CN115746954A - Emulsified essence, preparation method thereof and perfuming tube - Google Patents
Emulsified essence, preparation method thereof and perfuming tube Download PDFInfo
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- CN115746954A CN115746954A CN202211302777.4A CN202211302777A CN115746954A CN 115746954 A CN115746954 A CN 115746954A CN 202211302777 A CN202211302777 A CN 202211302777A CN 115746954 A CN115746954 A CN 115746954A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000003094 microcapsule Substances 0.000 claims abstract description 53
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 50
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000000463 material Substances 0.000 claims abstract description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 239000011787 zinc oxide Substances 0.000 claims abstract description 25
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 239000011162 core material Substances 0.000 claims abstract description 24
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 15
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 14
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 14
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 14
- 239000003755 preservative agent Substances 0.000 claims abstract description 14
- 230000002335 preservative effect Effects 0.000 claims abstract description 14
- 239000002562 thickening agent Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 238000001694 spray drying Methods 0.000 claims abstract description 10
- 125000000129 anionic group Chemical group 0.000 claims abstract description 6
- 239000003792 electrolyte Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 64
- 239000008367 deionised water Substances 0.000 claims description 52
- 229910021641 deionized water Inorganic materials 0.000 claims description 52
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000005406 washing Methods 0.000 claims description 29
- 239000000839 emulsion Substances 0.000 claims description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 239000006185 dispersion Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 16
- 239000012498 ultrapure water Substances 0.000 claims description 16
- 239000002105 nanoparticle Substances 0.000 claims description 15
- 239000004408 titanium dioxide Substances 0.000 claims description 15
- 108010073771 Soybean Proteins Proteins 0.000 claims description 14
- 235000019710 soybean protein Nutrition 0.000 claims description 14
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 14
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 12
- 238000004108 freeze drying Methods 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 11
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 10
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 10
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- 238000004945 emulsification Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 229940075507 glyceryl monostearate Drugs 0.000 claims description 7
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 239000002304 perfume Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 3
- 239000003945 anionic surfactant Substances 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 238000000643 oven drying Methods 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 238000004513 sizing Methods 0.000 abstract description 3
- YQEMORVAKMFKLG-UHFFFAOYSA-N glycerine monostearate Natural products CCCCCCCCCCCCCCCCCC(=O)OC(CO)CO YQEMORVAKMFKLG-UHFFFAOYSA-N 0.000 abstract 1
- SVUQHVRAGMNPLW-UHFFFAOYSA-N glycerol monostearate Natural products CCCCCCCCCCCCCCCCC(=O)OCC(O)CO SVUQHVRAGMNPLW-UHFFFAOYSA-N 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 229940071440 soy protein isolate Drugs 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 82
- 235000019504 cigarettes Nutrition 0.000 description 24
- 239000000203 mixture Substances 0.000 description 21
- 238000005303 weighing Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 239000003205 fragrance Substances 0.000 description 9
- 238000009210 therapy by ultrasound Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 4
- 230000006378 damage Effects 0.000 description 4
- 238000007493 shaping process Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- 239000004368 Modified starch Substances 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003571 electronic cigarette Substances 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Landscapes
- Cosmetics (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses an emulsified essence and a preparation method thereof, and a perfuming tube, wherein the method comprises the steps of (1) preparing modified nano silicon dioxide and titanium dioxide nanowires; (2) Mixing the titanium dioxide nanowires with anionic electrolyte to obtain negative charge titanium dioxide nanowires, and then modifying the modified nano-silica and the negative charge titanium dioxide nanowires to obtain soy protein isolate to obtain a wall material solution; (3) Neutralizing glycerol monostearate with essence ethanol to obtain a core material solution, slowly adding the core material solution into the wall material solution, and performing spray drying to obtain essence microcapsules; (4) Preparing flower-shaped nano zinc oxide, and adding the essence microcapsule to obtain a composite essence microcapsule; (5) And adding an emulsifier, a thickener, a weighting agent, an antioxidant and a preservative into the composite essence microcapsule to prepare the emulsified essence. The emulsified essence prepared by the invention has high attachment rate on the filter stick of the perfuming pipe, and the cooling and sizing efficiency of the filter stick of the perfuming pipe is improved.
Description
Technical Field
The invention relates to the technical field of emulsified essence processing, in particular to emulsified essence, a preparation method thereof and a perfuming pipe.
Background
With the international cigarette inhibition call and the increasing concern of cigarette consumers on the self health, the low-tar and low-harm cigarette becomes the mainstream of the cigarette in the future world, but the harm and tar reduction is accompanied with the loss of the cigarette aroma and the deterioration of the comfort degree, while the cigarette flavoring and charging can set off and supplement the cigarette aroma, increase the smoke concentration, improve the taste, remove and cover the offensive odor, reduce the irritation, endow the product with the characteristic aroma of beautiful appearance, highlight the personalized style of the cigarette product, and the development and application of the cigarette flavoring and charging are one of the most key technologies for keeping the cigarette aroma and taste in the harm and tar reduction work. The cooling, sizing and perfuming technology is a safe and effective perfuming technology, and the perfuming is completed by immersing the filter stick into emulsified essence, loading the emulsified essence on the filter stick, and devolatilizing and drying. When the cigarette is burnt and smoked, the aroma molecules are desorbed into the main stream smoke under the action of suction pressure, so that the cigarette flavoring effect is achieved.
