CN116622441A - Semi-dry distillation natural spice and preparation method and application thereof - Google Patents
Semi-dry distillation natural spice and preparation method and application thereof Download PDFInfo
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- CN116622441A CN116622441A CN202310529188.8A CN202310529188A CN116622441A CN 116622441 A CN116622441 A CN 116622441A CN 202310529188 A CN202310529188 A CN 202310529188A CN 116622441 A CN116622441 A CN 116622441A
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- 238000000197 pyrolysis Methods 0.000 title claims abstract description 138
- 235000013599 spices Nutrition 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000796 flavoring agent Substances 0.000 claims abstract description 24
- 235000019634 flavors Nutrition 0.000 claims abstract description 20
- 239000002304 perfume Substances 0.000 claims description 58
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 42
- 235000019504 cigarettes Nutrition 0.000 claims description 31
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 30
- 239000002609 medium Substances 0.000 claims description 30
- 239000003571 electronic cigarette Substances 0.000 claims description 25
- 239000002245 particle Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 24
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 23
- 239000002904 solvent Substances 0.000 claims description 23
- 239000012141 concentrate Substances 0.000 claims description 20
- 238000002791 soaking Methods 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 18
- 240000007154 Coffea arabica Species 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 12
- 235000016213 coffee Nutrition 0.000 claims description 12
- 235000013353 coffee beverage Nutrition 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002390 rotary evaporation Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 6
- 244000119298 Emblica officinalis Species 0.000 claims description 5
- 235000015489 Emblica officinalis Nutrition 0.000 claims description 5
- 239000008213 purified water Substances 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 244000241257 Cucumis melo Species 0.000 claims description 4
- 240000004584 Tamarindus indica Species 0.000 claims description 4
- 235000004298 Tamarindus indica Nutrition 0.000 claims description 4
- 229940119429 cocoa extract Drugs 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 229940057917 medium chain triglycerides Drugs 0.000 claims description 4
- 229940062013 tamarind extract Drugs 0.000 claims description 4
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 3
- 240000002547 Rosa roxburghii Species 0.000 claims description 3
- 235000000640 Rosa roxburghii Nutrition 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 235000009470 Theobroma cacao Nutrition 0.000 claims description 3
- 244000299461 Theobroma cacao Species 0.000 claims description 3
- 239000010962 carbon steel Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 235000009847 Cucumis melo var cantalupensis Nutrition 0.000 claims description 2
- 235000009815 Momordica Nutrition 0.000 claims description 2
- 241000218984 Momordica Species 0.000 claims description 2
- 235000013399 edible fruits Nutrition 0.000 claims description 2
- 244000061176 Nicotiana tabacum Species 0.000 claims 1
- 239000000779 smoke Substances 0.000 abstract description 15
- 235000019505 tobacco product Nutrition 0.000 abstract description 4
- 230000003313 weakening effect Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 31
- 241000208125 Nicotiana Species 0.000 description 22
- 238000011156 evaluation Methods 0.000 description 17
- 239000007789 gas Substances 0.000 description 11
- 238000000605 extraction Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 230000001953 sensory effect Effects 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000000391 smoking effect Effects 0.000 description 4
- 206010013911 Dysgeusia Diseases 0.000 description 3
- 239000003205 fragrance Substances 0.000 description 3
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 description 2
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- 244000207740 Lemna minor Species 0.000 description 1
- 235000006439 Lemna minor Nutrition 0.000 description 1
- 235000001855 Portulaca oleracea Nutrition 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 240000006023 Trichosanthes kirilowii Species 0.000 description 1
- 235000009818 Trichosanthes kirilowii Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 235000019568 aromas Nutrition 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 235000020289 caffè mocha Nutrition 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/08—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in rotating vessels; Atomisation on rotating discs
- B01D3/085—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in rotating vessels; Atomisation on rotating discs using a rotary evaporator
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/51—Methods thereof
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
-
- 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
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/21—Mixing of ingredients for cosmetic or perfume compositions
-
- 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
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Botany (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a semi-dry distillation natural spice, a preparation method and application thereof. The semi-dry distillation natural spice provided by the invention can improve the smoke layering sense of main stream smoke of tobacco products, increase the baking aroma of the smoke, improve the definition of the smoke, endow the smoke with different flavors by different types of semi-dry distillation natural spices, soften the smoke and enable the smoke to be more full on the premise of not weakening the original aroma.
