CN108835710B - Cigarette filter tip with controllable smoke temperature and low-temperature non-combustion and preparation method thereof - Google Patents

Cigarette filter tip with controllable smoke temperature and low-temperature non-combustion and preparation method thereof Download PDF

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CN108835710B
CN108835710B CN201810739602.7A CN201810739602A CN108835710B CN 108835710 B CN108835710 B CN 108835710B CN 201810739602 A CN201810739602 A CN 201810739602A CN 108835710 B CN108835710 B CN 108835710B
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polylactic acid
temperature
acid particles
particles
cigarette
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CN108835710A (en
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李雅明
姜俊全
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Wuhan Shuimuhong New Material Co ltd
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Wuhan Shuimuhong New Material Co ltd
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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/061Use of materials for tobacco smoke filters containing additives entrapped within capsules, sponge-like material or the like, for further release upon smoking
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/02Manufacture of tobacco smoke filters
    • A24D3/0204Preliminary operations before the filter rod forming process, e.g. crimping, blooming
    • A24D3/0212Applying additives to filter materials
    • A24D3/0225Applying additives to filter materials with solid additives, e.g. incorporation of a granular product
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/08Use of materials for tobacco smoke filters of organic materials as carrier or major constituent
    • A24D3/10Use of materials for tobacco smoke filters of organic materials as carrier or major constituent of cellulose or cellulose derivatives

Abstract

The invention relates to a cigarette filter tip rod with controllable smoke temperature and low-temperature non-combustion and a preparation method thereof. The polylactic acid particles with a certain particle size are uniformly embedded into the cigarette tows according to a certain proportion to prepare the low-temperature non-combustible cigarette filter rod with excellent performance, so that the problems that the existing like products are generally poor in flue gas temperature regulation and control, easy to block a flue gas channel, poor in flue gas inhalation taste and the like are solved. The polylactic acid material, the glyceryl triacetate and other environment-friendly modified auxiliary agents introduced by the invention have the advantages of good biocompatibility, biodegradability, safety, environment protection and the like, and the materials are nontoxic to human bodies and accord with the principle of green economy.

