CN111218099A - A kind of cellulose diacetate composite stereotyped phase change material and its preparation method and application - Google Patents
A kind of cellulose diacetate composite stereotyped phase change material and its preparation method and application Download PDFInfo
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- 229920001747 Cellulose diacetate Polymers 0.000 title claims abstract description 126
- 239000012782 phase change material Substances 0.000 title claims abstract description 88
- 239000002131 composite material Substances 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 35
- 239000000779 smoke Substances 0.000 claims abstract description 33
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 230000008859 change Effects 0.000 claims abstract description 17
- 238000007493 shaping process Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000004020 conductor Substances 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 68
- 239000002245 particle Substances 0.000 claims description 48
- 239000000243 solution Substances 0.000 claims description 38
- 239000002202 Polyethylene glycol Substances 0.000 claims description 30
- 229920001223 polyethylene glycol Polymers 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000003517 fume Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 230000004580 weight loss Effects 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims 2
- 238000004513 sizing Methods 0.000 abstract description 29
- 230000000694 effects Effects 0.000 abstract description 13
- 239000012071 phase Substances 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 239000007790 solid phase Substances 0.000 abstract description 4
- 238000004146 energy storage Methods 0.000 abstract description 3
- 230000007704 transition Effects 0.000 abstract description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 50
- 239000008118 PEG 6000 Substances 0.000 description 31
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 description 31
- 229920001030 Polyethylene Glycol 4000 Polymers 0.000 description 23
- 238000010438 heat treatment Methods 0.000 description 16
- 239000000523 sample Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- 241000208125 Nicotiana Species 0.000 description 10
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 10
- 230000009467 reduction Effects 0.000 description 10
- 238000002485 combustion reaction Methods 0.000 description 9
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- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000007605 air drying Methods 0.000 description 6
- 239000013068 control sample Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 238000011068 loading method Methods 0.000 description 6
- 239000010949 copper Substances 0.000 description 5
- 229920002472 Starch Polymers 0.000 description 4
- 231100000252 nontoxic Toxicity 0.000 description 4
- 230000003000 nontoxic effect Effects 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- 238000002411 thermogravimetry Methods 0.000 description 4
- 229920000875 Dissolving pulp Polymers 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000012496 blank sample Substances 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 229920000747 poly(lactic acid) Polymers 0.000 description 3
- 239000004626 polylactic acid Substances 0.000 description 3
- 229920006381 polylactic acid film Polymers 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 229920006221 acetate fiber Polymers 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000013074 reference sample Substances 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 238000007416 differential thermogravimetric analysis Methods 0.000 description 1
- HFCSXCKLARAMIQ-UHFFFAOYSA-L disodium;sulfate;hydrate Chemical compound O.[Na+].[Na+].[O-]S([O-])(=O)=O HFCSXCKLARAMIQ-UHFFFAOYSA-L 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000003471 mutagenic agent Substances 0.000 description 1
- 231100000707 mutagenic chemical Toxicity 0.000 description 1
- 230000003505 mutagenic effect Effects 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 235000019505 tobacco product Nutrition 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/02—Polyalkylene oxides
-
- 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
- A24D3/0212—Applying additives to filter materials
- A24D3/0225—Applying additives to filter materials with solid additives, e.g. incorporation of a granular product
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
Abstract
The invention discloses a cellulose diacetate composite sizing phase-change material for reducing the smoke temperature of a heated non-combustible cigarette, and a preparation method and application thereof. The cellulose diacetate composite sizing phase-change material is prepared from 10-50% of cellulose diacetate, 50-90% of phase-change material and 1-5% of heat-conducting material by a solvent blending method. The cellulose diacetate composite shaping phase-change material has a rigid net structure and high-melting-point cellulose diacetate, so that the material has the characteristics of excellent thermal stability and solid-solid phase change; the phase transition from the PEG branched chain crystalline state to the amorphous state enables the material to realize the function of heat absorption and energy storage; the addition of the heat-conducting metal powder improves the heat-conducting property of the material and achieves the effect of rapid cooling. The smoke containing resistance of the cellulose diacetate composite sizing phase-change material is similar to iQOS raw smoke, the temperature of the smoke from the first mouth to the fourth mouth can be obviously reduced, and the temperature of the smoke from the first mouth can be reduced to 36 ℃.
