CN105686069B - A kind of tobacco extract and preparation method thereof and its purposes - Google Patents
A kind of tobacco extract and preparation method thereof and its purposes Download PDFInfo
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- CN105686069B CN105686069B CN201610180305.4A CN201610180305A CN105686069B CN 105686069 B CN105686069 B CN 105686069B CN 201610180305 A CN201610180305 A CN 201610180305A CN 105686069 B CN105686069 B CN 105686069B
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- tobacco
- citric acid
- extract
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 100
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 99
- 239000000284 extract Substances 0.000 title claims abstract description 75
- 238000000605 extraction Methods 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 239000002699 waste material Substances 0.000 claims abstract description 26
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 117
- 239000012141 concentrate Substances 0.000 claims description 41
- 239000012074 organic phase Substances 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 25
- 239000003960 organic solvent Substances 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 16
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 10
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims description 9
- 229960002715 nicotine Drugs 0.000 claims description 9
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims description 9
- 102000004169 proteins and genes Human genes 0.000 claims description 9
- 108090000623 proteins and genes Proteins 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- 239000000460 chlorine Substances 0.000 claims description 7
- 229910052801 chlorine Inorganic materials 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 229910052700 potassium Inorganic materials 0.000 claims description 7
- 229910002651 NO3 Inorganic materials 0.000 claims description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 239000004480 active ingredient Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000010865 sewage Substances 0.000 abstract description 4
- 230000000116 mitigating effect Effects 0.000 abstract 1
- 235000019504 cigarettes Nutrition 0.000 description 16
- 239000002351 wastewater Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 230000000391 smoking effect Effects 0.000 description 5
- 230000001953 sensory effect Effects 0.000 description 4
- 239000000835 fiber Substances 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 238000003809 water extraction Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 235000014633 carbohydrates Nutrition 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 150000007529 inorganic bases Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 231100000989 no adverse effect Toxicity 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 241000208292 Solanaceae Species 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000010893 paper waste Substances 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/26—Use of organic solvents for extraction
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The present invention relates to the present invention relates to a kind of method that utilization waste tobacco stem liquid prepares tobacco extract, methods described includes the steps such as concentration, extraction, back extraction, concentration.The invention further relates to the tobacco extract obtained according to the preparation method, and application of the tobacco extract in reconstituted tobacoo production.Equipment needed for the technology is simple, and operation is simple, active ingredient in waste tobacco stem liquid is obtained further with mitigating its treatment pressure of sewage, on the other hand for reconstituted tobacoo production provides new raw material.
Description
【Technical field】
The invention belongs to technical field of tobacco processing.More particularly it relates to a kind of preparation side of tobacco extract
Method, further relates to the tobacco extract obtained according to the preparation method, and the tobacco extract is in reconstituted tobacoo is produced
Purposes.
【Background technology】
Tobacco is Solanaceae class herbaceous plant, and Nicotiana has more than 60 kind, and tobacco leaf mainly contains 1~3% cigarette by weight
Alkali, 5~15% protein, 11% cellulose, 20% hemicellulose, 12~16% organic acids, 2~7% fat, 0.52~
2.61% polyacid tannin matter, 12% pectin and ash content 10%.Tobacco leaf is applied directly in production of cigarettes, not only raw tobacco material into
This height, and it is unfavorable for reducing tar and reducing harm.Therefore, the 1950's, reconstituted tobacoo technology is risen, by reconstituted tobacoo with certain
Ratio is incorporated into production of cigarettes, can not only be reduced cigarette cost, be economized in raw materials, and can improve cigarette filling capacity and
Flammability, while the flue gas composition of cigarette can be changed, reduces tar content, so as to change cigarette interior quality.
The production technology of maturation reconstituted tobacoo is mainly and uses paper process at present, will tobacco be soaked in water extraction,
The insoluble matters such as tobacco water solubility thing and baccy fiber are carried out into separation of solid and liquid through squeezing, it is thin that gained solid is made fiber through copy paper again
Piece chip base, gained liquid is concentrated again to be made tobacco water solubility thing concentrate, dip-coating or spray after adding other blending materials
It is coated onto in thin slice chip base, reconstituted tobacoo most is obtained through drying, cutting afterwards.The primary raw material of reconstituted tobacoo production is whole cigarette life
Offal, offal, discarded tobacco leaf, tobacco chippings discarded during product etc., extraction process mainly has water extraction, alcohol extracting method etc., no
Which kind of extracting method pipe uses, and finally can all produce waste water, and contains certain active ingredient in waste water, and directly treatment is not only caused
Waste, and treatment pressure of sewage can be increased.
