CN112795428A - Lotus-fragrance-style tobacco essence and preparation method and application thereof - Google Patents

Lotus-fragrance-style tobacco essence and preparation method and application thereof Download PDF

Info

Publication number
CN112795428A
CN112795428A CN202110141532.7A CN202110141532A CN112795428A CN 112795428 A CN112795428 A CN 112795428A CN 202110141532 A CN202110141532 A CN 202110141532A CN 112795428 A CN112795428 A CN 112795428A
Authority
CN
China
Prior art keywords
lotus
fresh
mixing
liquid
ethanol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN202110141532.7A
Other languages
Chinese (zh)
Inventor
郝红玲
戴亚
何爱民
李杰辉
苏国岁
王龙
冯文宁
林洁
张艳芳
阎瑾
陈伟华
李远根
马戎
张晓静
卜一凡
寇天舒
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HEBEI CHINA TOBACCO INDUSTRY CO LTD
Original Assignee
HEBEI CHINA TOBACCO INDUSTRY CO LTD
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by HEBEI CHINA TOBACCO INDUSTRY CO LTD filed Critical HEBEI CHINA TOBACCO INDUSTRY CO LTD
Priority to CN202110141532.7A priority Critical patent/CN112795428A/en
Publication of CN112795428A publication Critical patent/CN112795428A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/0003Compounds of unspecified constitution defined by the chemical reaction for their preparation
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/24Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • A24B15/26Use of organic solvents for extraction
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/12Steaming, curing, or flavouring tobacco
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Preparation Of Fruits And Vegetables (AREA)
  • Fats And Perfumes (AREA)
  • Seasonings (AREA)

Abstract

The invention discloses an essence for cigarette with lotus fragrance style and a preparation method and application thereof, wherein the essence is prepared by fully and uniformly mixing prepared fresh lotus essential oil, fresh lotus dew and cigarette filter tip flavoring liquid according to a proportion, and the essence for cigarette with lotus fragrance style can be applied to a filter tip core wire or added into a filter tip bead explosion and then is rolled into a cigarette; the fresh lotus flower juice contains various water-soluble alcohols and other substances, has elegant fragrance, can improve the mellowness of smoke, improves the taste of cigarettes, can increase the fragrance of the existing cigarettes, and improves the mellowness and the fineness and the softness of the smoke.