Description

Cigarette filter tip with controllable smoke temperature and low-temperature non-combustion and preparation method thereof
Technical Field
The invention relates to the technical field of adsorption filter materials and tobacco, in particular to a cigarette filter rod with controllable smoke temperature and low-temperature non-combustion and a preparation method thereof.
Background
There are often tens of carcinogens in smoke produced by the burning of conventional smoking articles. Related researches show that the generation of various chemical substances in the smoke is closely related to the burning temperature of the cigarettes, and the hazard index of the cigarettes is increased along with the increase of the burning temperature of the cigarettes. In addition, smoke generated by combustion diffuses in the air to form second-hand smoke. The heating non-burning cigarette is a novel cigarette product. Unlike conventional cigarettes, low temperature cigarettes designed with the thought of heating without burning can heat the tobacco just enough to emit a taste without lighting the tobacco. In general, a common cigarette can generate a plurality of harmful substances at high temperature during smoking, while a low-temperature cigarette is smoked below 400 ℃ and the harmful substances are greatly reduced. Under the international environment and the large background of smoking control, the research and the development and the application of the heating non-burning cigarettes have important significance.
According to the recently issued survey data of European Rui International, a globally known consultation company, the heated nonflammable cigarette product will be the fastest growing product in the next 5 years, and its sales will reach $154 billion in 2021, well over $20 billion in 2016, with an increase of up to 691%. The study also showed that: japan is the largest market for heated non-combustible tobacco products worldwide, accounting for 96% of the global sales of such products; germany is the second major market, and the united states will exceed germany in 2021; the third and fourth major markets are swiss and portuguese, respectively, which are also the fastest growing markets. Based on the heating non-combustion device and the heating rod thereof, which are not required to be ignited, for increasing production of large-scale tobacco enterprises worldwide are started. In fact, the international company of philips morris tobacco, producing IQOS (squaring) heating non-combustibles, which has invested a tremendous amount of money in 2017 to build new factories in the eastern germany, and which also produces heating non-combustibles and its associated heating rods in italy, swiss and greece. A similar product GLO-Gelu was introduced by Inmei tobacco corporation in Korea market, and a heating non-combustible device Ploom TECH-Pu Lu Mu was introduced by Nippon tobacco International corporation in domestic market.
In recent years, a plurality of domestic tobacco manufacturing enterprises and research institutions successively enter the research and development field of novel tobacco products and obtain patents. However, no specific technical requirement is made on the temperature of the inhaled smoke in the design of the conventional low-temperature cigarette system, and most of the conventional filter design thought of the cigarette filter tip is adopted. For example, chinese patent CN2014104676403 discloses a smoking material for low-temperature non-combustible cigarettes and a preparation method thereof, the smoking material is obtained by pulverizing tobacco raw materials into powder, performing microwave expansion granulation, then fully and uniformly mixing with spice plant particles, tobacco essence, starch adhesive, propylene glycol and tobacco starch humectant to obtain a semi-finished smoking material, and finally performing compression molding. For example, chinese patent 2015100278401 discloses a smoking device for electrically heating non-combustible tobacco, which heats a tobacco product at a low temperature by means of electric heating, so that the tobacco product releases tobacco aroma under the premise of not burning, and the smoker can obtain satisfaction and reduce the harm of active and passive smoking to human body.
The smoke generated by the traditional cigarette combustion is mainly cooled by the back-end tobacco shred and the filter tip rod in the filtering process, so that the proper smoking temperature of a human body is achieved. The heating of the non-combustible cigarettes is carried out in a heating device with the baking temperature of 200-400 ℃, and the generated smoke is also required to be subjected to cooling treatment in a filter section of a cigarette holder, so that the temperature suitable for human body contact is reached, and meanwhile, the requirements of smokers on the taste of the smoke are met. In order to fully ensure the effective utilization rate of the smoke of the low-temperature heating tobacco products inhaled by a human body, the smoke adsorption rate of the filtering section needs to be reduced as much as possible, namely the filtering section can be cooled and is required to be adsorbed as little as possible.
The low temperature non-combustible cigarette IQOS developed by philips morris tobacco international includes a tobacco product segment, a hollow filter segment, and a polylactic acid material segment. Wherein the length of the tobacco product section is about 11mm, and the section mainly contributes to smoke; the length of the hollow filter tip section is about 8mm, and the hollow filter tip mainly plays a certain role in cooling and heat insulation; the polylactic acid material section is formed by folding and rolling a polylactic acid sheet with the thickness of about 0.05mm, the filling rate is about 30%, the porosity is about 70%, the smoke contact area is about 4000 square millimeters, and the polylactic acid material section is used as a smoke channel to play a supporting role and a cooling role. The product adopts polylactic acid material to certainly paste environment-friendly labels on low-temperature non-combustible cigarettes, and further utilizes physical characteristics of low glass transition temperature, low melting temperature and the like of the polylactic acid to effectively reduce the smoking temperature of smoke, and similar technology also comprises CN201510502839X, CN2013800033776. However, this polylactic acid material melts when exposed to the initial, too high temperature of the flue gas, resulting in the flue gas channel being blocked, and therefore, a sufficient distance must be provided from the heat generator, which is why the IQOS article must have a hollow filter segment designed between the front end of the polylactic acid and the heat generator. Even so, after the sucking is finished, the front polylactic acid film is still partially melted, and the phenomenon that part of smoke channels are blocked occurs. In addition, the research and test results also show that the smoke temperature of the IQOS product of Philips Moris tobacco International company is not ideal enough, and the mouth feel is slightly scalded.