The present inventor, by test of many times, is developed in reconstituted tobacoo production process to solve the above problems
The treatment technology of waste water, can not only mitigate the pressure of wastewater treatment, can more be prepared as raw material with waste water a kind of new
Tobacco extract, the tobacco extract can be back to reconstituted tobacoo production.
【The content of the invention】
[technical problem to be solved]
It is an object of the invention to provide a kind of method that utilization waste tobacco stem liquid prepares tobacco extract.
It is a further object to provide a kind of tobacco extract.
It is a further object to provide the purposes of the tobacco extract.
[technical scheme]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of preparation method of tobacco extract.The step of preparation method, is as follows:
(1) concentrate
Waste tobacco stem liquid is removed by filtration residue, then is concentrated in vacuo, then to concentration offal liquid in add hydrogen-oxygen
Changing sodium water solution makes its pH value adjust to 10~13, obtains a kind of alkaline concentrate;
(2) extract
Add ethyl acetate or dichloromethane organic solvent to be extracted in the alkaline concentrate obtained toward step (1), press
Extraction 2~4 times is repeated according to similarity condition, is separated, extract merges, and obtains a kind of organic phase;
(3) it is stripped
Add aqueous citric acid solution to be stripped in the organic phase obtained toward step (2), repeat anti-according to similarity condition
Extraction 2~4 times, separates, and strip aqueous merge, and obtain a kind of citric acid anti-stripping agent;
(4) tobacco extract is prepared
The citric acid anti-stripping agent that step (3) is obtained is concentrated in vacuo, until the solid content in concentrate is
By weight 54~60%, so obtain described tobacco extract.
Another preferred embodiment of the invention, in step (1), original volume is concentrated into by waste tobacco stem liquid
1/8~1/10.
Another preferred embodiment of the invention, in step (1), the waste tobacco stem liquid for removing residue is in temperature
Degree 50~60 DEG C with 0.05~0.12MPa of vacuum under conditions of be concentrated in vacuo.
Another preferred embodiment of the invention, in step (1), the concentration of the sodium hydrate aqueous solution is
In mass 10~40%.
Another preferred embodiment of the invention, in step (2), the alkaline concentrate is organic molten with described
The volume ratio of agent is 3~5:1.
Another preferred embodiment of the invention, in step (3), the concentration of the aqueous citric acid solution be with
Quality meter 4~6%.
Another preferred embodiment of the invention, in step (3), aqueous citric acid solution and the organic phase
Volume ratio is 1:3~5.
Another preferred embodiment of the invention, in step (4), described citric acid anti-stripping agent is in temperature
Concentrated under conditions of 50~60 DEG C of degree and vacuum 0.05~0.12MPa.
The invention further relates to the tobacco extract that the preparation method is obtained.
Described tobacco extract contains 54~60% solid contents, more than 10% nicotine, 0.7~1.0% total in mass
It is sugar, 0.3~1.0% reduced sugar, 0.02~0.2% nitrate, 0.05~0.8% potassium, less than 0.25% chlorine, 0.5~1.0% total
Nitrogen and less than 0.1% protein.
The invention further relates to purposes of the described tobacco extract in reconstituted tobacoo is produced.
The present invention is described in more detail below.
The present invention relates to a kind of preparation method of tobacco extract.The step of preparation method, is as follows:
(1) concentrate
Waste tobacco stem liquid is removed by filtration residue, then is concentrated in vacuo, then to concentration offal liquid in add hydrogen-oxygen
Changing sodium water solution makes its pH value adjust to 10~13, obtains a kind of alkaline concentrate.