Description

Lotus-fragrance-style tobacco essence and preparation method and application thereof
Background
Lotus (Nymphaeaceae) Nelumbo (Nelumbbo) perennial herb plants of the Nymphaeaceae family, the lotus is originally produced in China, is wild or cultivated, has a long history and rich resources, and is widely distributed in Shandong, Hunan, Hubei, Zhejiang, Guangdong, Hebei and the like in yellow river, Yangtze river and Zhujiang river basin. Lotus is a medicinal and edible plant, and lotus seeds, lotus coats, lotus seedcases, lotus stamens, lotus plumule, lotus leaves, lotus stalks, lotus nodes and the like of the lotus can be used as medicines. The lotus has ornamental value, and the lotus petals have the medicinal effects of promoting blood circulation, stopping bleeding, eliminating dampness, dispelling wind, clearing away the heart-fire, cooling blood, relieving fever, detoxifying and the like.
In the traditional cigarette flavoring technology, spice liquid is mainly added into tobacco shreds, the spice liquid added in the mode is partially lost in the cigarette combustion process, and meanwhile, as the reaction of a complex material system at high temperature is difficult to expect, part of the spice liquid can generate some bad sensory effects. As a new cigarette flavoring mode, such as flavoring of a filter stick core wire, flavoring of a filter stick bead blasting and the like, the defects in the existing flavoring mode can be overcome to a certain extent: when the cigarette is smoked, smoke passes through the filter tip and synergistically acts on a consumer with essence substances contained in the core wire or the crushed exploded bead, so that the perfuming and aroma-supplementing process is completed, and the loss of the essence and the aroma in the combustion process of the tobacco is effectively avoided.
The cigarette perfuming fragrance can provide special mood, induce memory, excite resonance and enrich feelings. The lotus has elegant flower color and far-reaching fragrance. The lotus has high ornamental value and deep culture bottom, and in Chinese culture, the lotus becomes a culture symbol bearing the pursuit of people for beauty and high cleanliness.
CN10507755B discloses a preparation method and application of a green lotus flavor plant cigarette material, which selects natural plants lotus, lotus leaf and lotus seed, and adds various raw materials of green lotus as slices into cigarettes. The raw materials used in the method are lotus flowers, lotus leaves and the like, the lotus flowers, lotus leaves and the like can be used as thin sheets to be blended into cigarettes, the safety performance is strong, the style characteristics of the materials with the flavor of the green lotus can be highlighted, the fragrance of the cigarettes is coordinated, the tar and harm reducing effects of the cigarettes can be effectively improved, the cigarettes can have typical faint scent and sweet fragrance, the stimulation is reduced, and the smoke is fine and soft. However, in the technical scheme, the lotus, lotus leaf, lotus seed and other raw materials are adopted instead of the lotus extract, so that a large amount of fragrance components are possibly lost in the production processes of pulping, drying and the like of the slices, and the natural and pure fragrance of the lotus is difficult to obtain.
CN107641557A discloses essence for lotus pond moonlight artistic conception cigarettes and a preparation method and application thereof, and the essence is prepared by mixing and compounding prepared lotus leaf extract, lotus flower extract, honeysuckle flower extract and chrysanthemum flower extract. The cigarette product added with the tobacco essence has the advantages of good tobacco shred gloss and plumpness, obviously reduced burning sensation and pungent taste of the cigarette, and increased special aroma of the cigarette. However, the related lotus leaf and lotus flower extracts are ethanol extracts of the lotus leaf and lotus flower, wherein the lotus leaf and lotus flower mainly contain polar components, so that the defects of few types of aroma components, low content, large addition amount, lack of cigarette smoking comfort level and the like exist.
Disclosure of Invention
The invention provides a technical scheme for adding lotus fragrance style tobacco essence into a cigarette filter, wherein the essence flavored by the filter directly enters the mouth of a smoker along with the smoking airflow without burning, the flavoring amount can be accurately controlled, the fragrance style of the cigarette is enhanced, the stimulation is reduced, the fragrance is fused with the consumption feeling, and the smoking comfort and the safety of the cigarette are improved.
In order to achieve the aim of the invention, the lotus-fragrance tobacco essence is characterized by comprising the following components in parts by weight: 1-60 parts of fresh lotus essential oil, 1-100 parts of fresh lotus dew and 1000000 parts of cigarette filter flavoring liquid, wherein the cigarette filter flavoring liquid consists of Zimbabwe tobacco extract, sophora flower extract, jujube honey extract and absolute ethyl alcohol, and the volume of the cigarette filter flavoring liquid is 4:3:1: 990-1000.
The preparation method of the lotus fragrance style tobacco essence is characterized by comprising the following steps:
A. preparation of fresh lotus essential oil:
a. uniformly spraying 1-20% of enzymolysis liquid with mass concentration in fresh lotus petals and a filament raw material from which impurities such as receptacle, lotus seeds and the like are removed, and carrying out enzymolysis for 3-4 h at 30-38 ℃, wherein the enzymolysis liquid is an aqueous solution of cellulase, hemicellulase and pectinase, and the weight parts of the cellulase, hemicellulase and pectinase are as follows: 0.1-1: 0.05-0.5: 0.08-0.9, wherein the fresh lotus petals and the fresh lotus filaments are prepared from the raw materials and the enzymatic hydrolysate in parts by weight: 100-200: 1;
b. crushing the mixture of the petals and the filaments after enzymolysis to 20-40 meshes, then carrying out sealed refrigeration at 10-15 ℃ and 60-65% humidity for 2-48 hours, adding 95% ethanol, introducing 100-110 ℃ water vapor, and distilling for 3-4 hours to obtain fresh lotus essential oil, wherein the weight part ratio of the ethanol to the mixture of the petals and the filaments after enzymolysis is 0.1-1: 100, and the flow rate of the water vapor is 16 kg/h;
B. preparation of fresh lotus flower syrup:
a. uniformly spraying 1-20% of enzymolysis liquid with mass concentration in fresh lotus petals and a filament raw material from which impurities such as receptacle, lotus seeds and the like are removed, and carrying out enzymolysis for 3-4 h at 30-38 ℃, wherein the enzymolysis liquid is an aqueous solution of cellulase, hemicellulase and pectinase, and the weight parts of the cellulase, hemicellulase and pectinase are as follows: 0.1-1: 0.05-0.5: 0.08-0.9, wherein the fresh lotus petals and the fresh lotus filaments are prepared from the raw materials and the enzymatic hydrolysate in parts by weight: 100-200: 1;
b. crushing the mixture of the petals and the filaments after enzymolysis to 20-40 meshes, then carrying out sealed refrigeration at 10-15 ℃ and 60-65% humidity for 2-48 hours, adding 95% ethanol, then introducing 100-110 ℃ steam for distillation, and distilling for 3-4 hours to obtain fresh lotus flower syrup, wherein the weight part ratio of the ethanol to the mixture of the petals and the filaments after enzymolysis is 0.1-1: 100, and the flow rate of the steam is 16 kg/h;
c. respectively collecting front dew distilled within 0.1-1 h after the distillation is started and back dew distilled within 1-0.1 h before the distillation is finished;
d. mixing the front dew and the rear dew obtained by distillation, adding n-hexane into the mixed liquid of the front dew and the rear dew, extracting at 20-30 ℃, and then concentrating the extract liquid at 30-50 ℃ and 0.8Mpa under reduced pressure to remove n-hexane to obtain fresh lotus dew, wherein the volume ratio of the n-hexane to the mixed liquid of the front dew and the rear dew is 0.2-1: 1;
C. preparing cigarette filter tip flavoring liquid:
a. mixing Zimbabwe tobacco leaves with 95% ethanol according to the material-liquid ratio of 1:8, performing reflux extraction at 80 ℃ for 60min, mixing Zimbabwe tobacco leaves with 80% ethanol according to the material-liquid ratio of 1:8, performing reflux extraction at 80 ℃ for 60min, and combining the two extracting solutions to obtain Zimbabwe tobacco extract;
b. mixing fresh sophora japonica flower with 95% ethanol at a ratio of 1:8, extracting under reflux at 80 deg.C for 60min, mixing fresh sophora japonica flower with 80% ethanol at a ratio of 1:8, extracting under reflux at 80 deg.C for 60min, and mixing the two extractive solutions to obtain sophora japonica extract;
c. mixing Mel Jujubae with 95% ethanol at a ratio of 1:8, reflux-extracting at 80 deg.C for 60min, mixing Mel Jujubae with 80% ethanol at a ratio of 1:8, reflux-extracting at 80 deg.C for 60min, and mixing the extractive solutions to obtain extract;
d. uniformly mixing Zimbabwe tobacco extract, sophora flower extract, jujube flower honey extract and absolute ethyl alcohol in a volume ratio of 4:3:1: 990-1000 to prepare cigarette filter tip flavoring liquid;
D. and uniformly mixing the prepared fresh lotus essential oil, fresh lotus dew and cigarette filter tip flavoring liquid according to the weight part ratio of 1-60: 1-100: 1000000 to obtain the lotus flavor tobacco essence.
The application of the essence for lotus flavor style cigarettes prepared by the method is characterized in that the prepared essence for lotus flavor style cigarettes is applied to a filter tip core wire in an application amount of 0.1-0.5 g/m, or is added into a filter tip bead in an addition amount of 2.0-5.0 uL.
The invention achieves the technical progress that:
1. the lotus extract commonly used in the prior art is the ethanol extract of the lotus, the ethanol extract only contains polar components in the lotus fragrance components, the content of the fragrance components is high, the addition amount is small, and the addition amount in ppm order can achieve the effect of strengthening the fragrance style characteristics of cigarettes, thereby being convenient for production, application and popularization.
2. The invention adopts the flavoring mode of the filter core wire and the filter blasting bead, and the added essence can directly enter smoke along with suction without combustion, thereby keeping the original flavor of the lotus.
3. The workshop self-grinding incense stick quantitative adding equipment-quantitative pump ensures the uniformity and consistency of essence addition.
4. According to the invention, through gas chromatography-mass spectrometry analysis, the fresh lotus essential oil contains a large amount of natural aroma components (chemical components of setose, costustoot, flower fragrance, spicy fragrance, milk fragrance, medicine fragrance, baking fragrance and the like) and main components of high-grade spices, such as acetaldehyde diethyl acetal, alpha-phellandrene, pinene, beta-myrcene, D-limonene, eucalyptol, gamma-terpinene, thymol, nonanal, beta-cyclocitral, cis-jasmone, vanillin, lauric acid, caryophyllene oxide, farnesol, ethyl palmitate and the like, and especially farnesol has the function of softening and smoothing smoke; through gas chromatography-mass spectrometry analysis, the fresh lotus flower syrup contains isoamyl alcohol, eucalyptol, phenethyl alcohol, guaiacol, vanillin and the like, and most of alcohol substances, and the water-soluble alcohol substances not only have elegant fragrance, but also can improve the alcohol content and the property of smoke, improve the taste of cigarettes, increase the fragrance of the existing cigarettes, and improve the alcohol content and the property of smoke and the fineness and softness.
The prepared fresh lotus essential oil, the fresh lotus dew and the cigarette filter tip flavoring liquid are fully and uniformly mixed according to a proportion to prepare the lotus flavor style cigarette essence, the lotus flavor style cigarette essence is applied to a filter tip core wire or added into a filter tip bead blasting to be rolled into a cigarette product, the original flavor of lotus can be kept, the stimulation is reduced, the comfort level and the safety of the cigarette are improved, meanwhile, the flavor art and the consumption feeling are fused, and the good quality represented by lotus is endowed to the cigarette.
Detailed Description
In order that the invention may be more clearly understood, reference will now be made to the following examples.
Example 1:
A. preparation of fresh lotus essential oil:
a. removing impurities such as receptacle and semen Nelumbinis from fresh flos Nelumbinis collected from white lake, and retaining petal and filament;
b. accurately weighing 50g of cellulase, 25g of hemicellulase and 45g of pectinase, mixing, adding 1000ml of water, uniformly stirring, and uniformly spraying on 100kg of the petal and filament materials;
c. carrying out enzymolysis on the petals and the filaments sprayed with the enzymolysis liquid at 35 ℃ for 3.5 hours;
