CN109700072B - Biodegradable composite filter tip material capable of regulating and controlling temperature of cigarette filter tip and preparation method thereof - Google Patents
Biodegradable composite filter tip material capable of regulating and controlling temperature of cigarette filter tip and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a biodegradable composite filter tip material capable of regulating and controlling the temperature of a cigarette filter tip and a preparation method thereof, wherein the biodegradable composite filter tip material is obtained by adding nano particles with high heat conductivity coefficient by taking a high polymer material with excellent biodegradability as a base material; the polymer material is a polymer material PVA with excellent biodegradability; the nano particles are one of BN, AlN and GO. The method can prepare the polymer-based composite material which is cheap, safe, harmless, excellent in heat transfer capacity and suitable for the cigarette filter. The novel cigarette filter tip can effectively reduce the problem of cigarette mainstream smoke, and has the characteristics of low addition, obvious cooling effect, remarkable reduction of harmful substances in smoke and the like.
Description
Technical Field
The invention relates to a biodegradable composite filter tip material capable of regulating and controlling the temperature of a cigarette filter tip and a preparation method thereof, belonging to the technical field of cigarettes.
Background
As a bridge between smokers and smoke, cigarette filters are important media for reducing tar and harm. The aerosol particles released in the burning process of the cigarette are filtered after physical actions such as direct interception, inertial collision, diffusion and deposition and the like in the filter tip, so that the intake of harmful substances by human bodies is reduced. Studies have shown that flue gas temperature has a significant effect on the velocity of intercepted aerosol particles, re-agglomeration of small size particles, condensation deposition of small particles of flue gas species, and the like. Furthermore, researchers have found that smoke temperatures in the filter region can reach as high as 70-80 ℃ in the first 2-3 puffs near the end of a puff, while the temperature at the filter end can even reach over 100 ℃ in the deep-draw mode. Too high filter temperature not only produces great influence to the filter tip to the effect of holding back of flue gas aerosol particulate matter in the filter tip, also can reduce the recognition degree of consumer to flue gas sensory quality simultaneously. Therefore, the effective regulation and control of the smoke temperature of the cigarette filter has an important effect on the improvement of the interception efficiency and the product quality.
For a long time, consumers are used to treat the smoked cigarette butts as garbage, and the smoked cigarette butts are generally directly discarded in the environment. However, the commonly used cellulose acetate and polypropylene-based filter tip materials in the current market are difficult to biodegrade in natural environment, and are easy to cause environmental pollution. In addition, the cellulose acetate filter tip is a chemical product obtained by taking high-quality wood as a raw material and is not easy to regenerate, while the polypropylene filter tip is made of petroleum as a raw material and consumes non-renewable resources. Therefore, from the viewpoint of improving environmental pollution or resource shortage, the development of a novel filter tip material which is continuously regenerated, safe and environment-friendly and has good biodegradability is a problem which needs to be considered and solved by the whole cigarette production industry.
Polyvinyl alcohol (PVA) is a high molecular material with excellent biodegradation performance all the time, and is internationally recognized 100 percent fully biodegradable plastic. The biodegradable plastic has wide sources, can be obtained through an oil route and a coal and natural gas route, is a mature, stable and transparent raw material industrial system, and has obvious price advantage compared with other biodegradable plastics. In addition, PVA has good grease and gas barrier properties, and can block most of gases except water vapor and ammonia gas, various fat substances and chemical solvents, so that PVA can play a role in particularly blocking as a packaging material. Meanwhile, PVA also has the advantages of high strength, high light transmittance, static resistance and the like. At present, no report is found on the preparation of cigarette filter materials by using PVA-based degradable macromolecules.
Generally, the polymer material itself has a low thermal conductivity. Therefore, the temperature of the cigarette filter tip section cannot be well reduced by using a single polymer base material, so that the interception effect of the filter tip on harmful substances in smoke is difficult to further improve. A great deal of research at home and abroad shows that a continuous heat transfer network is formed by adding two-dimensional lamellar nano particles with high heat conductivity coefficient into a matrix, and the heat transfer capability of a high polymer base material can be greatly improved. The physical barrier network formed by the uniformly dispersed nano particles also has a barrier effect on the diffusion of harmful substances generated by the combustion of tobacco, so that the intake of the harmful substances by a human body is reduced. And adding proper nano particles with high thermal conductivity coefficient into the filter base material so as to construct a continuous and uniform heat transfer network. It is beneficial to reduce the smoke temperature of the cigarette and improve the efficiency of intercepting harmful substances. At present, such designs have not been reported.
