CN111387545B - Preparation method of novel filter stick capable of reducing release amount of crotonaldehyde in smoke - Google Patents
Preparation method of novel filter stick capable of reducing release amount of crotonaldehyde in smoke Download PDFInfo
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- CN111387545B CN111387545B CN202010390984.4A CN202010390984A CN111387545B CN 111387545 B CN111387545 B CN 111387545B CN 202010390984 A CN202010390984 A CN 202010390984A CN 111387545 B CN111387545 B CN 111387545B
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- filter stick
- crotonaldehyde
- smoke
- release amount
- reducing
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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
- A24D3/0204—Preliminary operations before the filter rod forming process, e.g. crimping, blooming
-
- 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
- A24D3/02—Manufacture of tobacco smoke filters
- A24D3/0275—Manufacture of tobacco smoke filters for filters with special features
Abstract
The invention relates to a preparation method of a novel filter stick capable of reducing the release amount of crotonaldehyde in smoke. The novel filter stick can be directly formed into a filter stick with specific circumference and length in a filter stick forming die, has certain strength and can meet the requirement of cigarette tipping; the filter stick is provided with a micron-sized large hole, and the holes are communicated with each other, so that cigarette smoke can be transmitted; after the epoxy group reacts with the amination reagent, the filter stick has an amino functional group, so that the release amount of crotonaldehyde in smoke can be reduced; the strength of the filter stick can be improved by adopting the silicon dioxide nano particles as the particle emulsifier; 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 capable of reducing the release amount of crotonaldehyde in smoke.
Background
Crotonaldehyde is one of main harmful components of cigarette mainstream smoke, and by researching the relationship between the release amount of the harmful components and the biological activity of the smoke, the research project of a cigarette harmfulness index system finds that crotonaldehyde is one of the most main harmful components influencing the harmfulness of the cigarette mainstream smoke, so that the reduction of the crotonaldehyde content in the cigarette smoke has important significance for reducing the harmfulness of the cigarette.
Many related researches are also carried out at home and abroad on how to reduce crotonaldehyde in cigarette smoke. Patent CN104941606B discloses an adsorbent for reducing the release amount of crotonaldehyde in cigarette mainstream smoke, which belongs to a molecular sieve-polyether sulfone composite material. Patent CN107286275B discloses an amino resin for selectively reducing the release amount of HCN and crotonaldehyde in cigarette smoke, wherein the amino resin is polymethyl methacrylate resin spheres with amino groups grafted on the surface. Hydrophobic nano-SiO 2 prepared by Feng Bao et al (Feng Bao, yellow Tai Song, Zhoukxing, etc.. hydrophobic nano-SiO 2 selectively reduces harmful ingredient content in cigarette smoke [ J ] tobacco technology, 2011(10):49-53.) is added into tobacco shreds and filters respectively to study the harm reduction effect. Research shows that the release amount of phenol and crotonaldehyde added into tobacco shreds can be reduced by 27.2% and 12.4%. Patents CN102178351A, CN102119786A and CN102178350A disclose that adding soybean fibrin particles, soybean meal particles and fibroin into a filter tip can reduce the release amount of crotonaldehyde in smoke by 16.2-33.8%, and reduce other harmful substances in smoke differently, so that the smoke has obvious sweet feeling, the irritation of the smoke is reduced, and the richness and the fineness of the cigarette flavor are increased. Patent CN106858709B discloses a method for preparing amino acid ionic liquid for selectively reducing crotonaldehyde in cigarette mainstream smoke, which synthesizes tetraalkylammonium hydroxide type amino acid ionic liquid through acid-base neutralization reaction of carboxyl of amino acid and hydroxide radical of tetraalkylammonium hydroxide. Patent CN102942654A discloses a preparation method of an adsorbent for effectively reducing crotonaldehyde content in cigarette smoke, which takes n-butyl aldehyde as a dummy template, methacrylic acid, acrylamide, 2-vinylpyridine or 4-vinylpyridine as a functional monomer, methanol as a pore-forming solvent and ethylene glycol dimethacrylate as a cross-linking agent, and the adsorbent is synthesized by a precipitation polymerization method.
At present, a filter stick made of a diacetate fiber tow and a polypropylene tow are generally adopted as a filter tip of a cigarette, and the diacetate fiber tow and the polypropylene tow are firstly prepared and then are molded into a filter stick for a conventional cigarette (the diameter is generally 7.7mm), a filter stick for a medium cigarette (the diameter is generally 7.0mm or 6.0mm) or a filter stick for a fine cigarette (the diameter is generally 5.4mm) by a filter stick molding 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.
