A biodegradable polysaccharide-based fiber filter and a method for preparing the same

Abstract

The application relates to a biodegradable polysaccharide-based fiber filter and a preparation method thereof, which comprises 0.1-5 g of konjac glucomannan, 0.1-10 g of starch, 1-5 g of wood pulp fiber, 0.1-10 g of agar, 0.01-1 g of polyvinyl alcohol, 1-30 g of glycerol and 0.01-2 g of functional substances in 100 ml of water, wherein the functional substances comprise one or more of pyrrolidone compounds and surfactants, the pyrrolidone compounds comprise one or more of polyvinyl pyrrolidone and pyrrolidone carboxylate, and the surfactants comprise fatty alcohol polyoxyethylene ether sulfate, fatty alcohol polyoxyethylene ether carboxylate and the like. The raw materials for preparing the filter are natural polysaccharides extracted from nature and non-toxic and harmless chemical substances, so the filter can be degraded by microorganisms in nature, and no toxic and harmful substances are generated; meanwhile, the prepared filter can reduce traditional cigarette smoke tar by 5-25%, has a good adsorption effect on the smoke tar, and thus reduces the harm of the smoke tar.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of filter, in particular to a biodegradable polysaccharide-based fiber filter and a preparation method thereof. BACKGROUND

[0002] In the tobacco industry, the main harm of traditional cigarette smoke comes from a large amount of tar produced in the combustion process. The tar content of acetate fiber is poor due to its structural characteristics, and increasing the gram weight of acetate fiber will also cause some components in the smoke to be adsorbed by acetate fiber, thereby affecting the taste of smoking. This is also an important factor restricting the development of tar reduction and harm reduction technology in the tobacco industry.

[0003] Tar is a combination of the main harmful components in smoke, which can directly enter the blood circulation through contact with the skin and mucous membrane, causing protein denaturation, cell damage and loss of vitality, and has a strong irritating effect and carcinogenic effect on the skin and respiratory mucosa. It is listed as one of the index compounds of harmful substances in cigarette smoke and needs to be strictly controlled.

[0004] Therefore, how to reduce the tar in cigarette smoke has become a problem that needs to be solved. SUMMARY

[0005] The present application provides a biodegradable polysaccharide-based fiber filter and a preparation method thereof, which can reduce the tar in traditional cigarette smoke by 5-25%, and has a good adsorption effect on the tar in the smoke, thereby reducing the harm caused by the tar in the smoke.

[0006] In a first aspect, a biodegradable polysaccharide-based fiber filter is provided, comprising: 0.1-5 g of konjac glucomannan, 0.1-10 g of starch, 1-5 g of wood pulp fiber, 0.1-10 g of agar, 0.01-1 g of polyvinyl alcohol, 1-30 g of glycerol, and 0.01-2 g of functional substances, wherein the functional substances include one or more of a pyrrolidone-based compound and a surfactant, the pyrrolidone-based compound includes one or more of polyvinyl pyrrolidone and pyrrolidone carboxylate, and the surfactant includes one or more of fatty alcohol polyoxyethylene ether sulfate, fatty alcohol polyoxyethylene ether carboxylate, fatty acid methyl ester sulfonate, sodium secondary alkyl sulfonate, triglycerol monostearate, sodium starch octenyl succinate, sodium lauroyl glutamate, and sodium caseinate.

[0007] Further, the average molecular weight of the polyvinyl pyrrolidone is 8000-1.3 million.

[0008] Further, the pyrrolidone carboxylate includes one or more of 2-pyrrolidone-5-sodium carboxylate, L-pyrrolidone-5-sodium carboxylate, and potassium pyrrolidone carboxylate.

[0009] Further, the wood pulp fiber comprises one or more of coniferous fiber, broadleaf fiber, grafted cellulose, carboxymethylated cellulose and hydroxypropylated cellulose.

[0010] Further, the coniferous fiber comprises one or more of Pinus massoniana, Larix, Pinus koraiensis and Picea.

[0011] Further, the broadleaf fiber comprises one or more of birch, poplar, linden, eucalyptus and maple.

