1. The mouthpiece adhesive for the slow-release fragrance-holding cigarette is characterized by comprising a slow-release fragrance-holding milk fragrance spice which takes silicon dioxide microspheres with modified supermolecular structures as carriers;

the modified silica microspheres with the supermolecular structure are prepared by physically coating silica nanospheres with the supermolecular structure with mastic resin and chemically modifying vanillin.

2. The nozzle gum for the slow-release aroma-holding cigarette according to claim 1, wherein the slow-release aroma-holding milk flavor further comprises a biotech milk flavor and a mixed milk flavor.

3. The nozzle rubber for the slow-release cigarette, according to claim 2, is characterized in that the mass of the modified silica microsphere powder with the supermolecular structure is 4-15 times of that of the mixed milk-flavor essence and spice.

4. The preparation method of the nozzle rubber for the slow-release cigarette holder according to claim 1, which is characterized by comprising the following steps of:

s1, preparing silicon dioxide nano microspheres;

s2, performing supramolecular modification on the silicon dioxide nano-microsphere prepared in the S1;

s3, carrying out physical coating and chemical modification on the silica nano-microsphere with the supermolecular structure of S2;

s4, mixing the modified supermolecular structure nano-microspheres prepared in S3 with biotechnology milk flavor and mixed milk flavor and fragrance flavor to obtain slow-release and milk-holding flavor, and adding cigarette mouthpiece adhesive to prepare the slow-release and cigarette-holding mouthpiece adhesive.

5. The method for preparing the nozzle rubber for the slow-release cigarette-holding according to claim 4, wherein in step S1, the silicon dioxide nano-microspheres are prepared by catalyzing tetraethyl orthosilicate with L-histidine as a catalyst.

6. The method for preparing the nozzle adhesive for the slow-release cigarette holder according to claim 4, wherein in step S2, the silica nanospheres prepared in step S1 are modified into a supramolecular structure by using 3-aminopropyltrimethoxysilane.

7. The method for preparing the nozzle rubber for the slow-release cigarette holder according to claim 4, wherein in step S3, the supramolecular silica nanospheres obtained in step S2 are physically coated and chemically modified by mastic resin and vanillin respectively.

8. The preparation method of the nozzle rubber for the slow-release fragrance-holding cigarette according to claim 4, wherein in step S4, the use amount of the slow-release fragrance-holding milk fragrance spice is 15-35 parts; the using amount of the cigarette mouthpiece adhesive is 65-85 parts.

9. The preparation method of the nozzle rubber for the slow-release cigarette holder according to claim 4, wherein in step S4, the mixed milk-flavor essence is prepared by mixing 1:1 mass ratio of delta-sunflower lactone and 3-hydroxy-2-butanone.

10. The use of the nozzle gum for sustained-release cigarette according to any one of claims 1 to 3 in cigarette production.

Background

The adhesive is an important auxiliary material for cigarette production. The adhesive is classified into lap joint adhesive, nozzle adhesive, packaging adhesive and the like according to the use purpose, and white latex, hot melt adhesive and the like are classified according to physical and chemical properties. The cigarette mouthpiece adhesive is one of white latex. The cigarette flavoring technology is mainly applied to tobacco raw materials or filter tips and the like, and regarding the application research of the flavoring technology of the cigarette holder adhesive, Chinese patent CN104312497B discloses a cigarette holder adhesive for efficiently loading mint essence and a preparation process thereof, and the mint essence has high loading capacity; CN 107699155A discloses a cumin flavor cigarette mouthpiece adhesive and a preparation method thereof, wherein cumin ultrafine powder is added into the mouthpiece adhesive to flavor cigarettes. However, the volatile spices are directly mixed with the tipping glue and used in cigarette tipping paper, and have the defects of easy volatilization during normal-temperature storage, low stability, low and non-lasting heat-release aroma characteristics and the like.

The application of the frankincense slow-release spice in the cigarette mouthpiece adhesive is not reported. The main components of milk fat are fatty acid triglyceride, unsaturated fatty acid triglyceride, ketoacid triglyceride, hydroxy acid triglyceride, etc., which are hydrolyzed into various saturated and unsaturated fatty acids under the action of lipase, wherein C4, C6, C8, C10, C12 and C14 are rich in content, have high fragrance contribution degree, and are the main factors of frankincense. The keto acid and the hydroxy acid generate various methyl ketones and even carbon lactone in further reaction, and the contribution to the formation of milk fragrance is also large. However, the milk flavor prepared by lipase hydrolysis has high fragrance intensity and obvious characteristics, but the flavor is monotonous, and oil flavor and rancidity flavor are easy to appear. The milk flavor produced by microbial fermentation has rich and natural fragrance, but has low fermentation yield, insufficient fragrance intensity and weak characteristics. Therefore, it is necessary to research a method for enhancing aroma and richly retaining aroma by using the cigarette mouthpiece adhesive, and improving the slow-release capacity of aroma retention so that the cigarette has good aroma enhancing and retaining effects.

