CN105504077A - Integrated preparation method of tobacco polysaccharide - Google Patents
Integrated preparation method of tobacco polysaccharide Download PDFInfo
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- CN105504077A CN105504077A CN201510917532.6A CN201510917532A CN105504077A CN 105504077 A CN105504077 A CN 105504077A CN 201510917532 A CN201510917532 A CN 201510917532A CN 105504077 A CN105504077 A CN 105504077A
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- tobacco
- filtering membrane
- membrane
- integrated preparation
- extractor
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 62
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 61
- 150000004676 glycans Chemical class 0.000 title claims abstract description 33
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 33
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000012528 membrane Substances 0.000 claims abstract description 56
- 238000001914 filtration Methods 0.000 claims abstract description 45
- 238000000605 extraction Methods 0.000 claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000001802 infusion Methods 0.000 claims abstract description 12
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 11
- 239000002033 PVDF binder Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- CUYTYLVEYFUAAX-UHFFFAOYSA-N 4-methylbenzenesulfonic acid;sodium Chemical compound [Na].CC1=CC=C(S(O)(=O)=O)C=C1 CUYTYLVEYFUAAX-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000003851 corona treatment Methods 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 4
- -1 wherein Substances 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 235000019504 cigarettes Nutrition 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 5
- 238000004737 colorimetric analysis Methods 0.000 description 5
- 239000008103 glucose Substances 0.000 description 5
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 235000014633 carbohydrates Nutrition 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940088623 biologically active substance Drugs 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 235000019633 pungent taste Nutrition 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to an integrated preparation method of tobacco polysaccharide, which comprises the following steps: adding the tobacco raw material and an extracting agent into an extraction tank, and starting a circulating pump to circularly flow; heating the extraction tank, closing the circulating pump, starting the infusion pump, and conveying the extractant to sequentially pass through a first filtering membrane and a second filtering membrane which are arranged at intervals; concentrating and drying the liquid in the recovery tank to obtain tobacco polysaccharide; wherein the first filter membrane has a pore size of 5 xl 04～3×l05A PVDF tubular membrane from Dalton; the second filtration membrane had a pore size of 1 xl 04～3×l04A PVDF tubular membrane from Dalton. The scheme has the advantages of few operation steps, simple and convenient flow, short extraction time, low extraction cost, low energy consumption, high impurity removal efficiency and easy realization of industrial production.
Description
Technical field
The present invention relates to an extraction process growing tobacco polysaccharide, be specifically related to an integrated preparation method growing tobacco polysaccharide.
Background technology
Tobacco is Solanaceae Nicotiana plant, is the natural phant that a kind of utility value is very high, is also widely cultivated as a kind of important cash crop simultaneously.Chinese tobacco cultivated area and output rank first in the world, and tobacco planting and Product processing play an important role in the national economic development.In the Bian receipts and production process of tobacco, except for except the tobacco leaf of production of cigarettes, the resources such as a large amount of inferior grade tobacco leaves, cigarette stalk, offal, tobacco stem are had to fail to be utilized effectively as tankage every year, or abandon in field, or dried burning, also result in the significant wastage of natural resources while bringing pollution to environment.Current China is faced with severe environment situation, and environmental pollution has become the problem that the whole people show great attention to, and the efficiency utilization of resource and recycle will be the directions of each industry development from now on, also will be the direction of tobacco industry development.
Tobacco polysaccharide, as a kind of biologically active substance of functional component in tobacco leaf, has multiple pharmacological effect.The water-soluble sugar contained in tobacco occupies an important position in production of cigarettes, first, when cigarette burns and sucks can in and alkaline components in flue gas, regulate smoke pH, reduce the pungency of flue gas; Secondly, carbohydrate is latent aromatic substance important in tobacco, cracking can occur when cigarette burns and sucks, and produces many important aroma components, as furans, small molecules aldoketones etc.; 3rd, carbohydrate with the total free aminoacids generation Maillard reaction in tobacco, can also produce camerlsed, covers assorted gas beastly; Finally, tobacco glucide also plays a key effect in humid keeping performance, has remarkably influenced to the organoleptic quality of cigarette and the steady quality of cigarette product.
