CN113180275A - Tobacco sheet by rolling method and preparation method thereof - Google Patents

Tobacco sheet by rolling method and preparation method thereof Download PDF

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Publication number
CN113180275A
CN113180275A CN202110522103.4A CN202110522103A CN113180275A CN 113180275 A CN113180275 A CN 113180275A CN 202110522103 A CN202110522103 A CN 202110522103A CN 113180275 A CN113180275 A CN 113180275A
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fibers
tobacco
fiber
modified
tobacco sheet
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CN202110522103.4A
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Inventor
危培
晏群山
杨德勇
舒灏
乐喜
王子维
陈一桢
彭瑞
杨弘熙
胡超
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China Tobacco Hubei Industrial LLC
Hubei Xinye Tobacco Sheet Development Co Ltd
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China Tobacco Hubei Industrial LLC
Hubei Xinye Tobacco Sheet Development Co Ltd
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Priority to CN202110522103.4A priority Critical patent/CN113180275A/en
Publication of CN113180275A publication Critical patent/CN113180275A/en
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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/14Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products

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  • Cigarettes, Filters, And Manufacturing Of Filters (AREA)
  • Manufacture Of Tobacco Products (AREA)

Abstract

The invention belongs to the field of tobacco products, and particularly relates to a rolling tobacco sheet and a preparation method thereof. The tobacco sheet by the rolling method is obtained by uniformly mixing modified fibers with negatively charged groups on the surface and tobacco raw materials and then pressing. The method comprises the following steps: (1) carrying out negative charge modification on the surface of the fiber raw material; (2) and (2) uniformly mixing the modified fiber obtained in the step (1) with a tobacco raw material, pressing by using a roller press, and drying to obtain the tobacco sheet by using the roller pressing method. According to the invention, plant fibers are used as raw materials, and negative electricity groups are introduced to the surfaces of the fibers through a chemical modification method, so that the negative electricity of the fibers is improved, the electrostatic repulsion acting force among the fibers is improved, the length-diameter ratio of the fibers is reduced, and the fibers are uniformly mixed with components such as tobacco powder, an adhesive, an atomizing agent and the like, so that the fibers are uniformly dispersed in a slice, no obvious fiber flocculation exists, no white spots exist in the slice, and the texture is uniform.

