阅读说明：本技术 一种烟用爆珠壁材及其制备方法 (Bead blasting wall material for cigarettes and preparation method thereof ) 是由 邵佩 张雨迎 王盼 王俊 潘婷婷 于 2021-09-08 设计创作，主要内容包括：本发明公开了一种烟用爆珠壁材及其制备方法。本发明以仙草胶、纳米壳聚糖和淀粉作为制备壁材的主要原料,基于淀粉与仙草胶的氢键作用主导复合凝胶网络结构的形成,带正电荷的壳聚糖与带负电荷的仙草胶之间产生静电引力作用形成静电复合物,三元复合体系加强了网络结构的交联度,仙草胶与淀粉相互作用形成凝胶网络结构束缚了自由水的移动,同时添加纳米壳聚糖后纳米壳聚糖在三元复合体系中形成具有高度取向的结晶域,使得水蒸气和氧气的传输路径延长,从而减少了每单位时间内氧气和水蒸气的渗透量,由此制备的壁材不但稳定性好,而且具有较好的耐水性。(The invention discloses a bead blasting wall material for cigarettes and a preparation method thereof. The invention takes the mesona blume gum, the nano chitosan and the starch as main raw materials for preparing the wall material, the formation of a composite gel network structure is guided based on the hydrogen bond action of the starch and the mesona blume gum, an electrostatic compound is formed by the electrostatic attraction action between the positively charged chitosan and the negatively charged mesona blume gum, the cross-linking degree of the network structure is enhanced by a ternary composite system, the gel network structure formed by the interaction of the mesona blume gum and the starch restrains the movement of free water, and simultaneously, after the nano chitosan is added, a highly oriented crystalline domain is formed in the ternary composite system, so that the transmission path of water vapor and oxygen is prolonged, thereby reducing the permeation amount of oxygen and water vapor in unit time, and the prepared wall material has good stability and better water resistance.)

1. The bead blasting wall material for the cigarettes is characterized by comprising, by weight, 5-10 parts of mesona blume gum, 4-5 parts of nano chitosan, 3-5 parts of starch, 0.5-1.5 parts of a plasticizer and 70-80 parts of a solvent.

2. The wall material for popping beads for cigarettes as claimed in claim 1, wherein the starch is amylose.

3. The wall material for exploding beads for cigarette as claimed in claim 1, wherein the plasticizer is one or a mixture of glycerol, stearic acid, stearate and lauryl sulfate.

4. The wall material for the blasting bead for the cigarette as claimed in claim 3, wherein the plasticizer is preferably one or a mixture of stearate and dodecyl sulfate.

5. The wall material for exploding beads for cigarette as claimed in claim 1, wherein the solvent is one or a mixture of deionized water and acetic acid.

6. The wall material for exploding beads for cigarette as claimed in claim 5, wherein the solvent is preferably acetic acid.

7. The preparation method of the wall material for the blasting bead for the cigarette as claimed in any one of claims 1 to 6, which comprises the following steps:

taking a certain amount of starch for gelatinization to obtain a mixed solution A;

adding mesona blume gum into the mixed solution A, and uniformly stirring to obtain a mixed solution B;

and adding the nano chitosan and the plasticizer into the mixed solution B, uniformly stirring, and ultrasonically removing bubbles to obtain the explosion bead wall material.

8. The preparation method of the wall material for the blasting bead for the cigarette as claimed in claim 7, wherein the mixed solution B is acidic.

9. The preparation method of the wall material for the blasting bead for the cigarette as claimed in claim 8, wherein the pH of the mixed solution B is 5.5-6.

Technical Field

The invention belongs to the technical field of cigarette production, and particularly relates to a bead blasting wall material for cigarettes and a preparation method thereof.

Background

The cigarette blasting bead is used for realizing the artificially controllable characteristic flavor release in the cigarette smoking process, reducing the influence of the external environment on the smoking taste and the loss of essence caused by the external environment, enriching the smoking taste of the cigarette, realizing the functions of increasing the aroma and keeping the moisture in the smoking process and the like. The cigarette bead is prepared by wrapping various tobacco essences in a micro closed spherical capsule in a solid, liquid or gas form according to a natural polymer material or a synthetic polymer material, and implanting one or more easily-broken flavor capsules in the production process of the filter tip.