Disclosure of Invention
Aiming at the outstanding problems that the prior cigarette filter easily causes environmental pollution due to poor biodegradability, and the filter interception effect is poor and the cigarette sensory quality is poor due to overhigh smoke temperature in the cigarette smoking process, the invention provides a biodegradable composite filter material capable of regulating and controlling the temperature of the cigarette filter and a preparation method thereof.
The biodegradable composite filter tip material capable of regulating and controlling the temperature of the cigarette filter tip is prepared by adding nano particles with high heat conductivity coefficient by using a high polymer material with excellent biodegradability as a base material.
The polymer material is preferably PVA which is a polymer material having excellent biodegradability
One or more of (a).
The nano particles are one of BN, AlN and GO.
The mass of the nano particles is 5-50wt% of the mass of the high molecular material.
The preparation method of the biodegradable composite filter tip material capable of regulating and controlling the temperature of the cigarette filter tip comprises the following steps:
step 1: dissolving a high polymer material PVA in deionized water at 65-85 ℃ to prepare a high polymer solution with the concentration of 15-25 wt%;
step 2: in order to improve the dispersion effect of the nano particles with high thermal conductivity in the base material and avoid the formation of serious agglomeration, the nano particles are modified to obtain modified nano particles; the modification process is as follows:
for BN, because few reactive groups (such as hydroxyl groups) exist on the surface of the BN, a non-covalent bond modification method is adopted, and the method specifically comprises the following steps: dispersing a certain amount of BN powder in 500mL of water, carrying out ultrasonic treatment for 8-10h in an CQX25-06 ultrasonic cleaner, then adding a PEI modifier, wherein the mass ratio of BN to PEI modifier is 1:2-4, and continuing ultrasonic treatment for 4 h; and after the reaction is finished, centrifuging to remove the BN which is not peeled off, and performing suction filtration and drying on the obtained filtrate to obtain the modified BN. The PEI modifier is one or a mixture of more of PEI600, PEI1800, PEI10000 and PEI 70000. There is a lewis acid-base interaction between BN and PEI.
For AlN, a surfactant modification method is adopted, and the method specifically comprises the following steps: dispersing proper AlN powder in 200mL of water, carrying out ultrasonic treatment for 8-10h, adding a surfactant, and continuing the ultrasonic treatment for 5h, wherein the mass ratio of AlN to the surfactant is 1: 4-6; after the reaction is finished, removing the AlN which is not peeled off by centrifugation, and filtering and drying the obtained filtrate to obtain the modified AlN. The surfactant is one or a mixture of cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and tetradecyl trimethyl ammonium chloride.
The GO surface contains more hydroxyl active groups, so a silane coupling agent grafting modification method is adopted, and the method specifically comprises the following steps: dispersing a proper amount of GO in 200mL of ethanol, carrying out ultrasonic treatment for 8-10h, then adding a silane coupling agent, wherein the mass ratio of GO to the silane coupling agent is 1:3-5, and continuing to carry out ultrasonic reaction for 5 h; and after the reaction is finished, centrifuging, washing with ethanol and deionized water in sequence, and drying to obtain the modified GO. The silane coupling agent is one or a mixture of more of vinyl triethoxysilane, vinyl trimethoxysilane, vinyl tri (beta-methoxyethoxy) silane and gamma-aminopropyl triethoxysilane.
And step 3: ultrasonically dispersing the modified nano particles in deionized water to obtain uniform dispersion liquid; adding the obtained dispersion liquid into the polymer solution prepared in the step (1), and continuing to perform ultrasonic stirring to uniformly mix the added two particles with the matrix material to obtain a composite solution;
and 4, step 4: and (3) processing the composite solution obtained in the step (3) through electrostatic spinning or double-screw extrusion molding to prepare the filter tip material with high porosity.