The polymer intercommunicated porous material has good potential of becoming a novel filter stick, and is particularly represented as follows: (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) after the epoxy group reacts with the amination reagent, the filter stick has an amino functional group, so that the release amount of crotonaldehyde in smoke can be reduced; (4) the strength of the filter stick can be improved by adopting the silicon dioxide nano particles as the particle emulsifier; (5) 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; (6) adopts a radiation polymerization method, does not add a chemical initiator, and has the functions of disinfection and sterilization.
Disclosure of Invention
The invention aims to provide a preparation method of a novel filter stick capable of reducing the release amount of crotonaldehyde in smoke, and the preparation method is used for solving the problem that the preparation process of the filter stick is complex when acetate fiber tows and polypropylene tows are firstly prepared and then are molded by filter stick molding equipment in the conventional acetate fiber tow filter stick and polypropylene tow filter stick.
The invention is realized by the following technical scheme:
a preparation method of a novel filter stick capable of reducing the release amount of crotonaldehyde in smoke comprises the following specific steps:
1) preparing an oil phase, wherein the oil phase comprises the following components: 2-8 ml of glycidyl methacrylate, 0-3 ml of methyl methacrylate, 0-3 ml of 2-ethylhexyl acrylate, 0.5-5 ml of a cross-linking agent and 1-10 g of a particle emulsifier;
2) preparing an aqueous phase, wherein the composition of the aqueous phase is 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, introducing nitrogen for 10-20 min, and sealing;
4) putting the filter stick mould filled with the high internal phase emulsion in the step 3) into a mould of 1.3 multiplied by 1015Bq60In a Co source, the dosage rate is 20-80 Gy/min, and the irradiation time is 24-48 h;
5) adding excessive amination reagent into the filter stick-shaped solid product obtained in the step 4), and reacting for 24-48 hours at the temperature of 40-60 ℃;
6) extracting the product obtained in the step 5) with water and ethanol for 24 hours respectively, and drying in a vacuum oven to obtain the novel filter stick capable of reducing the release amount of crotonaldehyde in smoke.
The cross-linking agent is one or more of ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate or glycerol tri (alpha-methacrylic acid) ester.
The particle emulsifier is silicon dioxide nano particles with the surfaces modified by a modifier.
The modifier is a polymerizable modifier prepared by opening double bonds in oleic acid to generate dihydroxy and then carrying out esterification reaction with acrylic acid.
The inorganic salt is one of calcium chloride, sodium chloride or magnesium sulfate.
The amination reagent is ethylenediamine or propylenediamine.
The invention has the beneficial effects that:
(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) after the epoxy group reacts with the amination reagent, the filter stick has an amino functional group, so that the release amount of crotonaldehyde in smoke can be reduced;
(4) the strength of the filter stick can be improved by adopting the silicon dioxide particles as the particle emulsifier;
(5) 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;
(6) adopts a radiation polymerization method, does not add a chemical initiator, and has the functions of disinfection and sterilization.
Detailed Description
The technical solutions of the present invention are described in detail below by examples, and the following examples are only exemplary and can be used only for explaining and explaining the technical solutions of the present invention, but not construed as limiting the technical solutions of the present invention.
In the application, the particle emulsifier is silica nanoparticles with the surface modified by a modifier, wherein the modifier is a polymerizable modifier prepared by opening double bonds in oleic acid to generate dihydroxy and then carrying out esterification reaction with acrylic acid, and the specific reaction equation is as follows:
example 1
Preparing an oil phase, wherein the oil phase comprises 8ml of glycidyl methacrylate, 2ml of methyl methacrylate, 0.5ml of ethylene glycol dimethacrylate and 5g of modifier modified silica nanoparticles.
An aqueous phase was prepared by uniformly mixing 64ml of water with 0.5g of calcium 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 7.7mm and length of 100mm, introducing nitrogen for 10min, and sealing.
In the technical scheme of the application, the forming die of the filter stick can be changed as required, for example, the diameter is 7.0mm or 6.0mm or 5.4mm, the length is 100mm or 120mm or 144mm, or the die of other models can be used, the model of the filter stick die does not affect the implementation of the technical scheme of the application, and the same is true in the following embodiments of the application or other cases of implementing your filter stick die.