[0012] Further, the starch comprises one or more of potato starch, corn starch, mung bean starch, grafted starch and carboxymethylated starch.

[0013] Further, the polyvinyl alcohol has a molecular weight ranging from 25,000 to 250,000.

[0014] In a second aspect, a preparation method of the biodegradable polysaccharide-based fiber filter is provided, and the method comprises the following steps:

[0015] The wood pulp fiber is dispersed in water, and then cooled to a first temperature;

[0016] The konjac glucomannan, starch and agar are added, stirred and dissolved, then glycerol is added, and the temperature is raised to a second temperature to obtain a substance A;

[0017] The polyvinyl alcohol is added to the substance A, stirred and uniformly mixed, and then cooled to a third temperature to obtain a substance B;

[0018] The functional substance is added to the substance B, stirred and uniformly mixed, and then sequentially subjected to extrusion molding, low-temperature freezing and vacuum freeze-drying to obtain the biodegradable polysaccharide-based fiber filter.

[0019] Further, the temperature of the water is 60-100℃.

[0020] Further, the first temperature is 20-40℃.

[0021] Further, the second temperature is 70-95℃.

[0022] Further, the third temperature is 0-40℃.

[0023] Further, the temperature of the low-temperature freezing is -5 to -60℃.

[0024] The technical scheme provided by the present application has the following beneficial effects:

[0025] The biodegradable polysaccharide-based fiber filter and the preparation method thereof provided by the embodiments of the present application are all made of natural substances existing in nature, such as konjac glucomannan, starch, wood pulp fiber from plants, and agar from algae compounds, and thus can be degraded by microorganisms in nature.

[0026] The filter made of the polysaccharide-based fiber has a porous structure, which makes the filter have a very high porosity and specific surface area, and can effectively reduce harmful components in smoke, and can selectively adsorb some harmful components in tar by adding some functional substances.

[0027] The polyvinylpyrrolidone is a non-ionic high molecular compound, is an N-vinyl amide polymer, has a strong polarity and a formed hydrogen-bonded piperidine group, can perform complexation reaction with specific phenolic substances in tar, and thus reduces harmful components in tar; in addition, the high molecular polyvinylpyrrolidone can form a dense film on the pore structure of the aerogel, and can adsorb some harmful components in tar.

[0028] The pyrrolidone carboxylate is an anionic compound, can perform complexation reaction with phenolic substances in tar through specific groups to reduce harmful components in tar, and there are also a large number of cationic compounds in smoke tar; the pyrrolidone carboxylate can reduce the content of tar in smoke through the interaction of ionic bonds, and has the effect of reducing tar and reducing harm.

[0029] In summary, the present application can reduce tar in traditional cigarette smoke by 5-25%, has a good adsorption effect on tar in smoke, and thus reduces the harm of tar in smoke. BRIEF DESCRIPTION OF DRAWINGS

[0030] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed in the embodiment description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor.

[0031] Figure 1 The preparation method flow chart of the biodegradable polysaccharide-based fiber filter provided by the embodiments of the present application. DETAILED DESCRIPTION

[0032] To make the purposes, technical solutions, and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative work belong to the scope of protection of the present application.

[0033] The embodiment of the present application provides a biodegradable polysaccharide-based fiber filter, including 0.1-5 g of konjac glucomannan, 0.1-10 g of starch, 1-5 g of wood pulp fiber, 0.1-10 g of agar, 0.01-1 g of polyvinyl alcohol, 1-30 g of glycerol, and 0.01-2 g of functional substances, wherein the functional substances include one or more of a pyrrolidone-based compound and a surfactant, the pyrrolidone-based compound includes one or more of polyvinyl pyrrolidone and pyrrolidone carboxylate, and the surfactant includes one or more of fatty alcohol polyoxyethylene ether sulfate, fatty alcohol polyoxyethylene ether carboxylate, fatty acid methyl ester sulfonate, sodium secondary alkyl sulfonate, triglycerol monostearate, sodium starch octenyl succinate, sodium lauroyl glutamate, and sodium caseinate. The above materials are all naturally occurring substances in nature, such as konjac glucomannan, starch, and wood pulp fiber from plants, and agar from algal compounds, and thus can be degraded by microorganisms in nature.