Description
Technical Field
The invention belongs to the field of tobacco flavor. More particularly, the present invention relates to a semi-dry distilled natural perfume, to a method for preparing the semi-dry distilled natural perfume, and to the use of the semi-dry distilled natural perfume.
Background
With the development of the cigarette industry technology, cigarettes are not limited to single tobacco aroma, and the exogenous aroma substances of the tobacco are added into the cigarettes, so that the aroma style can be enriched, the beneficial components are increased, and the aroma of the cigarettes is more elegant and unique. Moreover, smokers also enjoy receiving gracefully coordinated exogenous aromas in cigarettes.
The semi-dry distillation natural spice preparation method is an extraction process between distillation and carbonization processes, the extractive aroma substances are carried out by steam by means of distillation principle, meanwhile, baking burnt aroma in the reaction substances is continuously extracted under carbonization conditions, and the two are mixed to form special aroma with the extractive flavor and compatible with the original aroma of tobacco products, so that the layering sense and plumpness of smoke are increased, and the sensory experience of smokers on the tobacco products is met. Through literature search, no research report on the application of the tobacco to tobacco is available up to the present time.
Disclosure of Invention
Technical problem to be solved
The invention aims to provide a semi-dry distillation natural spice.
It is another object of the present invention to provide a method for preparing the semi-distilled natural perfume.
It is a further object of the present invention to provide the use of said semi-dry distillation natural perfume.
Technical proposal
The invention is realized by the following technical scheme.
The invention relates to a preparation method of semi-dry distillation natural perfume.
The preparation method comprises the following preparation steps:
A. pretreatment of
Preparing natural perfume into particles with the granularity of 10-20 meshes or water extract or alcohol extract;
B. soaking
Uniformly mixing the natural spice particles or extractum obtained in the step A with a semi-dry distillation medium, and soaking for 30-60 min at room temperature to obtain a mixture;
C. semi-destructive distillation
The mixture obtained in the step B is subjected to half dry distillation for 0.5 to 2.0 hours in semi-dry distillation equipment at the temperature of 120 to 200 ℃ and the heating rate of 5 to 10 ℃/min, volatile gas generated in the semi-dry distillation process is condensed, and condensate is collected;
D. concentrating
Evaporating and concentrating the condensate obtained in the step C by using a rotary evaporation device until the water content is below 5% by weight, and obtaining a concentrate according to the volume ratio of the solvent to the concentrate of 1:0.1 to 20 portions of the natural perfume are dissolved by using a solvent, and the solution is filtered and collected to be the semi-dry distillation natural perfume.
According to a preferred mode of the invention, in step a, the natural flavor is a tobacco, coffee, cocoa, tamarind, grosvenor momordica, phyllanthus emblica, cantaloupe or rosa roxburghii natural flavor.
According to another preferred mode of the present invention, in the step a, the extract is a cocoa extract, tamarind extract, fructus momordicae extract, coffee extract or zimbabwe extract.
According to another preferred mode of the invention, in step B, said semi-dry distillation medium is one or more semi-dry distillation media selected from distilled water, propylene glycol, glycerol or medium chain triglycerides.
According to another preferred mode of the invention, in step B, the weight ratio of natural perfume particles or extract to semi-dry distillation medium is 1:0.5 to 10.0.
According to another preferred mode of the present invention, in the step C, the semi-dry distillation apparatus is a glass reaction vessel, a carbon steel reaction vessel, a stainless steel reaction vessel or a steel lining reaction vessel semi-dry distillation apparatus.
According to another preferred mode of the invention, in step D, the condensate obtained in step C is concentrated to a water content of less than 5% by weight using a rotary evaporation device at a temperature of 40-80 ℃ and a pressure of-0.07 to-0.02 MPa.
According to another preferred mode of the present invention, in the step D, the solvent is propylene glycol, purified water, glycerol or alcohol having a concentration of 50 to 95% by volume.
The invention also relates to the semi-dry distillation natural perfume prepared by the preparation method.