Disclosure of Invention

In order to solve the problems, the invention provides the nozzle adhesive for the slow-release and fragrance-holding cigarette and the preparation method and application thereof.

The invention is realized by the following technical scheme: a nozzle gum for slow-release cigarette comprises slow-release milk flavor with modified silica microspheres with supramolecular structure as carrier;

the modified silica microspheres with the supermolecular structure are prepared by physically coating silica nanospheres with the supermolecular structure with mastic resin and chemically modifying vanillin.

The invention has the following excellent technical scheme: the slow-release aroma-holding milk flavor also comprises a biotechnology milk flavor and a mixed milk flavor essence.

The invention has the following excellent technical scheme: the mass of the modified silica microsphere powder with the supermolecular structure is 4-15 times of that of the mixed milk flavor essence.

The invention also provides a preparation method of the nozzle adhesive for the slow-release cigarette, which comprises the following steps:

s1, preparing silicon dioxide nano microspheres;

s2, performing supramolecular modification on the silicon dioxide nano-microsphere prepared in the S1;

s3, carrying out physical coating and chemical modification on the silica nano-microsphere with the supermolecular structure of S2;

s4, mixing the modified supermolecular structure nano-microspheres prepared in S3 with biotechnology milk flavor and mixed milk flavor and fragrance flavor to obtain slow-release and milk-holding flavor, and adding cigarette mouthpiece adhesive to prepare the slow-release and cigarette-holding mouthpiece adhesive.

The invention has the following excellent technical scheme: in the step S1, L-histidine is used as a catalyst to catalyze tetraethyl orthosilicate to prepare the silicon dioxide nano microspheres.

The invention has the following excellent technical scheme: in the step S2, 3-aminopropyltrimethoxysilane is adopted to modify the silica nano-microspheres prepared in the step S1 into supramolecular structures.

The invention has the following excellent technical scheme: in the step S3, the supramolecular silica nanospheres of the step S2 are physically coated and chemically modified with mastic resin and vanillin, respectively.

The invention has the following excellent technical scheme: in the step S4, the use amount of the slow-release fragrance-holding milk fragrance is 15-35 parts; the using amount of the cigarette mouthpiece adhesive is 65-85 parts.

The invention has the following excellent technical scheme: in the step S4, the mixed milk flavor essence is formed by mixing the ambroside and the 3-hydroxy-2-butanone in a mass ratio of 1: 1.

An application of a cigarette holder gum for sustained-release cigarette in cigarette production.

The invention has the beneficial effects that:

the slow-release fragrance-holding milk flavor takes modified silicon dioxide microsphere powder with a supermolecular structure as a carrier, the carrier adopts natural L-histidine to catalyze and synthesize silicon dioxide nano microspheres, the silicon dioxide nano microspheres are modified into the supermolecular structure by 3-aminopropyltrimethoxysilane, then heated and melted masticated resin is added for physical coating, vanillin is heated for reaction for chemical modification, and the adsorbability and the dispersion uniformity of the carrier are improved.

Firstly, uniformly coating mastic resin on the surface of the supermolecule silicon dioxide nano microsphere, changing the surface property of the supermolecule silicon dioxide nano microsphere, reducing agglomeration and increasing the monodispersion stability of the nano microsphere; then, vanillin is adopted to modify the surface of the supramolecular silica microsphere, and the aldehyde group is connected with the oxygen-containing functional group on the surface of the supramolecular silica nanoparticle, so that the physical-coated nanoparticle has better dispersity and is more uniform, chemical modification is more rapidly carried out, and more vanillin is promoted to be combined with the supramolecular nanoparticle, so that the adsorption surface area is greatly increased, the adsorption performance of the nanoparticle on perfume substances is improved, and the loading capacity and the normal-temperature stability of adsorbed perfume are further enhanced; meanwhile, due to the phase change property of the mastic resin, the mastic resin can absorb heat and melt into a molten state when being heated, thereby enhancing the heat release property of the adsorbed spice and keeping the balanced and lasting characteristic aroma heat release.