For example, the Chinese patent with publication number CN110760388A discloses a production formula and a preparation method of an electronic cigarette emulsified essence, wherein the emulsified essence comprises edible essence, an antioxidant, an emulsifier, modified starch, a thickening agent, a preservative and deionized water, and the whole viscosity of the emulsified essence is increased and the whole emulsifying capacity is improved by adopting a one-by-one stirring mode, so that the obtained essence is more suitable for the taste of the public in terms of both fragrance and mouthfeel; the emulsified essence is used for cooling and sizing the filter stick of the cigarette, although the emulsified essence can endow the cigarette with certain fragrance, the attachment efficiency of the emulsified essence on the filter stick is lower, the processing period is longer, in addition, the emulsified essence is adsorbed on the filter stick and then is easy to desorb, and in the storage period of the cigarette, the fragrance in the emulsified essence can be volatilized and lost in a large quantity, so that the fragrance of the cigarette is lightened when the cigarette is burnt and the taste of the cigarette is poor.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of emulsified essence, the prepared emulsified essence can be used for cooling, shaping and perfuming of a perfuming pipe, the adhesion rate of the emulsified essence on a perfuming pipe filter stick is high, the cooling and shaping efficiency of the perfuming pipe filter stick is improved, and the fragrance retention of the perfuming pipe after perfuming is improved.
Necessarily, the invention also provides the emulsified essence prepared by the preparation method.
More necessarily, the invention also provides a perfuming pipe prepared by applying the emulsified essence.
The technical scheme provided by the invention is as follows:
a preparation method of emulsified essence comprises the following steps:
(1) Modifying nano-silica by adopting an anionic surfactant to obtain modified nano-silica, and synthesizing a titanium dioxide nanowire by taking isopropyl titanate, ultrapure water and sodium hydroxide as raw materials;
(2) Mixing the titanium dioxide nanowires with anionic electrolyte to obtain negative charge titanium dioxide nanowires, adding the modified nano-silica and the negative charge titanium dioxide nanowires into deionized water, and adding soybean protein isolate after ultrasonic dispersion to obtain a wall material solution;
(3) Adding essence into ethanol, adding glyceryl monostearate, mixing, adjusting pH to 7 to obtain core material solution, slowly adding the core material solution into the wall material solution, and spray drying to obtain essence microcapsule;
(4) Preparing flower-like nano zinc oxide with a wurtzite structure by a hydrothermal method, adding the flower-like nano zinc oxide into deionized water, adding essence microcapsules after ultrasonic dispersion, and obtaining composite essence microcapsules through ultrasonic dispersion and mechanical stirring;
(5) At normal temperature, adding deionized water into the composite essence microcapsules, stirring and mixing, sequentially adding an emulsifier, a thickening agent, a weighting agent, an antioxidant and a preservative during stirring, performing circulating ultrasonic emulsification for 10-20min to obtain a primary emulsion, homogenizing the emulsion by a homogenizer, standing, and filtering to obtain the required emulsified essence.
In the step (1), the preparation method of the modified nano-silica comprises the following specific operations:
adding nano silicon dioxide into sodium dodecyl sulfate solution, adjusting pH to 4-5 with acetic acid solution, stirring at 80-86 deg.C for 5-8h, centrifuging, repeatedly washing with distilled water, oven drying, and grinding;
wherein the dosage proportion of the nano silicon dioxide to the sodium dodecyl sulfate solution is (1-5) g: (200-600) mL; the concentration of the sodium dodecyl sulfate solution is 0.5-0.8wt%.
In the step (1), the preparation method of the titanium dioxide nanowire specifically comprises the following operations:
adding isopropyl titanate and ultrapure water into a container, stirring at room temperature for 30-50min, performing centrifugal separation after the reaction is finished, repeatedly washing with ultrapure water, performing freeze drying to obtain titanium dioxide nanoparticles, adding the titanium dioxide nanoparticles and a sodium hydroxide solution into a hydrothermal reaction kettle, reacting at 120-130 ℃ for 4-6h, performing centrifugal separation after the reaction is finished, repeatedly washing with dilute hydrochloric acid and water to be neutral, and performing freeze drying to obtain the titanium dioxide nanoparticles;
the mass ratio of the isopropyl titanate to the ultrapure water is 4: (10-15); the dosage ratio of the titanium dioxide nano particles to the sodium hydroxide solution is (1-4) g: (20-60) mL; the concentration of the sodium hydroxide solution is 10-13mol/L.
In the step (2), the preparation method of the wall material solution specifically comprises the following operations:
adding titanium dioxide nanowires into an anionic electrolyte sodium dodecyl benzene sulfonate solution, ultrasonically dispersing, centrifuging, washing and drying to obtain negative charge titanium dioxide nanowires, adding the modified nano silicon dioxide and negative charge titanium dioxide nanowires obtained in the step (1) into deionized water, ultrasonically dispersing, adding soybean protein isolate, and stirring at 78-82 ℃ for 30-50 min;
in the wall material solution, the dosage proportion of the modified nano-silica, the negative charge titanium dioxide nanowire, the deionized water and the soybean protein isolate is (1-3) g: (5-8) g: (180-230) mL: (20-40) g;
the concentration of the sodium dodecyl benzene sulfonate solution is 1-5mg/mL, and the addition amount of the sodium dodecyl benzene sulfonate solution is 20-30mL.
