CN114249632A - Novel process for purifying solanesol based on chemically modified diatomite - Google Patents
Novel process for purifying solanesol based on chemically modified diatomite Download PDFInfo
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- CN114249632A CN114249632A CN202111561624.7A CN202111561624A CN114249632A CN 114249632 A CN114249632 A CN 114249632A CN 202111561624 A CN202111561624 A CN 202111561624A CN 114249632 A CN114249632 A CN 114249632A
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- solanesol
- modified diatomite
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- diatomite
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 57
- AFPLNGZPBSKHHQ-UHFFFAOYSA-N Betulaprenol 9 Natural products CC(C)=CCCC(C)=CCCC(C)=CCCC(C)=CCCC(C)=CCCC(C)=CCCC(C)=CCCC(C)=CCCC(C)=CCO AFPLNGZPBSKHHQ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- AFPLNGZPBSKHHQ-MEGGAXOGSA-N solanesol Chemical compound CC(C)=CCC\C(C)=C\CC\C(C)=C\CC\C(C)=C\CC\C(C)=C\CC\C(C)=C\CC\C(C)=C\CC\C(C)=C\CC\C(C)=C\CO AFPLNGZPBSKHHQ-MEGGAXOGSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 33
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000011049 filling Methods 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 6
- 230000007935 neutral effect Effects 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 229930014626 natural product Natural products 0.000 description 4
- 239000005909 Kieselgur Substances 0.000 description 3
- 241000208125 Nicotiana Species 0.000 description 3
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 3
- 230000005526 G1 to G0 transition Effects 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000001257 hydrogen Chemical group 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000206761 Bacillariophyta Species 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000035 biogenic effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229920000344 molecularly imprinted polymer Polymers 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
Abstract
The invention discloses a new process for purifying solanesol based on chemically modified diatomite, which comprises the following steps: (1) grinding 3.0g of diatomite into fine powder with the particle size of 500-800 meshes, adding 8-12ml of any strong acid except hydrofluoric acid into the fine powder to form a solution, filling the solution into a first closed container, placing the first closed container in a constant-temperature water bath, oscillating for 45-55min at normal temperature, washing the oscillated solution to be neutral, filtering by using a screen with the aperture of 20-25 mu m, and drying the obtained filtrate to constant weight to obtain modified diatomite; (2) adding 0.3-0.8g of modified diatomite obtained in the step (1) into 50ml of an extract containing solanesol to form a mixed solution, filling the mixed solution into a third closed container, placing the third closed container into a constant-temperature water bath, shaking for 45-55min at normal temperature, filtering the mixed solution after shaking to obtain filter residues, wherein the aperture of a mesh screen for filtering is 10-15 mu m; (3) washing the filter residue with a washing solution to obtain solanesol, wherein the washing solution is a solution in which the solanesol is easily dissolved; the process can greatly reduce the separation cost.
Description
Technical Field
The invention relates to a technology for separating and purifying solanesol in a tobacco extract, in particular to a novel process for purifying solanesol based on chemically modified diatomite.
Background
Diatomite is a biogenic siliceous sedimentary rock and mainly comprises microalgae such as diatom before tens of thousands of years. These diatoms belong to single-celled microalgae, which are typically only 10 to tens of microns in shape. The density of the diatomite is 1.9-2.35 g/cm3, the bulk density is 0.34-0.56 g/cm3, the specific surface area is 10-60 m2/g, the pore volume is 0.46-0.98 cm3/g, and the melting point is 1650-1750 ℃. The specific porous structure of diatomaceous earth can be observed under an electron microscope (as shown in figure 1). The shell has micropores ranging from dozens of nanometers to several microns, loose texture, high porosity and strong adsorption capacity.
Diatomaceous earth has stable chemical properties and does not react with any strong acid other than hydrofluoric acid. As the surface and the pores of the diatomite contain a large amount of hydroxyl, hydrogen bonds can be formed among the hydroxyl, and the diatomite has certain reaction activity and is faintly acid. The separation of natural products mostly adopts macroporous resin as a stationary phase, the preparation cost is high, the processing process is complex, the waste is not suitable for treatment, and a certain problem of environmental pollution can be caused.
Disclosure of Invention
In view of the above, the present invention aims to provide a new process for purifying solanesol based on chemically modified diatomite, which can greatly reduce the separation and purification cost of solanesol, improve the efficiency of molecular separation of solanesol, and avoid environmental pollution caused by waste.
The purpose of the invention is realized by the following technical scheme:
a new process for purifying solanesol based on chemically modified diatomite comprises the following steps:
(1) grinding 3.0g of diatomite into fine powder with the particle size of 500-800 meshes, adding 8-12ml of any strong acid except hydrofluoric acid into the fine powder to form a solution, filling the solution into a first closed container, placing the first closed container in a constant-temperature water bath, oscillating for 45-55min at normal temperature, washing the oscillated solution to be neutral, filtering by using a screen with the aperture of 20-25 mu m, and drying the obtained filtrate to constant weight to obtain modified diatomite;
(2) adding 0.3-0.8g of modified diatomite obtained in the step (1) into 50ml of an extract containing solanesol to form a mixed solution, filling the mixed solution into a third closed container, placing the third closed container into a constant-temperature water bath, shaking for 45-55min at normal temperature, filtering the mixed solution after shaking to obtain filter residues, wherein the aperture of a mesh screen for filtering is 10-15 mu m;
(3) and washing the filter residue by using a washing solution to obtain the solanesol, wherein the washing solution is a solution in which the solanesol is easy to dissolve.