And (3) electrostatic spinning is carried out by adding the composite solution obtained in the step (3) into a sample injector of an electrostatic spinning machine, wherein the spinning voltage is 16-22kV, the distance from a spray head to a receiving plate is 9-15cm, and the injection speed is 0.01-0.1 mm/min.
The twin-screw extrusion molding comprises the following steps: and (3) carrying out air drying on the composite solution obtained in the step (3) to obtain a blocky composite material, melting at a high temperature, adding into a double-screw extruder, and carrying out extrusion molding to obtain the filter tip material. In order to increase the contact area between the filter tip and the smoke, a honeycomb-shaped mold is adopted during double-screw extrusion molding to obtain a filter tip material with a special pore channel structure; the parameters of the double-screw extruder are as follows: diameter D is 35mm, length-diameter ratio L/D is 36, coaxial speed is variable, and temperature range: at the temperature of 120 ℃ and 250 ℃, the extrusion speed is 200 r/min.
The filter tip material prepared by the method can be directly used as a cigarette filter tip material.
Compared with the prior art, the invention has the beneficial effects that:
the high molecular filter tip base material adopted by the invention has excellent biodegradability, and the discarded filter tip can be degraded into substances such as carbon dioxide, water and the like under the conditions of enzyme, microorganism and the like, so that the environmental pollution can not be caused; according to the invention, the nano particles with high heat conductivity coefficient are added into the filter tip base material for the first time, and can form a continuous heat conduction network with the nano particles in the base material; the cigarette filter with high specific surface area and porosity can be obtained by adopting electrostatic spinning and extrusion molding processing technologies; the invention prepares a biodegradable polymer-based cigarette filter for the first time, and the filter can effectively control the temperature of the mainstream smoke of the cigarette to be about 40 ℃.
Detailed Description
The following examples are intended to further illustrate the present disclosure, but not to limit the scope of the claims.
Example 1:
1. preparation of modified BN: 0.5g of BN is taken and dispersed in 200mL of water, and ultrasonic treatment is carried out for 8-10 h. Then 1.5g of PEI-10000 is added, and the ultrasonic treatment is continued for 5 h. After the reaction was completed, the unpeeled BN was removed by centrifugation at 3500 rpm. And carrying out suction filtration on the filtrate, and drying to obtain a final product.
2. Preparing a composite polymer solution: adding a proper amount of modified BN into 100mL of water, and continuously carrying out ultrasonic treatment for 6-8h to obtain a dispersion liquid A. Weighing a certain amount of PVA master batch, completely dissolving the PVA master batch in 100mL of water, heating to 75 ℃, and ultrasonically stirring uniformly to obtain a solution B, wherein the concentration of the PVA master batch is 15 wt%. Adding the solution B into the solution A, and continuing to perform ultrasonic treatment for 4 hours to uniformly mix the two added particles with the matrix. The amount of modified nanoparticles was 5wt% of the polymer.
3. Composite filter tip material forming
Electrostatic spinning preparation of cigarette filter tip material: 10mL of the composite solution was taken and added to a sample injector of an electrospinning machine to carry out electrospinning. The spinning voltage is 18kV, the distance from the nozzle to the receiving plate is 13cm, and the injection speed is 0.1 mm/min.
Preparing a filter tip material with a special pore structure: and drying the composite solution at 70 ℃ to obtain the blocky composite material. Melting the obtained block at the high temperature of 125 ℃, and extruding and cooling the block by using a double-screw extruder and a honeycomb briquette-shaped die to obtain the composite filter tip material.
Example 2:
1. preparation of modified BN: 0.5g of BN is taken and dispersed in 200mL of water, and ultrasonic treatment is carried out for 8-10 h. Then 2.0g of PEI-12000 was added and sonication continued for 5 h. After the reaction was completed, the unpeeled BN was removed by centrifugation at 3500 rpm. And carrying out suction filtration on the filtrate, and drying to obtain a final product.
2. Preparing a composite polymer solution: adding a proper amount of modified BN into 100mL of water, and continuously carrying out ultrasonic treatment for 6-8h to obtain a dispersion liquid A. Weighing a certain amount of PVA master batch, completely dissolving the PVA master batch in 100mL of water, heating to 75 ℃, and ultrasonically stirring uniformly to obtain a solution B, wherein the concentration of the PVA master batch is 18 wt%. Adding the solution B into the solution A, and continuing to perform ultrasonic treatment for 4 hours to uniformly mix the two added particles with the matrix. The amount of the modified nanoparticles is 10 wt% of the amount of the polymer.