In the step (3), the preparation method of the core material solution specifically comprises the following operations:
adding essence into ethanol, adding glyceryl monostearate, stirring at 60-70 deg.C for 10-30min, adjusting pH to 7 with sodium hydroxide solution, and cooling to 30-35 deg.C;
in the core material solution, the proportion of the essence, the ethanol and the glycerin monostearate is (5-10) g: (80-120) mL: (0.3-0.8) g; the concentration of the ethanol is 50-60wt%.
Wherein, under the stirring state, slowly adding the core material solution into the wall material solution, stirring at 35-40 ℃ for 30-50min, then dispersing at 13000-18000/min for 3-6min at a high speed, and spray drying the obtained solution;
the mass ratio of the core wall is 1: (7-10); in the spray drying, the air inlet temperature is 140-150 ℃, the air outlet temperature is 60-70 ℃, and the feeding flow is 8-12mL/min.
In the step (4), the preparation method of the flower-like nano zinc oxide specifically comprises the following operations:
dissolving zinc nitrate hexahydrate in deionized water at room temperature, continuously stirring, adding ammonia water to adjust the pH value to 8.0-8.5 to obtain a precursor solution, adding cetyl trimethyl ammonium bromide into the deionized water, stirring, mixing with the precursor solution, placing the formed reaction solution in a reaction kettle for reaction for 10-15h, cooling to room temperature after the reaction is finished, repeatedly washing a product with the deionized water and ethanol, and drying;
in the precursor solution, the proportion of the zinc nitrate hexahydrate to the deionized water is (12-16) g: (600-800) mL; the dosage proportion of the hexadecyl trimethyl ammonium bromide to the deionized water is (0.05-0.08) g: (20-50) mL; in the reaction liquid, the mass ratio of the zinc nitrate hexahydrate to the hexadecyl trimethyl ammonium bromide is (12-16): (0.05-0.08); the reaction temperature is 150-160 ℃.
In the step (4), the preparation method of the composite essence microcapsule specifically comprises the following operations:
adding flower-like nano zinc oxide into deionized water to obtain a dispersion, adding the essence microcapsule into the dispersion, and performing ultrasonic dispersion and mechanical stirring;
the dosage proportion of the flower-shaped nano zinc oxide, the deionized water and the essence microcapsule is (10-20) g: (150-260) mL: (3-8) g.
In the step (5), the preparation method of the emulsified essence comprises the following specific operations:
at normal temperature, adding the composite essence microcapsules into deionized water, stirring and mixing at the rotating speed of 600-800r/min, sequentially adding an emulsifier, a thickener, a weighting agent, an antioxidant and a preservative in the stirring process, stirring for 5-10min, performing circulating ultrasonic emulsification for 10-20min to obtain a primary emulsion, homogenizing the emulsion by a homogenizer at the homogenizing pressure of 15-25MPa, standing the homogenized emulsion, and filtering;
the composite essence microcapsule, the weighting agent, the antioxidant, the emulsifier, the deionized water, the thickening agent and the preservative are mixed according to the mass ratio of (20-40): (2-5): (1-3): (15-30): (50-80): (3-6): (2-4).
An emulsified essence is prepared by the preparation method.
The perfuming pipe is prepared by applying the emulsified essence prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the soybean protein isolate is modified by using nano-silica, the modified soybean protein isolate is used as a wall material of the microcapsule, and the essence is used as a core material to prepare the microcapsule, wherein the silicon-oxygen bond, hydroxyl and silicon atom containing empty bonding orbit contained in the nano-silica can be combined with amino and other groups of the soybean protein isolate to form a hydrogen bond and a coordination bond, so that the intermolecular structure is more compact, the space is reduced, the wall material is endowed with special performance, the mechanical property of the wall material is improved, the air permeability of the wall material is reduced, the fragrance of the essence in the microcapsule can be slowly and durably released, the slow release effect is achieved, and the emulsified essence has lasting fragrance; meanwhile, in order to further improve the strength of the wall material, so that the microcapsule can keep the structural stability and is not easy to damage to cause loss of the essence, the titanium dioxide nanowires are added into the wall material, and a cross-linked reticular structure is formed by mutually overlapping and winding the titanium dioxide nanowires, so that the effects of dispersing and transmitting stress can be achieved, the resistance of the wall material to the outside is improved, and the wall material is not easy to damage; meanwhile, the length-diameter ratio and a large number of active sites of the titanium dioxide nanowire are beneficial to the attachment of the nano-silicon dioxide on the surface of the nano-silicon dioxide, so that the microstructure corroded on the surface of the titanium dioxide nanowire can be filled and repaired, the integrity of the titanium dioxide nanowire structure and the roughness of the surface are improved, the effect of improving the dispersion and transmission stress of the net-shaped structure constructed by the titanium dioxide nanowire is facilitated, the bonding strength of the lap winding of the titanium dioxide nanowire is facilitated, the stability of the net-shaped structure can be enhanced, and the wall material of the microcapsule has better strength.