The extraction of current tobacco polysaccharide adopts lixiviate, filtration, centrifugal, the sequence of operations process such as alcohol precipitation and Sevage method deproteinated to obtain more.But the operation steps of these methods is many, and extraction time is many, flow process is too loaded down with trivial details, and extraction time is oversize.
Summary of the invention
For the deficiencies in the prior art part, the object of the present invention is to provide the integrated preparation method that grows tobacco polysaccharide.
Technical scheme of the present invention is summarized as follows:
The one integrated preparation method growing tobacco polysaccharide, comprising:
S1: tobacco material and extraction agent are joined in extractor, ON cycle pump circulates in extractor to make extraction agent, accelerates the extraction efficiency to tobacco material, and the time length circulated is 10 ~ 50min;
S2: extractor is heated to 50 ~ 80 DEG C, close recycle pump, open infusion pump, by extraction agent conveying successively through spaced first filtering membrane and the second filtering membrane, wherein, liquid under first filtering membrane interception is returned in extractor, the liquid through the second filtering membrane is returned in extractor, will the first filtering membrane be passed but be directed in withdrawing can by the liquid under the second filtering membrane interception;
S3: concentrate drying is carried out to the liquid in withdrawing can and namely obtains tobacco polysaccharide;
Wherein, described first filtering membrane is aperture is 5 × l0
4~ 3 × l0
5the PVDF tubular membrane of Dalton; Described second filtering membrane is aperture is 1 × l0
4~ 3 × l0
4the PVDF tubular membrane of Dalton.
Preferably, the integrated preparation method of described tobacco polysaccharide, wherein, the pressure of described infusion pump is 0.10 ~ 0.25MPa.
Preferably, the integrated preparation method of described tobacco polysaccharide, wherein, described extraction agent is water.
Preferably, the integrated preparation method of described tobacco polysaccharide, wherein, the consumption of described extraction agent is 10 ~ 30 times of tobacco material gross weight.
Preferably, the integrated preparation method of described tobacco polysaccharide, wherein, described first filtering membrane before use, immerses in the aqueous solution containing 0.01M p-methyl benzenesulfonic acid sodium.
Preferably, the integrated preparation method of described tobacco polysaccharide, wherein, described second filtering membrane before use, carries out corona treatment to it, and corona applied voltage size is 0.1 ~ 0.2V.
The invention has the beneficial effects as follows:
1, the characteristic of membrane separation technique realizes accurately being separated to the physical aspect of material according to screening principle, and process is easy to control, and is adapted to suitability for industrialized production;
2, the present invention adopts combined films isolation technique can effectively remove macromole impurity, tradition alcohol deposition method is when purified polysaccharide, only can remove the small molecular weight impurity being dissolved in ethanol, the removal to macromole impurity cannot be completed, the macropore filter membrane that the present invention adopts effectively can be tackled in extracting solution and obtain the macromolecular substance such as protein, pectin, and impurity-eliminating effect is better;
3, the present invention uses membrane separation technique to instead of traditional alcohol precipitation technology, saves a large amount of ethanol, reduces because using increasing of the security risk that causes of ethanol and production cost, also reduce simultaneously ethanol reclaim needed for energy consumption, shorten the production cycle;
4, the aperture filter membrane of the present invention's employing is while having retained tobacco polysaccharide target components, is also the process of a low temperature without phase transformation, decreases later stage concentrate drying required time, reduce energy consumption;
5, dynamic circulation extraction is separated integrated by the present invention with combined films, the multistep traditional technologys such as extraction, concentrated, separation are simplified, decrease filtration, the equipment such as concentrated, and shorten the process time, improve extraction and isolation efficiency, in filtration efficiency, the aspect such as solvent, energy expenditure all shows obvious advantage.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, can implement according to this with reference to specification sheets word to make those skilled in the art.