The cigarette bead has the core effect of the aroma components in the capsule, and although the aroma components are various and can be matched with aroma substances with various flavors, the wall materials forming the outer layer of the capsule have different barrier effects on the aroma substances with different properties, so that the wall materials are not suitable for the aroma substances with certain components, and the development of the taste of certain bead beads is limited. For example, the commonly used wall materials include plant gums, starches and derivatives thereof, proteins, various cellulose derivatives and the like, and the gel is mainly formed by forming a three-dimensional network structure by functional groups on various substances through the interaction between molecular chains, so that the fragrance substances are wrapped and blocked from the outside. When the three-dimensional network structure formed is unstable or has more voids, the migration of the fragrance substance out of the three-dimensional network structure or the migration of air or water in the external environment into the fragrance substance may affect the quality of the fragrance substance.

The cigarette blasting beads can be divided into ester solubility and alcohol solubility according to the properties of core materials, and the corresponding wrapping systems comprise an oil phase wrapping an oil phase and an oil phase wrapping a water phase. The ester-soluble essence and spice adopts a wrapping system of a water-phase wrapping oil-phase system, the blasting beads can not wrap a water-soluble or alcohol-soluble core material, and the wall material of the blasting beads has hydrophilicity and is easy to swell in an H bond combination mode. The wall material of the alcohol-soluble core material preferably has a compact internal microstructure, has a low dissolution coefficient and a low diffusion coefficient for water, and has fewer internal structure pores or gaps on the microstructure of the material, so that the water molecules have fewer 'escape' paths, and the barrier property is better.

Therefore, the development of a blasting bead wall material with good stability and capable of improving coating performance and water resistance is a problem to be solved at present.

Disclosure of Invention

Aiming at the problems, the invention aims to provide the bead blasting wall material for the cigarettes and the preparation method thereof.

The mesona chinensis benth is a herbal perennial root plant used as both medicine and food, the mesona chinensis benth is prepared by extracting leaves, stems and roots of the mesona chinensis benth serving as raw materials by hot water or alkali liquor, the main component of the mesona chinensis benth is mesona benth polysaccharide, and the mesona chinensis benth contains functional components such as polyphenol, flavonoid, terpenoids and the like, and has good antioxidation, bacterium and mould inhibition effects and unique gel characteristics.

The amino group in the chitosan molecular structure has stronger reactivity than the acetamido group in the chitin molecule, so that the polysaccharide has excellent biological function. Chitosan is linear alkaline polysaccharide, which is protonated in acetic acid solution to carry positive charge, and Mesona gum is an anionic polysaccharide containing uronic acid structure, and can form electrostatic compound with chitosan. Meanwhile, the mesona chinensis benth gum serving as a novel anionic polysaccharide gum rich in uronic acid structures can interact with starch to form composite gel.

The starch and the mesona blume gum form a network structure through hydrogen bond interaction, the network structure is further crosslinked by adding the chitosan, and the network structure of the composite gel is jointly reinforced, so that the gel network structure formed by the interaction of the mesona blume gum and the starch and the chitosan has a smaller gap size, the movement of free water is restrained, and more hydrophilic groups such as carboxyl and hydroxyl in molecules and water molecules form hydrogen bonds to restrain the movement of the free water.

The invention takes the mesona blume gum, the nano chitosan and the starch as main raw materials for preparing the wall material, the formation of a composite gel network structure is guided based on the hydrogen bond action of the starch and the mesona blume gum, an electrostatic compound is formed by the electrostatic attraction action between the positively charged chitosan and the negatively charged mesona blume gum, the cross-linking degree of the network structure is enhanced by a ternary composite system, the gel network structure formed by the interaction of the mesona blume gum and the starch restrains the movement of free water, and simultaneously, after the nano chitosan is added, a highly oriented crystalline domain is formed in the ternary composite system, so that the transmission path of water vapor and oxygen is prolonged, the permeation amount of the oxygen and the water vapor in each unit time is reduced, and the prepared wall material has better water resistance.

In order to achieve the purpose, the invention provides a wall material for blasting beads for cigarettes, which comprises, by weight, 5-10 parts of mesona blume gum, 4-5 parts of nano chitosan, 3-5 parts of starch, 0.5-1.5 parts of a plasticizer and 70-80 parts of a solvent.

The nano chitosan contains abundant hydroxyl and amino, and is beneficial to the crosslinking of a network structure in a reaction system.

The invention has the following excellent technical scheme: the starch is amylose.

