CN111543672B - Preparation method of novel filter stick capable of reducing release amount of phenol in smoke and filter stick product - Google Patents
Preparation method of novel filter stick capable of reducing release amount of phenol in smoke and filter stick product Download PDFInfo
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- CN111543672B CN111543672B CN202010435004.8A CN202010435004A CN111543672B CN 111543672 B CN111543672 B CN 111543672B CN 202010435004 A CN202010435004 A CN 202010435004A CN 111543672 B CN111543672 B CN 111543672B
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/02—Manufacture of tobacco smoke filters
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/02—Manufacture of tobacco smoke filters
- A24D3/0229—Filter rod forming processes
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/08—Use of materials for tobacco smoke filters of organic materials as carrier or major constituent
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
Abstract
A method for preparing a novel filter stick capable of reducing the release amount of phenol in smoke and a filter stick product are provided, wherein the novel filter stick capable of reducing the release amount of phenol in smoke is directly prepared in a specific filter stick mould through high internal phase emulsion polymerization. Compared with the conventional common tow filter stick, the tow is prepared firstly and then the tow is formed into the filter stick by filter stick forming equipment, so that the filter stick is substantially different. The novel filter stick can be directly formed into a filter stick in a mould, has certain strength and can meet the requirement of cigarette connection; the prepared novel filter stick is provided with a large hole with a micron size, and the smoke can be transmitted by the communication of the hole and the hole; iron oxide nanoparticles are used as a particle emulsifier, iron ions and epoxy groups can react with phenol, so that the release amount of phenol in smoke is reduced, and the strength of the filter stick can be increased; the particle emulsifier is modified by a modifier, and the modifier has polymerizable double bonds and is beneficial to the polymerization of high internal phase emulsion; adopts a radiation polymerization method, does not add a chemical initiator, and has the functions of disinfection and sterilization.
Description
Technical Field
The invention belongs to the technical field of filter stick preparation, and particularly relates to a preparation method of a novel filter stick prepared by high internal phase emulsion polymerization and a filter stick product.
Background
Phenol is one of main harmful components in cigarette main stream smoke, volatile phenol compounds in the cigarette smoke are mainly generated in the burning process of cigarettes, and the research on cigarette harmfulness index system finds that phenol is one of the most main harmful components influencing the harmfulness of the cigarette main stream smoke by researching the relation between the release amount of the harmful components and the biological activity of the smoke, so that the reduction of the phenol content in the cigarette smoke has important significance for reducing the harmfulness of the cigarettes.
Many related researches are also carried out at home and abroad on how to reduce phenol in the cigarette smoke. Chitosan-Fe was studied in the agricultural science of Anhui, 2009(10) 4371-43722+The complex has strong adsorption effect on harmful components in the smoke, which shows that the complex has strong adsorption effect on moisture, phenol and HCN in the smoke. The CN 101531779 patent researches a macroporous and microporous hybrid starch granule, and the macroporous and microporous hybrid starch granule is added into a filter element of a cigarette filter to prepare a binary or ternary composite filter, so that the delivery amount of tar, phenol, hydrocyanic acid and carbon monoxide in smoke can be effectively reduced. In the patent CN101015394A, common expanded activated carbon fibers are used as carriers, aluminum nitrate or ferric nitrate or the mixture of the aluminum nitrate and the ferric nitrate with different amounts is dispersed on the carriers by an expanding and dipping method, and modified activated carbon fibers with different loading amounts of Al2O3, Fe2O3 and Al2O3-Fe2O3 are prepared by roasting to prepare composite filter tips, which can reduce tar, phenol, pyrocatechol, hydroquinone, resorcinol, p-m-cresol, O-cresol and the like in smoke. The CN 101664228A selects a deep-cavity calixarene compound as an additive material, and can simultaneously selectively reduce benzo [ a ] in the cigarette smoke by utilizing the molecular recognition effect and the cavity size selection effect of the calixarene