The invention also relates to the application of the semi-dry distillation natural perfume in the traditional cigarettes, heating non-combustible products and electronic cigarettes, and the addition amount of the semi-dry distillation natural perfume in the traditional cigarettes is 0.01-5.0% by weight; the addition amount of the additive in the heating non-combustible product is 0.1 to 10 percent by weight; the addition amount of the additive in the electronic cigarette is 0.1-50.0% by weight.
The present invention will be described in more detail below.
The invention relates to a preparation method of semi-dry distillation natural perfume.
The preparation method comprises the following preparation steps:
A. pretreatment of
Preparing natural perfume into particles with the granularity of 10-20 meshes or water extract or alcohol extract;
according to the invention, the natural perfume is a natural perfume of tobacco, coffee, cocoa, tamarind, fructus momordicae, phyllanthus emblica, trichosanthes kirilowii or rosa roxburghii. The tobacco raw materials used in the invention are tobacco raw materials such as flue-cured tobacco, burley tobacco, sun-cured tobacco or aromatic tobacco which are commonly used in the current tobacco technical field, and the coffee raw materials used in the invention are coffee raw materials such as small-grain coffee, blue mountain coffee, mocha coffee or golden mannite which are commonly used in the current tobacco technical field. The tamarind fruit, the fructus momordicae, the phyllanthus emblica and the sour melon or the roxburgh rose which are used in the invention are all products sold in the market at present.
The particle size is 10-20 meshes. If the particle size is smaller than 10 meshes, the extraction medium is not easy to soak into the bottom of the material, so that the material at the bottom is not extracted; if the particle size is larger than 20 meshes, the extraction medium is not easy to permeate into the particles, so that the extraction effect is poor; therefore, it is reasonable that the particle size is 10 to 20 mesh;
the water extract or the alcohol extract used in the invention are all products sold in the market at present, such as cocoa extract sold by Shaoxing Kokoku bridge green source perfume Limited under the trade name of cocoa extract, tamarind extract sold by Shaoxing Koku bridge green source perfume Limited under the trade name of tamarind extract, fructus Siraitiae Grosvenorii extract sold under the trade name fructus Siraitiae Grosvenorii extract by Shaoxing Kochiae Green Source perfume Limited company, coffee extract sold under the trade name coffee extract by Shanxi Meifeng Fengda ecological agriculture Limited company, zimbabwe tobacco extract sold under the trade name Zimbabwe tobacco extract by Shanghai Meifeng chemical technology Limited company.
B. Soaking
Uniformly mixing the natural spice particles or extractum obtained in the step A with a semi-dry distillation medium, and soaking for 30-60 min at room temperature to obtain a mixture;
according to the invention, the main purpose of soaking the natural spice particles or the extract in the semi-dry distillation medium is to enable the medium to fully soak the natural spice or fully mix the natural spice with the extract, so that the extraction efficiency and the extraction yield are improved.
The semi-dry distillation medium is one or more selected from distilled water, propylene glycol, glycerol or medium chain triglyceride. The semi-dry distillation media used in the present invention are all products sold in the current market, such as propylene glycol sold under the trade name propylene glycol by the company of the chemical industry, inc. of Guangzhou, and glycerol sold under the trade name glycerol by the company of the chemical industry, inc. of Guangzhou, and medium chain triglycerides sold under the trade name medium chain triglycerides by the company of the biological technology, inc. of Shandong Duckweed.
