigarette flavor of S3 to obtain the superfine powder of the composite porous heat-release cigarette flavor.

The invention has the following excellent technical scheme: in step S1, the waste tobacco material is first pressurized and heated to obtain a tobacco sample, and then malic acid is added to the tobacco sample and the tobacco sample is calcined at high temperature to obtain the porous material.

The invention has the following excellent technical scheme: in the step S1, the pressurizing and heating system is 200-500 MPa, 180-225 ℃, and the heating is carried out for 2-5 h; the high-temperature calcination condition is 800-1000 ℃ and 1-2 h.

The invention has the following excellent technical scheme: before proceeding to step S2, the phase change material is first heated and melted.

The invention has the following excellent technical scheme: in the step S2, the heating temperature is 80-95 ℃; the dipping time is 0.5-1.5 h.

The invention has the beneficial effects that:

the invention adopts the high-pressure heating of the tobacco stem, tobacco leaf and other powder, then adds malic acid to calcine at high temperature to prepare the tobacco porous material, heats and soaks the supported phase-change material myristic acid, enhances the uniform adsorption stability of the spice, greatly improves the quick and stable heat release performance of the spice, then soaks and uniformly adsorbs the spice such as dill aldehyde, syringaldehyde and the like to prepare the spice for the composite porous heat release cigarette, so that the characteristic spicy fragrance is stably stored at normal temperature, and is quickly and stably released when being heated.

According to the invention, the myristic acid is adopted to introduce carboxyl on the surface of the porous material, so that active sites on the surface of the porous material are increased, and then the myristic acid is combined with aldehyde groups in the spice, and the adsorption property and the normal temperature stability of the spice are enhanced.

The invention adds the ultramicro powder of the compound porous spice for the cigarette into the glycerol triacetate, is applied to the cigarette industrial production on line, provides natural and strong spicy characteristic aroma, has good stability at normal temperature, has obvious, lasting and uniform heat release spicy characteristic during burning or heating, coordinates and enriches the cigarette aroma, and improves the sensory quality of cigarette smoking.

Detailed Description

In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.

Example 1 preparation of composite porous Heat-releasing perfume for cigarettes

(1) Preparation of the porous material: cutting waste tobacco stems and tobacco stems in the tobacco industry, mixing the cut waste tobacco stems and tobacco stems with waste tobacco leaf scraps, putting the mixture into a pressurizing and heating system (heating for 3.5 hours at 200 ℃) under 300 MPa, taking out 70 parts of samples and 3 parts of malic acid, adding the mixture into 27 parts of water at 90 ℃, uniformly mixing, soaking for 6 hours under heat preservation, carrying out suction filtration, removing filtrate, freezing solid insoluble substances at-20 ℃ for 6 hours, carrying out vacuum drying and dehydration, and heating to 900 ℃ for 1.5 hours by adopting a muffle furnace to obtain the porous carbon material of the tobacco. More disordered carbon in the porous carbon is converted into ordered graphitized carbon by hydrothermal graphitization and organic acid carbonization, so that the specific surface area and the adsorption capacity of the material are increased.

(2) Preparing a porous-phase-change composite material: firstly, heating 16 parts of gum tragacanth, 18 parts of myristic acid and 1 part of sodium chloride to 90 ℃ for melting, then putting 45 parts of the tobacco porous carbon material in the step (1) into a container, heating and stirring at a constant speed (150 rpm) for 1 h;

(3) preparing the composite porous heat-release cigarette flavor: dispersing 20 parts of spicy spices (including dill aldehyde, nutmeg oil, clove basil oil and syringaldehyde) in 50 parts of absolute ethyl alcohol, slowly adding into the porous-phase change composite material prepared in the step (2) while heating and stirring, performing ultrasonic treatment for 10 min with the power of 30 KW, volatilizing the ethyl alcohol, naturally cooling to room temperature, and solidifying to obtain the composite porous heat-release spice for cigarettes;

(4) preparing the composite porous heat-release cigarette flavor superfine powder: and (3) carrying out low-temperature high-speed shearing, rubbing and crushing on the composite porous heat-release cigarette flavor in the step (3) by adopting a low-temperature colloid mill to obtain the composite porous heat-release cigarette flavor superfine powder.