According to the invention, titanium dioxide nanowires are mixed with anionic electrolyte to enable the titanium dioxide nanowires to have negative charges, the mixture is added into a wall material solution to enable microcapsules to have negative charges, then zinc nitrate and cetyl trimethyl ammonium bromide are used as raw materials, flower-shaped nano zinc oxide with a wurtzite structure is prepared by a hydrothermal method, the flower-shaped nano zinc oxide is adsorbed on the microcapsules by utilizing the positive charges of the flower-shaped nano zinc oxide, and a coating layer consisting of nano zinc oxide is formed on the surface of the microcapsules through electrostatic interaction.
According to the emulsified essence, a coating layer with a loose structure constructed by nano zinc oxide is formed on the surface of a microcapsule embedded with the essence by utilizing the electrostatic effect, so that the specific surface area and the surface roughness of the microcapsule are increased, the emulsified essence can be better, quickly and firmly attached to a flavoring pipe filter stick under the capillary action, the cooling and shaping efficiency of the flavoring pipe filter stick is improved, meanwhile, the essence is embedded, so that the influence of external factors on the essence can be reduced, the essence is protected, and the slow release of the fragrance of the essence can be realized by utilizing certain air permeability of the wall material of the microcapsule, so that the flavoring pipe has better fragrance holding property after being flavored; moreover, after the microcapsules and the nano zinc oxide are subjected to electrostatic adsorption, the formed composite essence microcapsules have the same electrical property, and the composite essence microcapsules can stably exist and are not easy to agglomerate by utilizing the repulsion of the same electrical property, so that the stability of the emulsified essence is improved.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The material sources used in the embodiment of the invention are as follows:
nano silicon dioxide, CAS No. 7631-86-9, EC No. 238-878-4, pubChem No. 24261, cat No. S490064-100g, aladdin. Other materials the materials used in the examples of the present invention and comparative examples were commercially available from sources not otherwise specified.
Example 1
The preparation method of the emulsified essence specifically comprises the following steps:
(1) Adding 1g of nano silicon dioxide into 200mL of lauryl sodium sulfate solution with the concentration of 0.5wt%, adjusting the pH value to 4 by using acetic acid solution with the concentration of 10wt%, stirring for 5h at 80 ℃, repeatedly washing by using distilled water after centrifugation, drying for 10h at 60 ℃, and grinding to obtain modified nano silicon dioxide;
mixing isopropyl titanate and ultrapure water according to a mass ratio of 4:10, adding the mixture into a container, stirring the mixture at room temperature of 400r/min for 30min, after the reaction is finished, performing centrifugal separation, repeatedly washing the mixture with ultrapure water, performing freeze drying to obtain titanium dioxide nanoparticles, adding 1g of the titanium dioxide nanoparticles and 20mL of a 10mol/L sodium hydroxide solution into a hydrothermal reaction kettle, reacting the mixture at 120 ℃ for 4h, after the reaction is finished, performing centrifugal separation, repeatedly washing the mixture with dilute hydrochloric acid and water to be neutral, and performing freeze drying to obtain titanium dioxide nanowires;
(2) Adding titanium dioxide nanowires into 20mL of sodium dodecyl benzene sulfonate solution with the concentration of 1mg/mL, carrying out ultrasonic treatment for 3min at 300W after mixing, washing and drying after centrifuging to obtain negative-charge titanium dioxide nanowires, adding 1g of modified nano-silica and 5g of negative-charge titanium dioxide nanowires into 180mL of deionized water, carrying out ultrasonic treatment for 2h at 500W, then adding 20g of soybean protein isolate into the formed dispersion, and stirring for 30min at 500r/min at 78 ℃ to obtain a wall material solution;
(3) Adding 5g of essence into 80mL of 50wt% ethanol, adding 0.3g of glyceryl monostearate, stirring at 60 ℃ for 10min at 500r/min, adjusting the pH to 7 by using 1mol/L sodium hydroxide solution, cooling to 30 ℃ to obtain a core material solution, wherein the mass ratio of the core wall is 1:7, slowly adding the core material solution into the wall material solution under the stirring state of 500r/min, stirring for 30min at 35 ℃, then dispersing for 3min at a high speed of 13000/min, and performing spray drying on the obtained solution, wherein the air inlet temperature is 140 ℃, the air outlet temperature is 60 ℃, and the feed flow is 8mL/min to obtain the essence microcapsule;
(4) Weighing 12g of zinc nitrate hexahydrate, dissolving the zinc nitrate hexahydrate in 600mL of deionized water at room temperature, continuously stirring to obtain a mixed solution, adding 23wt% of ammonia water to adjust the pH value to 8 to obtain a precursor solution, weighing 0.05g of hexadecyl trimethyl ammonium bromide, adding the hexadecyl trimethyl ammonium bromide into 20mL of deionized water, stirring for 30min at a speed of 80r/min, mixing with the precursor solution, continuously stirring for 2h, placing the formed reaction solution in a reaction kettle, reacting for 10h at 150 ℃, cooling to room temperature after the reaction is finished, repeatedly washing a product with deionized water and ethanol, and drying to obtain flower-shaped nano zinc oxide;
weighing 10g of flower-like nano zinc oxide, adding into 150mL of deionized water, performing ultrasonic dispersion for 10min at 200W to obtain dispersion liquid, adding 3g of essence microcapsules into the dispersion liquid, continuing to perform ultrasonic dispersion for 1min, and stirring at 80r/min for 30min to obtain composite essence microcapsules;
(5) According to the mass ratio of 20:2:1:15:50:3:2, weighing the composite essence microcapsules, the weighting agent, the antioxidant, the emulsifier, the deionized water, the thickener and the preservative respectively, adding the composite essence microcapsules into the deionized water at normal temperature, stirring and mixing at the rotating speed of 600r/min, sequentially adding the emulsifier, the thickener, the weighting agent, the antioxidant and the preservative in the stirring process, stirring for 5min, performing circulating ultrasonic emulsification for 10min to obtain a primary emulsion, homogenizing the emulsion by a homogenizer at the homogenizing pressure of 15MPa, standing and filtering the homogenized emulsion to obtain the required emulsified essence.