In this step, the weight ratio of the natural perfume particles or extract to the semi-dry distillation medium is 1:0.5 to 10.0. If the weight ratio of the natural spice particles or the extract to the semi-dry distillation medium is more than 1:0.5, the medium cannot fully soak the natural spice particles or the extractum, so that the heating is uneven, and the semi-dry distillation effect is affected; if the weight ratio of the natural spice particles or the extract to the semi-dry distillation medium is less than 1:10.0, too much medium and too long heating time lead to unreasonable energy utilization and waste; therefore, the weight ratio of the natural spice particles or the extract to the semi-dry distillation medium is 1:0.5 to 10.0 is reasonable;
the soaking time of the natural spice particles or the extract in the semi-dry distillation medium is 30-60 min. If this soaking time is shorter than 30 minutes, it is difficult to ensure that the medium is completely saturated with natural perfume particles or extract; if the soaking time is longer than 60min, waste is caused to production and experiment time; therefore, this soaking time is suitably 30 to 60 minutes;
C. semi-destructive distillation
The mixture obtained in the step B is subjected to half dry distillation for 0.5 to 2.0 hours in semi-dry distillation equipment at the temperature of 120 to 200 ℃ and the heating rate of 5 to 10 ℃/min, volatile gas generated in the semi-dry distillation process is condensed, and condensate is collected;
the semi-dry distillation apparatus should be a separation apparatus having a structure capable of performing both semi-dry distillation and gas condensation, and in particular, the semi-dry distillation apparatus structure is disclosed in document CN115161111a as a perfume dry distillation extraction device. The semi-dry distillation apparatus used in the present invention is a glass reaction vessel, a carbon steel reaction vessel, a stainless steel reaction vessel or a steel lining reaction vessel, which are all products currently commercially available, for example, products sold under the trade name glass reaction vessel by Henan China, yi-Tech Co., ltd.
The mixture obtained in the step B is subjected to half dry distillation in the kettle body of the half dry distillation equipment.
In this section, the mixture is half-distilled at a temperature of 120 to 200 ℃ and a heating rate of 5 to 10 ℃/min for 0.5 to 2.0 hours. When the heating rate and the semi-dry distillation time are in the ranges, if the semi-dry distillation temperature is lower than 120 ℃, the macromolecular substance cracking effect can not be achieved, and the semi-dry distillation purpose can not be achieved; if the semi-dry distillation temperature is higher than 200 ℃, the semi-dry distillation is excessively cracked and gelatinized to generate bad smell, and the quality of the spice is affected; therefore, a semi-dry distillation temperature of 120 to 200℃is suitable; when the semi-dry distillation temperature and the semi-dry distillation time are in the ranges, if the temperature rising rate is lower than 5 ℃/min, the semi-dry distillation temperature rising time is too long, and the production efficiency is affected; if the heating rate is higher than 10 ℃/min, the heating is too fast, the temperature is not easy to control, and the separation effect of the semi-dry distillation substances is affected; therefore, a heating rate of 5 to 10℃per minute is suitable; when the semi-dry distillation temperature and the heating rate are in the ranges, if the semi-dry distillation time is shorter than 0.5h, the semi-dry distillation degree is insufficient, most of water in distillate is easily caused, and the product yield is low; if the half dry distillation time is longer than 2.0h, the half dry distillation is excessive, bad burnt smell is generated, and the product quality is affected; therefore, a half-dry distillation time of 0.5 to 2.0 hours is preferable.
Volatile gases generated during the semi-dry distillation are condensed into a condensate at a low temperature in a condensing tube portion of the semi-dry distillation apparatus.
D. Concentrating
Evaporating and concentrating the condensate obtained in the step C by using a rotary evaporation device until the water content is below 5% by weight, and obtaining a concentrate according to the volume ratio of the solvent to the concentrate of 1:0.1 to 20 portions of the natural perfume are dissolved by using a solvent, and the solution is filtered and collected to be the semi-dry distillation natural perfume.
According to the invention, the condensate obtained in step C is concentrated to a water content of less than 5% by weight using a rotary evaporation apparatus sold under the trade name rotary evaporator by the company Zhengzhou Huate instruments and Equipment Co., ltd. Under the conditions of a temperature of 40 to 80℃and a pressure of-0.07 to-0.02 MPa, the water content being detected according to the standard analytical method of the oven method.
The resulting concentrate was prepared in a solvent to concentrate volume ratio of 1:0.1 to 20 is dissolved by using a solvent, wherein the solvent is propylene glycol, purified water, glycerol or alcohol with the concentration of 50 to 95 percent by volume, and the propylene glycol, the purified water and the glycerol are all products sold in the current market. If the solvent to concentrate volume ratio is greater than 1:0.1, the fragrance intensity is too low; if the solvent to concentrate volume ratio is less than 1:20, too little solvent does not act to dissolve the concentrate; thus, the solvent to concentrate volume ratio is 1:0.1 to 20 is preferable.