The primary raw material of tobacco sheets by paper making method production is offal, offal, the low order discarded during whole production of cigarettes
Tobacco leaf, tobacco chippings etc., extraction process are mainly water extraction, alcohol extracting method etc., no matter using which kind of extracting method, finally can all produce
Raw waste water.The general character of this existing paper waste of waste water, for example, contain fiber fines, while there is tobacco wastewater colourity high, useless again
The features such as containing the nicotine unfavorable to growth of microorganism in water, while paper process tobacco wastewater water quality is different and raw with tobacco leaf species
Produce process variation very big, its CODCrAnd BOD5Concentration is high, rich in the carbohydrate and tar based on polysaccharide, nicotine, phenols and
Benzene ring substance, biodegradability is fair, and colourity is relatively deep (being in rufous), and SS is higher, and oxidation-reduction potential is higher, and waste water is easily degenerated
Go bad.If directly treatment not only causes to waste this waste water, and can increase treatment pressure of sewage.Because this waste water contains
There are the debris such as big content of starting materials fragment, disintegrating slag, it is necessary to carry out filter cleaner to these waste water before concentration.What filtering was used sets
Standby is all product usually used in technical field of waste water processing, in extensive sale in the market.
According to the present invention, the waste tobacco stem liquid for removing residue is in 50~60 DEG C of temperature and 0.05~0.12MPa of vacuum
Under conditions of be concentrated in vacuo.
In the present invention, it is necessary to waste tobacco stem liquid is concentrated into the 1/8~1/10 of original volume.If waste tobacco stem liquid is concentrated
Volume is more than 1/8, then can consume more extraction phase organic solvents;If waste tobacco stem liquid concentration volume is less than 1/10, extract
Serious emulsification phenomenon can be produced when taking, is unfavorable for layering.Therefore, waste tobacco stem liquid be concentrated into original volume 1/8~1/10 be close
Reason.
The equipment that the step is used in vacuum concentration is the product sold in the market, such as by Shanghai Asia Rong Sheng
Change the product of instrument plant's sale.
Then, its pH value is made to adjust to 10~13 toward addition sodium hydrate aqueous solution in concentration offal liquid.According to the present invention,
It is every the pH value of the concentration offal liquid to be adjusted to 10~13, while not born to the quality of tobacco extract of the present invention
The inorganic base that face rings may be used to the present invention, and these inorganic bases are also all within protection scope of the present invention.
In the present invention, using sodium hydrate aqueous solution by it is described concentration offal liquid pH value adjust to 10~13 it is main
Purpose is stalk liquid small molecular is alkalized into free state, is easy to the extraction of organic solvent.If the pH of the concentration offal liquid
When value regulation is to less than 10, then alkalize insufficient, extraction yield is low;If the concentration offal liquid pH value is adjusted during to more than 13,
Then cause to waste, alkalescence is too strong in addition, active ingredient can partial destruction;Therefore, the pH value of the concentration offal liquid is adjusted to 10
~13 is appropriate.
When the pH value of the concentration offal liquid is adjusted, using the concentration of sodium hydrate aqueous solution be in mass 10~
40%.If sodium hydrate aqueous solution concentration exceedes its scope, addition volume can be excessive when too low, increased organic solvent use
Amount, causes local concentration too high when too high, destroy active ingredient.
(2) extract
Add ethyl acetate or dichloromethane organic solvent to be extracted in the alkaline concentrate obtained toward step (1), press
Extraction 2~4 times is repeated according to similarity condition, is separated, extract merges, and obtains a kind of organic phase.
The purpose for extracting alkaline concentrate using organic solvent is that extraction active ingredient goes the removal of impurity.It is all according to the present invention
Can be used for extracting alkaline concentrate, realize its purpose, while being had no adverse effect to the quality of tobacco extract of the present invention
Organic solvent may be used to the present invention, these organic solvents are also all within protection scope of the present invention.
According to the present invention, in extraction, the alkaline concentrate and the volume ratio of the organic solvent are 3~5:1.If
Alkaline concentrate is more than 3 with the volume ratio of organic solvent:1, then extract insufficient;If the body of alkaline concentrate and organic solvent
Product is than being less than 5:1, then cause organic solvent to waste;Therefore, alkaline concentrate and the volume ratio of organic solvent are 3~5:1 is suitable
's.
The equipment that this extraction step is used is usually used in chemical technology field, in the product sold in the market
Product.
(3) it is stripped
Add aqueous citric acid solution to be stripped in the organic phase obtained toward step (2), repeat anti-according to similarity condition
Extraction 2~4 times, separates, and strip aqueous merge, and obtain a kind of citric acid anti-stripping agent.