[0034] The smoke contains a large amount of cationic compounds, and thus adding anionic surfactants such as fatty alcohol polyoxyethylene ether sulfate, fatty alcohol polyoxyethylene ether carboxylate, fatty acid methyl ester sulfonate, and sodium secondary alkyl sulfonate in the degradable polysaccharide-based filter can adsorb a part of harmful ingredients by using the charge effect between the two. Secondly, since aromatic hydrocarbons exist in the smoke tar, and sodium lauroyl glutamate and sodium caseinate contain a large amount of amino groups, a large amount of aromatic hydrocarbon substances can be combined by using the substitution reaction between the amino groups and the hydrocarbons, thereby playing a tar-reducing role.

[0035] The sodium secondary alkyl sulfonate is sodium alkyl sulfonate including 12 carbon atoms to 16 carbon atoms.

[0036] It should be noted that the above water needs to be heated into hot water for use in preparation, so as to disperse the wood pulp fiber.

[0037] In the present application, the filter prepared by using the polysaccharide-based fiber has a porous structure, which makes the filter have a very high porosity and specific surface area, can effectively reduce the harmful ingredients in the smoke, and can selectively adsorb some harmful ingredients in the tar in the smoke by adding some functional substances.

[0038] The polyvinylpyrrolidone is a non-ionic polymer compound, is an N-vinyl amide polymer, has a strong polarity and a hydrogen-bonded piperidine group, can perform a complexation reaction with specific phenolic substances in the tar, and thus reduces harmful components in the tar; in addition, the high-molecular polyvinylpyrrolidone can form a dense film on the pore structure of the aerogel and can adsorb some harmful components in the tar.

[0039] The pyrrolidone carboxylate is an anionic compound, can perform a complexation reaction with phenolic substances in the tar through specific groups to reduce harmful components in the tar, and there are also a large number of cationic compounds in the tar, the pyrrolidone carboxylate can reduce the content of the tar in the smoke through the interaction of the ionic bonds, and thus reduces the tar and the harm.

[0040] The average molecular weight of the polyvinylpyrrolidone is 8000-1.3 million; the type includes K13-K18, K16-K18, K23-K27, K29-K32 and K90.

[0041] The pyrrolidone carboxylate includes one or more of 2-pyrrolidone-5-carboxylic acid sodium, L-pyrrolidone-5-carboxylic acid sodium and pyrrolidone carboxylic acid potassium.

[0042] The wood pulp fiber has various options, for example, the wood pulp fiber includes one or more of coniferous fiber, broadleaf fiber, grafted cellulose, carboxymethylated cellulose and hydroxypropylated cellulose.

[0043] The coniferous fiber includes one or more of Pinus massoniana, Larix, Pinus koraiensis and Picea; the broadleaf fiber includes one or more of birch, poplar, linden, eucalyptus and maple.

[0044] The starch has various options, for example, the starch includes one or more of potato starch, corn starch, mung bean starch, grafted starch and carboxymethylated starch.

[0045] The molecular weight of the polyvinyl alcohol is 25-250 thousand.

[0046] The alcoholysis degree of the polyvinyl alcohol is mainly related to the molecular weight of the polyvinyl alcohol, the greater the molecular weight, the lower the alcoholysis degree, and the viscosity also changes; the purpose of adding the polyvinyl alcohol is to improve the appearance of the filter rod section, make the section appearance more uniform, and is beneficial to increase the elasticity of the core material of the filter rod.

[0047] Referring to Figure 1 The application also provides a preparation method of the biodegradable polysaccharide-based fiber filter rod.

[0048] 101: Disperse wood pulp fibers in water and cool to a first temperature.

[0049] The water is heated to disperse the wood pulp fibers, and the temperature can be determined according to actual needs, for example, the water is heated to 60-100°C to ensure that the wood pulp fibers are fully expanded.

[0050] The first temperature can be determined according to actual needs, for example, the first temperature is 20-40°C.