d. crushing the petals and the filaments after enzymolysis to 40 meshes, performing sealed refrigeration at the temperature of 11 ℃ and the humidity of 60% for 15 hours, then performing direct steam distillation on the petals and the filaments after the sealed refrigeration treatment by using a distillation still, arranging a perforated basket between a steam inlet and a steam outlet, placing the petals and the filaments after the refrigeration treatment in the perforated basket, adding 200mL of 95% ethanol entrainer, adding the entrainer ethanol to promote evaporation of volatile components in the distillation process, then introducing 100-110 ℃ steam, performing distillation at the steam flow rate of 16kg/h, adjusting the amount of condensed water in the distillation extraction process to keep the steam condensed water temperature at about 70 ℃, when the amount of fresh lotus essential oil in an oil-water separator is more than 1mL, collecting fresh lotus essential oil by using a separating funnel, closing the condensed water after distillation for 3.5 hours, then continuing to introduce the steam for 0.5 hour, collecting the fresh lotus essential oil attached in the discharge pipeline for 5-6 times, and accumulating to obtain 12mL of fresh lotus essential oil, wherein the relative density of the fresh lotus essential oil is 0.6-0.85 g/mL.
B. Preparation of fresh lotus flower syrup:
a. removing impurities such as receptacle and semen Nelumbinis from fresh flos Nelumbinis collected from white lake, and retaining petal and filament;
b. accurately weighing 50g of cellulase, 25g of hemicellulase and 45g of pectinase, mixing, adding 1000ml of water, stirring uniformly, and spraying uniformly on 100kg of the petal and filament materials;
c. carrying out enzymolysis on the petal and filament materials sprayed with the enzymolysis liquid at 35 ℃ for 3.5 h;
d. crushing the enzymatically hydrolyzed petal and filament materials to 40 meshes, sealing and refrigerating for 15 hours at the temperature of 11 ℃ and the humidity of 60%, putting the crushed materials into a distillation kettle, arranging a perforated basket between a water vapor inlet and a water vapor outlet, putting the refrigerated petal and filament materials into the perforated basket, adding 200ml of 95% ethanol entrainer, adding the entrainer ethanol to promote evaporation of volatile components in the distillation process, introducing 100-110 ℃ water vapor, distilling for 3.5 hours at the water vapor flow rate of 16kg/h, and adjusting the amount of condensed water in the distillation extraction process so that the temperature of the steam condensed water is kept at about 70 ℃;
e. respectively collecting 5L of front distillate distilled within 0.2h after the distillation starts and 5L of back distillate distilled within 0.5h before the distillation finishes;
f. mixing the front dew and the rear dew obtained by distillation, adding 5L of n-hexane into the mixed liquid of the front dew and the rear dew, performing continuous liquid-liquid extraction at 25 ℃, extracting for 2-3 times, and combining the extract liquor;
g. concentrating the above extractive solution at 50 deg.C under 0.8Mpa under reduced pressure to remove n-hexane, and obtaining refined fresh lotus flower syrup 40 mL.
C. Preparing cigarette filter tip flavoring liquid:
a. preparing Zimbabwe tobacco extract: mixing Zimbabwe tobacco leaves with 95% ethanol according to the material-liquid ratio of 1:8, performing reflux extraction at 80 ℃ for 60min, mixing Zimbabwe tobacco leaves with 80% ethanol according to the material-liquid ratio of 1:8, performing reflux extraction at 80 ℃ for 60min, and combining the two extracting solutions to obtain Zimbabwe tobacco extract;
b. preparing a sophora flower extract: mixing fresh sophora japonica flower with 95% ethanol at a ratio of 1:8, extracting under reflux at 80 deg.C for 60min, mixing fresh sophora japonica flower with 80% ethanol at a ratio of 1:8, extracting under reflux at 80 deg.C for 60min, and mixing the two extractive solutions to obtain sophora japonica extract;
c. preparing a jujube flower honey extract: mixing Mel Jujubae with 95% ethanol at a ratio of 1:8, reflux-extracting at 80 deg.C for 60min, mixing Mel Jujubae with 80% ethanol at a ratio of 1:8, reflux-extracting at 80 deg.C for 60min, and mixing the extractive solutions to obtain extract;
d. sequentially dissolving 4mL of Zimbabwe tobacco extract, 3mL of sophora flower extract and 1mL of jujube honey extract into 990mL of absolute ethyl alcohol, and then adding the absolute ethyl alcohol to complement to 1L to obtain cigarette filter tip flavoring liquid;
D. preparing and perfuming essence for lotus fragrance style cigarettes:
5uL of prepared fresh lotus essential oil, 10uL of fresh lotus dew and 1L of cigarette filter tip flavoring liquid are uniformly mixed at normal temperature and normal pressure to prepare the essence for the lotus flavor style cigarette, and the essence for the lotus flavor style cigarette is applied to a filter tip core wire in an application amount of 0.1-0.5 g/m by utilizing self-grinding flavor wire essence quantitative adding equipment, wherein the application amount of the essence for the lotus flavor style cigarette is 0.12 g/m.
The flavored filter tip core wire is connected with a cigarette formula cigarette of a certain brand to form a cigarette (sample 1), the cigarette smoke analysis result of the sample 1 is shown in a table 1, and the sensory smoking evaluation result is shown in a table 2 and a table 3.
Embodiment 2 this embodiment is different from embodiment 1 in that,
A. preparation of fresh lotus essential oil:
a. removing impurities such as receptacle and semen Nelumbinis from fresh flos Nelumbinis, and retaining petal and filament;
b. accurately weighing 30g of cellulase, 50g of hemicellulase and 80g of pectinase, mixing, adding 1000ml of water, stirring uniformly, and spraying uniformly on 100kg of the petal and filament materials;
c. carrying out enzymolysis on the petals and the filaments sprayed with the enzymolysis liquid at 33 ℃ for 4 hours;
d. crushing the petals and the filaments after enzymolysis to 30 meshes, performing sealed refrigeration at 13 ℃ and 63% humidity for 20 hours, then performing direct steam distillation on the petals and the filaments after the sealed refrigeration treatment by using a distillation still, arranging a perforated basket between a steam inlet and a steam outlet, placing the petals and the filaments after the refrigeration treatment in the perforated basket, adding 150mL of 95% ethanol entrainer, adding the entrainer ethanol to promote evaporation of volatile components in the distillation process, then introducing 100-110 ℃ steam, performing distillation at a steam flow rate of 16kg/h, adjusting the amount of condensed water in the distillation extraction process to keep the temperature of the steam condensed water at about 70 ℃, when the amount of fresh lotus essential oil in an oil-water separator is more than 1mL, collecting fresh lotus essential oil by using a separating funnel, closing the condensed water after 3.5 hours of distillation, and then continuing to introduce the steam for 0.5 hours, collecting fresh lotus essential oil attached in a discharge pipeline for 5-6 times, and accumulating to obtain 10mL of fresh lotus essential oil, wherein the relative density of the fresh lotus essential oil is 0.6-0.85 g/mL.