Description

Tobacco sheet by rolling method and preparation method thereof
Technical Field
The invention belongs to the field of tobacco products, and particularly relates to a rolling tobacco sheet and a preparation method thereof.
Background
The tobacco sheet prepared by the rolling method can effectively retain the smoke agent and endogenous components in the tobacco sheet, has great application value in novel tobacco products (such as heating non-combustion cigarettes), but the improvement of the quality is limited by the problem of poor strength. In the production process of the rolled sheet, the strength of the sheet is generally improved by a fiber adding method, namely adding plant fibers (such as wood pulp fibers, bagasse fibers, cut tobacco stems and the like) into the sheet as a reinforcing phase. However, because the hydrophilic action among fibers is strong, the mutual repulsive acting force is lacked, and the length-diameter ratio of the fibers is high, the fibers are easy to flocculate under the condition of high concentration, and are difficult to uniformly disperse in the sheet, so that the full play of the enhancement effect is limited, the appearance quality of the sheet is reduced, and the quality of the cigarette product is influenced.
Therefore, uniform dispersion of the fibers in the rolled sheet is important to improve the performance and quality of the rolled sheet in all aspects. Early researchers improved the dispersion uniformity of fibers in the sheet by optimizing the production process, designing defibering or mixing equipment, soaking fibers with alkali liquor and the like. For example, Zhang Cai Yun et al defiber the dispersed pulp sheet with an autonomously designed defibering apparatus. Journal literature "Zhang Cai Yun, Liu Dian Yun, Zhang Wei, Chen Lian Fang. Research on a tobacco sheet fiber adding method by a rolling method. Tobacco technology, 2001(11):3-5. "; shao Chun Ju, etc. is mixed with powdered tobacco after dispersing fiber with medium solution, and the periodical literature "Shao Chun Ju, Wang Qing Hai, Xuhai Tao, etc. And (3) researching a sheet fiber adding process by a rolling method. Tobacco technology, 2001(11):6-7. "; chen's inflammation, etc. uses the ' wet-decomposing dry-adding ' process to defiber and mix it with tobacco powder, and the journal literature ' Chen's inflammation, Ji Ming Xiang, etc. is known in the past. An application experiment of a wet-decomposition dry-fiber-adding process of a tobacco sheet by a rolling method. Tobacco technology, 2000(08):13-14. "; patent No. CN101933649A discloses a process method for improving the shatter resistance of a rolled sheet, and the inventor of the invention uses alkali liquor to soak fibers to realize high-efficiency defibration, thereby improving the toughness and shatter resistance of the sheet.
The research mainly improves the dispersion uniformity of the fibers in the sheet by a physical method, thereby achieving the purpose of improving the quality of the tobacco sheet. However, these methods are not sufficient enough to improve the uniformity of dispersion of the tobacco sheet, and at the same time, the strength and the quality of the tobacco sheet are not sufficient.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a rolling tobacco sheet and a preparation method thereof. The method provides that the uniform dispersion of the fibers in the rolled sheet is realized by starting from fiber raw materials through chemical modification to improve the surface charge amount of the fibers and properly reducing the length-diameter ratio of the fibers, so that the quality of the rolled sheet is improved.
In order to solve the problems, the invention adopts the following technical scheme:
a rolled tobacco sheet is prepared by uniformly mixing modified fibers with negatively charged groups on the surface and tobacco raw materials.
The invention also provides a preparation method of the rolled tobacco sheet, which comprises the following steps:
s1: carrying out negative charge modification on the surface of the fiber raw material;
s2: and (5) uniformly mixing the modified fibers obtained in the step (S1) with the tobacco raw materials, and pressing and drying the mixture by using a rolling machine to obtain the tobacco sheet by using the rolling method.
Preferably, the modification method for modifying the fiber in step S1 is one of oxidation, carboxymethylation, and phosphorylation.
Preferably, in the modified fiber, the ion content of the oxidized fiber and the carboxymethylated fiber is 0.6-1.3 mmol/g, and the ion content of the phosphorylated fiber is 1.2-1.8 mmol/g.
Preferably, in the step S2, the fiber adding amount of the modified fiber is 1 to 3wt% of the tobacco raw material.
Preferably, the oxidation method for preparing the modified fiber comprises the following steps: the fiber raw material is subjected to catalytic oxidation in a TEMPO/NaClO/NaBr system.
Preferably, the method for preparing the modified fiber by the carboxymethyl method comprises the following steps: and carrying out substitution reaction on the fiber raw material under an alkaline condition by using chloroacetic acid as an etherifying agent.
Preferably, the method for preparing the modified fiber by phosphorylation comprises the following steps: disodium hydrogen phosphate, sodium dihydrogen phosphate and urea are co-present, and phosphate groups are introduced into the fiber raw material in the form of esters.
Preferably, the fiber raw material is any one of bleached softwood pulp, bleached hardwood pulp and bleached bagasse pulp.