[0051] 102: Add konjac glucomannan, starch, and agar to the mixture, stir to dissolve, then add glycerol and heat to a second temperature to obtain substance A.

[0052] The second temperature can be 70-95°C to ensure sufficient swelling.

[0053] In addition, the konjac glucomannan is added again after cooling to a first temperature lower than the second temperature. The reason is that konjac glucomannan is a polysaccharide with strong water absorption. If the konjac glucomannan powder is added at a high temperature in the early stage, the konjac glucomannan will swell rapidly, the solution viscosity will increase rapidly, and the powder will be clumped, which is not conducive to the dispersion of other substances.

[0054] 103: Add polyvinyl alcohol to substance A, stir until uniform, and cool to a third temperature to obtain substance B.

[0055] The third temperature can be 0-40°C. If the temperature is too high, the proportion of free water in the glue solution will be too high, the liquid flowability will increase, and the material will easily flow out of the mold during extrusion molding, which is not conducive to the extrusion molding of the material. Therefore, through optimization, the effect of 0-40°C will be better.

[0056] 104: Add functional substances to substance B, stir until uniform, and then perform extrusion molding, low-temperature freezing, and vacuum freeze-drying to obtain a biodegradable polysaccharide-based fiber filter.

[0057] The low-temperature freezing temperature is -5 to -60°C. The freezing temperature is used to control the growth of ice crystals, thereby controlling the appearance of the cross section and the suction resistance of the mandrel.

[0058] Example 1

[0059] A biodegradable polysaccharide-based fiber filter includes 1.1 g of konjac glucomannan, 2 g of starch, 2 g of wood pulp fibers, 0.5 g of agar, 0.03 g of polyvinyl alcohol, 1.5 g of glycerol, and 0.05 g of a pyrrolidone compound, which includes polyvinylpyrrolidone, per 100 ml of water.

[0060] The preparation method of the biodegradable polysaccharide-based filter tip comprises the following steps:

[0061] 101: disperse the wood pulp fibers with water at 80℃, and then cool to 30℃;

[0062] 102: add konjac glucomannan, starch and agar again, stir and dissolve, then add glycerol, and heat to 92℃ to obtain substance A;

[0063] 103: add polyvinyl alcohol to substance A, stir until uniform, then cool to 40℃ to obtain substance B;

[0064] 104: add pyrrolidone compound to substance B, stir until uniform, then perform extrusion molding, low-temperature freezing and vacuum freeze-drying in sequence, to obtain the biodegradable polysaccharide-based filter tip, and the temperature of the low-temperature freezing is -20℃.

[0065] Example 2

[0066] Example 2 differs from Example 1 in that the amount of polyvinylpyrrolidone added is 0.1g.

[0067] Example 3

[0068] Example 3 differs from Example 1 in that the amount of polyvinylpyrrolidone added is 0.15g.

[0069] Example 4

[0070] Example 4 differs from Example 1 in that the amount of polyvinylpyrrolidone added is 0.2g.

[0071] The above Examples 1 to 4 are detected according to GB / T 19609-2004 Determination of total particulate matter and tar in cigarettes for routine analysis using smoking machine, GB / T 23203.1-2013 Determination of moisture in total particulate matter of cigarettes, GB / T 23355-2009 Determination of nicotine in total particulate matter of cigarettes - Gas chromatographic method, and GB / T 23356-2009 Determination of carbon monoxide in the gas phase of cigarette smoke - Non-dispersive infrared method. The detection instruments used include RM200A rotary smoking machine, RM200A2 rotary smoking machine and HP 7890 gas chromatograph.

[0072] The tobacco control sample used is a commercially available cigarette.

[0073] The detection results are shown in Table 1:

[0074] Table 1

[0075]

[0076] According to the tar test data of Examples 1 to 4 and the tobacco control sample, it is calculated that the tar content of Example 1 is reduced by 7.69% relative to the tobacco control sample, the tar content of Example 2 is reduced by 12.10%, the tar content of Example 3 is reduced by 17.61%, and the tar content of Example 4 is reduced by 22.77%. It can be seen that the addition of polyvinylpyrrolidone can effectively reduce the tar in the smoke of traditional cigarettes, has a good adsorption effect on the tar in the smoke, and thus reduces the harm caused by the tar in the smoke.