According to the invention, the modified silica microsphere powder with a supermolecular structure is used as a slow release material, so that the adsorption performance of the perfume is enhanced, the normal-temperature stability of the milk-flavor perfume is improved, the retention rate and absolute amount of the milk-flavor perfume are high after the cigarette product is placed for a period of time, when a consumer sucks the cigarette product, the heated smoke passes through the filter tip, so that the milk-flavor resin in the filter tip glue is heated and melted, the absolute amount of the improved milk-flavor perfume is rapidly and uniformly released, and the consumer feels that the milk-flavor characteristic in the mainstream smoke is obvious and lasting.

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

The preparation method of the mouth connecting glue for the slow-release cigarette comprises the following specific steps:

(1) preparing the silicon dioxide nano microspheres: 0.21 part of L-histidine and 10 parts of distilled water were weighed and mixed in a vessel, and magnetons were put therein and stirred at room temperature for 10 min at 100 rpm to form a homogeneous solution. Adding 1 part of tetraethyl orthosilicate, sealing the container, stirring for 15 min at room temperature and the rotating speed of 500 rpm to obtain the silicon dioxide nano microspheres.

The method adopts natural alkalescent amino acid-L-histidine as a catalyst, and carries out catalytic synthesis at a slower speed than acid and alkali catalysts, so that silicon spheres with uniform size can be obtained, the batch stability of the nano microspheres is improved, the product quality is more stable, and meanwhile, the method has no acid and alkali pollution and residue, does not need to recover, has simpler process, and is green, natural and environment-friendly.

(2) Supramolecular modification: and (2) dispersing 1 part of the silicon dioxide nano microsphere powder in the step (1) in 10 parts of absolute ethyl alcohol, then adding 1.1 part of 3-aminopropyltrimethoxysilane, heating for 5 min by microwave with the power of 100W, then stirring for 12 h at room temperature at 100 rpm, filtering, washing by using absolute ethyl alcohol, and then drying in vacuum at 65 ℃ to obtain the silicon dioxide nano microsphere powder with the supermolecular structure.

3-aminopropyl trimethoxy silane is added, long-chain alkyl functional groups are introduced to the surface of a silicon dioxide carrier, and a supermolecule effect is constructed between the carrier and additives such as spice and the like, so that the loading capacity and the normal-temperature loading stability of the additive spice are improved, and the slow-release fragrance-holding effect is enhanced. The supermolecule modification is carried out by adopting microwave heating, so that the carrier material is more uniformly dispersed, the reaction is quicker, the efficiency is higher, and the reaction time is shortened.

(3) Physical coating and chemical modification of the silica microspheres with supramolecular structures: and (3) adding 11 parts of the supermolecule silicon dioxide microsphere powder prepared in the step (2) and 10 parts of distilled water, keeping the temperature of 75-90 ℃, heating, condensing and refluxing, stirring at the rotation speed of 550 rpm for 6 hours, then adding 2.6 parts of vanillin, heating and stirring under the same condition for 6 hours, putting into an oven, and keeping the temperature at 60 ℃ overnight to obtain the modified supermolecule structure microsphere powder.

(4) Preparing the mouth connecting glue for the slow-release cigarette: sequentially adding biotechnological milk flavor, delta-decalactone, 3-hydroxy-2-butanone (mixed milk flavor) and the prepared supermolecular structure microsphere powder (the mass of the microsphere powder is 4 times of that of the mixed milk flavor) in a mass ratio of 1:1:1 into a 75% ethanol solution, heating with microwave for 5 min at a power of 500W to volatilize the solvent to obtain the slow-release flavor-holding milk flavor, and adding 15 parts of the slow-release flavor-holding milk flavor into 85 parts of cigarette mouthpiece adhesive to obtain the slow-release flavor-holding cigarette mouthpiece adhesive.

The biotechnological milk flavor is rich in natural milk flavor and strong in style characteristic, and is prepared by taking cream, cream ester, cream oil or cheese as raw materials, adding 0.1% by mass of biological agents (lipase, Lactobacillus reuteri active dry powder and Streptococcus butyrosporangium lactate active dry powder in a mass ratio of 0.5:1: 1), 1% by mass of citric acid and 0.1% by mass of glutamic acid, uniformly mixing and stirring, fermenting and performing enzymolysis for 12 hours at 45 ℃ and pH 5, performing vacuum suction filtration to obtain a fermentation filtrate, and performing vacuum freeze drying to obtain biotechnological milk flavor powder which is natural and soft in flavor and has obvious milk flavor characteristic.