Description
Technical Field
The invention relates to the technical field of a temperature-reducing material for heating non-combustible cigarettes, in particular to a cellulose diacetate composite sizing phase-change material for reducing the smoke temperature of the heating non-combustible cigarettes and application thereof.
Background
With the continuous concern of people on health problems caused by smoking and the gradual implementation of international and domestic tobacco control policies, a new concept tobacco product, namely a cigarette which is not burnt by heating, comes from year to year, and represents products such as Feimu iQOS, Glo of Enmei tobacco and Revo of Reynolds company. The cigarette without combustion is a low-temperature cigarette designed by taking the concept of 'heating without combustion', can heat tobacco leaves or tobacco materials to the extent of just releasing nicotine without igniting the tobacco leaves or the tobacco materials, obviously reduces the content of carcinogenic components and the content of mutagen in smoke because the tobacco is not combusted, and greatly reduces the harm to human bodies.
At present, all large transnational tobacco enterprises shift strategic emphasis to the novel tobacco field, particularly, after fimo international releases iQOS in Japan, the fiom international not only occupies a small market share, but also rapidly drives the rise and development of the heating non-combustion cigarette industry, and more resources at home and abroad are put into the field. The iQOS matched cigarette adopts the polylactic acid film as a material for cooling the smoke, but the cooling effect of the polylactic acid film is not obvious, the smoke of the first three mouths is higher, and the smoke is easy to melt and shrink when being heated, so that the smoking experience of a user is greatly influenced. Therefore, the reduction of the smoke temperature of the cigarette which is not burnt during heating is a difficult point of a novel tobacco technology, and the preparation of the non-toxic and harmless shaping phase-change material is the key of the technical application.
For example, fimo international patent CN104203015B, which describes an aerosol-generating article having an aerosol-cooling element, defines that the aerosol-cooling element is formed from a pleated, gathered polymeric sheet, but the first smoke temperature of its iQOS cigarette is 54-60 ℃, and the phenomenon of suction overheating still exists. For example, Chinese patent CN209376709U discloses a temperature-reducing filter rod and a cigarette which is not burned when heated, wherein a first rod and a solid second rod, the surfaces of which are coated with temperature-reducing materials and which comprise a plurality of through holes, are combined to form a temperature-reducing section, so that the temperature of the smoke of the first three openings can be reduced to 42 ℃ from 60-65 ℃ of iQOS of a reference sample. And Chinese patent CN108143004A, which describes a material for cooling cigarette smoke by heating and non-burning and its application, polylactic acid, montmorillonite, carbon fiber, sodium sulfate hydrate and copper powder are mixed uniformly and then made into cooling line by using screw extruder, the filter stick comprises 15mm cooling section and 3mm acetate fiber section, and the smoke temperature at the filter end is detected by using ISO mode suction, the result shows that the smoke temperature is reduced to 33 ℃ from 47 ℃ of the reference sample. However, the diameter of the cigarette in the patent is 23mm, the shrinkage rate of the cooling material is still 2.6%, and the smoking resistance and the specific cooling effect of the cigarette are not indicated. Furthermore, Chinese patent CN110372916A discloses a starch-based cooling material and application thereof, wherein the starch-based cooling material is prepared by the cooperation of starch, polylactic acid and polyalcohol, and a filter stick comprises a cooling section of 23mm and an acetate fiber section of 7 mm. The temperature difference between the two ends of the starch substrate tube is 70-120 ℃, and the temperature difference between the two ends of the pure polylactic acid is 68 ℃. However, the patent does not specify the diameter and the size of the smoking resistance of the cigarette, and does not describe the specific cooling effect in detail.