[0077] Example 5

[0078] A biodegradable polysaccharide-based fiber filter, comprising, per 100 ml of water: 1.1 g of konjac glucomannan, 2 g of starch, 2 g of wood pulp fiber, 0.5 g of agar, 0.03 g of polyvinyl alcohol, 1.5 g of glycerol, and 0.05 g of a pyrrolidone-based compound, the pyrrolidone-based compound comprising a pyrrolidone carboxylate.

[0079] A preparation method of the above biodegradable polysaccharide-based fiber filter, comprising the following steps:

[0080] 101: After dispersing the wood pulp fiber with water at 80°C, the temperature is lowered to 30°C;

[0081] 102: Konjac glucomannan, starch, and agar are added again, and after stirring and dissolving, glycerol is added, and the temperature is raised to 70°C to obtain substance A;

[0082] 103: Polyvinyl alcohol is added to substance A, and after stirring and uniformity, the temperature is lowered to 10°C to obtain substance B;

[0083] 104: A pyrrolidone-based compound is added to substance B, and after stirring and uniformity, extrusion molding, low-temperature freezing, and vacuum freeze-drying are sequentially performed, to obtain a biodegradable polysaccharide-based fiber filter, the temperature of the low-temperature freezing being -5°C.

[0084] Example 6

[0085] Example 6 differs from Example 5 in that, in step 104, the temperature of the low-temperature freezing is -20°C.

[0086] Example 7

[0087] Example 7 differs from Example 5 in that, in step 104, the temperature of the low-temperature freezing is -40°C.

[0088] Example 8

[0089] Example 8 differs from Example 5 in that, in step 104, the temperature of the low-temperature freezing is -60°C.

[0090] Comparative Example 1:

[0091] The difference between Comparative Example 1 and Example 5 is that the temperature of the low-temperature freezing in step 104 is 0℃.

[0092] Comparative Example 2:

[0093] The difference between Comparative Example 2 and Example 5 is that the temperature of the low-temperature freezing in step 104 is -70℃.

[0094] The above Examples 5 to 8 and Comparative Examples 1 to 2 are detected according to GB / T 19609-2004 Determination of total particulate matter and tar for cigarettes using a smoking machine, GB / T 23203.1-2013 Determination of moisture in total particulate matter of cigarettes, GB / T 23355-2009 Determination of nicotine in total particulate matter of cigarettes-Gas chromatographic method, and GB / T 23356-2009 Determination of carbon monoxide in the gas phase of cigarette smoke-Non-dispersive infrared method. The detection instruments used include RM200A rotary smoking machine, RM200A2 rotary smoking machine, and HP7890 gas chromatograph.

[0095] The tobacco control sample is a commercially available cigarette.

[0096] The detection results are shown in Table 2:

[0097] Table 2

[0098]

[0099]

[0100] From the above test data, when the freezing temperature is higher than 0 to -5℃, large cracks appear in the aerogel cross section, the smoke trapping effect is too poor, and the aerogel cannot be formed when the freezing temperature is higher than 0℃; when the freezing temperature is lower than -60℃, the suction resistance of the aerogel is too large, and the smoke cannot pass through.

[0101] Therefore, the temperature of the low-temperature freezing is set to -5 to -60℃. The growth of ice crystals can be controlled by the freezing temperature, so as to control the appearance of the cross section and the suction resistance of the mandrel.

[0102] According to the tar test data of Examples 5 to 8 and the tobacco control sample, it is calculated that the tar content of Example 5 is reduced by 5.28% compared with the tobacco control sample, the tar content of Example 6 is reduced by 7.13%, the tar content of Example 7 is reduced by 11.27%, and the tar content of Example 8 is reduced by 15.14%. It can be seen that the addition of polyvinylpyrrolidone under different freezing temperatures can effectively reduce the tar in the smoke of traditional cigarettes and has a good adsorption effect on the tar in the smoke, thereby reducing the harm of tar in the smoke.