The invention also relates to the semi-dry distillation natural perfume prepared by the preparation method.
The invention also relates to application of the semi-dry distillation natural perfume in traditional cigarettes, heating non-combustible products and electronic cigarettes.
The addition amount of the semi-dry distillation natural perfume in the traditional cigarette is 0.01-5.0% by weight; in the traditional cigarettes, if the addition amount of the semi-dry distillation natural spice is less than 0.01%, the aroma intensity is insufficient, and no obvious aroma enhancement effect is achieved; if the addition amount of the semi-dry distillation natural spice is higher than 5.0%, the aroma intensity is too high and the application cost is high; therefore, it is appropriate that the addition amount of the semi-dry distilled natural perfume is 0.01 to 5.0%;
the addition amount of the semi-dry distillation natural perfume in the heating non-combustible product is 0.1-10.0% by weight. In the heated non-combustible product, if the addition amount of the semi-destructive distillation natural perfume is less than 0.1%, no obvious flavoring effect is obtained; if the addition amount of the semi-dry distillation natural spice is higher than 10.0%, the aroma intensity is too high and the application cost is high; therefore, it is preferable that the amount of the semi-distilled natural perfume to be added is 0.1 to 10.0%.
The addition amount of the semi-dry distillation natural perfume in the electronic cigarette is 0.1-50.0% by weight. In the electronic cigarette, if the addition amount of the semi-dry distillation natural spice is less than 0.1%, no obvious aroma enhancement effect is achieved; if the addition amount of the semi-dry distillation natural spice is higher than 50.0%, the aroma intensity is too high and the application cost is high; therefore, it is preferable that the amount of the semi-distilled natural perfume to be added is 0.1 to 50%.
According to GB 5606.4-2005 part 4 of cigarette: sensory technology requirements, the traditional cigarettes, heated non-combustible products and electronic cigarettes with or without the semi-distilled natural flavors of the invention are compared and smoked by a smoking group consisting of 7 smokers, and the smoking results are described in the detailed description.
Advantageous effects
The beneficial effects of the invention are as follows: the semi-dry distillation natural spice provided by the invention can improve the smoke layering sense of main stream smoke of tobacco products, increase the baking aroma of the smoke, improve the definition of the smoke, endow the smoke with different flavors by different types of semi-dry distillation natural spices, soften the smoke and enable the smoke to be more full on the premise of not weakening the original aroma.
Detailed Description
The invention will be better understood by the following examples.
Example 1: the invention relates to the preparation of semi-dry distillation natural spice
The implementation steps of this embodiment are as follows:
A. pretreatment of
Preparing the flue-cured tobacco into natural spice extract by adopting an alcohol extraction method;
B. soaking
The weight ratio of the natural spice extract to the semi-dry distillation medium is 1:6.8, uniformly mixing the natural spice extract obtained in the step A with a semi-dry distillation medium consisting of distilled water and propylene glycol (volume ratio is 1:1), and soaking for 40min at room temperature to obtain a mixture;
C. semi-destructive distillation
The mixture obtained in the step B is subjected to semi-dry distillation for 1.0h in semi-dry distillation equipment sold by Henan Yi-Tech Co., ltd under the trade name of glass reaction kettle at the temperature of 172 ℃ and the heating rate of 10 ℃/min, volatile gas generated in the semi-dry distillation process is condensed under the low temperature condition, and condensate is collected;
D. concentrating
The condensate obtained in step C was concentrated to a water content of 4.8% by weight at a temperature of 70 ℃ and a pressure of-0.07 MPa using a rotary evaporation apparatus sold under the trade name rotary evaporator by the company of the wharf instruments, zheng, and the resulting concentrate was further prepared according to a solvent to concentrate volume ratio of 1:20.0 using propylene glycol solvent, filtering, collecting the solution which is the semi-dry distillation natural perfume.
The tobacco flavor semi-dry distillation spice prepared in the embodiment has the additive amount of 5.0% by weight in the traditional cigarette; its addition in the heated non-combustible product was 7.0% by weight; the addition amount of the additive in the electronic cigarette is 15.0% by weight.
