CN116064194B - Mint-flavored tipping paper essence and preparation method thereof - Google Patents
Mint-flavored tipping paper essence and preparation method thereof Download PDFInfo
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- CN116064194B CN116064194B CN202310159670.7A CN202310159670A CN116064194B CN 116064194 B CN116064194 B CN 116064194B CN 202310159670 A CN202310159670 A CN 202310159670A CN 116064194 B CN116064194 B CN 116064194B
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- tipping paper
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- enol
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000004698 Polyethylene Substances 0.000 claims abstract description 69
- -1 polyethylene Polymers 0.000 claims abstract description 69
- 229920000573 polyethylene Polymers 0.000 claims abstract description 69
- 239000000463 material Substances 0.000 claims abstract description 58
- 239000011162 core material Substances 0.000 claims abstract description 44
- 239000001525 mentha piperita l. herb oil Substances 0.000 claims abstract description 40
- 235000019477 peppermint oil Nutrition 0.000 claims abstract description 40
- 239000003094 microcapsule Substances 0.000 claims abstract description 38
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims description 57
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 51
- 150000002085 enols Chemical class 0.000 claims description 48
- 238000010438 heat treatment Methods 0.000 claims description 35
- 238000001816 cooling Methods 0.000 claims description 33
- 239000000839 emulsion Substances 0.000 claims description 27
- 238000001694 spray drying Methods 0.000 claims description 26
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- GHBFNMLVSPCDGN-UHFFFAOYSA-N rac-1-monooctanoylglycerol Chemical compound CCCCCCCC(=O)OCC(O)CO GHBFNMLVSPCDGN-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000010008 shearing Methods 0.000 claims description 17
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 14
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 claims description 13
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 13
- 235000006679 Mentha X verticillata Nutrition 0.000 claims description 12
- 235000002899 Mentha suaveolens Nutrition 0.000 claims description 12
- 235000001636 Mentha x rotundifolia Nutrition 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical group C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000796 flavoring agent Substances 0.000 claims description 8
- 235000019634 flavors Nutrition 0.000 claims description 8
- 229940087068 glyceryl caprylate Drugs 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 8
- 239000003999 initiator Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 4
- UFLHIIWVXFIJGU-ARJAWSKDSA-N (Z)-hex-3-en-1-ol Chemical compound CC\C=C/CCO UFLHIIWVXFIJGU-ARJAWSKDSA-N 0.000 claims description 3
- ZSPTYLOMNJNZNG-UHFFFAOYSA-N 3-Buten-1-ol Chemical compound OCCC=C ZSPTYLOMNJNZNG-UHFFFAOYSA-N 0.000 claims description 3
- UFLHIIWVXFIJGU-UHFFFAOYSA-N hex-3-en-1-ol Natural products CCC=CCCO UFLHIIWVXFIJGU-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000013270 controlled release Methods 0.000 abstract description 3
- 239000000686 essence Substances 0.000 description 50
- 239000000243 solution Substances 0.000 description 41
- 235000019504 cigarettes Nutrition 0.000 description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 238000002844 melting Methods 0.000 description 16
- 230000008018 melting Effects 0.000 description 16
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 13
- 239000002775 capsule Substances 0.000 description 11
- 230000000391 smoking effect Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000003921 oil Substances 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- 238000011049 filling Methods 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 235000019198 oils Nutrition 0.000 description 8
- FSUXYWPILZJGCC-IHWYPQMZSA-N (z)-pent-3-en-1-ol Chemical compound C\C=C/CCO FSUXYWPILZJGCC-IHWYPQMZSA-N 0.000 description 6
- 235000016257 Mentha pulegium Nutrition 0.000 description 6
- 244000246386 Mentha pulegium Species 0.000 description 6
- 235000004357 Mentha x piperita Nutrition 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 125000005456 glyceride group Chemical group 0.000 description 6
- 229940075507 glyceryl monostearate Drugs 0.000 description 6
- 235000001050 hortel pimenta Nutrition 0.000 description 6
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 241000208125 Nicotiana Species 0.000 description 3
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 3
- 239000003205 fragrance Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical group CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 229940075529 glyceryl stearate Drugs 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000008368 mint flavor Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000019476 oil-water mixture Nutrition 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000007762 w/o emulsion Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0007—Aliphatic compounds
- C11B9/0015—Aliphatic compounds containing oxygen as the only heteroatom
-
- 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
- A24D1/00—Cigars; Cigarettes
- A24D1/002—Cigars; Cigarettes with additives, e.g. for flavouring
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/025—Applications of microcapsules not provided for in other subclasses
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Dispersion Chemistry (AREA)
- Paper (AREA)
Abstract
The invention provides a mint-flavored tipping paper essence and a preparation method thereof, wherein the mint-flavored tipping paper essence comprises microcapsule wall materials and core materials wrapped in the microcapsule wall materials, the core materials comprise peppermint oil, an emulsifying agent and a solvent, the wall materials are enol-grafted modified polyethylene, and the mint-flavored tipping paper essence disclosed by the invention adopts the enol-grafted modified polyethylene as the microcapsule wall materials, so that the temperature controlled release performance of the essence is improved.