The flavor components of the collected fresh lotus essential oil were analyzed by GC/MS method, and the flavor components were not significantly different from those of example 1.
B. Preparation of fresh lotus flower syrup:
a. removing impurities such as receptacle and semen Nelumbinis from fresh flos Nelumbinis, and retaining petal and filament;
b. accurately weighing 30g of cellulase, 50g of hemicellulase and 80g of pectinase, mixing, adding 1000ml of water, stirring uniformly, and spraying uniformly on 100kg of the petal and filament materials;
c. carrying out enzymolysis on the petal and filament materials sprayed with the enzymolysis liquid at 33 ℃ for 4 h;
d. crushing the enzymatically hydrolyzed petal and filament materials to 30 meshes, sealing and refrigerating the petals and the filament materials for 20 hours at 13 ℃ and 63% humidity, putting the petals and the filament materials into a distillation kettle, arranging a perforated basket between a water vapor inlet and a water vapor outlet, putting the refrigerated petal and filament materials into the perforated basket, adding 150ml of 95% ethanol entrainer, adding the entrainer ethanol to promote evaporation of volatile components in the distillation process, introducing 100-110 ℃ water vapor, distilling the mixture for 3.5 hours at the water vapor flow rate of 16kg/h, and adjusting the amount of condensed water in the distillation extraction process to keep the temperature of the steam condensed water at about 70 ℃;
e. respectively collecting 5L of front distillate distilled within 0.2h after the distillation starts and 5L of back distillate distilled within 0.5h before the distillation finishes;
f. mixing the front dew and the rear dew obtained by distillation, adding 10L of n-hexane into the mixed liquid of the front dew and the rear dew, performing continuous liquid-liquid extraction at 20 ℃, extracting for 2-3 times, and combining the extract liquor;
g. concentrating the above extractive solution at 45 deg.C under 0.8Mpa under reduced pressure to remove n-hexane, and obtaining refined fresh lotus flower syrup 40 mL.
The GC/MS analysis of the extracted fresh lotus flower water shows that the fragrance components of the fresh lotus flower water are not obviously different from those of the fresh lotus flower water in the example 1.
C. Preparing cigarette filter tip flavoring liquid:
a. preparing Zimbabwe tobacco extract: mixing Zimbabwe tobacco leaves with 95% ethanol according to the material-liquid ratio of 1:8, performing reflux extraction at 80 ℃ for 60min, mixing Zimbabwe tobacco leaves with 80% ethanol according to the material-liquid ratio of 1:8, performing reflux extraction at 80 ℃ for 60min, and combining the two extracting solutions to obtain Zimbabwe tobacco extract;
b. preparing a sophora flower extract: mixing fresh sophora japonica flower with 95% ethanol at a ratio of 1:8, extracting under reflux at 80 deg.C for 60min, mixing fresh sophora japonica flower with 80% ethanol at a ratio of 1:8, extracting under reflux at 80 deg.C for 60min, and mixing the two extractive solutions to obtain sophora japonica extract;
c. preparing a jujube flower honey extract: mixing Mel Jujubae with 95% ethanol at a ratio of 1:8, reflux-extracting at 80 deg.C for 60min, mixing Mel Jujubae with 80% ethanol at a ratio of 1:8, reflux-extracting at 80 deg.C for 60min, and mixing the extractive solutions to obtain extract;
d. sequentially dissolving 4mL of Zimbabwe tobacco extract, 3mL of sophora flower extract and 1mL of jujube honey extract into 990mL of absolute ethyl alcohol, and then adding the absolute ethyl alcohol to complement to 1L to obtain the cigarette filter tip flavoring liquid.
D. Preparing and perfuming essence for lotus fragrance style cigarettes:
the prepared fresh lotus essential oil 10uL, fresh lotus dew 50uL and cigarette filter tip flavoring liquid 1L are uniformly mixed at normal temperature and normal pressure to prepare the essence for the lotus flavor style cigarette, then the bead blasting is prepared according to the addition amount of 2.0-5.0 uL in each bead blasting, the addition amount of the essence for the lotus flavor style cigarette in the bead blasting is 3.5uL, the bead blasting added with the essence for the lotus flavor style cigarette is added in the filter tip forming process to obtain a filter tip containing the bead blasting, the filter tip and a certain brand formula cigarette are rolled to form a cigarette (sample 2), the cigarette smoke analysis result of the sample 2 is shown in table 1, and the sensory evaluation result is also shown in tables 2 and 3. The "blank" in tables 1, 2 and 3 is the cigarette without lotus extract, and the blank is the same as the raw and auxiliary materials and processing manner used in samples 1 and 2.
Example 3: the present embodiment is different from embodiment 1 in that,
A. preparation of fresh lotus essential oil:
a. removing impurities such as receptacle and semen Nelumbinis from fresh flos Nelumbinis, and retaining petal and filament;
b. accurately weighing 60g of cellulase, 40g of hemicellulase and 50g of pectinase, mixing, adding 1000ml of water, stirring uniformly, and spraying uniformly on 100kg of the petal and filament materials;
c. carrying out enzymolysis on the petals and the filaments sprayed with the enzymolysis liquid at 38 ℃ for 3 hours;
d. crushing the petals and the filaments after enzymolysis to 20 meshes, performing sealed refrigeration for 8 hours at 15 ℃ and 65% humidity, then performing direct steam distillation on the petals and the filaments after the sealed refrigeration treatment by using a distillation still, arranging a perforated basket between a steam inlet and a steam outlet, placing the petals and the filaments after the refrigeration treatment in the perforated basket, adding 550mL of 95% ethanol entrainer, adding the entrainer ethanol to promote evaporation of volatile components in the distillation process, then introducing 100-110 ℃ steam, performing distillation at a steam flow rate of 16kg/h, adjusting the amount of condensed water in the distillation extraction process to keep the temperature of the steam condensed water at about 70 ℃, when the amount of fresh lotus essential oil in an oil-water separator is more than 1mL, collecting fresh lotus essential oil by using a separating funnel, closing the condensed water after 3.5 hours of distillation, and then continuing to introduce the steam for 0.5 hours, collecting fresh lotus essential oil attached in a discharge pipeline for 5-6 times, and accumulating to obtain 9mL of fresh lotus essential oil, wherein the relative density of the fresh lotus essential oil is 0.6-0.85 g/mL.