[0103] In the description of the present application, it should be noted that the terms "upper", "lower", and the like are used for indicating the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application. Unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connecting" should be interpreted broadly, for example, can be fixed connection, can also be detachable connection, or integrally connected; can be mechanical connection, can also be electrical connection; can be directly connected, can also be indirectly connected through an intermediate medium, can be the internal communication of two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0104] It should be noted that in the present application, relational terms such as "first" and "second", and the like are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply that there is any such actual relationship or order between these entities or operations. Moreover, the terms "comprising", "including" or any other variant thereof are intended to cover non-exclusive inclusion, so that a process, method, article or apparatus including a series of elements includes not only those elements, but also other elements not explicitly listed, or other elements inherent in such a process, method, article or apparatus. Without more limitations, the element defined by the statement "comprising a" does not exclude the presence of other identical elements in the process, method, article or apparatus including the element.

[0105] The above is only a specific embodiment of the present application, which enables those skilled in the art to understand or implement the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to these embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features applied herein.

Claims

1. A biodegradable polysaccharide-based fiber filter tip, characterized in that: Each 100ml of water contains: 0.1-5g of konjac glucomannan, 0.1-10g of starch, 1-5g of wood pulp fiber, 0.1-10g of agar, 0.01-1g of polyvinyl alcohol, 1-30g of glycerol, and 0.01-2g of functional substances. The functional substances include one or more of pyrrolidone-based compounds and surfactants. The pyrrolidone-based compounds include one or more of polyvinylpyrrolidone and pyrrolidone carboxylates. The surfactants include fatty alcohol polyoxyethylene ether sulfate, fatty alcohol polyoxyethylene ether carboxylates, fatty acid methyl ester sulfonate, sodium secondary alkyl sulfonate, triglyceride monostearate, sodium octyl succinate starch, sodium lauroyl glutamate, and sodium caseinate. The sodium secondary alkyl sulfonate is an alkyl sulfonate containing 12 to 16 carbon atoms. The molecular weight of the polyvinyl alcohol ranges from 25,000 to 250,000. The preparation method of polysaccharide-based fiber filter tip includes the following steps: After dispersing the wood pulp fibers in water, the temperature is lowered to 20~40℃, where the water temperature is 60~100℃; Add konjac glucomannan, starch and agar, stir to dissolve, then add glycerol and heat to 70~95℃ to obtain substance A; Polyvinyl alcohol was added to substance A, and after stirring until homogeneous, the temperature was lowered to 0-40℃ to obtain substance B. Functional substances are added to substance B, and after stirring evenly, the mixture is sequentially extruded, low-temperature frozen, and vacuum freeze-dried to obtain a biodegradable polysaccharide-based fiber filter tip. The low-temperature freezing temperature is -5 to -60°C.

2. The biodegradable polysaccharide-based fiber filter tip as described in claim 1, characterized in that: The average molecular weight of the polyvinylpyrrolidone is 8,000 to 1,300,000.

3. The biodegradable polysaccharide-based fiber filter tip as described in claim 1, characterized in that: The pyrrolidone carboxylates include one or more of sodium 2-pyrrolidone-5-carboxylate, sodium L-pyrrolidone-5-carboxylate, and potassium pyrrolidone carboxylate.

4. The biodegradable polysaccharide-based fiber filter tip as described in claim 1, characterized in that: The wood pulp fiber includes one or more of the following: softwood fiber, broadleaf fiber, grafted cellulose, carboxymethylated cellulose, and hydroxypropylated cellulose.

5. The biodegradable polysaccharide-based fiber filter tip as described in claim 4, characterized in that: The needle fibers include one or more of Masson pine, larch, red pine and spruce; And / or, the broad-leaved fiber includes one or more of birch, poplar, linden, eucalyptus and maple.

6. The biodegradable polysaccharide-based fiber filter tip as described in claim 1, characterized in that: The starch includes one or more of potato starch, corn starch, mung bean starch, grafted starch, and carboxymethylated starch.

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