Description
Technical Field
The invention relates to the technical field of essences, in particular to a mint-flavored tipping paper essence and a preparation method thereof.
Background
The tipping paper is a cigarette auxiliary material which is used for wrapping and connecting a cigarette filter tip and a cigarette part, is different from the cigarette paper, does not generally participate in the combustion of the cigarette, but directly contacts with the mouth of a smoker of the cigarette, and essence on the surface of the tipping paper is mainly released in the process of contacting with the mouth of the smoker to supplement the fragrance of the cigarette, so that the defect of insufficient fragrance concentration before and after the combustion of the cigarette paper can be overcome.
The mint-flavored cool essence is widely applied to tobacco shreds and cigarette paper, however, the main active ingredient of the conventional mint essence is mint oil, and the mint oil is generally attached to the surface of tipping paper in a printing and coating mode, so that the mint oil applied in the mode is easy to volatilize, and the long-acting preservation effect of the flavor is poor. The microcapsule technology can carry out good encapsulation treatment on the peppermint oil component, avoids the quick volatilization of the peppermint oil, can improve the retention time of essence when being applied to the tipping paper essence technology, but the essence encapsulated by the microcapsule is slowly released, so that the experience of a cigarette taster is greatly reduced, and the problem of how to lead the microcapsule to controllably rupture and release the essence when in use is the technical problem to be solved at present.
Disclosure of Invention
In view of the above, in one aspect, the present invention provides a mint-flavored tipping paper essence, which aims to solve the problem that the mint-flavored essence applied to tipping paper cannot be controllably released.
The technical scheme of the invention is realized as follows: the invention provides a mint-flavored tipping paper essence, which is microcapsule type and comprises microcapsule wall materials and a core material wrapped in the microcapsule wall materials, wherein the core material comprises peppermint oil, an emulsifying agent and a solvent, and the wall materials are enol-grafted modified polyethylene and have a structure shown in a formula I: the core material comprises peppermint oil, an emulsifying agent and a solvent, wherein the wall material is enol grafted modified polyethylene and has a structure of formula I:
wherein R is 1 is-H, -CH 3 、-CH 2 One of OH, n and m are positive integers not less than 1.
In some embodiments, the number average molecular weight of the enol graft modified polyethylene is 3000-6000.
In some embodiments, the D50 particle size of the mint flavored tipping paper flavor is 5-30 μm.
In some embodiments, the core material comprises 5-10 parts by weight of peppermint oil, 0.1-0.5 parts by weight of an emulsifier, and 40-60 parts by weight of a solvent.
In some embodiments, the emulsifier comprises at least one of glyceryl monostearate, glyceryl monocaprylate, and span 60.
In some embodiments, the emulsifying agent comprises glyceryl monostearate, glyceryl monocaprylate, and span 60, the glyceryl stearate: glycerol monocaprylate: the mass ratio of span 60 is 1: (4-5): (2-3).
In some embodiments, the solvent is water.
On the other hand, the invention also provides a preparation method of the mint-flavored tipping paper essence, which comprises the following steps:
dissolving enol grafted modified polyethylene in toluene, and heating to 90-95 ℃ to obtain a wall material solution;
step two, dissolving the enol grafted modified polyethylene in toluene, and heating to 90-95 ℃ to obtain a wall material solution;
and thirdly, maintaining the high-speed shearing and stirring conditions of the core material emulsion, adding the wall material solution into the core material emulsion, maintaining the shearing and stirring temperature to be 85 ℃, and performing spray drying at a cooling rate of 5-10 ℃/h to obtain the mint-flavored tipping paper essence.
In some embodiments, the mass ratio of enol graft modified polyethylene to toluene is 1:10, the volume ratio of the wall material solution to the core material solution is 1:10.
in some embodiments, the conditions of spray drying include: the spray air inlet temperature is 120-130 ℃, and the air outlet temperature is 50-60 ℃.
Compared with the prior art, the mint-flavored tipping paper essence has the following beneficial effects:
the mint-flavored tipping paper essence adopts a microcapsule structure, wherein the wall material adopts polyethylene with the structure of formula I, and has a melting point which is closer to the use temperature of a cigarette holder, so that the capsule wall of the microcapsule is easy to be heated and broken in the smoking process, thereby releasing peppermint oil when the cigarette is ignited, improving the storage time of the peppermint oil essence in tipping paper, simultaneously ensuring the efficient release of the peppermint oil in the use process, and secondly, the polyethylene microcapsule wall material with the structure of formula I has better printing and attaching effects and is easier to attach on the surface of tipping paper compared with the conventional polyethylene.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
The invention relates to a mint flavor tipping paper essence, which adopts a microcapsule structure and comprises microcapsule wall materials and a core material wrapped in the microcapsule wall materials, wherein the core material consists of peppermint oil, an emulsifying agent and a solvent, the wall materials are enol grafted modified polyethylene, and the wall materials have a structure shown in a formula I:
wherein: r is R 1 is-H, -CH 3 、-CH 2 One of OH, n and m are positive integers not less than 1.