The tobacco-flavor semi-dry distillation flavor prepared in this example was evaluated in conventional cigarettes, heated non-combustible products, and electronic cigarettes according to the methods described in the present specification, the evaluation results in conventional cigarettes are shown in table 1, the evaluation results in heated non-combustible products are shown in table 2, and the evaluation results in electronic cigarettes are shown in table 3.
Example 2: the invention relates to the preparation of semi-dry distillation natural spice
The implementation steps of this embodiment are as follows:
A. pretreatment of
Preparing natural perfume of the phyllanthus emblica extract into an extract by adopting an alcohol extraction method;
B. soaking
The weight ratio of the natural spice extract to the semi-dry distillation medium is 1:0.05, uniformly mixing the natural spice extract obtained in the step A with a propylene glycol semi-dry distillation medium, and soaking for 30min at room temperature to obtain a mixture;
C. semi-destructive distillation
The mixture obtained in the step B is subjected to semi-dry distillation for 2.0 hours in semi-dry distillation equipment sold by Henan Yi-Tech Co., ltd under the trade name of glass reaction kettle at the temperature of 120 ℃ and the heating rate of 5 ℃/min, volatile gas generated in the semi-dry distillation process is condensed under the low temperature condition, and condensate is collected;
D. concentrating
Concentrating the condensate obtained in step C to a water content of 4.6% by weight at a temperature of 60 ℃ and a pressure of-0.06 MPa using a rotary evaporation apparatus sold under the trade name rotary evaporator by the company of the wharf instruments, zheng, the concentrate obtained being further prepared according to a solvent to concentrate volume ratio of 1:0.1 dissolution with glycerol solvent, filtration and collection of the solution was the semi-distilled natural perfume.
The tobacco flavor semi-dry distillation spice prepared in the embodiment has the additive amount of 0.01 percent by weight in the traditional cigarette; its addition in the heated non-combustible product was 0.1% by weight; the addition amount of the additive in the electronic cigarette is 35.0% by weight.
The tobacco-flavor semi-dry distillation flavor prepared in this example was evaluated in conventional cigarettes, heated non-combustible products, and electronic cigarettes according to the methods described in the present specification, the evaluation results in conventional cigarettes are shown in table 1, the evaluation results in heated non-combustible products are shown in table 2, and the evaluation results in electronic cigarettes are shown in table 3.
Example 3: the invention relates to the preparation of semi-dry distillation natural spice
The implementation steps of this embodiment are as follows:
A. pretreatment of
Crushing the sour melon by a pulverizing machine to obtain 10-20 mesh particles;
B. soaking
The weight ratio of the natural spice particles to the semi-dry distillation medium is 1:3.4, uniformly mixing the natural spice particles obtained in the step A with a semi-dry distillation medium of a mixture of propylene glycol and medium chain triglyceride (volume ratio is 2:1), and soaking for 50min at room temperature to obtain a mixture;
C. semi-destructive distillation
The mixture obtained in the step B is subjected to semi-dry distillation for 1.5 hours at the temperature of 146 ℃ and the heating rate of 7 ℃/min in semi-dry distillation equipment sold by the environment-friendly equipment limited responsibility company under the trade name of stainless steel reaction kettles, volatile gas generated in the semi-dry distillation process is condensed at a low temperature, and condensate is collected;
D. concentrating
Concentrating the condensate obtained in step C to a water content of 4.9% by weight at a temperature of 80 ℃ and a pressure of-0.05 MPa using a rotary evaporation apparatus sold under the trade name rotary evaporator by the company of Ministry of Kogyo-Kagaku, the obtained concentrate being further subjected to a solvent to concentrate volume ratio of 1:7.0 dissolving with purified water solvent, filtering, collecting the solution which is the semi-dry distillation natural perfume.
The tobacco flavor semi-dry distillation spice prepared in the embodiment has the additive amount of 2.0% by weight in the traditional cigarette; its addition in the heated non-combustible product was 3.0% by weight; the addition amount of the additive in the electronic cigarette is 0.1% by weight.