In view of the above, it is very important to develop a shaping phase-change material which has the advantages of simple preparation process, no pollution in the preparation process, easy industrial production and good effect of reducing the temperature of smoke of a cigarette which is not burnt by heating.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to overcome the defects of the prior art and provides the cellulose diacetate composite sizing phase-change material particles which have the advantages of nontoxic and harmless raw materials, simple preparation process, no pollution in the preparation process, easy industrial production and obvious effect of reducing the smoke temperature of the cigarette which is not burnt by heating.
The technical scheme is as follows: the invention is realized by the following technical scheme: the cellulose diacetate composite sizing phase-change material is prepared from the following raw materials in percentage by mass through a solvent blending method: 10-50% of cellulose diacetate, 50-90% of phase change material and 1-5% of heat conduction material.
Further, the phase change material is polyethylene glycol, and the molecular weight of the polyethylene glycol is 2000-10000.
Further, the heat conducting material is copper powder or silver powder, and the particle size is 200-600 meshes.
The preparation method of the cellulose diacetate composite sizing phase-change material comprises the following steps:
(1) a solvent blending method is adopted to prepare CDA acetone solution and PEG acetone solution with equal mass fractions, and the specific operation is as follows: dissolving Cellulose Diacetate (CDA) in an acetone solution at room temperature, and placing the solution in a vibrator to vibrate for 1h to obtain a CDA acetone solution; dissolving polyethylene glycol (PEG) in an acetone solution at 40 ℃, and stirring in a water bath for 1h to obtain a PEG acetone solution;
(2) slowly dripping a certain mass of CDA acetone solution into the PEG acetone solution, quickly stirring for 10 minutes, adding a certain mass of metal powder, and stirring in a sealed water bath at 40 ℃ for 6 hours;
(3) after stirring, transferring the mixed solution to a culture dish, putting the culture dish into a fume hood for air drying, and then putting the culture dish into a 50 ℃ oven for drying for 12 hours;
(4) and crushing, tabletting, crushing and sieving the prepared material to obtain cellulose diacetate composite sizing phase-change material particles with a certain diameter.
Furthermore, the cellulose diacetate composite shape-fixed phase-change material is granular, and the grain sizes are 10-20 meshes and 20-40 meshes.
Furthermore, the cellulose diacetate composite shaping phase-change material has good high-temperature resistance while keeping high phase-change enthalpy, and can keep stable form and no leakage at 170 ℃; high thermal stability, no weight loss and decomposition at 250 ℃.
The application of the cellulose diacetate composite sizing phase-change material is characterized in that cellulose diacetate composite sizing phase-change particles are added into a cooling section of a heating non-combustion cigarette iQOS filter tip.
Further, when the cellulose diacetate composite shaped phase change particles are added to a filter tip of a cigarette iQOS which is not burnt, sponge fixing material particles with certain length and pores are used in a temperature reduction section close to the cavity type container section, and the suction resistance is adjusted.
Furthermore, the sponge for fixing the particles and adjusting the suction resistance has the use length of 0-1.8cm, the cigarette loading suction resistance of 0.5-0.65kPa and is close to iQOS to heat the non-combustible cigarettes.
Has the advantages that: the cellulose diacetate composite shaping phase-change material has a rigid net structure and high-melting-point cellulose diacetate, so that the material has the characteristics of excellent thermal stability and solid-solid phase change; the phase transition from the PEG branched chain crystalline state to the amorphous state enables the material to realize the function of heat absorption and energy storage; the addition of the heat-conducting metal powder improves the heat-conducting property of the material and achieves the effect of rapid cooling. The smoke containing resistance of the cellulose diacetate composite sizing phase-change material is similar to iQOS raw smoke, the temperature of the smoke from the first mouth to the fourth mouth can be obviously reduced, and the temperature of the smoke from the first mouth can be reduced to 36 ℃.