The mint-flavored tipping paper essence provided by the embodiment adopts a microcapsule structure, the wall material of the structural material of the formula I has the characteristic that the core material can be released more quickly at the ambient temperature of a cigarette holder in the cigarette setting-off process, and the microcapsule is easy to break under the action of external force suitable for the use environment of the cigarette holder, so that the mint oil can be released controllably, and the controlled release aim is achieved.
In some embodiments, n: m=1 (3-10)
In some embodiments, the enol graft modified polyethylene of formula I has a dredged molecular weight of 3000-6000.
In some embodiments, the D50 particle size of the mint flavored tipping paper flavor is 5-30 μm.
In some embodiments, the profile is composed of 5-10 parts by weight of peppermint oil, 0.1-0.5 part by weight of emulsifier and 40-60 parts by weight of solvent.
In some embodiments, the emulsifier includes at least one of glyceryl monostearate, glyceryl monocaprylate, and span 60.
In some embodiments, the emulsifier is composed of glyceryl monostearate, glyceryl monocaprylate and span 60 in a mass ratio of 1: (4-5): (2-3).
In some embodiments, the solvent is water.
In some embodiments, the enol graft modified polyethylene of the structure of formula I is obtained by heating polyethylene, an initiator and an enol monomer in a solvent to initiate a reaction, and the specific preparation method comprises the following steps:
adding polyethylene and enol monomer into dimethylbenzene, heating to 130-140 ℃, maintaining the temperature and stirring to obtain a solution, slowly dripping an initiator into the solution under the nitrogen atmosphere in a stirring state, maintaining the temperature and reacting for 3-5h, cooling to 25 ℃ after the reaction is finished, adding acetone, filtering and drying to obtain the enol grafted modified polyethylene.
Wherein the enol monomer is selected from one of 3-butene-1-ol, cis-3-pentene-1-ol and cis-3-hexene-1-ol.
Polyethylene: enol monomer: and (3) an initiator: the mass ratio of the dimethylbenzene is 1: (0.3-0.4): (0.2-0.3): (8-10), wherein the initiator is dicumyl peroxide.
The number average molecular weight of the polyethylene is 1000-3000.
The invention also provides a preparation method of the mint-flavored tipping paper essence, which comprises the following steps:
s1, dissolving enol grafted modified polyethylene shown in a formula I in toluene, and heating to 90-95 ℃ to obtain a wall material solution;
s2, mixing and stirring peppermint oil, an emulsifying agent and a solvent according to a proportion, heating to 90-95 ℃, and shearing and stirring at 8000-12000rpm to obtain core emulsion;
s3, adding the wall material solution into the core material emulsion under the condition of maintaining high-speed shearing and stirring of the core material emulsion, slowly cooling to 85 ℃ under the condition of maintaining shearing and stirring, controlling the cooling rate to be 5-10 ℃/h, and then performing spray drying treatment to obtain the mint-flavored tipping paper essence.
In the above embodiment, the enol graft modified polyethylene of the wall material is dissolved in toluene, the obtained wall material solution is used as a part of the oil phase, the peppermint oil and the solvent are stirred at high speed under the action of the emulsifier to form a water-in-oil emulsion system, wherein part of the peppermint oil is dissolved in the water phase, part of the peppermint oil forms the oil phase, the wall material solution is mixed with the peppermint oil in the slow adding process to form an oil phase, the suspension emulsion system is formed under the high-speed stirring action, the slow cooling process gradually stabilizes the suspension system, meanwhile, the wall materials are prevented from being quickly formed and adhered to each other, after spray drying, the melting point of the enol graft modified polyethylene is between 80 ℃ and 85 ℃ in the oil phase which is covered by the outer layer, so that a capsule wall is formed firstly, the core material inside the capsule wall comprises water, part of the peppermint oil dissolved in the water, the emulsifier and part of the peppermint oil which is mutually dissolved with the emulsifier, the temperature of the microcapsule is gradually reduced in the latter half of spray drying, the microcapsule is finally dried, and the microcapsule system which is covered by the oil-water mixture is obtained.
In some embodiments, the mass ratio of enol graft modified polyethylene to toluene is 1:10 and the volume ratio of wall material solution to core material solution is 1:10.