3. Composite filter tip material forming
Electrostatic spinning preparation of cigarette filter tip material: 10mL of the composite solution was taken and added to a sample injector of an electrospinning machine to carry out electrospinning. The spinning voltage is 19kV, the distance from the nozzle to the receiving plate is 12cm, and the injection speed is 0.08 mm/min.
Preparing a filter tip material with a special pore structure: and drying the composite solution at 70 ℃ to obtain the blocky composite material. Melting the obtained block at the high temperature of 125 ℃, and extruding and cooling the block by using a double-screw extruder and a honeycomb briquette-shaped die to obtain the composite filter tip material.
Example 3:
1. preparing modified AlN: 0.5g of AlN is taken and dispersed in 200mL of water, and ultrasonic treatment is carried out for 8-10 h. Thereafter, 2.5g of cetyltrimethylammonium bromide was added and sonication was continued for 5 h. After the reaction, AlN that had not been peeled off was removed by centrifugation at 3500 rpm. And carrying out suction filtration on the filtrate, and drying to obtain a final product.
2. Preparing a composite polymer solution: adding a proper amount of modified AlN into 100mL of water, and continuously carrying out ultrasonic treatment for 6-8h to obtain a dispersion liquid A. Weighing a certain amount of PVA master batch, completely dissolving the PVA master batch in 100mL of water, heating to 65 ℃ and uniformly stirring by ultrasonic to obtain a solution B, wherein the concentration of the PVA master batch is 15 wt%. Adding the solution B into the solution A, and continuing to perform ultrasonic treatment for 4 hours to uniformly mix the two added particles with the matrix. The amount of modified nanoparticles was 5wt% of the polymer.
3. Composite filter tip material forming
Electrostatic spinning preparation of cigarette filter tip material: 10mL of the composite solution was taken and added to a sample injector of an electrospinning machine to carry out electrospinning. Spinning voltage is 17kV, the distance from the nozzle to the receiving plate is 15cm, and the injection speed is 0.1 mm/min.
Preparing a filter tip material with a special pore structure: and drying the composite solution at 70 ℃ to obtain the blocky composite material. And melting the obtained block at 185 ℃, and extruding and cooling by using a double-screw extruder and a honeycomb briquette-shaped die to obtain the composite filter tip material.
Example 4:
1. preparing modified AlN: 0.5g of AlN is taken and dispersed in 200mL of water, and ultrasonic treatment is carried out for 8-10 h. Then 2.0g of sodium dodecyl sulfate was added and sonication was continued for 5 h. After the reaction, AlN that had not been peeled off was removed by centrifugation at 3500 rpm. And carrying out suction filtration on the filtrate, and drying to obtain a final product.
2. Preparing a composite polymer solution: adding a proper amount of modified AlN into 100mL of water, and continuously carrying out ultrasonic treatment for 6-8h to obtain a dispersion liquid A. Weighing a certain amount of PVA master batch, completely dissolving the PVA master batch in 100mL of water, heating to 65 ℃ and uniformly stirring by ultrasonic to obtain a solution B, wherein the concentration of the PVA master batch is 18 wt%. Adding the solution B into the solution A, and continuing to perform ultrasonic treatment for 4 hours to uniformly mix the two added particles with the matrix. The amount of the modified nanoparticles is 10 wt% of the amount of the polymer.
3. Composite filter tip material forming
Electrostatic spinning preparation of cigarette filter tip material: 10mL of the composite solution was taken and added to a sample injector of an electrospinning machine to carry out electrospinning. The spinning voltage is 18kV, the distance from the nozzle to the receiving plate is 16cm, and the injection speed is 0.12 mm/min.
Preparing a filter tip material with a special pore structure: and drying the composite solution at 70 ℃ to obtain the blocky composite material. And melting the obtained block at 185 ℃, and extruding and cooling by using a double-screw extruder and a honeycomb briquette-shaped die to obtain the composite filter tip material.