Drawings
FIG. 1 is a temperature rise test chart of a PEG6000/CDA composite phase change material;
FIG. 2 is a temperature rise test chart of the PEG4000/CDA composite phase change material;
FIG. 3 is an XRD spectrum of the PEG6000/CDA/Ag composite sizing material;
FIG. 4 is an XRD spectrum of the PEG4000/CDA/Cu composite sizing material;
FIG. 5 is an infrared spectrum of PEG 6000/CDA;
FIG. 6 is an infrared spectrum of PEG 4000/CDA;
FIG. 7 is a temperature rise test chart of the composite shape-stabilized phase-change material;
FIG. 8 is a graph of TG and DTG of PEG6000/CDA composite shape-stabilized phase-change material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below so that those skilled in the art can better understand the advantages and features of the present invention, and thus the scope of the present invention will be more clearly defined. The embodiments described herein are only a few embodiments of the present invention, rather than all embodiments, and all other embodiments that can be derived by one of ordinary skill in the art without inventive faculty based on the embodiments described herein are intended to fall within the scope of the present invention.
The cellulose diacetate composite shaping phase-change material for reducing the smoke temperature of a heated non-combustible cigarette is prepared from the following raw materials in percentage by mass by a solvent blending method: 10-50% of cellulose diacetate, 50-90% of phase change material and 1-5% of heat conduction material.
The phase change material is polyethylene glycol, and the molecular weight of the polyethylene glycol is 2000-10000. The heat conduction material is copper powder or silver powder, and the particle size is 200-600 meshes.
The preparation method of the cellulose diacetate composite sizing phase-change material comprises the following steps:
(1) a solvent blending method is adopted to prepare CDA acetone solution and PEG acetone solution with equal mass fractions, and the specific operation is as follows: dissolving Cellulose Diacetate (CDA) in an acetone solution at room temperature, and placing the solution in a vibrator to vibrate for 1 h; dissolving polyethylene glycol (PEG) in an acetone solution at 40 ℃, and stirring in a water bath for 1 h;
(2) slowly dripping a certain mass of CDA acetone solution into the PEG acetone solution, quickly stirring for 10 minutes, adding a certain mass of metal powder, and stirring in a sealed water bath at 40 ℃ for 6 hours;
(3) after stirring, transferring the mixed solution to a culture dish, putting the culture dish into a fume hood for air drying, and then putting the culture dish into a 50 ℃ oven for drying for 12 hours;
(4) and crushing, tabletting, crushing and sieving the prepared material to obtain cellulose diacetate composite sizing phase-change material particles with a certain diameter.
The preparation method has the advantages of simple preparation process, no pollution in the preparation process and easiness in industrial production, and the cellulose diacetate is the raw cigarette filter tip material and is non-toxic and harmless with the prepared composite sizing phase-change material.
The cellulose diacetate composite sizing phase change material prepared by the invention is granular, and the grain size is 10-20 meshes and 20-40 meshes. The cellulose diacetate composite shaping phase-change material has good high-temperature resistance while keeping higher phase-change enthalpy, and can keep stable form and no leakage at 170 ℃; high thermal stability, no weight loss and decomposition at 250 ℃.
The application of the cellulose diacetate composite sizing phase change particles is as follows: adding cellulose diacetate composite shaped phase change particles into a temperature reduction section of a heating non-combustion cigarette iQOS filter tip; when the cellulose diacetate composite shaped phase change particles are added to a filter tip of a cigarette iQOS which is not burnt by heating, sponge fixing material particles with certain length and pores are used in a cooling section close to the cavity type container section, and the suction resistance is adjusted. Wherein the sponge for fixing the particles and adjusting the suction resistance has the use length of 0-1.8cm, the cigarette loading suction resistance of 0.5-0.65kPa and is close to iQOS to heat the non-combustible cigarettes.
In the invention, the cellulose diacetate is a food grade raw material, and the phase-change material polyethylene glycol is a medicine grade raw material. Both are non-toxic and harmless. Dissolving Cellulose Diacetate (CDA) in an acetone solution at room temperature, and placing the solution in a vibrator to vibrate for 1 h; polyethylene glycol (PEG) was dissolved in acetone solution at 40 ℃ and stirred in a water bath for 1 h. The CDA acetone solution and the PEG acetone solution have equal mass fractions, and are both 9.3 percent.