In the present invention, the purpose being stripped using aqueous citric acid solution is extraction active ingredient.It is every according to the present invention
Can be used in present invention back extraction, while can to the organic acid that the quality of tobacco extract of the present invention has no adverse effect
For the present invention, these organic acids are also all within protection scope of the present invention.
The use of the concentration of aqueous citric acid solution is in mass 4~6% according to the present invention.If its concentration is higher than this
Scope, can cause to waste;If its concentration be less than this scope, can extraction yield it is low.Therefore, the concentration of aqueous citric acid solution is
4~6% is desirable.
The aqueous citric acid solution is 1 with the volume ratio of the organic phase:3~5.According to the present invention, in back extraction, lemon
Lemon aqueous acid is 1 with the volume ratio of organic phase:3~5.If aqueous citric acid solution is more than 1 with the volume ratio of organic phase:3, then
Cause to waste, increase concentration amount;If aqueous citric acid solution is less than 1 with the volume ratio of organic phase:5, then extract insufficient;Cause
This, aqueous citric acid solution is 1 with the volume ratio of organic phase:3~5 is feasible.
The equipment that this strip stage is used is the equipment that extraction step is used, therefore is repeated no more here.
(4) tobacco extract is prepared
The citric acid anti-stripping agent that step (3) is obtained is concentrated in vacuo, until the solid content in concentrate is
By weight 54~60%, so obtain described tobacco extract.
According to the present invention, described citric acid anti-stripping agent is in 50~60 DEG C of temperature and vacuum 0.05-0.12MPa
Under conditions of concentrated.If concentration condition exceedes the scope, concentration is slow, increases concentration time.
The equipment that the step is used in vacuum concentration is the product sold in the market.
The invention further relates to the tobacco extract that the preparation method is obtained.
The tobacco extract have detected using relevant national standard.Described tobacco extract contain in mass 54~
60% solid content, more than 10% nicotine, 0.7~1.0% total reducing sugar, 0.3~1.0% reduced sugar, 0.02~0.2% nitrate,
0.05~0.8% potassium, less than 0.25% chlorine, 0.5~1.0% total nitrogen and less than 0.1% protein.
The invention further relates to purposes of the described tobacco extract in reconstituted tobacoo is produced.When reconstituted tobacoo is produced,
Described tobacco extract is added in the raw material of production reconstituted tobacoo with addition in a conventional manner, tobacco is produced thin
Piece, is then added to produce qualified cigarette in cigarette producing process.
[beneficial effect]
Compared with prior art, the present invention mainly has the advantages that:
Equipment needed for the technology is simple, and operation is simple, and active ingredient obtains further profit on the one hand making waste tobacco stem liquid
With, mitigate treatment pressure of sewage, on the other hand provide new raw material for reconstituted tobacoo is produced.
Waste tobacco stem liquid by technical scheme treatment after, protein, carbohydrate in resulting tobacco extract
Content is very low, so as to reduce oral cavity throat excitement, effectively increases cigarette quality.
【Specific embodiment】
The present invention is will be better understood that by following embodiments.
Embodiment 1:The preparation of tobacco extract
The implementation steps of the embodiment are as follows:
(1) concentrate
Waste tobacco stem liquid is removed by filtration residue, reuse the equipment of present specification explanation 56 DEG C of temperature with it is true
Be concentrated in vacuo under conditions of reciprocal of duty cycle 0.07MPa, be concentrated into the 1/9 of original volume, then to concentration offal liquid in add concentration
For in mass 20% sodium hydrate aqueous solution its pH value is adjusted to 12, obtain a kind of alkaline concentrate;
(2) extract
The alkaline concentrate that step (1) is obtained is fitted into the extraction equipment of present specification explanation, then according to alkali
Property concentrate and organic solvent volume ratio be 1:4, ethyl acetate organic solvent is subsequently added into, extracted at room temperature, point
From the raffinate for obtaining repeats extraction 3 times according to similarity condition, separates, and raffinate is discarded, and these extracts are merged, and obtains
A kind of organic phase;
(3) it is stripped
Volume ratio according to aqueous citric acid solution and organic phase is 1:4, add concentration in the organic phase obtained toward step (2)
For in mass 4% aqueous citric acid solution be stripped, separate, the back extraction extraction raffinate for obtaining repeats anti-according to similarity condition
Extraction 2 times, is separated, and discards organic phase, and these strip aqueous are merged, and obtains a kind of citric acid anti-stripping agent;
(4) tobacco extract is prepared
The equipment illustrated using present specification, the citric acid anti-stripping agent that step (3) is obtained 56 DEG C of temperature with
It is concentrated in vacuo under conditions of vacuum 0.07MPa, until solid content in concentrate is by weight 58%, so
Obtain described tobacco extract.