Example 5:
1. preparing modified GO: 0.5g of GO is taken and dispersed in 200mL of ethanol, and ultrasonic treatment is carried out for 8-10 h. Thereafter, 2.0g of vinyltriethoxysilane was added and sonication was continued for 5 h. After the reaction is finished, centrifuging at 3500rpm, washing with ethanol and deionized water, and drying to obtain the final product.
2. Preparing a composite polymer solution: adding a proper amount of modified GO into 100mL of water, and continuously performing ultrasonic treatment for 6-8h to obtain a dispersion A. Weighing a certain amount of PVA master batch, completely dissolving the PVA master batch in 100mL of water, heating to 85 ℃, and ultrasonically stirring uniformly to obtain a solution B, wherein the concentration of the PVA master batch is 15 wt%. Adding the solution B into the solution A, and continuing to perform ultrasonic treatment for 4 hours to uniformly mix the two added particles with the matrix. The amount of modified nanoparticles was 5wt% of the polymer.
3. Composite filter tip material forming
Electrostatic spinning preparation of cigarette filter tip material: 10mL of the composite solution was taken and added to a sample injector of an electrospinning machine to carry out electrospinning. The spinning voltage is 18kV, the distance from the nozzle to the receiving plate is 15cm, and the injection speed is 0.1 mm/min.
Preparing a filter tip material with a special pore structure: and drying the composite solution at 70 ℃ to obtain the blocky composite material. And melting the obtained block at the high temperature of 150 ℃, and extruding and cooling by using a double-screw extruder and a honeycomb briquette-shaped die to obtain the composite filter tip material.
Example 6:
1. preparing modified GO: 0.5g of GO is taken and dispersed in 200mL of ethanol, and ultrasonic treatment is carried out for 8-10 h. Then 2.5g gamma-aminopropyl triethoxysilane was added and sonication continued for 5 h. After the reaction is finished, centrifuging at 3500rpm, washing with ethanol and deionized water, and drying to obtain the final product.
2. Preparing a composite polymer solution: adding a proper amount of modified GO into 100mL of water, and continuously performing ultrasonic treatment for 6-8h to obtain a dispersion A. Weighing a certain amount of PVA master batch, completely dissolving the PVA master batch in 100mL of water, heating to 85 ℃, and ultrasonically stirring uniformly to obtain a solution B, wherein the concentration of the PVA master batch is 18 wt%. Adding the solution B into the solution A, and continuing to perform ultrasonic treatment for 4 hours to uniformly mix the two added particles with the matrix. The amount of the modified nanoparticles is 10 wt% of the amount of the polymer.
3. Composite filter tip material forming
Electrostatic spinning preparation of cigarette filter tip material: 10mL of the composite solution was taken and added to a sample injector of an electrospinning machine to carry out electrospinning. The spinning voltage is 19kV, the distance from the nozzle to the receiving plate is 16cm, and the injection speed is 0.12 mm/min.
Preparing a filter tip material with a special pore structure: and drying the composite solution at 70 ℃ to obtain the blocky composite material. And melting the obtained block at the high temperature of 150 ℃, and extruding and cooling by using a double-screw extruder and a honeycomb briquette-shaped die to obtain the composite filter tip material.
The filter material obtained in example 2 showed better effect of lowering smoke temperature than in example 1, because the addition of more heat-conductive BN particles favoured the formation of a continuous and efficient heat transfer network in the matrix, thus providing a good heat evacuation. The continuous BN network can also provide more effective barrier effect, which is beneficial to the interception of harmful substances to the smoke. Likewise, by comparing examples 3, 4 and 5, 6, it can be found that the composite filter materials with high particle addition amount all show better effects of cooling down and trapping harmful substances. By comparing examples 2, 4, 6, it can be seen that the filter material containing graphite oxide nanoparticles has the best cooling effect at the same addition level, probably because graphite oxide itself has a higher thermal conductivity. Furthermore, the filter material containing graphite oxide also exhibits the best retention of harmful substances, probably due to its large lamella size and abundant surface functional groups.
