阅读说明：本技术 缓释香料及其制备方法 (Slow-release perfume and preparation method thereof ) 是由 魏敏 潘曦 宋旭艳 杨俊鹏 董爱君 李俊升 于 2020-07-15 设计创作，主要内容包括：本发明公开了缓释香料及其制备方法。该缓释香料包括缓释载体和分散于所述缓释载体中占缓释载体质量10～100wt%的致香物质；其中,所述缓释载体包含质量之比为1：9～99的石墨烯和选自琼脂、明胶、瓜儿豆胶、果蜡中一种或至少二种的载体主相材料。本申请缓释香料,以琼脂、明胶、瓜儿豆胶、果蜡具有生物相容性高分子材料为载体主相材料,于其中添加石墨烯,石墨烯的添加既能促进致香物质被导热,也能促进致香物质在载体主相材料中分散均匀性,由此在满足缓释香味的同时提高释放的速率。(The invention discloses a slow-release spice and a preparation method thereof. The slow-release spice comprises a slow-release carrier and a fragrant substance which is dispersed in the slow-release carrier and accounts for 10-100 wt% of the mass of the slow-release carrier; wherein, the slow release carrier comprises a mixture of 1: 9-99 of graphene and one or at least two carrier main phase materials selected from agar, gelatin, guar gum and fruit wax. According to the slow-release spice, the agar, the gelatin, the guar gum and the fruit wax are used as main phase materials of the carrier, the graphene is added, the addition of the graphene can promote the heat conduction of the fragrant substances and the dispersion uniformity of the fragrant substances in the main phase materials of the carrier, and therefore the slow-release spice is capable of meeting the requirement of releasing fragrance and improving the release rate.)

1. A slow-release spice is characterized by comprising a slow-release carrier and a fragrant substance which is dispersed in the slow-release carrier and accounts for 10-100 wt% of the mass of the slow-release carrier; wherein, the slow release carrier comprises a mixture of 1: 9-99 of graphene and one or at least two carrier main phase materials selected from agar, gelatin, guar gum and fruit wax.

2. The slow-release flavor according to claim 1, wherein the graphene has a sheet diameter of 0.5 to 5 μm.

3. The slow-release spice according to claim 1, wherein the graphene has a thickness of 1 to 3 nm.

4. The slow-release spice according to claim 1, wherein the slow-release carrier further comprises a siloxane coupling agent accounting for 4-12 wt% of the mass of the graphene.

5. The slow-release perfume according to claim 4, wherein the siloxane coupling agent is one or at least two of KH-550, KH-KH-570, KH-590.

6. The slow release flavor of claim 1, wherein the flavor-causing substance is one or at least two of menthol, ethyl maltol, vanillin, beta-damascone.

7. A process for the preparation of a slow release fragrance as claimed in claim 1, comprising the steps of:

making the carrier main phase material and the aroma substance into a molten state;

and mixing the graphene with the carrier main phase material in the molten state and the aroma substances, and cooling and molding.

8. The method according to claim 7, wherein the temperature for cooling and forming is room temperature.

Technical Field

The invention relates to the field of flavors and fragrances, in particular to a slow-release fragrance and a preparation method thereof.

Background

The tobacco shreds in the non-combustible tobacco product are heated but not combusted, so that the generation of a large amount of harmful compounds can be avoided while the characteristic flavor feeling of the tobacco is provided, and the health hazard of the tobacco product is reduced. Although a plurality of heat-not-combustible tobacco products appear on the market at present, most of the heat-not-combustible tobacco products still have difficulty in restoring the smoking mouthfeel of traditional tobacco. The use of flavourants is one of the important ways to enhance the mouthfeel of heat-not-combustible cigarette products. The flavour loading system of a heat-not-combustible cigarette is significantly different from a conventional cigarette due to the difference in operating temperature. For a heat not burn cigarette, the flavoring should be released quickly at a lower temperature. Meanwhile, the spice of the non-combustible cigarette should maintain higher stability at normal temperature.