Example 2
The preparation method of the emulsified essence specifically comprises the following steps:
(1) Adding 3g of nano-silica into 500mL of lauryl sodium sulfate solution with the concentration of 0.6wt%, adjusting the pH value to 4.5 by using acetic acid solution with the concentration of 13wt%, stirring for 7h at 85 ℃, repeatedly washing by using distilled water after centrifugation, drying for 13h at 65 ℃, and grinding to obtain modified nano-silica;
mixing isopropyl titanate and ultrapure water according to a mass ratio of 4:13, adding the mixture into a container, stirring the mixture for 40min at the room temperature of 500r/min, performing centrifugal separation after the reaction is finished, repeatedly washing the mixture with ultrapure water, performing freeze drying to obtain titanium dioxide nanoparticles, adding 3g of the titanium dioxide nanoparticles and 50mL of a sodium hydroxide solution with the concentration of 12mol/L into a hydrothermal reaction kettle, reacting the mixture for 5h at the temperature of 125 ℃, performing centrifugal separation after the reaction is finished, repeatedly washing the mixture with dilute hydrochloric acid and water to be neutral, and performing freeze drying to obtain titanium dioxide nanowires;
(2) Adding titanium dioxide nanowires into 30mL of sodium dodecyl benzene sulfonate solution with the concentration of 3mg/mL, carrying out ultrasonic treatment for 5min at 400W after mixing, washing and drying after centrifuging to obtain negative charge titanium dioxide nanowires, adding 2g of modified nano-silica and 7g of negative charge titanium dioxide nanowires into 210mL of deionized water, carrying out ultrasonic treatment for 3h at 700W, then adding 30g of soybean protein isolate into the formed dispersion, and stirring at 700r/min for 40min at 80 ℃ to obtain a wall material solution;
(3) Adding 8g of essence into 100mL of ethanol with the concentration of 55wt%, adding 0.5g of glyceryl monostearate, stirring at the temperature of 65 ℃ for 20min at 600r/min, adjusting the pH to 7 by using 1.3mol/L of sodium hydroxide solution, cooling to 32 ℃ to obtain a core material solution, wherein the mass ratio of the core material to the wall is 1: slowly adding the core material solution into the wall material solution under the stirring state of 600r/min, stirring for 40min at 38 ℃, dispersing for 5min at a high speed of 15000/min, and performing spray drying on the obtained solution, wherein the air inlet temperature is 145 ℃, the air outlet temperature is 65 ℃, and the feed flow is 10mL/min to obtain the essence microcapsules;
(4) Weighing 15g of zinc nitrate hexahydrate to be dissolved in 700mL of deionized water at room temperature, continuously stirring to obtain a mixed solution, adding 25wt% ammonia water to adjust the pH value to 8.2 to obtain a precursor solution, weighing 0.07g of hexadecyl trimethyl ammonium bromide to be added into 40mL of deionized water, stirring at 100r/min for 40min, mixing with the precursor solution, continuously stirring for 3h, placing the formed reaction solution into a reaction kettle, reacting at 155 ℃ for 13h, cooling to room temperature after the reaction is finished, repeatedly washing the product with deionized water and ethanol, and drying to obtain flower-shaped nano zinc oxide;
weighing 15g of flower-like nano zinc oxide, adding the flower-like nano zinc oxide into 230mL of deionized water, carrying out ultrasonic dispersion for 20min at 250W to obtain a dispersion solution, adding 5g of essence microcapsules into the dispersion solution, continuing the ultrasonic dispersion for 3min, and stirring at 120r/min for 40min to obtain composite essence microcapsules;
(5) According to the mass ratio of 30:3:2:25:70:5:3, weighing the composite essence microcapsules, the weighting agent, the antioxidant, the emulsifier, the deionized water, the thickener and the preservative respectively, adding the composite essence microcapsules into the deionized water at normal temperature, stirring and mixing at the rotating speed of 700r/min, sequentially adding the emulsifier, the thickener, the weighting agent, the antioxidant and the preservative in the stirring process, stirring for 7min, performing circulating ultrasonic emulsification for 15min to obtain a primary emulsion, homogenizing the emulsion by a homogenizer at the homogenizing pressure of 20MPa, standing and filtering the homogenized emulsion to obtain the required emulsified essence.