Claims (2)
1. A preparation method of a biodegradable composite filter tip material is characterized by comprising the following steps:
step 1: dissolving a high polymer material PVA in deionized water at 65-85 ℃ to prepare a high polymer solution with the concentration of 15-25 wt%;
step 2: in order to improve the dispersion effect of the nano particles with high thermal conductivity in the base material and avoid the formation of serious agglomeration, the nano particles are modified to obtain modified nano particles;
and step 3: ultrasonically dispersing the modified nano particles in deionized water to obtain uniform dispersion liquid; adding the obtained dispersion liquid into the polymer solution prepared in the step (1), and continuing to perform ultrasonic stirring to uniformly mix the added two particles with the matrix material to obtain a composite solution;
and 4, step 4: processing the composite solution obtained in the step (3) through electrostatic spinning or double-screw extrusion molding to prepare a filter tip material with high porosity;
the high polymer material is one or more of Mowiol PVA-210, Mowiol PVA-105, Mowiol PVA-224, Mowiol PVA-203, Mowiol PVA-117 and Mowiol PVA-103;
the nano particles are one of BN, AlN and GO; the mass of the nano particles is 5-50wt% of that of the high molecular material;
the modified nano-particle is prepared by the method comprising the following steps:
for BN, a non-covalent bond modification method is adopted, a certain amount of BN powder is dispersed in 500mL of water, ultrasonic treatment is carried out for 8-10h, then PEI modifier is added, the mass ratio of BN to PEI modifier is 1:2-4, and ultrasonic treatment is continued for 4 h; after the reaction is finished, centrifuging to remove the BN which is not peeled off, and carrying out suction filtration and drying on the obtained filtrate to obtain modified BN; the PEI modifier is one or a mixture of more of PEI600, PEI1800, PEI10000 and PEI 70000;
for AlN, a surfactant modification method is adopted, a proper amount of AlN powder is dispersed in 200mL of water, ultrasonic treatment is carried out for 8-10h, then a surfactant is added, the mass ratio of AlN to the surfactant is 1:4-6, and the ultrasonic treatment is continued for 5 h; after the reaction is finished, centrifuging to remove the AlN which is not stripped, and filtering and drying the obtained filtrate to obtain modified AlN; the surfactant is one or a mixture of cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and tetradecyl trimethyl ammonium chloride;
for GO, a silane coupling agent grafting modification method is adopted, a proper amount of GO is dispersed in 200mL of ethanol, ultrasonic treatment is carried out for 8-10h, then a silane coupling agent is added, the mass ratio of GO to the silane coupling agent is 1:3-5, and ultrasonic reaction is continued for 5 h; centrifuging after the reaction is finished, washing with ethanol and deionized water in sequence, and drying to obtain modified GO; the silane coupling agent is one or a mixture of more of vinyl triethoxysilane, vinyl trimethoxysilane, vinyl tri (beta-methoxyethoxy) silane and gamma-aminopropyl triethoxysilane;
the electrostatic spinning is to add the composite solution obtained in the step (3) into a sample injector of an electrostatic spinning machine for electrostatic spinning, wherein the spinning voltage is 16-22kV, the distance from a nozzle to a receiving plate is 9-15cm, and the injection speed is 0.01-0.1 mm/min;
the twin-screw extrusion molding comprises the following steps: blowing and drying the composite solution obtained in the step 3 to obtain a blocky composite material, melting at a high temperature, adding the blocky composite material into a double-screw extruder, and performing extrusion molding to obtain a filter tip material; the parameters of the double-screw extruder are as follows: diameter D =35mm, aspect ratio L/D =36, variable speed of coaxial shaft, temperature range: at the temperature of 120 ℃ and 250 ℃, the extrusion speed is 200 r/min.
2. The method of claim 1, wherein:
when the double screw extrusion molding is carried out, a honeycomb-shaped die is adopted.
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| CN111304765A (en) * | 2020-03-30 | 2020-06-19 | 安徽中烟工业有限责任公司 | Carbon/phase-change material composite membrane for reducing mainstream smoke temperature of cigarette filter and preparation method thereof |
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| US20120000481A1 (en) * | 2010-06-30 | 2012-01-05 | Dennis Potter | Degradable filter element for smoking article |
| GB201400990D0 (en) * | 2014-01-21 | 2014-03-05 | British American Tobacco Co | Filter materials and filters made therefrom |
| CN104389234B (en) * | 2014-09-12 | 2017-02-15 | 河南中烟工业有限责任公司 | Cigarette filter tip added with chitosan-graphene oxide composite material |
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