Specific example 1 preparation of PEG6000/CDA composite shape-stabilized phase-change material particles
Slowly dripping 10g of CDA acetone solution into 40g of PEG6000 acetone solution, and stirring in a sealed water bath at 40 ℃ for 6 hours; after stirring, transferring the mixed solution to a culture dish, putting the culture dish into a fume hood for air drying, and then putting the culture dish into a 50 ℃ oven for drying for 12 hours; and crushing the prepared material, tabletting, and sieving by a 20-40-mesh sieve after crushing to obtain 20-40-mesh particles of the cellulose diacetate composite sizing phase change material.
The application of the PEG6000/CDA composite shape-fixed phase-change material particles comprises the following steps: the sample particles of 20-40 meshes are filled into iQOS cigarette branches, and 5 cigarettes are put into a Y450AKC01 type draw resistance sorter to measure the average draw resistance. And (3) placing the heated non-burning cigarette filled with the phase change particles in a smoking machine of the S45000601 type to perform a simulated smoking test, and measuring and recording the temperature of the end of the filter tip by using a thermocouple. The PEG6000/CDA composite sizing phase-change material particles with 20-40 meshes can reduce the temperature of the first smoke at the filter tip from 58 ℃ of a control sample iQOS heated non-combustion cigarette product to 36 ℃, and the whole temperature reduction effect is better than that of the control sample.
Specific example 2 preparation of PEG4000/CDA composite shaped phase change material particles
Slowly dripping 15g of CDA acetone solution into 35g of PEG4000 acetone solution, and stirring in a sealed water bath at 40 ℃ for 6 hours; after stirring, transferring the mixed solution to a culture dish, putting the culture dish into a fume hood for air drying, and then putting the culture dish into a 50 ℃ oven for drying for 12 hours; and crushing the prepared material, tabletting, and sieving by a 10-20-mesh sieve after crushing to obtain the cellulose diacetate composite sizing phase change material particles of 10-20 meshes.
The application of PEG4000/CDA composite shaped phase change material particles comprises the following steps: the test method was the same as in example 1; the PEG4000/CDA composite sizing phase-change material particles with 10-20 meshes can reduce the temperature of the first mouth smoke at the filter tip from 54 ℃ of a control sample iQOS heating non-combustion cigarette product to 41 ℃, the suction resistance is 0.55kPa, and the temperature reduction effect of the first 8 mouths is obviously better than that of an iQOS blank sample.
Specific example 3 preparation of PEG6000/CDA/Ag composite shaped phase-change Material particles
Slowly dripping 10g of CDA acetone solution into 40g of PEG6000 acetone solution, quickly stirring for 10 minutes, adding a certain mass of metal powder, and stirring in a sealed water bath at 40 ℃ for 6 hours; after stirring, transferring the mixed solution to a culture dish, putting the culture dish into a fume hood for air drying, and then putting the culture dish into a 50 ℃ oven for drying for 12 hours; and crushing the prepared material, tabletting, and sieving by a 20-40-mesh sieve after crushing to obtain 20-40-mesh particles of the cellulose diacetate composite sizing phase change material.
The application of the PEG6000/CDA/Ag composite shaped phase-change material particles comprises the following steps: the test method was the same as in example 1; the PEG6000/CDA/Ag composite shaped phase-change material particles with 20-40 meshes can reduce the temperature of the first smoke at the filter tip from 58 ℃ of a control iQOS heated non-combustion cigarette product to 39 ℃, and the whole temperature reduction effect is better than that of the iQOS and a 1.8cm sponge blank sample.
Specific example 4 preparation of PEG4000/CDA/Cu composite shaped phase-change Material particles
Slowly dripping 15g of CDA acetone solution into 35g of PEG4000 acetone solution, quickly stirring for 10 minutes, adding a certain mass of metal powder, and stirring in a sealed water bath at 40 ℃ for 6 hours; after stirring, transferring the mixed solution to a culture dish, putting the culture dish into a fume hood for air drying, and then putting the culture dish into a 50 ℃ oven for drying for 12 hours; and crushing the prepared material, tabletting, and sieving by a 10-20-mesh sieve after crushing to obtain the cellulose diacetate composite sizing phase change material particles of 10-20 meshes.