compound]Pyrene and phenol emissions. The patent CN 101433818A invents a novel mesoporous material for adsorbing tar, phenol, tobacco-specific nitrosamine and the like in cigarette mainstream smoke. The mesoporous material is a mesoporous molecular sieve with 3-dimensional network microstructure and monolithic morphology, such as SBA-15, or a three-dimensional network microstructure and monolithic morphology SBA-15 mesoporous molecular sieve material which is plated with a liquid film or modified by metal oxide, such as zirconia. CN101919589A, CN101974124A, CN101919591A, CN101961646A and the like invent a series of high molecular additives for reducing the phenolic substances in the smoke of cigarettes. Such additivesThe additive is used for selectively reducing harmful substances of phenols in the smoke of the cigarettes by utilizing moisture in the material. U.S. patent (US6779529) discloses a cigarette filter comprising a fibrous filter segment, a selective adsorbent segment and a general adsorbent segment coaxially connected in series, wherein the selective adsorbent segment is formed by functionalizing a phenolic resin matrix with primary and secondary amines, and the filter is capable of removing specific components such as phenol from smoke. CN102617782B is polymerized by high internal phase emulsion of Methyl Methacrylate (MMA) to obtain an intercommunicated porous material (PolyMMA) of polymethyl methacrylate with ester functional groups, wherein the raw materials comprise methyl methacrylate, a cross-linking agent, a pore-foaming agent, an emulsifier, water, inorganic salt and an initiator; the material can effectively adsorb harmful substance phenol in the smoke. The material is added into a cigarette filter stick at a dose of 10-30mg per cigarette, so that the phenol release amount in the mainstream smoke of the cigarette can be selectively reduced by more than 25%, the tar release amount is basically unchanged or slightly reduced, and the smoking quality of the cigarette is not negatively affected, thereby achieving the purpose of selectively reducing the phenol release amount in the smoke of the cigarette. CN106632847B relates to a composite surface molecularly imprinted material capable of selectively reducing the release amount of phenol in cigarette mainstream smoke and a patent application of a preparation method thereof. The material is prepared by taking a gamma-MPS modified molecular sieve as a carrier, phenol as a template molecule, 4-Vpy as a functional monomer, AIBN as an initiator and EGDMA as a cross-linking agent through a hydrothermal synthesis method. The specific phenol adsorbent prepared by the invention has the recognition sites fixed on the surface of a molecular sieve carrier material, is beneficial to eluting and recognizing template molecules, and has the advantages of stable mechanical property, high mass transfer rate, good dispersibility, uniform particle size distribution and the like, thereby having high selectivity on phenol.
At present, the cigarette generally adopts a filter stick of a diacetate fiber tow and a filter stick of a polypropylene tow as filter tips. The two filter sticks are prepared by firstly preparing a diacetate fiber tow and a polypropylene tow, and then forming the diacetate fiber tow and the polypropylene tow into a filter stick (the diameter is generally 7.7 mm) for a conventional cigarette, a filter stick (the diameter is generally 7.0mm or 6.0 mm) for a medium cigarette or a filter stick (the diameter is 5.4 mm) for a fine cigarette by a filter stick forming device. However, the filter stick needs to be prepared into tows firstly and then formed into the filter stick, and the steps are complicated.
Polymer-interconnected porous materials (PolyHIPE) are prepared by mixing a high internal phase emulsion (HIPE, also known as an ultra-concentrated emulsion, the volume fraction of the dispersed phase is more than 74 percent, the liquid drops are mutually extruded to form polyhedral vacuoles separated by a continuous phase film containing a surfactant, and the continuous phase monomer is polymerized to obtain the interconnected porous material, wherein the polymer interconnected porous material usually contains three pores: (1) the pores formed by the dispersed phase template are called "cells" (void), and the pore diameter is in the micron order; (2) the pores formed between two adjacent cells are called window holes (windows), the pore diameter is in micron order, and the pores are communicated with each other; (3) the pores formed on the walls of the cells by adding a porogen to the continuous phase monomer are called "pores" (pores), the pore size is on the nanometer scale, and the existence of the pores greatly increases the surface area of the polymer interconnected porous material.