In the above embodiment, the grafted polyethylene capsule wall has good mechanical properties, and in order to further improve the controlled release property of the grafted polyethylene capsule wall, the amount of the wall material solution is controlled to be 10% of the amount of the core material solution, so that the thickness of the wall material is thinner, and the wall material is easier to break under the action of external force.
Meanwhile, in the above embodiment, in order to avoid the influence of the fast concentrated release of the peppermint oil component in the microcapsule after rupture to the feeling of the second half of smoking, the emulsifier includes at least one of monoglyceride stearate, monocaprylic acid glyceride and span 60, wherein the melting point of the monoglyceride stearate is similar to that of the grafted polyethylene of formula I, when the grafted polyethylene capsule wall is ruptured, the monoglyceride stearate can play a role of a certain capsule wall, so as to avoid the too fast release of the peppermint oil-water system in the capsule wall, the span 60 and monocaprylic acid glyceride have relatively lower melting points, when the span 60 or monocaprylic acid glyceride is used as the emulsifier, the solid span 60 and monocaprylic acid glyceride can also maintain the peppermint oil-water system in the capsule wall after the rupture of the microcapsule, so as to avoid the fast release of the peppermint oil-water system, when the capsule wall is ruptured, and when a certain temperature rise occurs in the use process of the cigarette holder, the span 60, the monocaprylic acid glyceride or the monocaprylic acid glyceride can cause the peppermint oil-water system to be released more quickly after being heated.
It is known that in the first half of smoking, the temperature of the high temperature region of the tobacco tip cannot be quickly transferred to the position of the cigarette holder, at this time, microcapsule essence on the surface of tipping paper releases peppermint oil through the slow release effect of the microcapsule essence and the quick release effect of the microcapsule which is partially broken due to stress, when the temperature of the high temperature region of the tobacco tip is gradually transferred to the position of the cigarette holder, the capsule wall of the microcapsule essence melts, and meanwhile, the speed of releasing the inner peppermint oil-water system by the microcapsule core material is increased, and the fragrance feeling of the second half of smoking can be improved by adopting staged release.
In some embodiments, the conditions of spray drying include: the temperature of spray air inlet is 120-130 ℃, and the temperature of air outlet is 50-60 ℃.
The essence of the embodiment adopts a water-in-oil system, and meanwhile, the melting point of the wall material is between 80 and 85 ℃ and the discharging temperature is 85 ℃, so that the temperature of spray air inlet is not too high, the microcapsule forming effect is good when the temperature of air outlet is controlled between 50 and 60 ℃, and the size of the microcapsule is maintained between 5 and 30 mu m, so that the microcapsule is easier to be used for applying the surface of tipping paper.
In the above examples, the graft modified polyethylene has a certain hydroxyl group, so that it has a certain hydrophilicity, and can improve the adhesion between the essence and the tipping paper.
In order to further illustrate the present invention, the following detailed description of the mint-flavored tipping paper essence and the preparation method thereof is provided in connection with specific examples, which are not to be construed as limiting the scope of protection of the present invention.
Example 1
Respectively adding 10 parts of polyethylene with average molecular weight of 1000 and 3 parts of 3-buten-1-ol into 80 parts of dimethylbenzene, heating to 130 ℃, keeping the temperature and stirring to obtain a solution, filling nitrogen into a reaction container for replacement under a stirring state, then dropwise adding 2 parts of dicumyl peroxide, keeping the temperature and reacting for 3 hours after the dropwise adding is finished, cooling to 25 ℃, adding 80 parts of acetone under stirring until solid is separated out, and filtering to obtain enol grafted modified polyethylene, wherein the number average molecular weight of the enol grafted modified polyethylene is 3000, and the melting point is 78.4 ℃;
step two, respectively mixing 10 parts of the enol graft modified polyethylene prepared in the step one with 100 parts of toluene, and heating to 90 ℃ to obtain a wall material solution; mixing 5 parts of peppermint oil, 0.1 part of monoglyceride stearate and 40 parts of water, heating to 90 ℃, and stirring in a high-speed shearing machine at 8000rpm to obtain core emulsion; slowly adding 1 volume of wall material solution into 10 volumes of core material emulsion, keeping stirring speed at 8000rpm, cooling to 85 ℃ according to cooling speed at 5 ℃/h after the addition, and spray drying to obtain mint-flavored tipping paper essence, wherein the spray drying conditions comprise: the inlet air temperature is 120 ℃, and the outlet air temperature is 50 ℃.