The application of the PEG4000/CDA/Cu composite shaped phase-change material particles comprises the following steps: the test method was the same as in example 1; the PEG4000/CDA/Cu composite sizing phase-change material particles with 10-20 meshes can reduce the temperature of the first mouth smoke at the filter tip from 54 ℃ of a control sample iQOS heating non-combustion cigarette product to 42 ℃, the suction resistance is only 0.529kPa, and the temperature reduction effect of the first 8 mouths is better than that of the control sample. And compared with a blank sponge sample (0.45kPa, 0.9cm), the overall cooling curve is lower than that of the blank sponge sample, and the prepared composite sizing phase-change material particles can obviously reduce the smoke temperature of the cigarette which is not combusted by heating.
The temperature rise test of the present invention is as follows: FIG. 1 is a photograph of a PEG6000/CDA composite phase change material during a temperature rise test. The experimental variable is only the mass ratio of the phase change material PEG6000 to the cellulose diacetate. The diagrams a, b, c, d and e respectively represent PEG6000/CDA composite phase change materials with the mass ratio of 90: 10, 85: 15, 80: 20, 70: 30 and 50: 50. It can be observed from the photo that the composite phase change materials with the mass ratio of 85: 15, 70: 30, 90: 10 and 50: 50 are transparent in turn in the process of continuously increasing the temperature, and the leakage phenomenon of other composite phase change materials is generated to a certain extent at 170 ℃ except that the composite phase change material with the mass ratio of 80: 20 is not obviously changed. This indicates that the PEG 6000: CDA mass ratio is 80: 20, and the composite phase change material has the best high temperature resistance effect. Therefore, the PEG6000/CDA composite phase change material with the mass ratio of 80: 20 is a cellulose diacetate shaping phase change material and has the characteristic of solid-solid phase change.
FIG. 2 is a photograph of the PEG4000/CDA composite phase change material during the temperature rise test. The experimental variable was simply the mass ratio of the phase change material PEG4000 to cellulose diacetate. The diagrams a, b, c, d and e respectively represent PEG4000/CDA composite phase change materials at mass ratios of 90: 10, 85: 15, 80: 20, 70: 30 and 50: 50. As can be seen from the photographs, the four groups of samples with the mass ratio of 90: 10, 85: 15, 80: 20 and 50: 50 all have melting phenomena with different degrees along with the continuous increase of the temperature, and the samples with the mass ratio of 70: 30 do not have obvious change. This indicates a mass ratio of 70: the PEG4000/CDA composite phase-change material prepared at 30 hours has good thermal stability, can resist the high temperature of 170 ℃ and is a sizing phase-change material.
The X-ray diffraction (XRD) analysis of the present invention is as follows: FIG. 3 is the XRD spectra of pure PEG6000, silver powder, PEG6000/CDA and PEG 6000/CDA/Ag. FIG. 4 is an XRD spectrum of PEG4000, copper powder, PEG4000/CDA and PEG4000/CDA/Cu composite shape-fixing phase-change material. It can be seen from fig. 3 that pure PEG6000 has strong peaks at 18.92 ° and 23.02 ° 2 θ, showing its crystalline structure. The addition of CDA reduced the intensity of the PEG6000 diffraction peak, indicating a decrease in crystallinity. The Ag powder has 3 obvious characteristic diffraction peaks at 2 theta of 38 degrees, 44.2 degrees and 64.4 degrees, and meanwhile, the XRD pattern of PEG6000/CDA/Ag also shows the corresponding characteristic peaks of the PEG6000 and the Ag powder. These results indicate that PEG of PEG6000/CDA/Ag branched chain is in crystalline state, and the introduction of Ag powder in the composite material does not affect the crystal structure.