Thus, the polymer interconnected porous material has good potential to be a novel filter rod.
Disclosure of Invention
The invention aims to provide a preparation method of a novel filter stick capable of reducing the release amount of phenol in smoke based on the prior art, and the novel filter stick capable of reducing the release amount of phenol in smoke is directly prepared in a specific filter stick mould through high internal phase emulsion polymerization.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a novel filter stick capable of reducing phenol release amount comprises the following specific steps:
(1) firstly preparing an oil phase, wherein the specific components and the mixture ratio are as follows: 2-8 ml of glycidyl methacrylate, 1-3 ml of methyl methacrylate, 1-3 ml of 2-ethylhexyl acrylate, 0-3 ml of hydrophilic monomer acrylic acid, 0.5-5 ml of cross-linking agent and 1-10 g of particle emulsifier; (wherein glycidyl methacrylate, methyl methacrylate and 2-ethylhexyl acrylate are all polymerized monomers which polymerize to form a polymer, and the hydrophilic monomer acrylic acid is mainly used for increasing the cell diameter)
(2) Then preparing a water phase, wherein the specific components and the mixture ratio are as follows: 40-90 ml of water and 0.1-1.5 g of inorganic salt;
(3) slowly adding the water phase into the oil phase at 500-700 rpm to form a high internal phase emulsion, transferring the high internal phase emulsion into a filter stick mold with the diameter of 7.7mm or 7.0mm or 6.0mm or 5.4mm and the length of 100mm or 120mm or 144mm, introducing nitrogen for 10-20 min, and sealing;
(4) radiation-induced polymerization was used to place the above-described mold containing the high internal phase emulsion into a 1.3X 1015 Bq 60In a Co source, the dosage rate is 20-80 Gy/min, and the irradiation time is 24-48 h;
(5) respectively extracting the filter stick-shaped solid product obtained in the step (4) with water and ethanol for 24 hours, and drying in a vacuum oven;
the cross-linking agent is ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate or glycerol tri (alpha-methacrylate).
The particle emulsifier is ferric oxide nano particles with the surface modified by a modifier, and the ferric oxide nano particles are prepared by a coprecipitation method.
The modifier is prepared by opening double bonds in oleic acid to generate dihydroxy, and then carrying out esterification reaction with acrylic acid. The specific reaction equation is as follows:
the inorganic salt is calcium chloride, sodium chloride or magnesium sulfate.
The filter stick product prepared by the method is of a hard structure and is formed by injection molding or pouring in a mold, the filter stick is provided with micron-sized large holes, the holes are communicated with each other, cigarette smoke can be transmitted, and iron ions and epoxy groups can react with phenol to reduce the release amount of phenol in the smoke.
The novel filter stick provided by the invention has the following advantages:
(1) the filter stick with the target circumference and length can be directly formed in a filter stick preparation mould, has certain strength, meets the requirement of cigarette tipping, and has simple and convenient preparation steps;
(2) the material has micron-sized macropores which are communicated with each other, so that the smoke transmission is facilitated;
(3) the iron oxide nanoparticles are used as the particle emulsifier, so that on one hand, iron ions and epoxy groups can react with phenol to reduce the release amount of phenol in smoke, and on the other hand, the strength of the filter stick can be increased;
(4) the filter stick contains the epoxy functional group, and the release amount of phenol can be reduced by the interaction of the epoxy group and the phenol.
(5) Adopts a radiation polymerization method, does not add a chemical initiator, and has the functions of disinfection and sterilization.
Detailed Description
The following examples further illustrate the essence of the present invention, but the present invention is not limited thereto.