The tobacco-flavor semi-dry distillation flavor prepared in this example was evaluated in conventional cigarettes, heated non-combustible products, and electronic cigarettes according to the methods described in the present specification, the evaluation results in conventional cigarettes are shown in table 1, the evaluation results in heated non-combustible products are shown in table 2, and the evaluation results in electronic cigarettes are shown in table 3.
Example 4: the invention relates to the preparation of semi-dry distillation natural spice
The implementation steps of this embodiment are as follows:
A. pretreatment of
Crushing the natural fructus rosae roxburghii perfume into particles with the granularity of 10-20 meshes by adopting a pulverizing machine crushing method;
B. soaking
The weight ratio of the natural spice extract to the semi-dry distillation medium is 1:10.0, uniformly mixing the natural spice extract obtained in the step A with a propylene glycol semi-dry distillation medium, and soaking for 60 minutes at room temperature to obtain a mixture;
C. semi-destructive distillation
The mixture obtained in the step B is subjected to semi-dry distillation for 0.5h in semi-dry distillation equipment sold by the environment-friendly equipment limited company under the trade name of stainless steel reaction kettles at the temperature of 200 ℃ and the heating rate of 8 ℃/min, volatile gas generated in the semi-dry distillation process is condensed under the low temperature condition, and condensate is collected;
D. concentrating
Concentrating the condensate obtained in step C to a water content of 4.2% by weight at a temperature of 50 ℃ and a pressure of-0.07 MPa using a rotary evaporation apparatus sold under the trade name rotary evaporator by the company of Ministry of Kogyo-Kagaku, the obtained concentrate being further subjected to a solvent to concentrate volume ratio of 1:14.0 using an alcohol solvent at a concentration of 85% by volume, filtering, and collecting the solution which is the semi-distilled natural perfume.
The tobacco flavor semi-dry distillation spice prepared in the embodiment has the additive amount of 4.0% by weight in the traditional cigarette; its addition in the heated non-combustible product was 10.0% by weight; the addition amount of the additive in the electronic cigarette is 50.0% by weight.
The tobacco-flavor semi-dry distillation flavor prepared in this example was evaluated in conventional cigarettes, heated non-combustible products, and electronic cigarettes according to the methods described in the present specification, the evaluation results in conventional cigarettes are shown in table 1, the evaluation results in heated non-combustible products are shown in table 2, and the evaluation results in electronic cigarettes are shown in table 3.
Table 1: evaluation results of traditional cigarette containing semi-dried distilled natural perfume of the invention
The smoking evaluation results listed in table 1 show that the application of the semi-dry distillation natural perfume in cigarettes obviously improves the sensory quality of the cigarettes, and compared with a blank control without the semi-dry distillation natural perfume, the semi-dry distillation natural perfume improves the baking aroma of the traditional cigarettes, gives the cigarettes coordinated flavor, and has certain improvements on miscellaneous gases, pungent aftertaste and the like, and the sensory experience is more pleasant.
Table 2: evaluation results of heated nonflammable products containing semi-distilled natural fragrances of the present invention
The suction evaluation results listed in table 2 show that the application of the semi-dry distillation natural perfume in the heating non-combustion products improves the sensory quality of the heating non-combustion products, and compared with a blank control without the semi-dry distillation natural perfume, the semi-dry distillation natural perfume improves the baking fragrance in the heating non-combustion products, and endows the heating non-combustion products with coordinated flavor, and in addition, miscellaneous gases, pungent aftertaste and the like are improved to a certain extent, so that the sensory experience is more pleasant.
Table 3: electronic cigarette smoking result containing semi-dry distillation natural perfume of the invention
The evaluation results listed in table 3 show that the application of the semi-dry distillation natural perfume in the electronic cigarette improves the sensory quality of the electronic cigarette, and compared with a blank control without the semi-dry distillation natural perfume, the semi-dry distillation natural perfume improves the baking aroma in the electronic cigarette, gives the electronic cigarette a coordinated flavor, and has improved miscellaneous gases, pungent aftertaste and the like, and the sensory experience is more pleasant.