Example 2

The preparation method of the mouth connecting glue for the slow-release cigarette comprises the following specific steps:

(1) preparing the silicon dioxide nano microspheres: 0.25 parts of L-histidine and 50 parts of distilled water were weighed and mixed in a container, and magnetons were put and stirred at 150 rpm for 15 min at room temperature to form a uniform solution. Adding 10 parts of tetraethyl orthosilicate, sealing the container, stirring at room temperature for 25 min, and rotating at the speed of 700 rpm to obtain the silicon dioxide nano microspheres.

(2) Supramolecular modification: and (2) dispersing 10 parts of the silicon dioxide nano microsphere powder in the step (1) in 50 parts of absolute ethyl alcohol, then adding 1.5 parts of 3-aminopropyltrimethoxysilane, heating for 10 min by microwave with the power of 300W, then stirring for 18 h at room temperature at 200 rpm, filtering, washing by using absolute ethyl alcohol, and finally drying in vacuum at the temperature of 75 ℃ to obtain the silicon dioxide nano microsphere powder with the supermolecular structure.

(3) Physical coating and chemical modification of the silica microspheres with supramolecular structures: and (3) adding 15 parts of mastic resin into 15 parts of the supermolecule microsphere powder prepared in the step (2) and 50 parts of distilled water, keeping the temperature of 85 ℃, heating, condensing and refluxing, stirring at the rotating speed of 450 rpm for 9 hours, then adding 3 parts of vanillin, continuously heating and stirring for 9 hours under the same condition, putting the mixture into an oven, and keeping the temperature at 70 ℃ overnight to obtain the microsphere powder with the modified supermolecule structure.

(4) Preparing the mouth connecting glue for the slow-release cigarette: sequentially adding biotechnological milk flavor, delta-malolactone and 3-hydroxy-2-butanone (mixed milk flavor) in a mass ratio of 1.5:1:1 and the microsphere powder (the mass of the microsphere powder is 10 times of that of the mixed milk flavor) with the modified supermolecular structure in (3) into an 85% ethanol solution, heating with microwave for 10 min at a power of 300W to volatilize the solvent to obtain the slow-release flavor-holding milk flavor, and adding 25 parts of the slow-release flavor-holding milk flavor into 75 parts of cigarette mouthpiece adhesive to obtain the slow-release flavor-holding cigarette mouthpiece adhesive.

Wherein, the biotechnology milk flavor has rich natural milk flavor and strong style characteristics. Cream, cream ester, cream oil or cheese is used as raw materials, 1.5% by mass of biological agents (lipase, lactobacillus reuteri active dry powder and streptococcus lactis active dry powder in a mass ratio of 1.5:1: 1), 2.5% of citric acid and 0.5% of glutamic acid are added, the raw materials are mixed and stirred uniformly, the mixture is fermented and enzymolyzed for 24 hours at the temperature of 48 ℃ and the pH value of 6, fermented filtrate is obtained by decompression and suction filtration, and the mixture is subjected to vacuum freeze drying to obtain the biotechnological milk flavor powder which is natural and soft in flavor and obvious in milk flavor characteristic.

Example 3

The preparation method of the mouth connecting glue for the slow-release cigarette comprises the following specific steps:

(1) preparing a silicon dioxide nano microsphere dispersion liquid: 0.3 part of L-histidine and 100 parts of distilled water were weighed and mixed in a container, and magnetons were put and stirred at 200 rpm for 20 min at room temperature to form a uniform solution. Adding 15 parts of tetraethyl orthosilicate, sealing the container, stirring at room temperature for 40 min, and rotating at 800 rpm to obtain the silicon dioxide nano microsphere dispersion liquid.

(2) Supramolecular modification: and (2) dispersing 15 parts of the silicon dioxide nano microsphere powder in the step (1) in 100 parts of absolute ethyl alcohol, adding 2 parts of 3-aminopropyltrimethoxysilane, heating for 15 min by microwave with the power of 100W, stirring for 24 h at room temperature at 300 rpm, filtering, washing by using the absolute ethyl alcohol, and finally drying in vacuum at 85 ℃ to obtain the silicon dioxide nano microsphere powder with the supermolecular structure.