Amylose has good transparency, flexibility, tensile strength and water insolubility. After the direct-connection starch is gelatinized, the direct-connection starch molecules obtain fluidity, a continuous phase of a direct-connection starch solution is formed in water, the continuous phase still exists in a particle or block form after being gelatinized compared with amylopectin, and is dispersed into a two-phase system in a water solution, the direct-connection starch solution is more favorable for forming a gel system, and the direct-connection starch solution is uniformly dispersed in the water phase, so that the direct-connection starch molecules can be fully contacted with the mesona chinensis benth glue molecules to form a uniform gel system, and the subsequent prepared wall material is favorable for forming a smooth and flat appearance.

The invention has the following excellent technical scheme: the plasticizer is one or more of glycerol, stearic acid, stearate and dodecyl sulfate.

The plasticizer is added to make the network structure plastic, to enhance its flexibility and to facilitate processing.

The invention has the following excellent technical scheme: the plasticizer is one or a mixture of stearate and dodecyl sulfate.

The stearate and the dodecyl sulfate with negative charges and the chitosan with positive charges interact with each other through static electricity, wherein the hydrophobic carbon chains on the stearate and the dodecyl sulfate further improve the repulsion of the blasting bead wall material to hydrophilic substances and reduce the permeability to water. Negatively charged-COO in stearate^-with-NH positively charged in the nano-chitosan³⁺Combining with novel anion containing uronic acid structure in Mesona Procumbens Hemsl to compete for-NH positively charged in nano chitosan³⁺The stearate is inserted into the three-dimensional network structure formed by the mesona blume gum, the starch and the nano chitosan, the electrostatic interaction between the mesona blume gum and the nano chitosan is reduced, the mobility of the three-dimensional network structure is improved, the plasticity of the wall material is improved, meanwhile, the hydrophobic carbon chains on the stearate and the dodecyl sulfate are distributed in the three-dimensional network structure to form a hydrophobic barrier, water molecules are difficult to enter the three-dimensional network structure, and the water-resistant stability of the wall material prepared by the method is improved.

The invention has the following excellent technical scheme: the solvent is one or a mixture of deionized water and acetic acid; acetic acid is preferred.

On one hand, acetic acid can effectively improve the acidity of the solution, and on the other hand, when the acetic acid is used as a solvent and a three-dimensional network structure is formed, free water in the network structure is replaced by the acetic acid, so that the water content in the network structure is reduced; in addition, the nano chitosan has poor dispersibility, and the addition of acetic acid can improve and accelerate the dispersibility of the nano chitosan in a reaction system, thereby being beneficial to the formation of gel.

The invention also provides a preparation method of the bead blasting wall material for the cigarettes, which comprises the following specific steps: weighing starch, dispersing in deionized water, gelatinizing at 60-80 deg.C for 30min to obtain a mixed solution A, adding mesona chinensis benth gum into the mixed solution A, mixing and stirring at 80 deg.C to obtain a mixed solution B, adding nano chitosan and plasticizer into the mixed solution B, stirring, and ultrasonically removing bubbles to obtain molten blasting bead wall material.

The invention has the following excellent technical scheme: the mixed solution B is acidic.

The invention has the following excellent technical scheme: the pH of the mixed solution B is 5.5-6. Under the acidic condition, the nano chitosan can be effectively protonated to enable-NH₂Form positively charged-NH₃ ⁺The nano chitosan and the novel anion with the structure of the mesona blume uronic acid are combined through electrostatic interaction, wherein when the pH is 5.5-6, the nano chitosan can be completely protonated, so that the electrostatic combination capability is highest.

According to the invention, the mesona blume gum, the nano chitosan and the starch are used as main raw materials for preparing the gel, the composite gel with a network structure is formed mainly based on the hydrogen bond action of the starch and the mesona blume gum, the electrostatic attraction action is generated between the nano chitosan with positive charge and the mesona blume gum with negative charge to form an electrostatic composite, and the ternary composite system enhances the crosslinking degree of the network structure, so that the network structure is compact, and the migration of substances is blocked. The hydrophilic Mesona gum and starch interact to form a gel network structure to restrict the movement of free water, and the nano chitosan forms a highly oriented crystalline domain in a ternary composite system after being added, so that the transmission path of water vapor and oxygen is prolonged, the permeation amount of oxygen and water vapor in unit time is reduced, and the wall material prepared by the method has good water resistance.

The invention has the beneficial effects that:

1. the wall material for blasting beads for cigarettes provided by the invention takes the mesona chinensis benth gum as a raw material, the mesona chinensis benth gum contains rich functional components such as polyphenol, flavonoid, terpenoids and the like, and has better antioxidation effect and bacteria and mould inhibition effect.