The infrared absorption spectrum of the present invention is measured as follows: FIG. 5 and FIG. 6 are the infrared spectra of PEG6000/CDA at the mass ratio of 80: 20 and PEG4000/CDA at the mass ratio of 70: 30 respectively. As can be seen from FIG. 5, pure PEG6000 at 2887cm-1The characteristic peak at (A) is due to C-H stretching vibration of methylene. 1112cm-1The peak at (A) is caused by the stretching vibration of C-O-C. While pure CDA was at 1732cm-1Stretching vibration peak at 1240cm of carbonyl-1In the presence of an acetyl ester bond, 1375cm-1And 1435cm-1Is in the position of-CH3Symmetric and asymmetric deformation vibration peaks. Compared with CDA alone, the carbonyl peak of the PEG6000/CDA composite sizing phase-change material is from 1732cm-1Move to a lower 1755cm-1It is suggested that hydrogen bonds may be partially formed between carbonyl and hydroxyl groups in the PEG and CDA blend system. All the characteristic absorption peaks of PEG and CDA appear in the spectra of PEG6000/CDA and PEG4000/CDA, and no new peak appears, which indicates that PEG and CDA are physically mixed well by using a solvent blending method.
The heat conductivity of the present invention was tested as follows: sequentially comparing the mass ratio of 70: 30 PEG4000/CDA composite shape-stabilized phase-change material and PEG4000/CDA composite shape-stabilized phase-change material added with 1 wt%, 3 wt% and 5 wt% copper powder are subjected to temperature rise test, the temperature of the sample is recorded every 10 seconds, and the heat conductivity of each sample is compared. As can be seen from FIG. 7, the temperature was raised to 70 ℃ and the sample with 5% copper powder added took only about 68 seconds, the sample with 3% copper powder added took about 95 seconds, the sample with 1% copper powder added took about 130 seconds, and the PEG4000/CDA composite shape-stabilized phase change material without copper powder took about 350 seconds, so it can be concluded that: when 0-5 wt% of copper powder is added, the higher the content of the copper powder is, the better the heat-conducting property of the cellulose diacetate composite shaping phase-change material is.
The differential thermogravimetric analysis (TG) of the present invention is as follows: the thermogravimetric curve of the PEG6000/CDA (80: 20) composite shaped phase change material is shown in FIG. 8. For the PEG6000/CDA composite shape-stabilized phase-change material, a TG curve and a DTG (differential curve) of TG are kept as horizontal straight lines before 250 ℃, which shows that the material has no obvious decomposition reaction and weight loss below 250 ℃, has good thermal stability and meets the application condition of being added to a temperature reduction section of a heating non-combustible cigarette.
The Differential Scanning Calorimeter (DSC) of the present invention is shown in the enthalpy change analysis table of the samples of Table 1 below.
Enthalpy change analysis of the samples of Table 1
The cigarette loading and resistance test of the invention is as follows: the sample particles were loaded into iQOS cigarettes, the sponge length and the cigarette loading quality were recorded, and 5 cigarettes were placed in a Y450AKC01 type draw resistance sorter for resistance measurements, the detailed data being recorded as shown in tables 2 and 3 below.
TABLE 2 resistance to draw, sponge length and cigarette loading quality for samples of 20-40 mesh particles
TABLE 3 resistance to draw, sponge length and cigarette loading quality for sample 10-20 mesh particles
The temperature reduction test of the simulated smoking machine disclosed by the invention is as follows: iQOS produced by Felmo international is adopted to heat non-burning cigarettes as a blank sample, and polylactic acid film sheets in iQOS are replaced by sponge samples with different lengths for comparison with a control sample. Table 4 and Table 5 show the temperature reduction test data of the front three ports of the simulated smoking machine for 20-40 and 10-20 mesh sample particles respectively.