Claims (10)
1. The preparation method of the semi-dry distillation natural perfume is characterized by comprising the following preparation steps of:
A. pretreatment of
Preparing natural perfume into particles with the granularity of 10-20 meshes or water extract or alcohol extract;
B. soaking
Uniformly mixing the natural spice particles or extractum obtained in the step A with a semi-dry distillation medium, and soaking for 30-60 min at room temperature to obtain a mixture;
C. semi-destructive distillation
The mixture obtained in the step B is subjected to half dry distillation for 0.5 to 2.0 hours in semi-dry distillation equipment at the temperature of 120 to 200 ℃ and the heating rate of 5 to 10 ℃/min, volatile gas generated in the semi-dry distillation process is condensed, and condensate is collected;
D. concentrating
Evaporating and concentrating the condensate obtained in the step C by using a rotary evaporation device until the water content is below 5% by weight, and obtaining a concentrate according to the volume ratio of the solvent to the concentrate of 1:0.1 to 20 portions of the natural perfume are dissolved by using a solvent, and the solution is filtered and collected to be the semi-dry distillation natural perfume.
2. The method according to claim 1, wherein in step a, the natural flavor is a natural flavor of tobacco, coffee, cocoa, tamarind, grosvenor momordica, emblic leafflower fruit, cantaloupe or rosa roxburghii.
3. The method according to claim 1, wherein in step a, the extract is a cocoa extract, tamarind extract, fructus momordicae extract, coffee extract or zimbabwe extract.
4. The process according to claim 1, wherein in step B, the semi-dry distillation medium is one or more semi-dry distillation media selected from distilled water, propylene glycol, glycerol or medium chain triglycerides.
5. The method according to claim 1, wherein in step B, the weight ratio of the natural perfume particles or extract to the semi-dry distillation medium is 1:0.5 to 10.0.
6. The method according to claim 1, wherein in the step C, the semi-dry distillation apparatus is a glass reaction vessel, a carbon steel reaction vessel, a stainless steel reaction vessel or a steel lining reaction vessel semi-dry distillation apparatus.
7. The process according to claim 1, wherein in step D, the condensate obtained in step C is concentrated to a water content of 5% by weight or less using a rotary evaporation apparatus at a temperature of 40 to 80℃and a pressure of-0.07 to-0.02 MPa.
8. The method according to claim 1, wherein in the step D, the solvent is propylene glycol, purified water, glycerol or alcohol having a concentration of 50 to 95% by volume.
9. A semi-distilled natural perfume prepared by the method according to any one of claims 1 to 8.
10. The use of the semi-dry distillation natural perfume according to claim 9 in conventional cigarettes, heated non-combustible products and electronic cigarettes, characterized in that its addition in conventional cigarettes is 0.01-5.0% by weight; the addition amount of the additive in the heating non-combustible product is 0.1 to 10 percent by weight; the addition amount of the additive in the electronic cigarette is 0.1-50.0% by weight.
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| CN1050213A (en) * | 1989-09-14 | 1991-03-27 | 韩连恩 | Semi-dry distillation gas producer and gas making method |
| CN110839947A (en) * | 2019-10-16 | 2020-02-28 | 云南中烟工业有限责任公司 | Extraction process of plant spice for cigarette without burning under heating |
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| CN114504119A (en) * | 2022-03-29 | 2022-05-17 | 南京林业大学 | Tobacco flavor extraction method |
| CN114703021A (en) * | 2022-03-21 | 2022-07-05 | 云南巴菰生物科技股份有限公司 | Emblic leafflower fruit extract and its preparing method and use |
| CN115161111A (en) * | 2022-08-23 | 2022-10-11 | 云南中烟工业有限责任公司 | Spices dry distillation extraction element |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1050213A (en) * | 1989-09-14 | 1991-03-27 | 韩连恩 | Semi-dry distillation gas producer and gas making method |
| CN110839947A (en) * | 2019-10-16 | 2020-02-28 | 云南中烟工业有限责任公司 | Extraction process of plant spice for cigarette without burning under heating |
| CN113717795A (en) * | 2021-09-27 | 2021-11-30 | 南京林业大学 | Novel multifunctional steam distillation-dry distillation integrated equipment |
| CN114703021A (en) * | 2022-03-21 | 2022-07-05 | 云南巴菰生物科技股份有限公司 | Emblic leafflower fruit extract and its preparing method and use |
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