The mold with the high internal and upper emulsion added was then placed in a 1.3X 10 position15Bq60In the Co source, the dosage rate is 36Gy/min, and the irradiation time is 24 h. And (3) placing the obtained solid product in an excessive ethylenediamine solution for reaction for 24 hours at 40 ℃, respectively extracting for 24 hours by using water and ethanol, and drying in a vacuum oven to obtain the final filter stick. Compared with the cigarette without the filter stick, the cigarette with the filter stick has the advantage that the crotonaldehyde release amount reduction rate of the main stream smoke reaches 30.5%.
Example 2
An oil phase was prepared consisting of 4ml of glycidyl methacrylate, 0.5ml of 2-ethylhexyl acrylate, 3ml of trimethylolpropane trimethacrylate, and 3g of modifier-modified silica nanoparticles.
An aqueous phase was prepared by mixing 60ml of water and 0.5g of sodium chloride uniformly.
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. The mold with the high internal phase emulsion added is then placed in a 1.3X 10 position15Bq60In the Co source, the dosage rate is 36Gy/min, and the irradiation time is 36 h.
And (3) placing the obtained solid product in an excessive propane diamine solution for reaction at 40 ℃ for 24h, respectively extracting with water and ethanol for 24h, and drying in a vacuum oven to obtain the final filter stick.
Example 3
An oil phase was prepared, which consisted of 5ml of glycidyl methacrylate, 2ml of methyl methacrylate, 1ml of glycerol tri (. alpha. -methacrylate) and 4g of modifier-modified silica nanoparticles.
An aqueous phase was prepared by mixing 70ml of water and 1.5g of magnesium sulfate uniformly.
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.
The mold with the high internal emulsion added is then placed in a 1.3X 1015Bq60In the Co source, the dosage rate is 36Gy/min, and the irradiation time is 36 h.
And (3) placing the obtained solid product in an excessive ethylenediamine solution for reaction for 24 hours at 50 ℃, respectively extracting 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 was prepared, which consisted of 6ml of glycidyl methacrylate, 2ml of methyl methacrylate, 1ml of glycerol tri (. alpha. -methacrylate) and 4g of modifier-modified silica nanoparticles.
An aqueous phase was prepared by mixing 70ml of water and 1.5g of magnesium sulfate uniformly.
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.
The mold with the high internal phase emulsion added is then placed in a 1.3X 10 position15Bq60In the Co source, the dosage rate is 36Gy/min, and the irradiation time is 48 h.
And (3) placing the obtained solid product in an excessive ethylenediamine solution for reaction for 24 hours at 50 ℃, respectively extracting for 24 hours by using water and ethanol, and drying in a vacuum oven to obtain the final filter stick.
Example 5
Preparing an oil phase, wherein the oil phase comprises 6ml of glycidyl methacrylate, 2ml of methyl methacrylate, 0.5ml of ethylene glycol dimethacrylate and 4g of modifier modified silica nanoparticles.
Then, an aqueous phase was prepared by uniformly mixing 64ml of water with 0.5g of calcium 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 7.7mm and length of 144mm, introducing nitrogen for 10min, and sealing.
The mold with the high internal phase emulsion added is then placed in a 1.3X 10 position15Bq60In the Co source, the dosage rate is 36Gy/min, and the irradiation time is 24 h.
And (3) placing the obtained solid product in an excessive ethylenediamine solution for reaction for 24 hours at 50 ℃, respectively extracting for 24 hours by using water and ethanol, and drying in a vacuum oven to obtain the final filter stick.
The novel filter stick prepared by the embodiments 1 to 5 can be directly formed into a filter stick with specific circumference and length in a filter stick forming die, has certain strength, and can meet the requirement of cigarette tipping; the prepared novel filter stick is provided with a micron-sized large hole, and the holes are communicated with each other, so that cigarette smoke can be transmitted; after the epoxy group reacts with the amination reagent, the filter stick has an amino functional group, so that the release amount of crotonaldehyde in smoke can be reduced; the strength of the filter stick can be improved by adopting the silicon dioxide nano particles as the particle emulsifier; 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.
The above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of by the inventive arts should be included in the scope of the present invention, and therefore, the scope of the present invention should be subject to the scope defined by the claims.