Example 3
The preparation method of the emulsified essence specifically comprises the following steps:
(1) Adding 5g of nano silicon dioxide into 600mL of lauryl sodium sulfate solution with the concentration of 0.8wt%, adjusting the pH value to 5 by using acetic acid solution with the concentration of 15wt%, stirring for 8h at 86 ℃, repeatedly washing by using distilled water after centrifugation, drying for 15h at 70 ℃, and grinding to obtain modified nano silicon dioxide;
mixing isopropyl titanate and ultrapure water according to a mass ratio of 4:15, adding the mixture into a container, stirring the mixture for 50min at the room temperature of 600r/min, performing centrifugal separation after the reaction is finished, repeatedly washing the mixture with ultrapure water, performing freeze drying to obtain titanium dioxide nanoparticles, adding 4g of the titanium dioxide nanoparticles and 60mL of 13mol/L sodium hydroxide solution into a hydrothermal reaction kettle, reacting the mixture for 6h at the temperature of 130 ℃, performing centrifugal separation after the reaction is finished, repeatedly washing the mixture with dilute hydrochloric acid and water to be neutral, and performing freeze drying to obtain titanium dioxide nanowires;
(2) Adding titanium dioxide nanowires into 25mL of 5mg/mL sodium dodecyl benzene sulfonate solution, carrying out ultrasonic treatment for 6min at 500W after mixing, carrying out washing and drying after centrifugation to obtain negative charge titanium dioxide nanowires, adding 3g of modified nano-silica and 8g of negative charge titanium dioxide nanowires into 230mL of deionized water, carrying out ultrasonic treatment for 4h at 800W, then adding 40g of soybean protein isolate into the formed dispersion, and stirring for 50min at 82 ℃ at 800r/min to obtain a wall material solution;
(3) Adding 10g of essence into 120mL of 60wt% ethanol, adding 0.8g of glyceryl monostearate, stirring at 70 ℃ for 30min at 700r/min, adjusting the pH to 7 by using 1.5mol/L sodium hydroxide solution, cooling to 35 ℃ to obtain a core material solution, wherein the mass ratio of the core wall is 1:10, slowly adding the core material solution into the wall material solution under the stirring state of 800r/min, stirring for 50min at 40 ℃, dispersing for 6min at a high speed of 18000/min, and performing spray drying on the obtained solution, wherein the air inlet temperature is 150 ℃, the air outlet temperature is 70 ℃, and the feed flow rate is 12mL/min to obtain the essence microcapsule;
(4) Weighing 16g of zinc nitrate hexahydrate, dissolving the zinc nitrate hexahydrate in 800mL of deionized water at room temperature, continuously stirring to obtain a mixed solution, adding 26wt% ammonia water to adjust the pH value to 8.5 to obtain a precursor solution, weighing 0.08g of hexadecyl trimethyl ammonium bromide, adding the hexadecyl trimethyl ammonium bromide into 50mL of deionized water, stirring for 50min at 130r/min, mixing with the precursor solution, continuously stirring for 5h, placing the formed reaction solution into a reaction kettle, reacting for 15h at 160 ℃, cooling to room temperature after the reaction is finished, repeatedly washing a product with deionized water and ethanol, and drying to obtain flower-shaped nano zinc oxide;
weighing 20g of flower-like nano zinc oxide, adding the flower-like nano zinc oxide into 260mL of deionized water, performing ultrasonic dispersion for 30min at 300W to obtain a dispersion solution, adding 8g of essence microcapsules into the dispersion solution, continuing performing ultrasonic dispersion for 5min, and stirring for 50min at 150r/min to obtain composite essence microcapsules;
(5) According to the mass ratio of 40:5:3:30:80:6: and 4, weighing the composite essence microcapsules, the weighting agent, the antioxidant, the emulsifier, deionized water, the thickener and the preservative respectively, adding the composite essence microcapsules into the deionized water at normal temperature, stirring and mixing at the rotating speed of 800r/min, sequentially adding the emulsifier, the thickener, the weighting agent, the antioxidant and the preservative in the stirring process, stirring for 10min, performing circulating ultrasonic emulsification for 20min to obtain a primary emulsion, homogenizing the emulsion by a homogenizer at the homogenizing pressure of 25MPa, standing and filtering the homogenized emulsion to obtain the required emulsified essence.
Comparative example 1: the comparative example is basically the same as example 1, except that the wall material solution does not contain the modified nano-silica, and the preparation method of the wall material solution comprises the following steps:
mixing isopropyl titanate and ultrapure water according to a mass ratio of 4:10, adding the mixture into a container, stirring the mixture for 30min at the room temperature of 400r/min, performing centrifugal separation after the reaction is finished, repeatedly washing the mixture with ultrapure water, and performing freeze drying to obtain titanium dioxide nanoparticles, adding 1g of the titanium dioxide nanoparticles and 20mL of a 10mol/L sodium hydroxide solution into a hydrothermal reaction kettle, reacting the mixture for 4h at the temperature of 120 ℃, performing centrifugal separation after the reaction is finished, repeatedly washing the mixture with dilute hydrochloric acid and water to be neutral, and performing freeze drying to obtain titanium dioxide nanowires;
adding titanium dioxide nanowires into a sufficient sodium dodecyl benzene sulfonate solution with the concentration of 1mg/mL, carrying out ultrasonic treatment for 3min at 300W after mixing, washing and drying after centrifuging to obtain negative charge titanium dioxide nanowires, adding 5g of negative charge titanium dioxide nanowires into 180mL of deionized water, carrying out ultrasonic treatment for 2h at 500W, then adding 20g of soybean protein isolate into the formed dispersion, and stirring for 30min at 78 ℃ at 500r/min to obtain a wall material solution.