The method illustrated using present specification, is tested and analyzed to tobacco extract manufactured in the present embodiment,
The tobacco extract contains 57.5% solid content, 12.7% nicotine, total reducing sugar 0.7%, reduced sugar 0.3%, nitric acid by weight
Salt 0.1%, potassium 0.3%, chlorine 0.08%, total nitrogen 0.5% and protein 0%.
Addition tobacco manufactured in the present embodiment is have detected according to GB5606.4-2005 Sensory Quality of Cigarette judgment criteria to carry
Take thing and prepare reconstituted tobacoo smoking result, its result is listed in the table below in 1.
Embodiment 2:The preparation of tobacco extract
The implementation steps of the embodiment are as follows:
(1) concentrate
Waste tobacco stem liquid is removed by filtration residue, reuse present specification explanation equipment temperature 50 C with it is true
Be concentrated in vacuo under conditions of reciprocal of duty cycle 0.05MPa, be concentrated into the 1/8 of original volume, then to concentration offal liquid in add concentration
For in mass 10% sodium hydrate aqueous solution its pH value is adjusted to 10, obtain a kind of alkaline concentrate;
(2) extract
The alkaline concentrate that step (1) is obtained is fitted into the extraction equipment of present specification explanation, then according to alkali
Property concentrate and organic solvent volume ratio be 1:3, dichloromethane organic solvent is subsequently added into, extracted at room temperature, point
From the raffinate for obtaining repeats extraction 2 times according to similarity condition, separates, and raffinate is discarded, and these extracts are merged, and obtains
A kind of organic phase;
(3) it is stripped
Volume ratio according to aqueous citric acid solution and organic phase is 1:3, add concentration in the organic phase obtained toward step (2)
For in mass 5% aqueous citric acid solution be stripped, separate, the back extraction extraction raffinate for obtaining repeats anti-according to similarity condition
Extraction 3 times, is separated, and discards organic phase, and these strip aqueous are merged, and obtains a kind of citric acid anti-stripping agent;
(4) tobacco extract is prepared
Using present specification illustrate equipment, the citric acid anti-stripping agent that step (3) is obtained temperature 50 C with
It is concentrated in vacuo under conditions of vacuum 0.05MPa, until solid content in concentrate is by weight 54%, so
Obtain described tobacco extract.
Tobacco extract manufactured in the present embodiment is tested and analyzed, the tobacco extract contains by weight
58.4% solid content, 13.6% nicotine, 0.8% total reducing sugar, 0.4% reduced sugar, 0.25% nitrate, 0.1% potassium, 0.08% chlorine,
0.8% total nitrogen and 0% protein.
Addition tobacco manufactured in the present embodiment is have detected according to GB5606.4-2005 Sensory Quality of Cigarette judgment criteria to carry
Take thing and prepare reconstituted tobacoo smoking result, its result is listed in the table below in 1.