Example 1
An oil phase consisting of 5ml of glycidyl methacrylate, 2ml of methyl methacrylate, 1ml of 2-ethylhexyl acrylate, 0.5ml of ethylene glycol dimethacrylate and 2.4g of modifier-modified iron oxide nanoparticles was prepared first, and an aqueous phase consisting of 64ml of water and 0.5g of calcium chloride was prepared. Slowly adding the water phase into the oil phase under high-speed stirring at 500rpm to form high internal phase emulsion, pouring into a filter stick forming mold with diameter of 7.7mm and length of 100mm, introducing nitrogen for 10min, and sealing. Then put it into 1.3X 1015 Bq 60In the Co source, the dosage rate is 36Gy/min, and the irradiation time is 24 h. And respectively extracting the obtained solid products for 24 hours by using water and ethanol, and drying in a vacuum oven to obtain the final filter stick. When the obtained filter stick is used for cigarette loading, compared with the cigarette without the filter stick, the reduction rate of the phenol release amount of the main stream smoke reaches 32.3%.
Example 2
First preparedThe oil phase was placed with 4ml of glycidyl methacrylate, 1ml of methyl methacrylate, 0.5ml of 2-ethylhexyl acrylate, 0.5ml of acrylic acid, 3ml of trimethylolpropane trimethacrylate, 3g of modifier-modified iron oxide nanoparticles, and then the aqueous phase was prepared with 60ml of water and 0.5g of sodium chloride. Slowly adding the water phase into the oil phase under high-speed stirring at 500rpm to form high internal phase emulsion, pouring into a filter stick forming mold with diameter of 7.0mm and length of 120mm, introducing nitrogen for 10min, and sealing. Then put it into 1.3X 1015 Bq 60In the Co source, the dosage rate is 36Gy/min, and the irradiation time is 36 h. And respectively extracting the obtained solid products for 24 hours by using water and ethanol, and drying in a vacuum oven to obtain the final filter stick.
Example 3
An oil phase consisting of 5ml of glycidyl methacrylate, 2ml of methyl methacrylate, 1ml of 2-ethylhexyl acrylate, 1ml of glycerol tri (. alpha. -methacrylic acid) ester and 4g of modifier-modified iron oxide nanoparticles was prepared, and then an aqueous phase consisting of 70ml of water and 1.5g of magnesium sulfate was prepared. Slowly adding the water phase into the oil phase under high-speed stirring at 700rpm to form high internal phase emulsion, pouring into a filter stick forming die with diameter of 6.0mm and length of 120mm, introducing nitrogen for 10min, and sealing. Then put it into 1.3X 1015 Bq 60In the Co source, the dosage rate is 36Gy/min, and the irradiation time is 36 h. And respectively extracting the obtained solid products for 24 hours by using water and ethanol, and drying in a vacuum oven to obtain the final filter stick.
Example 4
An oil phase is prepared, wherein the oil phase comprises 6ml of glycidyl methacrylate, 2ml of methyl methacrylate, 2ml of 2-ethylhexyl acrylate, 1ml of glycerol tri (alpha-methacrylic acid) ester and 4g of modifier modified iron oxide nanoparticles, and then an aqueous phase comprises 70ml of water and 1.5g of magnesium sulfate. Slowly adding the water phase into the oil phase under high-speed stirring at 700rpm to form high internal phase emulsion, pouring into a filter stick forming die with diameter of 5.4mm and length of 120mm, introducing nitrogen for 10min, and sealing. . Then put it into 1.3X 1015 Bq 60In a Co source, the dose rate is36Gy/min and 48h of irradiation time. And respectively extracting the obtained solid products for 24 hours by using water and ethanol, and drying in a vacuum oven to obtain the final filter stick.