Example 2
Respectively adding 10 parts of polyethylene with average molecular weight of 1000 and 3 parts of cis-3-penten-1-ol into 80 parts of dimethylbenzene, heating to 130 ℃, keeping the temperature and stirring to obtain a solution, filling nitrogen into a reaction container for replacement under a stirring state, then dropwise adding 2 parts of dicumyl peroxide, keeping the temperature and reacting for 3 hours after the dropwise adding is finished, cooling to 25 ℃, adding 80 parts of acetone under stirring until solid is separated out, and filtering to obtain enol grafting modified polyethylene, wherein the number average molecular weight of the enol grafting modified polyethylene is 4000, and the melting point is 77.6 ℃;
step two, respectively mixing 10 parts of the enol graft modified polyethylene prepared in the step one with 100 parts of toluene, and heating to 90 ℃ to obtain a wall material solution; mixing 5 parts of peppermint oil, 0.3 part of monoglyceride stearate and 40 parts of water, heating to 90 ℃, and stirring in a high-speed shearing machine at 8000rpm to obtain core emulsion; slowly adding 1 volume of wall material solution into 10 volumes of core material emulsion, keeping stirring speed at 8000rpm, cooling to 85 ℃ according to cooling speed at 5 ℃/h after the addition, and spray drying to obtain mint-flavored tipping paper essence, wherein the spray drying conditions comprise: the inlet air temperature is 120 ℃, and the outlet air temperature is 50 ℃.
Example 3
Respectively adding 10 parts of polyethylene with average molecular weight of 1000 and 3 parts of cis-3-hexene-1-ol into 80 parts of dimethylbenzene, heating to 130 ℃, keeping the temperature and stirring to obtain a solution, filling nitrogen into a reaction container for replacement under a stirring state, then dropwise adding 2 parts of dicumyl peroxide, keeping the temperature and reacting for 3 hours after the dropwise adding is finished, cooling to 25 ℃, adding 80 parts of acetone under stirring until solid is separated out, and filtering to obtain enol grafted modified polyethylene, wherein the number average molecular weight of the enol grafted modified polyethylene is 5000, and the melting point is 75.2 ℃;
step two, respectively mixing 10 parts of the enol graft modified polyethylene prepared in the step one with 100 parts of toluene, and heating to 90 ℃ to obtain a wall material solution; mixing 5 parts of peppermint oil, 0.3 part of monoglyceride stearate and 40 parts of water, heating to 90 ℃, and stirring in a high-speed shearing machine at 8000rpm to obtain core emulsion; slowly adding 1 volume of wall material solution into 10 volumes of core material emulsion, keeping stirring speed at 8000rpm, cooling to 85 ℃ according to cooling speed at 5 ℃/h after the addition, and spray drying to obtain mint-flavored tipping paper essence, wherein the spray drying conditions comprise: the inlet air temperature is 120 ℃, and the outlet air temperature is 50 ℃.
Example 4
Respectively adding 10 parts of polyethylene with average molecular weight of 3000 and 4 parts of cis-3-penten-1-ol into 100 parts of xylene, heating to 140 ℃, keeping the temperature and stirring to obtain a solution, filling nitrogen into a reaction container for replacement under a stirring state, then dropwise adding 3 parts of dicumyl peroxide, keeping the temperature and reacting for 5 hours after the dropwise adding is finished, cooling to 25 ℃, adding 100 parts of acetone under stirring until solid is separated out, and filtering to obtain enol grafted modified polyethylene, wherein the number average molecular weight of the enol grafted modified polyethylene is 5000, and the melting point is 77.2 ℃;
step two, respectively mixing 10 parts of the enol graft modified polyethylene prepared in the step one with 100 parts of toluene, and heating to 95 ℃ to obtain a wall material solution; mixing 5 parts of peppermint oil, 0.3 part of monoglyceride stearate and 40 parts of water, heating to 95 ℃, and stirring in a high-speed shearing machine at 8000rpm to obtain core emulsion; slowly adding 1 volume of wall material solution into 10 volumes of core material emulsion, keeping stirring speed at 8000rpm, cooling to 85 ℃ according to cooling speed at 5 ℃/h after the addition, and spray drying to obtain mint-flavored tipping paper essence, wherein the spray drying conditions comprise: the inlet air temperature is 120 ℃, and the outlet air temperature is 50 ℃.
Example 5
Respectively adding 10 parts of polyethylene with average molecular weight of 1000 and 3 parts of cis-3-penten-1-ol into 80 parts of dimethylbenzene, heating to 130 ℃, keeping the temperature and stirring to obtain a solution, filling nitrogen into a reaction container for replacement under a stirring state, then dropwise adding 2 parts of dicumyl peroxide, keeping the temperature and reacting for 3 hours after the dropwise adding is finished, cooling to 25 ℃, adding 80 parts of acetone under stirring until solid is separated out, and filtering to obtain enol grafting modified polyethylene, wherein the number average molecular weight of the enol grafting modified polyethylene is 4000, and the melting point is 77.6 ℃;
step two, respectively mixing 10 parts of the enol graft modified polyethylene prepared in the step one with 100 parts of toluene, and heating to 90 ℃ to obtain a wall material solution; mixing 5 parts of peppermint oil, 0.3 part of glyceryl monostearate, 0.2 part of glyceryl monocaprylate and 40 parts of water, heating to 90 ℃, and stirring in a high-speed shearing machine at 8000rpm to obtain core emulsion; slowly adding 1 volume of wall material solution into 10 volumes of core material emulsion, keeping stirring speed at 8000rpm, cooling to 85 ℃ according to cooling speed at 5 ℃/h after the addition, and spray drying to obtain mint-flavored tipping paper essence, wherein the spray drying conditions comprise: the inlet air temperature is 120 ℃, and the outlet air temperature is 50 ℃.