(3) Physical coating and chemical modification of the silica microspheres with supramolecular structures: and (3) adding 20 parts of the supermolecule microsphere powder prepared in the step (2) and 100 parts of distilled water, keeping the temperature of 90 ℃ for heating and condensing reflux, stirring at the rotating speed of 350 rpm for 12 h, then adding 3.5 parts of vanillin, continuously heating and stirring under the same condition for 12 h, then putting into an oven, and keeping the temperature at 80 ℃ overnight to obtain the modified supermolecule structure microsphere powder.

(4) Preparing the mouth connecting glue for the slow-release cigarette: sequentially adding biotechnological milk flavor, delta-decalactone, 3-hydroxy-2-butanone (mixed milk flavor) and the modified supermolecular structure nano microsphere powder (the mass of the microsphere powder is 15 times of that of the mixed milk flavor) in the mass ratio of 2:1:1 into 95% ethanol solution, heating with microwave for 15 min at a power of 500W to volatilize the solvent to obtain the slow-release flavor-holding milk flavor, and adding 35 parts of the slow-release flavor-holding milk flavor into 65 parts of cigarette mouthpiece adhesive to obtain the slow-release flavor-holding cigarette mouthpiece adhesive.

Wherein, the biotechnology milk flavor has rich natural milk flavor and strong style characteristics. Cream, cream ester, cream oil or cheese is used as a raw material, 3% by mass of biological agents (lipase, lactobacillus reuteri active dry powder and streptococcus lactis active dry powder in a mass ratio of 2:1: 1), 5% of citric acid and 1% of glutamic acid are added, the mixture is uniformly mixed and stirred, the temperature is 50 ℃, the pH value is 6.5, fermentation enzymolysis is carried out for 30 hours, the fermentation filtrate is obtained by decompression suction filtration, and vacuum freeze drying is carried out to obtain the biotechnological milk flavor powder which has natural and soft flavor and obvious milk flavor characteristics.

Comparative example 1

The preparation steps of the nozzle adhesive for the slow-release cigarette are the same as those of the example 3 except that the microsphere powder with the modified supermolecular structure is not added.

Comparative example 2

The preparation steps of the nozzle gum for the slow-release cigarette are the same as those of the example 3 except that the nano microsphere powder with the supermolecular structure is used for replacing the nano microsphere powder with the modified supermolecular structure.

Comparative example 3

The physical coating and chemical modification steps of the silica microspheres with supramolecular structures are not added with mastic resin, and the rest steps are the same as those of the example 3.

Evaluation of

1. Evaluation procedure

A. Retention rate

The storage conditions of the fragrance were simulated and the retention of the milky fragrance after 15 days in a forced air oven at a constant temperature of 40 ℃ in an open air environment was found by weighing and the retention was calculated, the retention = retention/initial amount.

B. Heat release amount

The prepared cigarette mouthpiece adhesive is placed for 15 days, and is heated at 80 ℃ for 10 min, and the actual heat release quality is calculated according to the original addition amount minus the retention amount.

The retention rate and heat release amount of the mouth piece adhesive for cigarettes prepared in examples and comparative examples were evaluated in comparison, and the results are shown in table 1.

C. Sensory evaluation

The cigarette mouthpiece adhesive prepared in the example 3, the comparative example 1, the comparative example 2 and the comparative example 3 is rolled into a cigarette according to the conventional process parameters, after the cigarette is placed for 15 days, the sensory evaluation is carried out by adopting 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 microsphere powder of modified supramolecular structure;

the retention rate and the heat release of the comparative example 2 are lower than those of the example 3, which shows that the modification of the nano microspheres with the supermolecular structure is the key for ensuring the normal temperature stability and the heat release of the cigarette mouthpiece adhesive;

the retention rate and the heat release amount of the comparative example 3 are lower than those of the example 3, which shows that the normal temperature stability and the heat release property of the cigarette mouthpiece adhesive can be further improved by carrying out physical coating and chemical modification on the supermolecular structural nanospheres compared with the supermolecular nanospheres which are only chemically modified.

As can be seen from table 2, the cigarette manufactured in example 3 has natural and distinct characteristic smell and flavor of natural, rich and pure milk flavor, is accompanied by sweet and sour flavor, has good stability at room temperature, has stable, uniform and strong style and characteristic of heat-released milk flavor during smoking, can coordinate and enrich the tobacco flavor and taste, improves flavor quality, and improves the taste comfort level.

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.