B. Preparation of fresh lotus flower syrup:
a. removing impurities such as receptacle and semen Nelumbinis from fresh flos Nelumbinis, and retaining petal and filament;
b. accurately weighing 60g of cellulase, 40g of hemicellulase and 50g of pectinase, mixing, adding 1000ml of water, stirring uniformly, and spraying uniformly on 100kg of the petal and filament materials;
c. carrying out enzymolysis on the petal and filament materials sprayed with the enzymolysis liquid at 38 ℃ for 3 h;
d. crushing the enzymatically hydrolyzed petal and filament materials to 20 meshes, sealing and refrigerating for 8 hours at 15 ℃ and 65% humidity, then putting the leaves and filament materials into a distillation kettle, arranging a perforated basket between a water vapor inlet and a water vapor outlet, putting the refrigerated petal and filament materials into the perforated basket, adding 550ml of 95% ethanol entrainer, adding the entrainer ethanol to promote evaporation of volatile components in the distillation process, then introducing 100-110 ℃ water vapor, and distilling for 3.5 hours at the water vapor flow rate of 16kg/h, wherein in the distillation extraction process, the amount of condensed water is adjusted to keep the temperature of the steam condensed water at about 70 ℃;
e. respectively collecting 5L of front distillate distilled within 0.2h after the distillation starts and 5L of back distillate distilled within 0.5h before the distillation finishes;
f. mixing the front dew and the rear dew obtained by distillation, adding 2L of n-hexane into the mixed liquid of the front dew and the rear dew, performing continuous liquid-liquid extraction at 30 ℃, extracting for 2-3 times, and combining the extract liquor;
g. concentrating the above extractive solution at 30 deg.C under 0.8Mpa under reduced pressure to remove n-hexane, and obtaining refined fresh lotus flower syrup 40 mL.
The GC/MS analysis of the extracted fresh lotus flower water shows that the fragrance components of the fresh lotus flower water are not obviously different from those of the fresh lotus flower water in the example 1.
C. Preparing cigarette filter tip flavoring liquid:
a. preparing Zimbabwe tobacco extract: mixing Zimbabwe tobacco leaves with 95% ethanol according to the material-liquid ratio of 1:8, performing reflux extraction at 80 ℃ for 60min, mixing Zimbabwe tobacco leaves with 80% ethanol according to the material-liquid ratio of 1:8, performing reflux extraction at 80 ℃ for 60min, and combining the two extracting solutions to obtain Zimbabwe tobacco extract;
b. preparing a sophora flower extract: mixing fresh sophora japonica flower with 95% ethanol at a ratio of 1:8, extracting under reflux at 80 deg.C for 60min, mixing fresh sophora japonica flower with 80% ethanol at a ratio of 1:8, extracting under reflux at 80 deg.C for 60min, and mixing the two extractive solutions to obtain sophora japonica extract;
c. preparing a jujube flower honey extract: mixing Mel Jujubae with 95% ethanol at a ratio of 1:8, reflux-extracting at 80 deg.C for 60min, mixing Mel Jujubae with 80% ethanol at a ratio of 1:8, reflux-extracting at 80 deg.C for 60min, and mixing the extractive solutions to obtain extract;
d. sequentially dissolving 4mL of Zimbabwe tobacco extract, 3mL of sophora flower extract and 1mL of jujube honey extract into 990mL of absolute ethyl alcohol, and then adding the absolute ethyl alcohol to complement to 1L to obtain cigarette filter tip flavoring liquid;
D. preparing and perfuming essence for lotus fragrance style cigarettes:
the prepared fresh lotus essential oil 1uL, the fresh lotus dew 100uL and the cigarette filter tip flavoring liquid 1L are uniformly mixed at normal temperature and normal pressure to prepare the lotus fragrance style cigarette essence, and the prepared lotus fragrance style cigarette essence is applied to a filter tip core wire in an application amount of 0.1-0.5 g/m by utilizing a self-grinding fragrance thread essence quantitative adding device, wherein the application amount of the lotus fragrance style cigarette essence is 0.35 g/m.
The flavored filter core wire is spliced with a cigarette (sample 3) with a certain brand of cigarette formula cigarette, the cigarette smoke analysis result of the sample 3 is shown in a table 1, the sensory evaluation result is shown in a table 2 and a table 3, and the evaluation is performed by 7 professional evaluation personnel according to a dark evaluation mode. The "blank" in tables 1, 2 and 3 is the cigarette without lotus extract, and the blank is the same as the raw and auxiliary materials and processing manner used in samples 1, 2 and 3.
Table 1 flue gas analysis results summary
Group of samples Blank space Sample 1 Sample 2 Sample 3
Suction port number (puff) 5.8 5.7 5.9 5.7
Total particulate matter (mg/count) 14.71 14.21 14.29 14.27
Moisture (mg/count) 2.21 1.96 2.10 2.09
Tar yield (mg/count) 11.5 11.3 11.2 11.1
Amount of nicotine in flue gas (mg/count) 0.98 1.00 0.99 0.99
Carbon monoxide (mg/count) 12.2 11.6 11.3 11.4
TABLE 2 summary of cigarette smoking results
Group of samples Evaluation of smoking effect
Blank space Strong smoke, strong satisfaction, good smoking resistance and comfortable aftertaste.
Sample 1 Fine and soft fragrance, conglobation, good harmony, mellow and sweet taste and comfortable aftertaste. .
Sample 2 The fragrance amount is increased, the lotus fragrance is light, the smoke is strong, the satisfaction is strong, and the aftertaste is comfortable.
Sample 3 Has good fragrance quality, improved fragrance amount, good compatibility, and comfortable aftertaste.
Figure DEST_PATH_IMAGE001
The result of the invention shows that the essence for cigarette with lotus fragrance style is added into the cigarette filter tip, the essence added into the filter tip directly enters the mouth of a smoker along with the smoking airflow without burning, the adding amount can be accurately controlled, simultaneously the cigarette fragrance style is strengthened, the stimulation is reduced, the comfort and the safety of the cigarette are improved, the fragrance art and the consumption feeling are fused, and the cigarette is endowed with the fine quality represented by lotus.
The above description is intended to describe in detail the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention, and all equivalent changes and modifications made within the technical spirit of the present invention should fall within the scope of the claims of the present invention.