Example 5
An oil phase consisting of 6ml of glycidyl methacrylate, 2ml of methyl methacrylate, 1ml of 2-ethylhexyl acrylate, 0.5ml of ethylene glycol dimethacrylate and 4g of modifier-modified iron oxide nanoparticles was prepared, and an aqueous phase consisting of 64ml of water and 0.5g of calcium chloride was prepared. Slowly adding the water phase into the oil phase under high-speed stirring at 500rpm to form high internal phase emulsion, pouring into a filter stick forming mold with diameter of 7.7mm and length of 144mm, introducing nitrogen for 10min, and sealing. Then put it into 1.3X 1015 Bq 60In the Co source, the dosage rate is 36Gy/min, and the irradiation time is 24 h. And respectively extracting the obtained solid products for 24 hours by using water and ethanol, and drying in a vacuum oven to obtain the final filter stick.
TPM, tar and phenol release amount in main stream smoke of surface cigarette respectively connected with acetate fiber filter stick and filter stick in application
| TPM (mg/count) | Tar (mg/count) | Phenol (microgram/count) | |
| Acetate fibre filter stick | 13.2 | 11.2 | 12.6 |
| Novel filter stick capable of reducing phenol release amount | 13.9 | 11.8 | 8.9 |
| Rate of decrease | -5.3% | -5.4% | 32.5% |
The results in the table show that after the cigarette is connected with the low smoke filtration efficiency filter stick, the filtration efficiency of the cigarette on smoke is reduced, and the release amount of TPM, tar and nicotine in main stream smoke is increased.
Claims (4)
1. A preparation method of a novel filter stick capable of reducing the release amount of phenol in cigarette smoke is characterized by comprising the following steps: the method comprises the following specific steps:
(1) firstly preparing an oil phase, wherein the specific composition and the specific mixture ratio are as follows: 2-8 ml of glycidyl methacrylate, 1-3 ml of methyl methacrylate, 1-3 ml of 2-ethylhexyl acrylate, 0-3 ml of hydrophilic monomer acrylic acid, 0.5-5 ml of cross-linking agent and 1-10 g of particle emulsifier; the particle emulsifier is iron oxide nanoparticles with the surface modified by a modifier, and the modifier is prepared by the following method: opening double bonds in oleic acid to generate dihydroxy, and then carrying out esterification reaction with acrylic acid to prepare a polymerizable modifier;
(2) then preparing a water phase, wherein the water phase comprises the following specific components in percentage by weight: 40-90 ml of water and 0.1-1.5 g of inorganic salt;
(3) slowly adding the water phase into the oil phase at 500-700 rpm to form a high internal phase emulsion, transferring the high internal phase emulsion into a filter stick mold with the diameter of 7.7mm or 7.0mm or 6.0mm or 5.4mm and the length of 100mm or 120mm or 144mm, introducing nitrogen for 10-20 min, and sealing;
(4) radiation-induced polymerization was used to place the above-described mold containing the high internal phase emulsion into a 1.3X 1015 Bq 60 CIn the o source, the dosage rate is 20-80 Gy/min, and the irradiation time is 24-48 h;
(5) and (4) respectively extracting the filter stick-shaped solid product obtained in the step (4) with water and ethanol for 24 hours, and drying in a vacuum oven.
2. The preparation method of a novel filter stick according to claim 1, which is characterized in that: the cross-linking agent is ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate or glycerol tri (alpha-methacrylate).
3. The preparation method of a novel filter stick according to claim 1, which is characterized in that: the inorganic salt is calcium chloride, sodium chloride or magnesium sulfate.
4. A novel filter stick product capable of reducing the release amount of phenol in cigarette smoke prepared by the method according to any one of claims 1 to 3, wherein the novel filter stick product is characterized in that: the filter stick product is of a hard structure and is formed by injection molding or pouring in a mold, the filter stick is provided with micron-sized large holes, the holes are communicated with each other, cigarette smoke can be transmitted, and iron ions and epoxy groups can react with phenol to reduce the release amount of phenol in the smoke.
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