This case proposes the integrated preparation method of the tobacco polysaccharide of an embodiment, comprising:
S1: tobacco material and extraction agent are joined in extractor, ON cycle pump circulates in extractor to make extraction agent, accelerates the extraction efficiency to tobacco material, and the time length circulated is 10 ~ 50min;
S2: extractor is heated to 50 ~ 80 DEG C, close recycle pump, open infusion pump, by extraction agent conveying successively through spaced first filtering membrane and the second filtering membrane, wherein, liquid under first filtering membrane interception is returned in extractor, the liquid through the second filtering membrane is returned in extractor, will the first filtering membrane be passed but be directed in withdrawing can by the liquid under the second filtering membrane interception;
S3: concentrate drying is carried out to the liquid in withdrawing can and namely obtains tobacco polysaccharide;
Wherein, the first filtering membrane is aperture is 5 × l0
4~ 3 × l0
5the PVDF tubular membrane of Dalton; Second filtering membrane is aperture is 1 × l0
4~ 3 × l0
4the PVDF tubular membrane of Dalton.
In the above-described embodiments, the pressure of infusion pump is preferably 0.10 ~ 0.25MPa.
In the above-described embodiments, extraction agent is preferably water.
In the above-described embodiments, the consumption of extraction agent is preferably 10 ~ 30 times of tobacco material gross weight.Tobacco material is preferably one or more mixing in the particle that produces in tobacco leaf, pipe tobacco or tobacco processing course tiny offal, cigarette ash, tobacco fragment, offal or other tobacco wastes.
As another embodiment of this case, wherein, the first filtering membrane before use, immerses in the aqueous solution containing 0.01M p-methyl benzenesulfonic acid sodium.The effect of p-methyl benzenesulfonic acid sodium is the charged group on activation pvdf membrane, is make the first filtering membrane have filtration velocity faster to tobacco polysaccharide.But it should be noted that the concentration of the aqueous solution of p-methyl benzenesulfonic acid sodium should be limited, if concentration is excessive, then will the strainability of pvdf membrane be caused to decline.
As the another embodiment of this case, wherein, the second filtering membrane before use, carries out corona treatment to it, and corona applied voltage size is 0.1 ~ 0.2V.The object of corona treatment is the activity in order to regulate charged group on pvdf membrane, to accelerate the second filtering membrane to micromolecular filtration velocity, prevents runner from blocking up, causes flow velocity to reduce, and increases energy consumption.But voltage swing should be defined, exceed preferred scope and decline causing the strainability of the second filtering membrane.
Embodiment 1
As stated above, tobacco material 1kg, water 10kg, 10min is extracted in circulation, and infusion pump pressure 0.10MPa, finally obtains solids 50.6g, with Glucose standards sample for standard, take phenolsulfuric acid as developer, the content adopting colorimetric method for determining wherein polysaccharide is 89.2%.
Embodiment 2
As stated above, tobacco material 1kg, water 30kg, 50min is extracted in circulation, and infusion pump pressure 0.25MPa, finally obtains solids 57.5g, with Glucose standards sample for standard, take phenolsulfuric acid as developer, the content adopting colorimetric method for determining wherein polysaccharide is 90.1%.
Embodiment 3
As stated above, tobacco material 1kg, water 30kg, 50min, infusion pump pressure 0.25MPa are extracted in circulation, and the first filtering membrane before use, immerses in the aqueous solution containing 0.01M p-methyl benzenesulfonic acid sodium; Finally obtaining solids 60.8g, with Glucose standards sample for standard, take phenolsulfuric acid as developer, and the content adopting colorimetric method for determining wherein polysaccharide is 91.4%.
Embodiment 4
As stated above, tobacco material 1kg, water 10kg, 10min, infusion pump pressure 0.10MPa are extracted in circulation, and the second filtering membrane before use, carries out corona treatment to it, and corona applied voltage size is 0.1V; Finally obtaining solids 53.3g, with Glucose standards sample for standard, take phenolsulfuric acid as developer, and the content adopting colorimetric method for determining wherein polysaccharide is 91.0%.
Embodiment 5
As stated above, tobacco material 1kg, water 20kg, 30min is extracted in circulation, infusion pump pressure 0.20MPa, the first filtering membrane before use, immerses in the aqueous solution containing 0.01M p-methyl benzenesulfonic acid sodium, second filtering membrane before use, carries out corona treatment to it, and corona applied voltage size is 0.2V; Finally obtaining solids 60.1g, with Glucose standards sample for standard, take phenolsulfuric acid as developer, and the content adopting colorimetric method for determining wherein polysaccharide is 92.2%.