The development of flavour-loaded systems for heat-not-combustible cigarettes has been a focus of recent years. The invention patent application No. 201910600458.3 proposes a volcanic rock-based fragrance loading system. The loading material has rich pore canal structure and can load a certain amount of perfume. The flavored volcanic rock is loaded in the tow rod to realize the release of the spice in a non-combustible state by heating. However, the carrier can carry a low proportion of perfume and only the perfume carrying and surface pores can be effectively released under the condition of non-combustible heating. The invention patent application No. 201911363441.7 proposes a konjac based flavor loading system. The technology removes starch and partial impurities from the thin-walled tissue under the cortex of the konjak bulb to leave polysaccharide substances and the original framework network of the konjak thin-walled tissue, mixes the konjak thin-walled tissue with chitosan aqueous solution again to swell and granulate to form a spice loading material, and carries out spice loading in a top spraying mode. The preparation process of the spice loading material is complex, and the production cost is high. At the same time, this way of perfuming makes it difficult to get the perfume inside the load material, which may lead to uncontrolled release of the perfume. Patent application No. 201910615640.6 discloses a mint-based tobacco sheet that releases a mint aroma when used in a non-combustible cigarette when heated. However, the perfume loading system is complex in component and consists of a plurality of auxiliary perfume bases and other base materials. The presence of these adjunct ingredients may affect the flavour of the menthol flavour. In addition, the ingredients of the perfume load system are less tunable. The invention patent application No. 201910091601.0 discloses a microcapsule based perfume delivery system. The perfume releasing system can effectively protect the perfume and realize the release of the perfume.

The above reported perfumes all contain slow release materials, and since the slow release materials achieve the purpose of slow release by coating or covering the aroma-generating substances, the perfume releases aroma at the smoking temperature very slowly compared with the perfume without the slow release materials, so that the rate of aroma release is greatly sacrificed while the slow aroma release is obtained, thereby causing the main stream smoke fragrance to be not rich enough.

Disclosure of Invention

The invention aims to provide a slow-release perfume and a preparation method thereof, which can improve the release rate while meeting the slow-release perfume.

The present inventors have found that high-molecular materials with high biocompatibility, represented by agar, gelatin, guar gum, fruit wax, have satisfactory effects of stabilizing a heat-fragrant substance, and can be used as a carrier main phase material. However, these carrier main phase materials generally exhibit poor thermal conductivity, and the heating of the aroma substances is derived from the conduction of the carrier main phase materials from the outside, which naturally impairs the heating of the aroma substances, and difficulties in aroma release of some of the aroma substances may also occur at operating (i.e., heating the puff of a non-combustible cigarette). On one hand, the graphene dispersed in the main phase material of the carrier can be used as heat-conducting particles to provide a high-efficiency heat-conducting channel for the fragrant substances, so that heat absorption required by heat release of the fragrant substances is promoted; on the other hand, graphene can show adsorption to the aroma substances through electrostatic interaction, pi-pi stacking, hydrophobic interaction, hydrogen bonding and van der waals force action, and can provide the aroma substances with 'transient habitats', so that the aroma substances can be improved, and local over-aggregation state can be generated due to the large compatibility difference with the carrier main phase material, and the over-aggregation state can reduce the dispersity and possibly cause heating nonuniformity; thereby increasing the rate of release by both of these aspects. Based on this, the invention of the present application has been completed.

According to a first aspect of the present invention, there is provided a slow release perfume comprising a slow release carrier and a fragrant substance dispersed in the slow release carrier in an amount of 10 to 100wt% based on the mass of the slow release carrier, such as 10wt%, 12wt%, 15wt%, 20wt%, 30wt%, 40wt%, 50wt%, 70wt%, 80wt%, 90wt%, 95wt%, 100 wt%; wherein, the slow release carrier comprises a mixture of 1: 9-99 of graphene and one or at least two carrier main phase materials selected from agar, gelatin, guar gum and fruit wax, wherein the carrier main phase materials can be 1: 9. 1: 9.5, 1: 10. 1: 15. 1: 20. 1: 30. 1: 50. 1: 70. 1: 80. 1: 90. 1: 95. 1: 99.

here, the graphene may be graphene oxide, or may be reduced graphene oxide or the like.