Claims (3)

1. The lotus-fragrance tobacco essence is characterized by comprising the following components in parts by weight: 1-60 parts of fresh lotus essential oil, 1-100 parts of fresh lotus dew and 1000000 parts of cigarette filter flavoring liquid, wherein the cigarette filter flavoring liquid consists of Zimbabwe tobacco extract, sophora flower extract, jujube honey extract and absolute ethyl alcohol, and the volume of the cigarette filter flavoring liquid is 4:3:1: 990-1000.
2. The preparation method of the essence for lotus-flavor cigarettes as claimed in claim 1, characterized by comprising the following steps:
A. preparation of fresh lotus essential oil:
a. uniformly spraying 1-20% of enzymolysis liquid with mass concentration in fresh lotus petals and a filament raw material from which impurities such as receptacle, lotus seeds and the like are removed, and carrying out enzymolysis for 3-4 h at 30-38 ℃, wherein the enzymolysis liquid is an aqueous solution of cellulase, hemicellulase and pectinase, and the weight parts of the cellulase, hemicellulase and pectinase are as follows: 0.1-1: 0.05-0.5: 0.08-0.9, wherein the fresh lotus petals and the fresh lotus filaments are prepared from the raw materials and the enzymatic hydrolysate in parts by weight: 100-200: 1;
b. crushing the mixture of the petals and the filaments after enzymolysis to 20-40 meshes, then carrying out sealed refrigeration at 10-15 ℃ and 60-65% humidity for 2-48 hours, adding 95% ethanol, then introducing 100-110 ℃ steam for distillation, and distilling for 3-4 hours to obtain fresh lotus essential oil, wherein the weight part ratio of the ethanol to the mixture of the petals and the filaments after enzymolysis is 0.1-1: 100, and the flow rate of the steam is 16 kg/h;
B. preparation of fresh lotus flower syrup:
a. uniformly spraying 1-20% of enzymolysis liquid with mass concentration in fresh lotus petals and a filament raw material from which impurities such as receptacle, lotus seeds and the like are removed, and carrying out enzymolysis for 3-4 h at 30-38 ℃, wherein the enzymolysis liquid is an aqueous solution of cellulase, hemicellulase and pectinase, and the weight parts of the cellulase, hemicellulase and pectinase are as follows: 0.1-1: 0.05-0.5: 0.08-0.9, wherein the fresh lotus petals and the fresh lotus filaments are prepared from the raw materials and the enzymatic hydrolysate in parts by weight: 100-200: 1;
b. crushing the mixture of the petals and the filaments after enzymolysis to 20-40 meshes, then carrying out sealed refrigeration at 10-15 ℃ and 60-65% humidity for 2-48 hours, adding 95% ethanol, then introducing 100-110 ℃ steam for distillation, and distilling for 3-4 hours to obtain fresh lotus flower syrup, wherein the weight part ratio of the ethanol to the mixture of the petals and the filaments after enzymolysis is 0.1-1: 100, and the flow rate of the steam is 16 kg/h;
c. respectively collecting front dew distilled within 0.1-1 h after the distillation is started and back dew distilled within 1-0.1 h before the distillation is finished;
d. mixing the front dew and the rear dew obtained by distillation, adding n-hexane into the mixed liquid of the front dew and the rear dew, extracting at 20-30 ℃, and then concentrating the extract liquid at 30-50 ℃ and 0.8Mpa under reduced pressure to remove n-hexane to obtain fresh lotus dew, wherein the volume ratio of the n-hexane to the mixed liquid of the front dew and the rear dew is 0.2-1: 1;
C. preparing cigarette filter tip flavoring liquid:
a. mixing Zimbabwe tobacco leaves with 95% ethanol according to the material-liquid ratio of 1:8, performing reflux extraction at 80 ℃ for 60min, mixing Zimbabwe tobacco leaves with 80% ethanol according to the material-liquid ratio of 1:8, performing reflux extraction at 80 ℃ for 60min, and combining the two extracting solutions to obtain Zimbabwe tobacco extract;
b. mixing fresh sophora japonica flower with 95% ethanol at a ratio of 1:8, extracting under reflux at 80 deg.C for 60min, mixing fresh sophora japonica flower with 80% ethanol at a ratio of 1:8, extracting under reflux at 80 deg.C for 60min, and mixing the two extractive solutions to obtain sophora japonica extract;
c. mixing Mel Jujubae with 95% ethanol at a ratio of 1:8, reflux-extracting at 80 deg.C for 60min, mixing Mel Jujubae with 80% ethanol at a ratio of 1:8, reflux-extracting at 80 deg.C for 60min, and mixing the extractive solutions to obtain extract;
d. uniformly mixing Zimbabwe tobacco extract, sophora flower extract, jujube flower honey extract and absolute ethyl alcohol in a volume ratio of 4:3:1: 990-1000 to prepare cigarette filter tip flavoring liquid;
D. and uniformly mixing the prepared fresh lotus essential oil, fresh lotus dew and cigarette filter tip flavoring liquid according to the weight part ratio of 1-60: 1-100: 1000000 to obtain the lotus flavor tobacco essence.
3. The application of the essence for lotus flavor style cigarettes prepared by the method of any one of claims 1 to 2, wherein the prepared essence for lotus flavor style cigarettes is applied to a filter core wire in an application amount of 0.1 to 0.5g/m, or is added into a filter bursting bead in an addition amount of 2.0 to 5.0 uL.
CN202110141532.7A 2021-02-02 2021-02-02 Lotus-fragrance-style tobacco essence and preparation method and application thereof Withdrawn CN112795428A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110141532.7A CN112795428A (en) 2021-02-02 2021-02-02 Lotus-fragrance-style tobacco essence and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110141532.7A CN112795428A (en) 2021-02-02 2021-02-02 Lotus-fragrance-style tobacco essence and preparation method and application thereof