Although embodiment of the present invention are open as above, but it is not restricted to listed in specification sheets and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and shown here embodiment.
Claims (6)
1. an integrated preparation method growing tobacco polysaccharide, is characterized in that, comprising:
S1: tobacco material and extraction agent are joined in extractor, ON cycle pump circulates in extractor to make extraction agent, accelerates the extraction efficiency to tobacco material, and the time length circulated is 10 ~ 50min;
S2: extractor is heated to 50 ~ 80 DEG C, close recycle pump, open infusion pump, by extraction agent conveying successively through spaced first filtering membrane and the second filtering membrane, wherein, liquid under first filtering membrane interception is returned in extractor, the liquid through the second filtering membrane is returned in extractor, will the first filtering membrane be passed but be directed in withdrawing can by the liquid under the second filtering membrane interception;
S3: concentrate drying is carried out to the liquid in withdrawing can and namely obtains tobacco polysaccharide;
Wherein, described first filtering membrane is aperture is 5 × l0
4~ 3 × l0
5the PVDF tubular membrane of Dalton; Described second filtering membrane is aperture is 1 × l0
4~ 3 × l0
4the PVDF tubular membrane of Dalton.
2. the integrated preparation method of tobacco polysaccharide according to claim 1, is characterized in that, the pressure of described infusion pump is 0.10 ~ 0.25MPa.
3. the integrated preparation method of tobacco polysaccharide according to claim 1, is characterized in that, described extraction agent is water.
4. the integrated preparation method of tobacco polysaccharide according to claim 1, is characterized in that, the consumption of described extraction agent is 10 ~ 30 times of tobacco material gross weight.
5. the integrated preparation method of tobacco polysaccharide according to claim 1, is characterized in that, described first filtering membrane before use, immerses in the aqueous solution containing 0.01M p-methyl benzenesulfonic acid sodium.
6. the integrated preparation method of tobacco polysaccharide according to claim 1, is characterized in that, described second filtering membrane before use, carries out corona treatment to it, and corona applied voltage size is 0.1 ~ 0.2V.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510917532.6A CN105504077A (en) | 2015-12-11 | 2015-12-11 | Integrated preparation method of tobacco polysaccharide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510917532.6A CN105504077A (en) | 2015-12-11 | 2015-12-11 | Integrated preparation method of tobacco polysaccharide |
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| Publication Number | Publication Date |
|---|---|
| CN105504077A true CN105504077A (en) | 2016-04-20 |
Family
ID=55712424
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510917532.6A Pending CN105504077A (en) | 2015-12-11 | 2015-12-11 | Integrated preparation method of tobacco polysaccharide |
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| Country | Link |
|---|---|
| CN (1) | CN105504077A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102781558A (en) * | 2009-11-25 | 2012-11-14 | 悉尼大学 | Membrane and membrane separation system |
| CN104271220A (en) * | 2011-12-07 | 2015-01-07 | 杜邦营养生物科学有限公司 | Nanofiltration methods for enhanced solute flux through pretreatment |
| CN104853833A (en) * | 2012-12-17 | 2015-08-19 | 巴斯夫欧洲公司 | Filtration systems and membranes with enhanced flux and method for their preparation |
-
2015
- 2015-12-11 CN CN201510917532.6A patent/CN105504077A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102781558A (en) * | 2009-11-25 | 2012-11-14 | 悉尼大学 | Membrane and membrane separation system |
| CN104271220A (en) * | 2011-12-07 | 2015-01-07 | 杜邦营养生物科学有限公司 | Nanofiltration methods for enhanced solute flux through pretreatment |
| CN104853833A (en) * | 2012-12-17 | 2015-08-19 | 巴斯夫欧洲公司 | Filtration systems and membranes with enhanced flux and method for their preparation |
Non-Patent Citations (1)
| Title |
|---|
| 卢玲巧: "大黄多糖集成化提取分离方法的研究", 《中国优秀硕士学位论文全文数据库医药卫生科技辑》 * |
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