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the invention, plant fibers are used as raw materials, and negative electricity groups are introduced to the surfaces of the fibers by chemical modification methods such as oxidation, carboxymethylation and phosphorylation, so that the negative electricity of the fibers is improved, and the electrostatic repulsion acting force between the fibers is improved; in addition, the introduction of the negative electricity groups enables the fibers to be cut off in the length direction and swell the cell walls of the fibers, so that the length of the fibers is reduced, the length-diameter ratio of the fibers is reduced, the fibers are promoted to be uniformly mixed with components such as tobacco powder, an adhesive, an atomizing agent and the like, and the dispersion uniformity of the fibers in the tobacco sheets is improved.
The tobacco sheet prepared by the rolling method provided by the invention has the advantages that the fibers are uniformly dispersed in the sheet, no obvious fiber flocculation is generated, no white spots are generated in the sheet, the texture is uniform, and the strength is obviously improved; the adding amount of fibers and adhesives (sodium carboxymethylcellulose, sodium alginate and the like) can be reduced on the premise of maintaining the tensile strength of the sheet, so that the smoking quality of the sheet is improved, and the smoking sensory evaluation score of the sheet is about 82-75 minutes, which is superior to that of a sheet added with fibril (75 minutes).
Drawings
Fig. 1 is an appearance view of tobacco sheets in examples and comparative examples.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
In the following examples, the carboxyl content of oxidized and carboxymethylated fibers and the charge content of phosphorylated fibers were measured according to the methods mentioned in the paper [ Houshu ] two methods for measuring sulfonic acid groups and carboxylic acid groups [ J ] Chinese paper, 1985(3):36-38 ], the Zeta potential of modified fibers was measured according to the national standard GB/T24993-.
Example 1
The fiber is chemically modified by an oxidation method: 10 g of oven-dried bleached bagasse pulp, 0.156 g of 2,2,6, 6-tetramethylpiperidine-N-oxide (TEMPO), 1.029 g of sodium bromide (NaBr), 48.857 g of sodium hypochlorite solution (NaClO, 5% available chlorine), 500 g of pure water were weighed out and placed in a flask, and after 1 hour of reaction at 25 ℃ and pH =10.5, the fibers were washed with pure water to neutrality for use. The carboxyl content of the prepared oxidized fiber is 1.31 mmol/g, the Zeta potential is-46.3 mV, the mass average length is 0.452 mm, the average width is 38.9 μm, and the length-diameter ratio is 11.6.
100 g of tobacco powder, 2.5g of the above oxidized fiber, 3g of Sodium Alginate (SA), 40 g of propylene glycol and 20 g of pure water were mixed, stirred for 5 minutes by a stirrer, pressed by a roller press, and dried in an air-blowing drying oven to prepare a rolled tobacco sheet having a moisture content of 9.8% and a thickness of 0.159 mm. The sheet has the advantages of uniform fiber dispersion, no fiber flocculation, no white spots, and uniform texture. The tensile strength was 589N/m.
Example 2
The fiber is chemically modified by a carboxymethylation method: 10 g of absolutely dry bleached bagasse pulp, 2.5g of sodium hydroxide (NaOH), 2.75g of chloroacetic acid (MCA), 300mL of absolute ethyl alcohol and 30 g of pure water are weighed and placed in a flask, a condensation reflux device is installed, the mixture reacts for 1 hour at the temperature of 90 ℃, and then the fibers are filtered and washed by pure water to be neutral for later use. The content of carboxyl group of carboxymethylation is 1.03 mmol/g, the Zeta potential is-41.6 mV, the average length of the proton is 0.591mm, the average width is 36.5 μm, and the length-diameter ratio is 16.2.
100 g of tobacco powder, 2.5g of the above carboxymethylated fibers, 2 g of sodium carboxymethylcellulose (CMC-Na), 20 g of glycerol and 20 g of pure water were mixed, stirred for 5 minutes by a stirrer, pressed by a roll press, and dried in an air-blast drying oven to prepare a rolled tobacco sheet having a moisture content of 8.9% and a thickness of 0.163 mm. The sheet has the advantages of uniform fiber dispersion, no fiber flocculation, no white spots, and uniform texture. The tensile strength was 562N/m.
Example 3
The fiber is chemically modified by a phosphorylation method: 10 g of oven-dried bleached bagasse pulp, 3.7 g of urea, 13.15 g of disodium hydrogen phosphate (Na)2HPO3) 11.11 g of sodium dihydrogen phosphate (NaH)2PO3) After 20 g of pure water was dissolved in a beaker and mixed uniformly, the mixed fibers were dried in a forced air drying oven at 70 ℃ for 2 hours. The dried mixture was placed in a flask, stirred at 120 ℃ until urea melted and reacted for 30 minutes. After the reaction is finished and the flask is cooled to room temperature, the fiber is filtered and washed by pure water to be neutral, and the conductivity of the filtrate is less than 20 mu S/cm for standby. The prepared phosphorylated fiber has the ion content of 1.51 mmol/g, the Zeta potential of-45.3 mV, the mass average length of 0.511 mm, the average width of 36.2 μm and the length-diameter ratio of 14.1.
Tobacco sheets were prepared as in example 2, except that 2.5g of the above phosphorylated fibers were used in place of the carboxymethylated fibers, and the sheets had uniform fiber dispersion, no fiber floc, no "white spots" and uniform texture. The tensile strength was 602N/m.
Example 4
The fiber is chemically modified by an oxidation method: 10 g of oven-dried bleached hardwood pulp (eucalyptus pulp), 0.156 g of 2,2,6, 6-tetramethylpiperidine-N-oxide (TEMPO), 1.029 g of sodium bromide (NaBr), 36.563 g of sodium hypochlorite solution (NaClO, 5% available chlorine content), 500 g of pure water were weighed out and placed in a flask, and after 1 hour of reaction at 25 ℃ and pH =10.5, the fibers were washed with pure water until neutral for use. The carboxyl content of the prepared oxidized fiber is 0.87 mmol/g, the Zeta potential is-39.1 mV, the mass average length is 0.652 mm, the average width is 18.2 μm, and the length-diameter ratio is 35.8.