Publications (1)

Publication Number Publication Date
CN112795428A true CN112795428A (en) 2021-05-14

Family

ID=75813634

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110141532.7A Withdrawn CN112795428A (en) 2021-02-02 2021-02-02 Lotus-fragrance-style tobacco essence and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN112795428A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113693263A (en) * 2021-08-30 2021-11-26 深圳市真味生物科技有限公司 Seabuckthorn flavone antioxidant electronic cigarette liquid and preparation method thereof
CN115232670A (en) * 2022-06-15 2022-10-25 河北中烟工业有限责任公司 Lotus essence and preparation method thereof
CN115725366A (en) * 2022-11-09 2023-03-03 河北中烟工业有限责任公司 Lotus-flavored essence for cigarettes and cigarettes

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2682006A1 (en) * 2011-03-02 2014-01-08 Feellife Bioscience International Co., Ltd Method for preparing gel-state water soluble flavoring essence used for cigarette
CN103966023A (en) * 2014-05-22 2014-08-06 广西平果华莲科技研究所 Method for extracting essence from lotus stamens
CN107641557A (en) * 2017-10-31 2018-01-30 鹰潭中投科技有限公司 MoonlIght on the Lotus Pond artistic conception flavouring essence for tobacco and its preparation method and application
CN108219943A (en) * 2018-01-24 2018-06-29 云南中烟工业有限责任公司 A kind of quick-fried pearl essential oil of cigarette and the method for preparing quick-fried pearl
CN111830145A (en) * 2020-03-10 2020-10-27 北京农业生物技术研究中心 Method for determining feeding ratio and distillation time of black-branch rose hydrosol

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2682006A1 (en) * 2011-03-02 2014-01-08 Feellife Bioscience International Co., Ltd Method for preparing gel-state water soluble flavoring essence used for cigarette
CN103966023A (en) * 2014-05-22 2014-08-06 广西平果华莲科技研究所 Method for extracting essence from lotus stamens
CN107641557A (en) * 2017-10-31 2018-01-30 鹰潭中投科技有限公司 MoonlIght on the Lotus Pond artistic conception flavouring essence for tobacco and its preparation method and application
CN108219943A (en) * 2018-01-24 2018-06-29 云南中烟工业有限责任公司 A kind of quick-fried pearl essential oil of cigarette and the method for preparing quick-fried pearl
CN111830145A (en) * 2020-03-10 2020-10-27 北京农业生物技术研究中心 Method for determining feeding ratio and distillation time of black-branch rose hydrosol

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
广西中烟工业有限责任公司: "《天然烟用精油》", 28 February 2019, 广西科学技术出版社 *
曾晓鹰,等: "《卷烟调香体系构建》", 28 February 2013, 西南交通大学出版社 *
沈丹彤,等: "酶解辅助水蒸汽蒸馏法提取紫枝玫瑰精油工艺研究", 《生物技术进展》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113693263A (en) * 2021-08-30 2021-11-26 深圳市真味生物科技有限公司 Seabuckthorn flavone antioxidant electronic cigarette liquid and preparation method thereof
CN115232670A (en) * 2022-06-15 2022-10-25 河北中烟工业有限责任公司 Lotus essence and preparation method thereof
CN115232670B (en) * 2022-06-15 2023-11-28 河北中烟工业有限责任公司 Lotus essence and preparation method thereof
CN115725366A (en) * 2022-11-09 2023-03-03 河北中烟工业有限责任公司 Lotus-flavored essence for cigarettes and cigarettes
CN115725366B (en) * 2022-11-09 2024-05-10 河北中烟工业有限责任公司 Lotus-flavored essence for cigarettes and cigarettes

Similar Documents

Publication Publication Date Title
CN112795428A (en) Lotus-fragrance-style tobacco essence and preparation method and application thereof
CN105146739B (en) The preparation method of a kind of mao of cigarette quintessence oil and application thereof
CN101999753B (en) Method for processing burley tobacco and application thereof to cigarette
CN110839947B (en) Extraction process of plant spice for cigarette without burning under heating
CN109082344A (en) Essence spice for cigarette, the cigarette paper containing the essence spice for cigarette and its application
CN106857904A (en) A kind of fragrant green tea processing technology
CN111418892A (en) Cigarette filter stick additive and application thereof
CN110628508A (en) Preparation method of compound plant extract for promoting production of body fluid and increasing moisture and cold-extraction electronic cigarette oil
CN112189875A (en) Polysweet fruit refined extract for cigarettes as well as preparation method and application thereof
CN109609278A (en) A kind of fritillary-loquat essence and its preparing purposes of the cigarette in quick-fried pearl
CN107637858A (en) A kind of plant for improving water extraction and alcohol precipitation method extraction causes perfumery and extracting method and application
CN101637303A (en) Lemon extract, preparation method thereof and application thereof in cigarette flavoring
CN108618192A (en) A kind of 15 are formulated electronic cigarette tobacco tar and preparation method thereof
CN111671135B (en) Tobacco component suitable for electronic cigarette atomized liquid and processing and application method thereof
CN106617253A (en) Method for preparing electronic cigarette essence from green tea
CN108865437B (en) Preparation method of perilla seed spice for cigarettes and application of perilla seed spice in cigarettes
CN102899167B (en) Tobacco flavor with uniform and stable fragrance and preparation method thereof
CN110358630B (en) Spice with fresh and spicy flavor for cigarettes, preparation method of spice and application of spice in cigarettes
CN115011410B (en) Schisandra chinensis branch spice, preparation method thereof and cigarette
CN112094693B (en) Passion fruit bead-blasting essence and application thereof
CN105768200B (en) Application of plumeria rubra and leaves in cigarette
CN108359531A (en) The quick-fried pearl essence of lily odor type and its application in cigarette
CN114410376A (en) Cigarette bead-blasting essential oil with pepper flavor and preparation method thereof
CN111329098B (en) Fumigating and flavoring method and application thereof in tobacco
CN114052283A (en) Abelmoschus manihot bead-blasting essence and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication

Application publication date: 20210514

WW01 Invention patent application withdrawn after publication