In order to solve the problems and simultaneously adapt to the development trend of cigarette products, the applicant creatively embeds pure/modified polylactic acid particles into a filter rod uniformly, and takes the polylactic acid particles as a heat absorption carrier, so that the smoke temperature is effectively reduced, and the problem of smoke channel blockage caused by melting of polylactic acid is avoided. When the contact area of the embedded polylactic acid particles and the smoke is large to a certain extent, the temperature of the smoke can be obviously reduced. In the smoke inhalation process, even if the front end temperature is higher, partial polylactic acid is softened or melted, enough gaps are reserved among polylactic acid particles, and large-area blockage or deformation cannot be generated, so that the smoke channel cannot be influenced. The filter tip rod embedded with polylactic acid particles can be directly used close to a tobacco heating body, a hollow filter tip section is not required to be additionally arranged, the structure is simpler, and the effect is better.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a cigarette filter rod with controllable smoke temperature and low-temperature non-combustion, which comprises a filter rod body formed by a cigarette tow and polylactic acid particles, wherein the polylactic acid particles are uniformly distributed in the filter rod body.
The mass filling percentage of the polylactic acid particles (namely, the mass of the polylactic acid particles/(the mass of the polylactic acid particles and the mass of the filter rod)) is 5-50%, preferably 15-30%.
The particle diameter of the polylactic acid particles is 10-100 meshes, preferably 40-60 meshes.
The intrinsic viscosity eta of the polylactic acid raw material for preparing the polylactic acid microsphere is 0.1-15dl/g, and the viscosity average molecular weight is 1000-1000000.
The polylactic acid particles are made of pure polylactic acid or modified polylactic acid, wherein the modified polylactic acid is prepared from pure polylactic acid and a plasticizer according to the following (100-X): x (X is more than or equal to 0 and less than or equal to 30) and the plasticizer is selected from polyethylene glycol, glyceryl triacetate, acetyl citrate, glycerin and other small molecular substances which are non-toxic to human inhalation.
The filter tip rod body is made of materials such as diacetate fiber tows, polypropylene fiber tows and the like.
The preparation method of the cigarette filter tip rod with controllable smoke temperature and low temperature non-combustion comprises the following steps:
(a) Preparing polylactic acid particles by using pure polylactic acid or modified polylactic acid;
(b) When the filter rod bundle for tobacco is processed and molded, polylactic acid particles and the filter rod bundles are mixed and molded, so that the polylactic acid particles are uniformly embedded in the filter rod body.
According to the scheme, the polylactic acid particles are obtained by extruding, granulating, crushing and sieving pure polylactic acid or modified polylactic acid, and the granulating mode is selected from underwater granulating, water ring granulating, centrifugal atomizing granulating and the like.
According to the scheme, the process for preparing polylactic acid particles from the modified polylactic acid is as follows: firstly, uniformly mixing pure polylactic acid and a plasticizer in shearing mixing equipment at 150-230 ℃, extruding and granulating, then mixing polylactic acid particles with liquid nitrogen to embrittle the polylactic acid particles, and finally crushing and sieving, wherein the shearing mixing equipment is one of a double-screw extruder, an internal mixer, a double-roll mill and the like.
According to the invention, polylactic acid particle materials with a certain particle size are uniformly embedded into the filter tip rod according to a certain proportion, so that the low-temperature non-combustible cigarette filter tip rod with excellent performance is prepared. The method fully utilizes the advantages of low melting point, low glass transition temperature, quick heat absorption, environmental protection, safety and the like of the polylactic acid material, and when the heated smoke passes through the filter tip, the polylactic acid particles can play the role of regulating and controlling the temperature of the smoke, improve the inhaled taste and avoid the phenomenon of blocking a smoke channel. Compared with the prior art, the invention has the following unexpected beneficial effects:
(1) Safe, nontoxic, environment-friendly and degradable. Based on the existing filter tip rod material, the environment-friendly modified auxiliary agents such as polylactic acid material which has good biocompatibility with human body, can be fully biodegraded, is safe and environment-friendly, and triacetin commonly used in tobacco industry are introduced, and the use of the materials is not only harmless to the human body, but also accords with the principle of green economy;
(2) The preparation method is simple, and has lower requirements on equipment and process improvement. The polylactic acid particles are uniformly distributed in the filter tip tows by adopting a powder embedded type adding technology, and the technology is very mature in the tobacco industry, and has simple technology and low production cost;
(3) Compared with the mode of arranging holes (CN 203618761U, CN203618762U and the like) in the filter rod, arranging a particle filling section/layer (CN 106174692A, CN103054190A, CN102885401A, CN106376968A and the like) in the middle or on the surface of the filter rod and directly taking polylactic acid as a raw material of the filter rod (such as CN103987283A, CN105177737A and the like), the method creatively uniformly embeds polylactic acid particles in the filter rod tow, can more effectively regulate and control the flue gas temperature, and prevents the occurrence of flue gas channel blockage.