In a typical embodiment, the graphene has a sheet diameter of 0.5 to 5 μm, such as 0.5 μm, 0.55 μm, 0.6 μm, 1 μm, 1.5 μm, 2 μm, 2.5 μm, 3 μm, 4 μm, 4.5 μm, 5 μm, and the like. Too large or too small a sheet diameter of graphene may affect the effect of heat conduction or improvement of dispersion of aroma substances.

In a typical embodiment, the graphene has a thickness of 1 to 3 nm, such as 1 nm, 1.5 nm, 2nm, 2.5nm, 2.8 nm, 3 nm, and the like. Too large or too small a thickness of the graphene may affect the heat conduction or improve the dispersion effect of the aroma substances.

In order to further promote the above-mentioned effect of graphene on the fragrant substance, a siloxane coupling agent may also be added. The addition of the siloxane coupling agent is to modify the graphene, and the siloxane coupling agent in the modified graphene material serves as a 'bridge' of a carrier main phase material and a fragrant substance. The siloxane coupling agent has a hydrophobic group and a hydrophilic group, the hydrophilic group (namely silicon hydroxyl generated by hydrolysis) can generate acting force such as molecular hydrogen bond and the like with the residual carboxyl, hydroxyl and other hydrophilic groups on the surface of the graphene, and the hydrophobic group (namely C-Si) can reduce and weaken the surface energy between the aroma substances and reduce the molecular compatibility difference between the aroma substances and the carrier main phase material, thereby promoting the dispersion of the aroma substances in the carrier main phase material.

In order to obtain the best effect, the addition amount of the siloxane coupling agent may be 4 to 12wt% based on the graphene mass, for example, specifically 4wt%, 4.5wt%, 5wt%, 6wt%, 8wt%, 9wt%, 10wt%, 11wt%, 11.5wt%, 12wt%, and the like.

Specific examples of the siloxane coupling agent include KH-550, KH-KH-570 and KH-590.

It will be appreciated that the foregoing fragrance-forming substances may be selected from conventional fragrance materials as desired. However, the fragrant substance is preferably one or at least two of menthol, ethyl maltol, vanillin, β -damascone from the viewpoint of exerting an effect of increasing the rate of release.

According to still another embodiment of the present application, a method for preparing the above-mentioned slow-release perfume comprises the steps of:

making the carrier main phase material and the aroma substance into a molten state;

and mixing the graphene with the carrier main phase material in the molten state and the aroma substances, and cooling and molding.

Here, the temperature of the cooling molding may be room temperature or the like, and the cooling method may be natural cooling or air cooling or the like.

In the case of adding the aforementioned siloxane coupling agent, the order of addition or timing of addition of the siloxane coupling agent may be: firstly, modifying with graphene to obtain siloxane modified graphene, and then mixing the siloxane modified graphene with a molten main phase material and a fragrant substance.

The modification of the siloxane-modified graphene specifically comprises the steps of putting the solid graphene and the siloxane coupling agent into a solvent, fully dispersing the solid graphene and the siloxane coupling agent (for example, ultrasonic oscillation is adopted), and drying the mixture into a solid phase, wherein the drying temperature can be 120-160 ℃.

It should be understood that the molten state refers to a fluid state in which the main phase material, the fragrant substance, and the like maintain a certain fluidity, and is not completely liquid. The temperature of the molten state is selected for processing requirements.

The invention has the beneficial effects that: according to the slow-release spice, the agar, the gelatin, the guar gum and the fruit wax are used as main phase materials of the carrier, the graphene is added, the addition of the graphene can promote the heat conduction of the fragrant substances and the dispersion uniformity of the fragrant substances in the main phase materials of the carrier, and therefore the slow-release spice is capable of meeting the requirement of releasing fragrance and improving the release rate.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.