Wherein the dill aldehyde, the nutmeg oil, the clove basil oil and the syringaldehyde in the step (3) are food-grade cigarette flavors in a mass ratio of 1:1:1: 1.

And (4) the compound porous cigarette flavor is subjected to low-temperature high-speed shearing, friction and crushing by adopting a low-temperature colloid mill to form superfine powder, active substances such as characteristic aroma components, antibacterial active components and the like are retained to the maximum extent, the compound porous cigarette flavor is convenient to store and transport, has good stability at normal temperature, is friendly to the environment and operators, locks characteristic aroma, does not emit strong irritant smell, and also enables the process of adding the compound porous cigarette flavor into cigarettes to be easier to realize and convenient to add.

Example 2 preparation of composite porous Heat-releasing perfume for cigarettes

(1) Preparation of the porous material: cutting waste tobacco stems and tobacco stems in the tobacco industry, mixing the cut waste tobacco stems and tobacco stems with waste tobacco leaf scraps, putting the mixture into a pressurizing and heating system (200 MPa, heating at 225 ℃ for 2 hours), taking out 50 parts of samples and 1 part of malic acid, adding 49 parts of water at 80 ℃, uniformly mixing, soaking for 12 hours in a heat preservation manner, carrying out suction filtration, removing filtrate, freezing solid insoluble substances at-20 ℃ for 8 hours, carrying out vacuum drying and dehydration, and heating to 1000 ℃ for 1 hour by adopting a muffle furnace to obtain a porous carbon material;

(2) preparing a porous-phase-change composite material: firstly, heating 15 parts of gum tragacanth, 14 parts of myristic acid and 1 part of sodium chloride to 80 ℃ for melting, then putting 40 parts of the tobacco biological porous carbon material in the step (1) into a container, heating and electrically stirring at a constant speed (100 rpm) for 1.5 h, ensuring that the liquid gum tragacanth and myristic acid fully cover the porous carbon and fully infiltrate into the carbon skeleton and pores;

(3) preparing the composite porous heat-release cigarette flavor: dispersing 30 parts of spicy spices (including dill aldehyde, nutmeg oil, clove basil oil and syringaldehyde) in 60 parts of absolute ethyl alcohol, slowly adding the materials into the porous-phase-change composite material prepared in the step (2) while heating and stirring, performing ultrasonic treatment for 15 min with the power of 40 KW, volatilizing the ethyl alcohol, naturally cooling to room temperature, and solidifying to obtain the composite porous heat-release spice for cigarettes;

(4) preparing the composite porous heat-release cigarette flavor superfine powder: and (3) carrying out low-temperature high-speed shearing, rubbing and crushing on the composite porous heat-release cigarette flavor in the step (3) by adopting a low-temperature colloid mill to obtain the composite porous heat-release cigarette flavor superfine powder.

Wherein the dill aldehyde, the nutmeg oil, the clove basil oil and the syringaldehyde in the step (3) are food-grade cigarette flavors in a mass ratio of 0.5:0.5:0.5: 1.

Example 3 preparation of composite porous Heat-releasing perfume for cigarettes

(1) Preparation of the porous material: cutting waste tobacco stems and tobacco stems in the tobacco industry, mixing the cut waste tobacco stems and tobacco stems with waste tobacco leaf scraps, putting the mixture into a pressurizing and heating system (heating for 5 hours at 180 ℃ under 500 MPa), taking out 90 parts of samples, 5 parts of malic acid and 5 parts of water at 95 ℃, uniformly mixing, preserving heat and infiltrating for 8 hours, carrying out suction filtration, removing filtrate, freezing solid insoluble substances at-20 ℃ for 4 hours, carrying out vacuum drying and dehydration, and heating to 800 ℃ for 2 hours by adopting a muffle furnace to obtain a porous carbon material of tobacco;