Comparative example 2: the comparative example is basically the same as example 1, except that the wall material solution does not contain the titanium dioxide nanowires, and the preparation method of the wall material solution is as follows;
adding 1g of nano silicon dioxide into 200mL of lauryl sodium sulfate solution with the concentration of 0.5wt%, adjusting the pH value to 4 by using acetic acid solution with the concentration of 10wt%, stirring for 5h at 80 ℃, repeatedly washing by using distilled water after centrifugation, drying for 10h at 60 ℃, and grinding to obtain modified nano silicon dioxide;
adding 1g of modified nano silicon dioxide into 180mL of deionized water, carrying out ultrasonic treatment for 2h by 500W, then adding 20g of soybean protein isolate into the formed dispersion, and stirring for 30min at the temperature of 78 ℃ at the speed of 500r/min to obtain a wall material solution.
Comparative example 3: this comparative example is essentially the same as example 1 except that step (4) is omitted and the composite perfume microcapsule of step (5) is replaced directly with the perfume microcapsule prepared in step (3).
Control group: refer to the emulsified essence prepared in the Chinese patent with publication No. CN110760388A, example 1.
Test experiment 1:
the emulsified perfume samples provided in examples 1 to 3, comparative examples 1 to 3 and the control were stored at room temperature, and the stability of each sample was observed and recorded, and the results are shown in table 1.
TABLE 1
As can be seen from the table 1, the emulsified essence provided by the invention is very stable, is not easy to agglomerate, and can be stably stored for a long time.
Test experiment 2:
the emulsified essence samples provided in examples 1 to 3, comparative examples 1 to 3 and the control were used to cool, shape and flavor the cigarette flavoring pipe filter rods, and were then devolatilized and dried, cut and assembled to cigarettes to obtain cigarette samples, which were stored in a dry environment for 24 months, taken out for use by participants and recorded the experience of the participants, with the results shown in table 2.
TABLE 2
As can be seen from the table 2, after the emulsified essence disclosed by the invention is used for cooling, shaping and perfuming the cigarette flavoring pipe filter stick, the cigarette flavoring pipe filter stick has good fragrance-holding property, and the taste of the cigarette is greatly improved.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (11)
1. The preparation method of the emulsified essence is characterized by comprising the following steps:
(1) Modifying nano-silica by adopting an anionic surfactant to obtain modified nano-silica, and synthesizing a titanium dioxide nanowire by taking isopropyl titanate, ultrapure water and sodium hydroxide as raw materials;
(2) Mixing the titanium dioxide nanowires with anionic electrolyte to obtain negative charge titanium dioxide nanowires, adding the modified nano-silica and the negative charge titanium dioxide nanowires into deionized water, and adding soybean protein isolate after ultrasonic dispersion to obtain a wall material solution;
(3) Adding essence into ethanol, adding glyceryl monostearate, mixing, adjusting pH to 7 to obtain core material solution, slowly adding the core material solution into the wall material solution, and spray drying to obtain essence microcapsule;
(4) Preparing flower-like nano zinc oxide with a wurtzite structure by a hydrothermal method, adding the flower-like nano zinc oxide into deionized water, adding essence microcapsules after ultrasonic dispersion, and obtaining composite essence microcapsules through ultrasonic dispersion and mechanical stirring;
(5) At normal temperature, adding deionized water into the composite essence microcapsules, stirring and mixing, sequentially adding an emulsifier, a thickening agent, a weighting agent, an antioxidant and a preservative during stirring, performing circulating ultrasonic emulsification for 10-20min to obtain a primary emulsion, homogenizing the emulsion by a homogenizer, standing, and filtering to obtain the required emulsified essence.
2. The method for preparing the emulsified essence according to claim 1, wherein the method comprises the following steps:
in the step (1), the preparation method of the modified nano-silica specifically comprises the following operations:
adding nano silicon dioxide into sodium dodecyl sulfate solution, adjusting pH to 4-5 with acetic acid solution, stirring at 80-86 deg.C for 5-8h, centrifuging, repeatedly washing with distilled water, oven drying, and grinding;
wherein the dosage ratio of the nano silicon dioxide to the sodium dodecyl sulfate solution is (1-5) g: (200-600) mL; the concentration of the sodium dodecyl sulfate solution is 0.5-0.8wt%.