Embodiment 3:The preparation of tobacco extract
The implementation steps of the embodiment are as follows:
(1) concentrate
Waste tobacco stem liquid is removed by filtration residue, reuse present specification explanation equipment temperature 60 C with it is true
Be concentrated in vacuo under conditions of reciprocal of duty cycle 0.12MPa, be concentrated into the 1/10 of original volume, then to concentration offal liquid in add concentration
For in mass 30% sodium hydrate aqueous solution its pH value is adjusted to 13, obtain a kind of alkaline concentrate;
(2) extract
The alkaline concentrate that step (1) is obtained is fitted into the extraction equipment of present specification explanation, then according to alkali
Property concentrate and organic solvent volume ratio be 1:4, ethyl acetate organic solvent is subsequently added into, extracted at room temperature, point
From the raffinate for obtaining repeats extraction 3 times according to similarity condition, separates, and raffinate is discarded, and these extracts are merged, and obtains
A kind of organic phase;
(3) it is stripped
Volume ratio according to aqueous citric acid solution and organic phase is 1:5, add concentration in the organic phase obtained toward step (2)
For in mass 6% aqueous citric acid solution be stripped, separate, the back extraction extraction raffinate for obtaining repeats anti-according to similarity condition
Extraction 4 times, is separated, and discards organic phase, and these strip aqueous are merged, and obtains a kind of citric acid anti-stripping agent;
(4) tobacco extract is prepared
Using present specification illustrate equipment, the citric acid anti-stripping agent that step (3) is obtained temperature 60 C with
It is concentrated in vacuo under conditions of vacuum 0.12MPa, until solid content in concentrate is by weight 60%, so
Obtain described tobacco extract.
Tobacco extract manufactured in the present embodiment is tested and analyzed, the tobacco extract contains by weight
60.0% solid content, 10.5% nicotine, 1% total reducing sugar, 0.5% reduced sugar, 0.07% nitrate, 0.1% potassium, 0.18% chlorine, 1%
Total nitrogen and 0.01% protein.
Addition tobacco manufactured in the present embodiment is have detected according to GB5606.4-2005 Sensory Quality of Cigarette judgment criteria to carry
Take thing and prepare reconstituted tobacoo smoking result, its result is listed in the table below in 1.
Embodiment 4:The preparation of tobacco extract
The implementation steps of the embodiment are as follows:
(1) concentrate
Waste tobacco stem liquid is removed by filtration residue, reuse the equipment of present specification explanation 53 DEG C of temperature with it is true
Be concentrated in vacuo under conditions of reciprocal of duty cycle 0.10MPa, be concentrated into the 1/9 of original volume, then to concentration offal liquid in add concentration
For in mass 40% sodium hydrate aqueous solution its pH value is adjusted to 11, obtain a kind of alkaline concentrate;
(2) extract
The alkaline concentrate that step (1) is obtained is fitted into the extraction equipment of present specification explanation, then according to alkali
Property concentrate and organic solvent volume ratio be 1:4, dichloromethane organic solvent is subsequently added into, extracted at room temperature, point
From the raffinate for obtaining repeats extraction 4 times according to similarity condition, separates, and raffinate is discarded, and these extracts are merged, and obtains
A kind of organic phase;
(3) it is stripped
Volume ratio according to aqueous citric acid solution and organic phase is 1:4, add concentration in the organic phase obtained toward step (2)
For in mass 5% aqueous citric acid solution be stripped, separate, the back extraction extraction raffinate for obtaining repeats anti-according to similarity condition
Extraction 3 times, is separated, and discards organic phase, and these strip aqueous are merged, and obtains a kind of citric acid anti-stripping agent;
(4) tobacco extract is prepared
The equipment illustrated using present specification, the citric acid anti-stripping agent that step (3) is obtained 53 DEG C of temperature with
It is concentrated in vacuo under conditions of vacuum 0.10MPa, until solid content in concentrate is by weight 56%, so
Obtain described tobacco extract.
Tobacco extract manufactured in the present embodiment is tested and analyzed, the tobacco extract contains by weight
59.1% solid content, 11.5% nicotine, 1% total reducing sugar, 0.4% reduced sugar, 0.16% nitrate, 0.2% potassium, 0.12% chlorine,
0.3% total nitrogen and 0.01% protein.
Addition tobacco manufactured in the present embodiment is have detected according to GB5606.4-2005 Sensory Quality of Cigarette judgment criteria to carry
Take thing and prepare reconstituted tobacoo smoking result, its result is listed in the table below in 1.