2. According to the invention, the nano chitosan is used as a raw material, and the nano chitosan with positive charges and the mesona blume gum with negative charges form an electrostatic compound, so that the crosslinking degree is improved, the compact structure of a network is improved, and the mechanical strength, rheological property and barrier property of the composite material are enhanced.

3. According to the invention, the fatty acid salt, such as stearate and dodecyl sulfate, is added as a plasticizer, so that on one hand, the plasticity of the wall material is improved, on the other hand, the hydrophobic carbon chains on the stearate and the dodecyl sulfate are distributed in the three-dimensional network structure to form a hydrophobic barrier, water molecules are difficult to enter the three-dimensional network structure, and the water-resistant stability of the wall material prepared by the method is further improved.

Detailed Description

The present invention will be described in further detail with reference to examples, which are not intended to limit the technical scope of the present invention. The invention can be used for other purposes by anyone skilled in the art within the technical scope of the invention disclosure, and the relevant changes of raw materials, process conditions and the like can be properly realized by taking the technical content into consideration, and the invention can not depart from the technical content, and all similar substitutes and modifications which are obvious to those skilled in the art are deemed to be included in the technical scope of the invention.

In order to better explain the invention, the following text further illustrates the main content of the invention in connection with specific laboratory examples, but the content of the invention is not limited to the following examples only.

The invention is further illustrated by the following examples:

example 1

A method for preparing a bead blasting wall material for cigarettes.

Weighing 5 parts of direct-connection starch, dispersing the direct-connection starch in 80 parts of acetic acid, gelatinizing at 70 ℃ for 40min to obtain a mixed solution A, then adding 5 parts of mesona blume into the mixed solution A, mixing and stirring uniformly at 80 ℃ to obtain a mixed solution B, adjusting the pH of the mixed solution B by using hydrochloric acid and a sodium hydroxide solution to 6, finally adding 5 parts of nano chitosan and 1 part of sodium stearate into the mixed solution B, stirring uniformly, and ultrasonically removing bubbles to obtain a molten blasting bead wall material.

Example 2

A method for preparing a bead blasting wall material for cigarettes.

Weighing 5 parts of direct-connection starch, dispersing the direct-connection starch in 40 parts of deionized water and 40 parts of acetic acid mixed solution, gelatinizing for 40min at 70 ℃ to obtain mixed solution A, then adding 5 parts of mesona blume into the mixed solution A, uniformly mixing and stirring at 80 ℃ to obtain mixed solution B, adjusting the pH of the mixed solution B to 6 with hydrochloric acid and sodium hydroxide solution, finally adding 5 parts of nano chitosan and 1 part of sodium stearate into the mixed solution B, uniformly stirring, and ultrasonically removing bubbles to obtain the molten blasting bead wall material.

Example 3

A method for preparing a bead blasting wall material for cigarettes.

Weighing 5 parts of direct-connection starch, dispersing the direct-connection starch in 80 parts of deionized water, gelatinizing at 70 ℃ for 40min to obtain a mixed solution A, then adding 5 parts of mesona blume into the mixed solution A, mixing and stirring uniformly at 80 ℃ to obtain a mixed solution B, adjusting the pH of the mixed solution B by using hydrochloric acid and a sodium hydroxide solution to 6, finally adding 5 parts of nano chitosan and 1 part of sodium stearate into the mixed solution B, stirring uniformly, and ultrasonically removing bubbles to obtain a molten explosion bead wall material.

Example 4

A method for preparing a bead blasting wall material for cigarettes.

Weighing 4 parts of direct-connection starch, dispersing the direct-connection starch in a mixed solution of 45 parts of deionized water and 25 parts of acetic acid, gelatinizing the mixed solution at 70 ℃ for 40min to obtain a mixed solution A, then adding 5 parts of mesona blume into the mixed solution A, mixing and stirring the mixture at 80 ℃ to obtain a mixed solution B, adjusting the pH value of the mixed solution B to 5.7 by using a hydrochloric acid and sodium hydroxide solution, finally adding 4.5 parts of nano chitosan and 1 part of sodium stearate into the mixed solution B, stirring the mixture uniformly, and removing bubbles by using ultrasonic waves to obtain a molten explosion bead wall material.

Comparative example 1

A method for preparing a bead blasting wall material for cigarettes.

Weighing 5 parts of direct-connection starch, dispersing the direct-connection starch in 80 parts of acetic acid, gelatinizing at 70 ℃ for 40min to obtain a mixed solution A, then adding 5 parts of mesona blume into the mixed solution A, mixing and stirring uniformly at 80 ℃ to obtain a mixed solution B, adjusting the pH6 of the mixed solution B by using hydrochloric acid and a sodium hydroxide solution, finally adding 0 part of nano chitosan and 1 part of sodium stearate into the mixed solution B, stirring uniformly, and ultrasonically removing bubbles to obtain a molten blasting bead wall material.