TABLE 4 sample temperature of three-mouth filter tip before 20-40 mesh particle cooling test
TABLE 5 sample temperature of three-mouth filter tip before 10-20 mesh particle cooling test
The cellulose diacetate composite shaping phase-change material has a rigid net structure and high-melting-point cellulose diacetate, so that the material has the characteristics of excellent thermal stability and solid-solid phase change; the phase transition from the PEG branched chain crystalline state to the amorphous state enables the material to realize the function of heat absorption and energy storage; the addition of the heat-conducting metal powder improves the heat-conducting property of the material and achieves the effect of rapid cooling. The smoke containing resistance of the cellulose diacetate composite sizing phase-change material is similar to iQOS raw smoke, the temperature of the smoke from the first mouth to the fourth mouth can be obviously reduced, and the temperature of the smoke from the first mouth can be reduced to 36.2 ℃ at most.
Claims (9)
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| CN202010146958.7A CN111218099A (en) | 2020-03-05 | 2020-03-05 | A kind of cellulose diacetate composite stereotyped phase change material and its preparation method and application |
| PCT/CN2020/100977 WO2020259713A1 (en) | 2020-03-05 | 2020-07-09 | Cellulose diacetate composite shape-stabilized phase change material and preparation method and use therefor |
| ZA2021/00219A ZA202100219B (en) | 2020-03-05 | 2021-01-13 | Cellulose diacetate composite shape-stabilized phase change material and preparation method and use therefor |
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| CN111945241A (en) * | 2020-08-25 | 2020-11-17 | 南通醋酸纤维有限公司 | Temperature-regulating composite material aggregate for cigarettes, preparation method and application |
| CN111944493A (en) * | 2020-08-25 | 2020-11-17 | 甘肃烟草工业有限责任公司 | Composite phase-change material for reducing cigarette smoke temperature and preparation method and application thereof |
| WO2020259713A1 (en) * | 2020-03-05 | 2020-12-30 | 南通大学 | Cellulose diacetate composite shape-stabilized phase change material and preparation method and use therefor |
| CN112280536A (en) * | 2020-09-18 | 2021-01-29 | 湖北中烟工业有限责任公司 | A kind of cooling energy storage phase change material used in novel tobacco filter rod and preparation method thereof |
| CN113174238A (en) * | 2021-04-13 | 2021-07-27 | 深圳市康吸科技有限公司 | Composite phase change material for rapidly reducing smoke temperature of electronic cigarette, preparation method of composite phase change material and electronic cigarette |
| CN113197334A (en) * | 2021-04-28 | 2021-08-03 | 河南中烟工业有限责任公司 | Preparation method of heating cigarette cooling section |
| CN114376266A (en) * | 2022-02-24 | 2022-04-22 | 杭州高烯科技有限公司 | One-section type cigarette holder |
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| WO2020259713A1 (en) * | 2020-03-05 | 2020-12-30 | 南通大学 | Cellulose diacetate composite shape-stabilized phase change material and preparation method and use therefor |
| CN111945241A (en) * | 2020-08-25 | 2020-11-17 | 南通醋酸纤维有限公司 | Temperature-regulating composite material aggregate for cigarettes, preparation method and application |
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| CN111944493B (en) * | 2020-08-25 | 2021-11-05 | 甘肃烟草工业有限责任公司 | Composite phase-change material for reducing cigarette smoke temperature and preparation method and application thereof |
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| CN113174238A (en) * | 2021-04-13 | 2021-07-27 | 深圳市康吸科技有限公司 | Composite phase change material for rapidly reducing smoke temperature of electronic cigarette, preparation method of composite phase change material and electronic cigarette |
| CN113174238B (en) * | 2021-04-13 | 2021-11-16 | 深圳市康吸科技有限公司 | Composite phase change material for rapidly reducing smoke temperature of electronic cigarette, preparation method of composite phase change material and electronic cigarette |
| CN113197334A (en) * | 2021-04-28 | 2021-08-03 | 河南中烟工业有限责任公司 | Preparation method of heating cigarette cooling section |
| CN114376266A (en) * | 2022-02-24 | 2022-04-22 | 杭州高烯科技有限公司 | One-section type cigarette holder |
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| ZA202100219B (en) | 2021-09-29 |
| WO2020259713A1 (en) | 2020-12-30 |
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