Table 1:Addition tobacco extract of the present invention prepares reconstituted tobacoo smoking result
Claims (8)
1. a kind of preparation method of tobacco extract, it is characterised in that as follows the step of the preparation method:
(1) concentrate
Waste tobacco stem liquid is removed by filtration residue, then under conditions of 50~60 DEG C and 0.05~0.12MPa of vacuum of temperature
It is concentrated in vacuo, is then made it to the sodium hydrate aqueous solution for adding concentration to be in mass 10~40% in concentration offal liquid
PH value is adjusted to 10~13, obtains a kind of alkaline concentrate;
(2) extract
Ethyl acetate or dichloromethane organic solvent is added to be extracted in the alkaline concentrate obtained toward step (1), according to same
Batten part repeats extraction 2~4 times, separates, and extract merges, and obtains a kind of organic phase;
(3) it is stripped
Add aqueous citric acid solution to be stripped in the organic phase obtained toward step (2), back extraction 2 is repeated according to similarity condition
~4 times, separate, strip aqueous merge, and obtain a kind of citric acid anti-stripping agent;
(4) tobacco extract is prepared
The citric acid anti-stripping agent that step (3) is obtained is concentrated in vacuo, until the solid content in concentrate is with weight
Gauge 54~60%, so obtains described tobacco extract.
2. preparation method according to claim 1, it is characterised in that in step (1), waste tobacco stem liquid is concentrated into original
The 1/8~1/10 of volume.
3. preparation method according to claim 1, it is characterised in that in step (2), the alkaline concentrate with it is described
The volume ratio of organic solvent is 3~5:1.
4. preparation method according to claim 1, it is characterised in that in step (3), the aqueous citric acid solution it is dense
Degree is in mass 4~6%.
5. preparation method according to claim 1, it is characterised in that in step (3), aqueous citric acid solution has with described
The volume ratio of machine phase is 1:3~5.
6. preparation method according to claim 1, it is characterised in that in step (4), described citric acid anti-stripping agent
Concentrated under conditions of 50~60 DEG C of temperature with 0.05~0.12MPa of vacuum.
7. the tobacco extract that the preparation method according to any one of claim 1-6 claim is obtained, it is characterised in that
Described tobacco extract contain in mass 54~60% solid contents, more than 10% nicotine, 0.7~1.0% total reducing sugar, 0.3~
1.0% reduced sugar, 0.02~0.2% nitrate, 0.05~0.8% potassium, less than 0.25% chlorine, 0.5~1.0% total nitrogen with
Less than 0.1% protein.
8. tobacco extract according to claim 7 produce reconstituted tobacoo in purposes.
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| CN106947595B (en) * | 2017-03-20 | 2020-08-28 | 河南中烟工业有限责任公司 | Subcritical reverse extraction method of tobacco original fragrance components |
| CN110283158B (en) * | 2019-07-11 | 2020-10-30 | 广东省金叶科技开发有限公司 | Method for recovering plant alkali from tobacco leaching liquor |
| CN110810894B (en) * | 2019-10-31 | 2022-03-01 | 上海烟草集团有限责任公司 | A kind of reconstituted tobacco leaf coating liquid and preparation method thereof |
| CN111620851A (en) * | 2020-06-17 | 2020-09-04 | 云南天爵汉麻生物科技有限公司 | Method for extracting nicotine from tobacco based on tertiary extraction method |
| CN113508919B (en) * | 2020-12-31 | 2023-05-02 | 上海零诺生物科技有限公司 | Tobacco extract and preparation method and application thereof |
| CN114605384B (en) * | 2022-03-02 | 2023-11-21 | 湖南省烟草公司郴州市公司 | Method for extracting nicotine |
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| KR0161777B1 (en) * | 1995-10-31 | 1998-11-16 | 박명규 | Tobacco flavor preparation method using tobacco extract |
| KR100217828B1 (en) * | 1996-07-24 | 1999-09-01 | 박명규 | Perfume manufacturing method comprising a low nicotine tobacco extract for tobacco flavor and tobacco extract |
| DK1267650T3 (en) * | 2000-03-10 | 2006-05-08 | British American Tobacco Co | tobacco Treatment |
| JP4821024B2 (en) * | 2002-07-18 | 2011-11-24 | ファセックス・コーポレーション | Reduction of components in tobacco |
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| CN103497837B (en) * | 2013-09-27 | 2016-03-23 | 福建中烟工业有限责任公司 | A kind of essential oil of the flower of Camellia sinensis, its preparation method and the application in cigarette thereof |
| CN105254609B (en) * | 2015-11-27 | 2017-07-11 | 江苏万村爱农农业科技有限公司 | The extracting method of blueberry anthocyanin |
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