Example 6
Respectively adding 10 parts of polyethylene with average molecular weight of 1000 and 3 parts of cis-3-penten-1-ol into 80 parts of dimethylbenzene, heating to 130 ℃, keeping the temperature and stirring to obtain a solution, filling nitrogen into a reaction container for replacement under a stirring state, then dropwise adding 2 parts of dicumyl peroxide, keeping the temperature and reacting for 3 hours after the dropwise adding is finished, cooling to 25 ℃, adding 80 parts of acetone under stirring until solid is separated out, and filtering to obtain enol grafting modified polyethylene, wherein the number average molecular weight of the enol grafting modified polyethylene is 4000, and the melting point is 77.6 ℃;
step two, respectively mixing 10 parts of the enol graft modified polyethylene prepared in the step one with 100 parts of toluene, and heating to 90 ℃ to obtain a wall material solution; mixing 5 parts of peppermint oil, 0.2 part of glyceryl monostearate, 0.1 part of glyceryl monocaprylate, 0.2 part of span 60 and 40 parts of water, heating to 90 ℃, and stirring in a high-speed shearing machine at a stirring speed of 8000rpm to obtain core emulsion; slowly adding 1 volume of wall material solution into 10 volumes of core material emulsion, keeping stirring speed at 8000rpm, cooling to 85 ℃ according to cooling speed at 5 ℃/h after the addition, and spray drying to obtain mint-flavored tipping paper essence, wherein the spray drying conditions comprise: the inlet air temperature is 120 ℃, and the outlet air temperature is 50 ℃.
Example 7
Respectively adding 10 parts of polyethylene with average molecular weight of 1000 and 3 parts of cis-3-penten-1-ol into 80 parts of dimethylbenzene, heating to 130 ℃, keeping the temperature and stirring to obtain a solution, filling nitrogen into a reaction container for replacement under a stirring state, then dropwise adding 2 parts of dicumyl peroxide, keeping the temperature and reacting for 3 hours after the dropwise adding is finished, cooling to 25 ℃, adding 80 parts of acetone under stirring until solid is separated out, and filtering to obtain enol grafting modified polyethylene, wherein the number average molecular weight of the enol grafting modified polyethylene is 4000, and the melting point is 77.6 ℃;
step two, respectively mixing 10 parts of the enol graft modified polyethylene prepared in the step one with 100 parts of toluene, and heating to 90 ℃ to obtain a wall material solution; mixing 5 parts of peppermint oil, 0.3 part of monoglyceride stearate and 40 parts of water, heating to 90 ℃, and stirring in a high-speed shearing machine at 12000rpm to obtain core emulsion; slowly adding 1 volume of wall material solution into 10 volumes of core material emulsion, keeping the stirring speed at 12000rpm, cooling to 85 ℃ according to the cooling speed of 5 ℃/h after the addition, and spray drying to obtain the mint-flavored tipping paper essence, wherein the spray drying conditions comprise: the inlet air temperature is 120 ℃, and the outlet air temperature is 50 ℃.
Example 8
Respectively adding 10 parts of polyethylene with average molecular weight of 1000 and 3 parts of cis-3-penten-1-ol into 80 parts of dimethylbenzene, heating to 130 ℃, keeping the temperature and stirring to obtain a solution, filling nitrogen into a reaction container for replacement under a stirring state, then dropwise adding 2 parts of dicumyl peroxide, keeping the temperature and reacting for 3 hours after the dropwise adding is finished, cooling to 25 ℃, adding 80 parts of acetone under stirring until solid is separated out, and filtering to obtain enol grafting modified polyethylene, wherein the number average molecular weight of the enol grafting modified polyethylene is 4000, and the melting point is 77.6 ℃;
step two, respectively mixing 10 parts of the enol graft modified polyethylene prepared in the step one with 100 parts of toluene, and heating to 90 ℃ to obtain a wall material solution; mixing 5 parts of peppermint oil, 0.3 part of monoglyceride stearate and 40 parts of water, heating to 90 ℃, and stirring in a high-speed shearing machine at 8000rpm to obtain core emulsion; slowly adding 1 volume of wall material solution into 10 volumes of core material emulsion, keeping stirring speed at 8000rpm, cooling to 85 ℃ according to cooling speed at 10 ℃/h after the addition, and spray drying to obtain mint-flavored tipping paper essence, wherein the spray drying conditions comprise: the inlet air temperature is 120 ℃, and the outlet air temperature is 50 ℃.