Drawings
Fig. 1 is a schematic view of the structure of a cigarette filter rod according to the present invention.
Wherein, the filter tip comprises a 1-filter tip rod, 2-polylactic acid microspheres and 3-filter tip rod tows.
Detailed Description
In order for those of ordinary skill in the art to fully understand the technical solutions and advantageous effects of the present invention, the following description is further given with reference to specific embodiments and drawings.
The polylactic acid material selected in this example was 4032D polylactic acid product produced by Nature works, inc. of America, which has a viscosity average molecular weight of 35000 and an intrinsic viscosity of 3.5dl/g. The mixing equipment used was SHJ-36 twin screw extruder manufactured by Nanj Jien, the drying equipment was DZF-6050 vacuum drying oven manufactured by Shanghai Santa instruments, inc., the pulverizing and granulating equipment was WF-250 stainless steel high-speed universal pulverizer manufactured by Changzhou spring pharmaceutical machinery, inc., and the filter tip forming equipment was KDF2 cigarette holder filter forming machine manufactured by Germany. Other raw materials are all commonly and commercially available.
And (3) filling polylactic acid raw materials in a stainless steel tray, and then pouring the polylactic acid into a vacuum drying oven for drying at a drying temperature of 60 ℃ for 12 hours. And after the drying is finished, mixing the polylactic acid and the glyceryl triacetate according to the mass ratio of 90:10, uniformly stirring, and sealing and preserving for standby, thus obtaining the modified polylactic acid premix. The same amount of pure polylactic acid raw material is also prepared for drying for standby according to the method.
Starting the double-screw extruder, and setting the temperature of each interval: the conveying section 130 ℃, the melting section 170 ℃, the mixing section 180 ℃, the exhausting section 175 ℃ and the homogenizing extrusion section 170 ℃. After the temperature of each temperature section reaches a set value and is kept for 30min, adding the mixed modified polylactic acid premix and pure polylactic acid from a feed hopper of a double-screw extruder in batches, extruding the molten mixture from the double-screw extruder in a linear shape, cooling the molten mixture to room temperature in an air cooling mode, and cutting and granulating the polylactic acid lines by a plastic granulator to obtain modified polylactic acid particles and pure polylactic acid particles respectively. Before crushing, the two particles are respectively cooled by liquid nitrogen to improve brittleness, the liquid nitrogen is poured into a plastic container filled with polylactic acid particles for a period of time during operation, and then the cooled polylactic acid particles are put into a stainless steel high-speed universal crusher to be crushed, so as to obtain modified polylactic acid particles and pure polylactic acid particles. Screening and grading with standard screens with different mesh numbers to obtain various pure polylactic acid/modified polylactic acid particulate materials with uniform size specifications.
And uniformly embedding and distributing the polylactic acid particles into the cigarette tows when the polylactic acid particles are clustered on a cigarette holder filter forming machine, wherein the equivalent quantity of the modified polylactic acid particles and the pure polylactic acid particles with the mesh number of 20 are taken. The mass fraction of polylactic acid particles in the obtained filter tip rod for cigarettes is 20%.
Example 2
Referring to the method of example 1, modified polylactic acid was prepared according to a mass ratio of polylactic acid to acetyl citrate of 80:20, and polylactic acid fine particles having a mesh number of 50 were prepared using the modified polylactic acid, and finally a filter rod for cigarettes having a mass fraction of polylactic acid fine particles of 30% was prepared.
Example 3
Referring to the method of example 1, modified polylactic acid was prepared according to a mass ratio of polylactic acid to glycerin of 85:15, and polylactic acid fine particles having a mesh number of 45 were prepared using the modified polylactic acid, and finally a filter rod for cigarettes having a mass fraction of polylactic acid fine particles of 15% was prepared.
Example 4
Referring to the method of example 1, modified polylactic acid was prepared according to a mass ratio of polylactic acid to polyethylene glycol of 75:25, and polylactic acid fine particles having a mesh number of 55 were prepared using the modified polylactic acid, and finally a filter rod for cigarettes having a mass fraction of polylactic acid fine particles of 25% was prepared.
For the above embodiments, a simple method is used to detect the temperature change of the flue gas and the melting and flue gas channel blockage conditions of the polylactic acid. And taking the IQOS low-temperature non-combustible cigarette as a reference comparison sample, and respectively replacing the filter rod of the IQOS low-temperature non-combustible cigarette with the filter rod prepared in each embodiment to prepare the cigarette. In order to facilitate the comparison of implementation effects, a cigarette holder filter rod with the same length as an IQOS product is adopted, a tobacco professional is invited to carry out suction evaluation test on all samples simultaneously, an electronic infrared temperature measuring instrument is adopted to detect the temperature change of smoke during the process, the filter tip is disassembled after the suction is finished, and the melting condition of polylactic acid is observed. The experimental results are shown in the following table:
TABLE 1 IQOS original filter rod and cigarette smoking evaluation test results table of the filter rod of the present invention
Figure BDA0001722910280000061
As can be seen from the table, the cigarette filter tip rod provided by the invention can be used for effectively regulating and controlling the smoke temperature, and the occurrence of the blockage of a smoke channel is basically avoided.