Evaluation of

(1) Influence of solvent on blasting bead for cigarette

Selecting chrysanthemum essential oil as essence core liquid, preparing the bead blasting wall materials obtained in the embodiment 1, the embodiment 2 and the embodiment 3 into bead blasting products by adopting a dripping pill method, and wrapping the essence core liquid in the wall materials by the hot-melt wall materials through the surface tension of liquid through dripping equipment to obtain the bead blasting for cigarettes. And condensing in cooling liquid to prepare spherical blasting beads, and then deoiling, drum drying, pill screening, selecting, balancing and packaging to obtain the final product, wherein the final product is applied to the cigarette filter.

The moisture content and sensory properties of the resulting puffed tobacco beads were evaluated as shown in table 1.

As can be seen from Table 1, the moisture content of the bead for cigarette blasting can be effectively controlled by changing the proportion of the solvent, and the hand feeling of the bead for blasting is influenced.

(2) Influence of adding nano chitosan on bead blasting for cigarettes

Selecting chrysanthemum essential oil as essence core liquid, preparing the bead blasting wall materials obtained in the embodiment 1 and the comparative example 1 into bead blasting products by adopting a dropping pill method, and wrapping the essence core liquid in the wall materials by the hot-melt wall materials through liquid surface tension through dropping equipment to obtain the bead blasting for cigarettes. And condensing in cooling liquid to prepare spherical blasting beads, then deoiling, drum drying, screening, selecting, balancing and packaging to obtain a final product, placing the products prepared by the two types of wall materials in an open environment with the humidity of 80% for 3 days, and then testing the moisture content of the whole blasting bead product so as to evaluate the barrier property of the wall material to water.

The water content detection method of the bead blasting product detects the water content in the bead blasting product by using GC-TCD (gas chromatography-thermal conductivity detector).

Step 1: preparing a standard solution by mixing the following components in a volume ratio of 1: 333 preparing absolute ethyl alcohol (internal standard)/isopropanol extract; weighing ultrapure water, preparing a standard stock solution with the concentration of 20mg/mL by using the extract liquor, and diluting the standard stock solution into a standard working solution with a certain concentration gradient.

Preparing an extraction liquid: adding 3mL of absolute ethyl alcohol internal standard into 1000mL of isopropanol solution, and uniformly mixing for later use.

Preparation of stock solution: 1.0g (about 1mL) of ultrapure water was precisely weighed out, and the volume of the extract solution was adjusted to 50 mL.

Preparing a primary stock solution: 10mL of the standard stock solution was accurately removed, and the volume of the solution was adjusted to 100mL with the extract.

Preparing a standard working solution: 2.5 mL, 5mL, 7.5 mL, 10mL, 12.5 mL, 15mL of the primary stock solution were removed, and the volume was adjusted to 50mL with the extract.

The above liquids are all prepared as required.

Step 2: pretreating a bead blasting product, namely putting 40-60 beads into a triangular flask with the volume of 150mL, mashing with a glass rod, adding 10-30 mL of isopropanol extract, and repeatedly washing the glass rod; vibrating for 20-40 min at 180r/min with a plug; standing for 2min, and filtering 2mL of supernatant with 0.22 μm organic phase filter membrane.

And step 3: instrumental detection, chromatographic column: porapak Q80/100 (PE corporation); sample inlet temperature: 250 ℃; detector temperature: 250 ℃; carrier gas: h2, 30 mL/min; sample introduction amount: 1 μ L.

And 4, step 4: quantitative method, each sample is measured twice in parallel, and blank samples are needed in each experiment. And drawing a standard curve according to the corresponding relation between the concentration ratio and the peak area ratio of the standard series solution and the internal standard substance. And then, the ratio of the peak area of the sample to be detected to the peak area of the internal standard is taken into the standard curve, and the concentration of the water in the sample is calculated.

As can be seen from table 2, the wall material of example 1 has a lower water content than the wall material of comparative example 1, indicating that the wall material added with nano chitosan has a better moisture barrier effect.

The embodiments of the present invention have been described above by way of example, but the description is only a preferred embodiment of the present invention and should not be construed as limiting the scope of the invention. All equivalent changes and modifications within the scope of the application of the present invention shall fall within the scope of the patent of the present invention.