3. The method of preparing an emulsified perfume according to claim 1 or 2, wherein:
in the step (1), the preparation method of the titanium dioxide nanowire specifically comprises the following operations:
adding isopropyl titanate and ultrapure water into a container, stirring at room temperature for 30-50min, performing centrifugal separation after the reaction is finished, repeatedly washing with ultrapure water, performing freeze drying to obtain titanium dioxide nanoparticles, adding the titanium dioxide nanoparticles and a sodium hydroxide solution into a hydrothermal reaction kettle, reacting at 120-130 ℃ for 4-6h, performing centrifugal separation after the reaction is finished, repeatedly washing with dilute hydrochloric acid and water to be neutral, and performing freeze drying to obtain titanium dioxide nanowires;
the mass ratio of the isopropyl titanate to the ultrapure water is 4: (10-15); the dosage ratio of the titanium dioxide nano particles to the sodium hydroxide solution is (1-4) g: (20-60) mL; the concentration of the sodium hydroxide solution is 10-13mol/L.
4. The method for preparing emulsified essence according to claim 3, wherein:
in the step (2), the preparation method of the wall material solution specifically comprises the following operations:
adding titanium dioxide nanowires into an anionic electrolyte sodium dodecyl benzene sulfonate solution, ultrasonically dispersing, centrifuging, washing and drying to obtain negative charge titanium dioxide nanowires, adding the modified nano silicon dioxide and negative charge titanium dioxide nanowires obtained in the step (1) into deionized water, ultrasonically dispersing, adding soybean protein isolate, and stirring at 78-82 ℃ for 30-50 min;
in the wall material solution, the dosage proportion of the modified nano-silica, the negative charge titanium dioxide nanowire, the deionized water and the soybean protein isolate is (1-3) g: (5-8) g: (180-230) mL: (20-40) g;
the concentration of the sodium dodecyl benzene sulfonate solution is 1-5mg/mL, and the addition amount of the sodium dodecyl benzene sulfonate solution is 20-30mL.
5. The method for preparing the emulsified essence according to claim 1, wherein the method comprises the following steps:
in the step (3), the preparation method of the core material solution specifically comprises the following operations:
adding essence into ethanol, adding glyceryl monostearate, stirring at 60-70 deg.C for 10-30min, adjusting pH to 7 with sodium hydroxide solution, and cooling to 30-35 deg.C;
in the core material solution, the proportion of the essence, the ethanol and the glycerin monostearate is (5-10) g: (80-120) mL: (0.3-0.8) g; the concentration of the ethanol is 50-60wt%.
6. The method for preparing emulsified essence according to claim 5, wherein:
slowly adding the core material solution into the wall material solution under stirring, stirring at 35-40 deg.C for 30-50min, dispersing at 13000-18000/min for 3-6min, and spray drying the obtained solution;
the mass ratio of the core wall is 1: (7-10); in the spray drying, the air inlet temperature is 140-150 ℃, the air outlet temperature is 60-70 ℃, and the feed flow is 8-12mL/min.
7. The method for preparing emulsified essence according to claim 5, wherein:
in the step (4), the preparation method of the flower-like nano zinc oxide specifically comprises the following operations:
dissolving zinc nitrate hexahydrate in deionized water at room temperature, continuously stirring, adding ammonia water to adjust the pH value to 8.0-8.5 to obtain a precursor solution, adding cetyl trimethyl ammonium bromide into the deionized water, stirring, mixing with the precursor solution, placing the formed reaction solution in a reaction kettle for reaction for 10-15h, cooling to room temperature after the reaction is finished, repeatedly washing a product with the deionized water and ethanol, and drying;
in the precursor solution, the proportion of the zinc nitrate hexahydrate to the deionized water is (12-16) g: (600-800) mL; the dosage ratio of the hexadecyl trimethyl ammonium bromide to the deionized water is (0.05-0.08) g: (20-50) mL; in the reaction liquid, the mass ratio of the zinc nitrate hexahydrate to the hexadecyl trimethyl ammonium bromide is (12-16): (0.05-0.08); the reaction temperature is 150-160 ℃.
8. The method for preparing emulsified essence according to claim 5, wherein:
in the step (4), the preparation method of the composite essence microcapsule specifically comprises the following operations:
adding flower-like nano zinc oxide into deionized water to obtain a dispersion, adding the essence microcapsule into the dispersion, and performing ultrasonic dispersion and mechanical stirring;
the dosage proportion of the flower-shaped nano zinc oxide, the deionized water and the essence microcapsule is (10-20) g: (150-260) mL: (3-8) g.
9. The method for preparing emulsified essence according to claim 5, wherein:
in the step (5), the preparation method of the emulsified essence comprises the following specific operations:
at normal temperature, adding the composite essence microcapsules into deionized water, stirring and mixing at the rotating speed of 600-800r/min, sequentially adding an emulsifier, a thickener, a weighting agent, an antioxidant and a preservative in the stirring process, stirring for 5-10min, performing circulating ultrasonic emulsification for 10-20min to obtain a primary emulsion, homogenizing the emulsion by a homogenizer at the homogenizing pressure of 15-25MPa, standing the homogenized emulsion, and filtering;
the composite essence microcapsule, the weighting agent, the antioxidant, the emulsifier, the deionized water, the thickening agent and the preservative are mixed according to the mass ratio of (20-40): (2-5): (1-3): (15-30): (50-80): (3-6): (2-4).
10. An emulsified essence, characterized by being prepared by the preparation method of any one of claims 1 to 9.
11. A perfuming tube, characterized in that: prepared by using the emulsified essence prepared by the preparation method according to any one of claims 1 to 9.
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