Claims (7)

1. The cigarette filter tip rod is characterized by comprising a filter tip rod body formed by cigarette tows and polylactic acid particles, wherein the polylactic acid particles are uniformly distributed in the filter tip rod tows; the polylactic acid particles are made of pure polylactic acid or modified polylactic acid, wherein the modified polylactic acid is prepared from pure polylactic acid and a plasticizer according to the following (100-X): the mass ratio of X is more than or equal to 0 and less than or equal to 30, and the plasticizer is one of polyethylene glycol, glyceryl triacetate, acetyl citrate and glycerin.
2. A smoke temperature controllable, low temperature non-combustible cigarette filter rod according to claim 1 and wherein: the mass percentage of polylactic acid particles in the filter tip rod body is 5-50%.
3. A smoke temperature controllable, low temperature non-combustible cigarette filter rod according to claim 1 and wherein: the particle size of the polylactic acid particles is 10-100 meshes.
4. A smoke temperature controllable, low temperature non-combustible cigarette filter rod according to claim 1 and wherein: the intrinsic viscosity eta of the polylactic acid raw material for preparing the polylactic acid microsphere is 0.1-15dl/g, and the viscosity average molecular weight is 1000-1000000.
5. A method for preparing a cigarette filter rod with controllable smoke temperature and low temperature non-combustion as claimed in any one of claims 1 to 4, comprising the steps of:
(a) Preparing polylactic acid particles by using pure polylactic acid or modified polylactic acid;
(b) When the filter rod bundle for the cigarette is processed and molded, polylactic acid particles and the filter rod bundles are mixed and molded, so that the polylactic acid particles are uniformly embedded in the filter rod body.
6. The method of manufacturing according to claim 5, wherein: the polylactic acid particles are obtained by extruding, granulating, crushing and sieving pure polylactic acid or modified polylactic acid, and the granulating mode is selected from one of underwater granulating, water ring granulating and centrifugal atomizing granulating.
7. The method according to claim 5, wherein the process for preparing polylactic acid particles from modified polylactic acid comprises the following steps: firstly, uniformly mixing pure polylactic acid and a plasticizer in shearing mixing equipment at 150-230 ℃, extruding and granulating, then mixing polylactic acid particles with liquid nitrogen to embrittle the polylactic acid particles, and finally crushing and sieving, wherein the shearing mixing equipment is selected from any one of a double-screw extruder, an internal mixer and a double-roll mill.
CN201810739602.7A 2018-07-06 2018-07-06 Cigarette filter tip with controllable smoke temperature and low-temperature non-combustion and preparation method thereof Active CN108835710B (en)

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CN112401298A (en) * 2019-08-27 2021-02-26 湖北中烟工业有限责任公司 Cooling filter rod and low-temperature cigarette with same
CN110893009A (en) * 2019-09-18 2020-03-20 索图电子(惠州)有限公司 Filter part for cigarette
CN110903619B (en) * 2019-11-12 2022-03-08 湖北中烟工业有限责任公司 Preparation method of modified PLA cooling material
CN112369665A (en) * 2020-01-16 2021-02-19 湖北中烟工业有限责任公司 Cigarette cooling section, preparation method thereof, cooling filter tip containing cigarette cooling section and low-temperature cigarette

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