Claims (4)
1. A preparation method of a novel filter stick capable of reducing the release amount of crotonaldehyde in smoke is characterized by comprising the following specific steps:
1) preparing an oil phase, wherein the oil phase comprises the following components: 2-8 ml of glycidyl methacrylate, 0-3 ml of methyl methacrylate, 0-3 ml of 2-ethylhexyl acrylate, 0.5-5 ml of a cross-linking agent and 1-10 g of a particle emulsifier;
2) preparing an aqueous phase, wherein the composition of the aqueous phase is 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, introducing nitrogen for 10-20 min, and sealing;
4) putting the filter stick mould filled with the high internal phase emulsion in the step 3) into a mould of 1.3 multiplied by 1015 Bq 60In a Co source, the dosage rate is 20-80 Gy/min, and the irradiation time is 24-48 h;
5) adding excessive amination reagent into the filter stick-shaped solid product obtained in the step 4), and reacting for 24-48 hours at the temperature of 40-60 ℃;
6) extracting the product obtained in the step 5) with water and ethanol for 24 hours respectively, and drying in a vacuum oven to obtain a novel filter stick capable of reducing the release amount of crotonaldehyde in smoke;
the particle emulsifier is silicon dioxide nano particles with the surfaces modified by a modifier;
the modifier is a polymerizable modifier prepared by opening double bonds in oleic acid to generate dihydroxy and then carrying out esterification reaction with acrylic acid.
2. The method for preparing a novel filter stick capable of reducing the release amount of crotonaldehyde in smoke according to claim 1, wherein the crosslinking agent is at least one of ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate or glycerol tri (alpha-methacrylate).
3. The method for preparing the novel filter stick capable of reducing the release amount of crotonaldehyde in smoke according to claim 1, wherein the inorganic salt is one of calcium chloride, sodium chloride or magnesium sulfate.
4. The method for preparing a novel filter stick capable of reducing the release amount of crotonaldehyde in smoke according to claim 1, wherein the amination reagent is ethylenediamine or propylenediamine.
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| CN202010390984.4A CN111387545B (en) | 2020-05-11 | 2020-05-11 | Preparation method of novel filter stick capable of reducing release amount of crotonaldehyde in smoke |
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| CN202010390984.4A CN111387545B (en) | 2020-05-11 | 2020-05-11 | Preparation method of novel filter stick capable of reducing release amount of crotonaldehyde in smoke |
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| CN111387545B true CN111387545B (en) | 2022-04-19 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| FR2932184B1 (en) * | 2008-06-09 | 2010-07-30 | Commissariat Energie Atomique | HIGH MECHANICAL POLYHIPED MATERIAL, PROCESS FOR PREPARING THE SAME, USEFUL EMULSION FOR ITS PREPARATION AND ARTICLE CONSISTING OF SUCH A MATERIAL |
| CN101979418B (en) * | 2010-12-07 | 2012-08-01 | 中国烟草总公司郑州烟草研究院 | Preparation method and application of poly-glycidyl methacrylate interosculated porous material |
| CN103431519B (en) * | 2013-08-29 | 2014-10-29 | 中国烟草总公司郑州烟草研究院 | Application of high content of epoxy group polyethylene glycidyl methacrylate interconnected porous materials in cigarettes |
| CN105273118B (en) * | 2014-07-15 | 2018-06-12 | 南通醋酸纤维有限公司 | A kind of PDGA resins and its preparation method and application |
| CN105622812B (en) * | 2014-10-30 | 2018-05-04 | 南通醋酸纤维有限公司 | A kind of aminated high-specific surface area polystyrene resin and its preparation method and application |
| CN104558438B (en) * | 2014-12-24 | 2017-01-18 | 中科院广州化学有限公司 | Methacrylate polymer-inorganic compound through hole material as well as preparation method and application thereof |
| EP3543263A4 (en) * | 2016-11-16 | 2019-11-27 | Zhejiang University | Polyolefin-based emulsifier and application thereof for preparing high internal phase emulsion and porous polymeric material |
| CN107115570B (en) * | 2017-03-30 | 2020-06-19 | 华南理工大学 | Nano composite biological scaffold with multi-stage controllable through hole structure and preparation method and application thereof |
| CN107674141B (en) * | 2017-11-21 | 2019-07-12 | 中国烟草总公司郑州烟草研究院 | One tobacco articles in vitro toxicology evaluates the preparation of three-dimensional cell bracket and the method for carrying out cell culture using it |
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