100 g of tobacco powder, 1g of the above oxidized fiber, 2 g of Sodium Alginate (SA), 20 g of propylene glycol and 20 g of pure water were mixed, stirred for 5 minutes by a stirrer, pressed by a roller press, and dried in an air-blast drying oven to prepare a rolled tobacco sheet having a moisture content of 8.6% and a thickness of 0.167 mm. The sheet has the advantages of uniform fiber dispersion, no fiber flocculation, no white spots, and uniform texture. The tensile strength was 416N/m.
Example 5
The fiber is chemically modified by a carboxymethylation method: weighing 10 g of absolutely dry bleached hardwood pulp (eucalyptus pulp), 1.5g of sodium hydroxide (NaOH), 1.65 gChloroacetic acid(MCA), 300mL of absolute ethyl alcohol and 30 g of pure water were placed in a flask, a condensation reflux apparatus was installed, and after 1 hour of reaction at 90 ℃, the fiber was washed with pure water to neutrality by filtration and used. The carboxyl content of the prepared carboxymethylated fiber is 0.62 mmol/g, the Zeta potential is-30.2 mV, the mass average length is 0.572mm, the average width is 16.3 μm, and the length-diameter ratio is 35.1.
100 g of tobacco powder, 3g of the above carboxymethylated fibers, 1.5g of sodium carboxymethylcellulose (CMC-Na), 30 g of propylene glycol and 20 g of pure water were mixed, stirred for 5 minutes by a stirrer, pressed by a roll press, and dried in an air-blast drying oven to prepare a rolled tobacco sheet having a moisture content of 9.1% and a thickness of 0.168 mm. The sheet has the advantages of uniform fiber dispersion, no fiber flocculation, no white spots, and uniform texture.
Example 6
The fiber is chemically modified by a phosphorylation method: weighing 10 g absolutely dry bleached hardwood pulp (eucalyptus pulp), 3.7 g urea, 15.78 g disodium hydrogen phosphate (Na)2HPO3) 13.33 g of sodium dihydrogen phosphate (NaH)2PO3) After 20 g of pure water was dissolved in a beaker and mixed uniformly, the mixed fibers were dried in a forced air drying oven at 70 ℃ for 2 hours. The dried mixture was placed in a flask, stirred at 120 ℃ until urea melted and reacted for 30 minutes. After the reaction is finished and the flask is cooled to room temperature, the fiber is filtered and washed by pure water to be neutral, and the conductivity of the filtrate is less than 20 mu S/cm for standby. The prepared phosphorylated fiber has the ion content of 1.8 mmol/g, the Zeta potential of-49.5 mV, the mass average length of 0.430 mm, the average width of 24.2 μm and the length-diameter ratio of 17.77.
100 g of tobacco powder, 1g of the above phosphorylated fiber, 3g of sodium carboxymethylcellulose (CMC-Na), 35 g of propylene glycol and 20 g of pure water were mixed, stirred for 5 minutes by a stirrer, pressed by a roll press, and dried in an air-blowing dry oven to prepare a rolled tobacco sheet having a moisture content of 9.8% and a thickness of 0.161 mm. The sheet has the advantages of uniform fiber dispersion, no fiber flocculation, no white spots, and uniform texture. The tensile strength was 602N/m.
Comparative example
In the preparation of rolled tobacco sheets, 1g of oven-dried bleached hardwood pulp (raw eucalyptus pulp) fibers were used in place of the phosphorylated fibers, as in example 6.
Evaluation of
1. Evaluation procedure
A. Ion content
The ion contents of oxidized, carboxymethylated fibres and phosphorylated fibres are determined as described in the paper [ Houyan ] two methods for the determination of sulfonic and carboxylic acid groups [ J ] paper of China, 1985(3):36-38 ].
B. Aspect ratio
The average length and the average width of the fiber are measured by a fiber analyzer; the fiber analyzer model was Morfi Compact, Techpap, France.
B. Tensile strength
The tensile strength of the tobacco sheet is tested by adopting GB/T12914 and 2018 national standards; the tensile strength tester model is CE062, Sweden L & W.
C. Sensory evaluation
The tobacco sheets prepared in the examples 1-6 and the comparative example are rolled into cigarettes according to the conventional process parameters, and the sensory evaluation is carried out by adopting the national standard YCT 138-.
2. Evaluation results
The evaluation results of the examples and comparative examples are shown in FIG. 1 and tables 1-2.
As can be seen from the appearance of the tobacco sheets prepared in the example and comparative example of FIG. 1, the tobacco sheets of the comparative example had poor uniformity of fiber dispersion, a certain amount of fiber flocks, and a density of "white spots" of about 4/100 cm2The tobacco sheets of the examples have uniform fiber dispersion, no fiber flocculation, no "white spots" and uniform texture, indicating that the introduction of negative charge groups on the surface of the fibrils improves the uniformity of fiber dispersion in the rolled sheet.
Figure DEST_PATH_IMAGE002
As can be seen from Table 1, the aspect ratio of the comparative example is significantly larger than that of example 6, and the tensile strength is significantly lower than that of example 6, which illustrates the technical contribution to the charge modification of the fibers;
example 3, which has a higher ionic content and tensile strength than example 2 and a lower fiber aspect ratio than example 2, shows that the technical contribution of the phosphorylated modified fibers is better than that of the carboxymethylated modification.
Figure DEST_PATH_IMAGE004
As can be seen from Table 2, the tobacco sheet made of the modified fibers had a sensory evaluation score of about 82-75 points in smoking, which is superior to the fibrillated sheet (75 points).
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.