(2) preparing a porous-phase-change composite material: heating 20 parts of gum tragacanth, 25 parts of myristic acid and 1 part of sodium chloride to 95 ℃ for melting, then putting 50 parts of the tobacco biological porous carbon material in the step (1) into a container, heating and electrically stirring at a constant speed (300 rpm for 0.5 h), ensuring that the liquid gum tragacanth and myristic acid fully cover the porous carbon and fully infiltrate into the carbon skeleton and pores;

(3) preparing the composite porous heat-release cigarette flavor: dispersing 5 parts of spicy spices (including dill aldehyde, nutmeg oil, clove basil oil and syringaldehyde) in 10 parts of absolute ethyl alcohol, slowly adding the materials into the porous-phase-change composite material prepared in the step (2) while heating and stirring, performing ultrasonic treatment for 5 min with the power of 20 KW, volatilizing the ethyl alcohol, naturally cooling to room temperature, and solidifying to obtain the composite porous heat-release spice for cigarettes;

(4) preparing the composite porous heat-release cigarette flavor superfine powder: and (3) carrying out low-temperature high-speed shearing, rubbing and crushing on the composite porous heat-release cigarette flavor in the step (3) by adopting a low-temperature colloid mill to obtain the composite porous heat-release cigarette flavor superfine powder.

Wherein the dill aldehyde, the nutmeg oil, the clove basil oil and the syringaldehyde in the step (3) are food-grade cigarette flavors in a mass ratio of 2:2:2: 1.

Comparative example 1

The preparation of the composite porous heat-release cigarette flavor is not added with the porous-phase change composite material, and the rest is the same as that in the example 3.

Comparative example 2

The preparation of the composite porous heat-release cigarette flavor uses a porous carbon material instead of a porous-phase change composite material, and the rest is the same as example 3.

Comparative example 3

The preparation of the porous-phase change composite material was carried out using a phase change material paraffin having no carboxyl functional group instead of myristic acid, as in example 3

Evaluation of

1. Evaluation procedure

A. Retention rate

Adding the prepared spice into glycerol triacetate for cigarettes, uniformly mixing, simulating the storage condition of the spice, standing for 15 days in a blast oven at the constant temperature of 40 ℃ in an open air environment, obtaining the retention of the spice by a weighing method, and then calculating the retention, wherein the retention = retention/addition.

B. Heat release amount

Adding the prepared spice into glycerol triacetate for cigarettes, uniformly mixing, standing for 15 days, and heating at 80 ℃ for 10 min to obtain the cigarette perfume with the actual heat release quality calculated by subtracting the retention amount from the initial addition amount.

C. Sensory evaluation

The triglycolate of the flavors for cigarettes prepared in example 3, comparative example 1, comparative example 2 and comparative example 3 was rolled into cigarettes according to the conventional process parameters, and after standing for 15 days, sensory evaluation was performed by using the sensory evaluation method of national standard YCT 138-.

2. Evaluation results

The evaluation results of the examples and comparative examples are shown in Table 1-2.

As can be seen from Table 1, the retention rate and the amount of heat release of comparative example 1 are significantly lower than those of example 3, which illustrates the technical contribution of adding the porous-phase change composite material;

the retention rate and the heat release amount of the comparative example 2 are lower than those of the example 3, which shows that the phase change material loaded on the porous material is the key for ensuring the normal temperature stability and the heat release property of the spice for the cigarette;

the retention rate and the heat release amount of the composite porous heat-release perfume of the example 3 are lower than those of the example 3, which shows that compared with the phase-change material which is loaded with the perfume and does not contain the carboxyl functional group, the phase-change material which is loaded with the carboxyl-containing phase-change material can further improve the normal temperature stability and the heat release property of the perfume product.

As shown in Table 2, the cigarette manufactured in example 3 provides natural and strong characteristic aroma with good stability at room temperature, and has obvious characteristic of releasing aroma when smoking or heating, and has harmonious and rich tobacco aroma.

Specific embodiments of the present invention have been described above in detail.

It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, any technical solutions that can be obtained by a person skilled in the art through logical analysis, reasoning or limited experiments in the prior art based on the inventive concept should be within the scope of protection defined by the claims.