Comparative example 1
Respectively mixing 10 parts of polyethylene with 4000 average molecular weight with 100 parts of toluene, and heating to 90 ℃ to obtain a wall material solution; mixing 5 parts of peppermint oil, 0.3 part of monoglyceride stearate and 40 parts of water, heating to 90 ℃, and stirring in a high-speed shearing machine at 8000rpm to obtain core emulsion; slowly adding 1 volume of wall material solution into 10 volumes of core material emulsion, keeping stirring speed at 8000rpm, cooling to 85 ℃ according to cooling speed at 5 ℃/h after the addition, and spray drying to obtain mint-flavored tipping paper essence, wherein the spray drying conditions comprise: the inlet air temperature is 120 ℃, and the outlet air temperature is 50 ℃.
The particle size distribution of the microcapsule essence prepared in the comparative example is shown in the following table:
| grouping | D10 | D50 | D90 |
| Example 1 | 2.7μm | 26.7μm | 33.6μm |
| Example 2 | 3.4μm | 25.8μm | 35.1μm |
| Example 3 | 3.3μm | 22.4μm | 33.9μm |
| Example 4 | 3.4μm | 24.3μm | 34.1μm |
| Example 5 | 3.1μm | 23.8μm | 34.6μm |
| Example 6 | 2.9μm | 24.5μm | 33.6μm |
| Example 7 | 1.3μm | 15.2μm | 22.4μm |
| Example 8 | 3.9μm | 28.9μm | 39.5μm |
| Comparative example 1 | 3.5μm | 34.3μm | 42.5μm |
Mixing the essence with the fixed amount prepared in the above examples and comparative examples in a polyvinyl alcohol aqueous solution to obtain a coating liquid with a concentration of 10wt%, coating the coating liquid on the surface of tipping paper and preparing cigarettes from tipping paper with the essence, respectively using the prepared cigarettes for smoking simulation, and measuring embedding rate of microcapsules on the same surface area of tipping paper of a cigarette holder part of cigarettes of 1min,5min and 10min, wherein the theoretical amount of microcapsules per unit area of tipping paper surface is calculated as follows:
theoretical amount of essence per unit area= (unit area/total area of tipping paper coated) x total amount of essence coated
Embedding rate of surface microcapsule of tipping paper per unit area= (theoretical amount of peppermint oil in essence per unit area-residual peppermint oil amount of essence per unit area) ×100%.
Meanwhile, the essences prepared in the examples and the comparative examples are respectively stored for 1 month, 3 months and 6 months, and the embedding rate before and after storage is measured, and the specific obtained results are as follows:
| grouping | Initial embedding rate | Embedding rate of 1 month | Embedding rate of 3 months | Embedding rate of 6 months |
| Example 1 | 86.7％ | 85.5％ | 82.6％ | 78.9％ |
| Example 2 | 92.6％ | 91.1％ | 89.6％ | 88.0％ |
| Example 3 | 93.1％ | 91.7％ | 90.5％ | 88.2％ |
| Example 4 | 93.5％ | 92.1％ | 91.1％ | 89.8％ |
| Example 5 | 93.6％ | 92.0％ | 91.2％ | 90.1％ |
| Example 6 | 95.2％ | 94.7％ | 94.0％ | 93.3％ |
| Example 7 | 92.1％ | 91.0％ | 89.4％ | 88.1％ |
| Example 8 | 92.5％ | 91.0％ | 89.1％ | 87.8％ |
| Comparative example 1 | 92.1％ | 91.5％ | 90.3％ | 89.8％ |
The data of the above examples show that the mint-flavored tipping paper essence provided by the invention has good initial embedding rate, and meanwhile, the embedding effect of the mint-flavored tipping paper essence is kept good in the long-term storage process, and the mint-flavored tipping paper essence has similar storage and maintenance effects as the conventional polyethylene shell microcapsules.