Claims (9)

1. A tobacco sheet by a rolling method is characterized in that the tobacco sheet is obtained by uniformly mixing modified fibers with negatively charged groups on the surface and tobacco raw materials and then pressing and forming the mixture.
2. A method of making a rolled tobacco sheet according to claim 1, comprising the steps of:
s1: carrying out negative charge modification on the surface of the fiber raw material;
s2: and (5) uniformly mixing the modified fibers obtained in the step (S1) with the tobacco raw materials, and pressing and drying the mixture by using a rolling machine to obtain the tobacco sheet by using the rolling method.
3. The method of claim 2, wherein the modification method of the modified fiber in step S1 is one of oxidation, carboxymethylation, and phosphorylation.
4. The method for preparing a rolled tobacco sheet according to claim 3, wherein the ion content of the oxidized fibers and the carboxymethylated fibers in the modified fibers is 0.6 to 1.3 mmol/g, and the ion content of the phosphorylated fibers is 1.2 to 1.8 mmol/g.
5. The method of claim 3, wherein in step S2, the modified fiber is added in an amount of 1-3 wt% of the tobacco material.
6. The method for preparing the rolled tobacco sheet according to claim 3, wherein the method for preparing the modified fiber by the oxidation method comprises the following steps: the fiber raw material is subjected to catalytic oxidation in a TEMPO/NaClO/NaBr system.
7. The method for preparing a rolled tobacco sheet according to claim 3, wherein the carboxymethyl method for preparing the modified fiber comprises the following steps: and carrying out substitution reaction on the fiber raw material under an alkaline condition by using chloroacetic acid as an etherifying agent.
8. The method for preparing rolled tobacco sheets according to claim 3, wherein the method for preparing modified fibers by phosphorylation comprises the following steps: disodium hydrogen phosphate, sodium dihydrogen phosphate and urea are coexisted, and phosphate groups are introduced into the fiber raw material in the form of ester.
9. The method of claim 2, wherein the fibrous material is any one of bleached softwood pulp, bleached hardwood pulp, and bleached bagasse pulp.
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