After the essence obtained in the above example was used for tipping paper for cigarette holder and subjected to simulated smoking test, the experimental data obtained were as follows:
the above embodiment data shows that the essence of the invention can improve the release of peppermint oil in the smoking process, especially when the smoking time is longer, the temperature of the cigarette holder is increased and the release of peppermint oil is accelerated, the embodiment 4 shows that when the dosage of enol monomer for grafting is higher, the embedding rate of the essence at the end of smoking is obviously reduced, the melting point of the wall material is probably reduced after the grafting rate is increased, and the release of peppermint oil is accelerated under the condition of temperature rise, and the data according to the embodiment 5 and the embodiment 6 show that the temperature control release effect of peppermint oil is better when a plurality of emulsifying agents with different melting points are adopted, and has good linear control release effect, especially when three emulsifying agents with different melting points are adopted, the release of peppermint oil is relatively uniform corresponding to the data of the embodiment 6, and is beneficial to improving the experience of a smoker when 1min,5min and 10min are adopted; from the data of examples 7 and 8, it can be seen that when the particle size of the flavor microcapsules is too small and the temperature is too high, the release of peppermint oil is too fast, which may result in too irritating peppermint taste to smokers in the later stages of smoking.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (8)
1. The mint-flavored tipping paper essence is characterized by comprising a microcapsule wall material and a core material wrapped in the microcapsule wall material, wherein the core material comprises peppermint oil, an emulsifying agent and a solvent, the wall material is enol-grafted modified polyethylene, and the preparation method of the wall material comprises the following steps:
adding polyethylene and enol monomer into dimethylbenzene, heating to 130-140 ℃, preserving heat and stirring to obtain a solution, slowly dripping an initiator into the solution under the nitrogen atmosphere in a stirring state, carrying out heat preservation reaction for 3-5h, cooling to 25 ℃ after the reaction is finished, adding acetone, filtering and drying to obtain enol grafted modified polyethylene;
wherein the enol monomer is selected from one of 3-butene-1-ol, cis-3-pentene-1-ol and cis-3-hexene-1-ol;
polyethylene: enol monomer: and (3) an initiator: the mass ratio of the dimethylbenzene is 1: (0.3-0.4): (0.2-0.3): (8-10) the initiator is dicumyl peroxide;
the number average molecular weight of the polyethylene is 1000-3000.
2. The mint-flavored tipping paper essence according to claim 1, wherein said mint-flavored tipping paper essence has a D50 particle size of 5-30 μm.
3. The mint flavored tipping paper essence according to claim 1, wherein the core comprises, by weight, 5-10 parts of peppermint oil, 0.1-0.5 part of an emulsifier and 40-60 parts of a solvent.
4. The mint flavored tipping paper flavor according to claim 1, wherein said emulsifier comprises at least one of monoglyceride stearate, glyceryl monocaprylate and span 60.
5. The mint flavored tipping paper flavor according to claim 4, wherein said emulsifier comprises monoglyceride stearate, glyceryl monocaprylate, and span 60, said monoglyceride stearate: glycerol monocaprylate: the mass ratio of span 60 is 1: (4-5): (2-3).
6. The mint flavored tipping paper flavor of claim 1, wherein said solvent is water.
7. A method for preparing a mint-flavored tipping paper flavor according to any one of claims 1 to 6, comprising the steps of:
s1, dissolving enol grafted modified polyethylene in toluene, and heating to 90-95 ℃ to obtain a wall material solution;
s2, mixing and stirring peppermint oil, an emulsifying agent and a solvent in proportion, heating to 90-95 ℃, and shearing and stirring at 8000-12000rpm to obtain core emulsion;
s3, maintaining high-speed shearing and stirring conditions of the core material emulsion, adding the wall material solution into the core material emulsion, maintaining shearing and stirring, cooling to 85 ℃, and performing spray drying at a cooling rate of 5-10 ℃/h to obtain the mint-flavored tipping paper essence, wherein the spray drying conditions comprise: the spray air inlet temperature is 120-130 ℃, and the air outlet temperature is 50-60 ℃.
8. The method for preparing mint flavored tipping paper essence according to claim 7, wherein the mass ratio of the enol graft modified polyethylene to toluene is 1:10, the volume ratio of the wall material solution to the core material solution is 1:10.
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| CN105085932A (en) * | 2015-07-10 | 2015-11-25 | 宁波大学 | Polyethylene-hyperbranched graft polymer and preparation method therefor |
| CN107164090A (en) * | 2017-05-31 | 2017-09-15 | 东南大学 | A kind of cigarette perfume microcapsule and preparation method |
| CN112390904A (en) * | 2019-08-19 | 2021-02-23 | 中国科学院上海有机化学研究所 | Polyethylene containing polar functional group and preparation method thereof |
| CN115634209A (en) * | 2021-07-20 | 2023-01-24 | 泓博元生命科技（深圳）有限公司 | Microcapsule powder stable in gastric acid and preparation method and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105085932A (en) * | 2015-07-10 | 2015-11-25 | 宁波大学 | Polyethylene-hyperbranched graft polymer and preparation method therefor |
| CN107164090A (en) * | 2017-05-31 | 2017-09-15 | 东南大学 | A kind of cigarette perfume microcapsule and preparation method |
| CN112390904A (en) * | 2019-08-19 | 2021-02-23 | 中国科学院上海有机化学研究所 | Polyethylene containing polar functional group and preparation method thereof |
| CN115634209A (en) * | 2021-07-20 | 2023-01-24 | 泓博元生命科技（深圳）有限公司 | Microcapsule powder stable in gastric acid and preparation method and application thereof |
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