Further, the strong acid added to the fine powder in the step (1) is hydrochloric acid having a concentration of 3 mol/L.
Further, the washing liquid in the step (3) is hexane.
Still further, the constant temperature water bath is a constant temperature water bath oscillator.
The invention has the beneficial effects that:
the invention relates to a new process for purifying solanesol based on chemical modified diatomite, which modifies diatomite by adopting any strong acid except hydrofluoric acid, so that the diatomite has the maximum specific surface area and pore volume, in addition, because the surface and the pores of the diatomite contain a large amount of hydroxyl groups, hydrogen bonds can be formed between the hydroxyl groups, the diatomite has certain reaction activity and is faintly acid and can become a solanesol molecularly imprinted polymer, the modified diatomite can be used as a stationary phase for separating the natural product solanesol, the use of resin materials can be reduced, the separation cost of the natural product can be greatly reduced, the separation efficiency is improved, the diatomite is a natural product and has wide acquisition channels, the diatomite is used as a modifier and only needs to be modified by any strong acid except hydrofluoric acid, and the separation process of the solanesol molecules by adopting the modified diatomite is easy, the efficiency is high.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof.
Drawings
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings, in which:
fig. 1 is an SEM image of the microstructure of diatomaceous earth.
FIG. 2 is a graph showing the effect of hydrochloric acid concentration on the adsorption performance of modified diatomaceous earth.
FIG. 3 is a graph showing the effect of treatment time on the adsorption performance of modified diatomaceous earth.
Detailed Description
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. It should be understood that the preferred embodiments are illustrative of the invention only and are not limiting upon the scope of the invention.
Example one
As shown in fig. 1-3, a new process for purifying solanesol based on chemically modified diatomite comprises the following steps:
(1) grinding 3.0g of diatomite into fine powder with the particle size of 500 meshes by using a grinding bottle, adding 12ml of sulfuric acid with the concentration of 3mol/L into the fine powder to form a solution, then placing the grinding bottle filled with the solution into a constant-temperature water bath oscillator, oscillating for 45min at normal temperature, washing the oscillated solution to be neutral, filtering by using a screen with the aperture of 20-25 mu m, and drying the obtained filtrate to constant weight to obtain modified diatomite;
(2) adding 0.3g of modified diatomite obtained in the step (1) into 50ml of an extract containing solanesol to form a mixed solution, filling the mixed solution into a third closed container, placing the third closed container into a constant-temperature water bath oscillator, oscillating for 55min at normal temperature, filtering the oscillated mixed solution to obtain filter residues, wherein the aperture of a mesh screen for filtering is 10-15 mu m;
(3) washing the filter residue with hexane to obtain solanesol.
Example two
As shown in fig. 1-3, a new process for purifying solanesol based on chemically modified diatomite comprises the following steps:
(1) grinding 3.0g of diatomite into fine powder with the particle size of 800 meshes by adopting a grinding bottle, adding 8ml of nitric acid with the concentration of 3mol/L into the fine powder to form a solution, then placing the grinding bottle filled with the solution into a constant-temperature water bath oscillator, oscillating for 55min at normal temperature, washing the oscillated solution to be neutral, filtering by using a screen with the aperture of 20-25 mu m, and drying the obtained filtrate to constant weight to obtain modified diatomite;
(2) adding 0.8g of modified diatomite obtained in the step (1) into 50ml of an extract containing solanesol to form a mixed solution, filling the mixed solution into a third closed container, placing the third closed container into a constant-temperature water bath oscillator, oscillating for 45min at normal temperature, filtering the oscillated mixed solution to obtain filter residues, wherein the aperture of a mesh screen for filtering is 10-15 mu m;
(3) washing the filter residue with hexane to obtain solanesol.
EXAMPLE III
As shown in fig. 1-3, a new process for purifying solanesol based on chemically modified diatomite comprises the following steps:
(1) grinding 3.0g of diatomite into fine powder with the particle size of 600 meshes by using a grinding bottle, adding 10ml of hydrochloric acid with the concentration of 3mol/L into the fine powder to form a solution, then placing the grinding bottle filled with the solution into a constant-temperature water bath oscillator, oscillating for 50min at normal temperature, washing the oscillated solution to be neutral, filtering by using a screen with the aperture of 20-25 mu m, and drying the obtained filtrate to constant weight to obtain modified diatomite;
(2) adding 0.5g of modified diatomite obtained in the step (1) into 50ml of tobacco extract containing solanesol to form a mixed solution, filling the mixed solution into a third closed container, placing the third closed container into a constant-temperature water bath oscillator, oscillating for 50min at normal temperature, filtering the oscillated mixed solution to obtain filter residues, wherein the aperture of a mesh screen for filtering is 10-15 mu m;
(3) washing the filter residue with hexane to obtain solanesol.
Determining the adsorption effect of the modified diatomite: putting 0.5g of modified diatomite obtained in the step (1) into a grinding flask containing 50ml of aniline solution, putting the grinding flask into a constant-temperature water bath oscillator, oscillating for 30 minutes at 25 ℃, taking out the grinding flask and filtering the solution in the grinding flask to obtain a filtrate, wherein the aperture of a screen mesh for filtering is 18 mu m, aniline is adsorbed by the modified diatomite, the modified diatomite in the step (2) is changed into a filtrate, and the adsorption effect of the modified diatomite on solanesol can be known according to the aniline concentration in the filtrate after the step (2), wherein solanesol is obtained by replacing solanesol in the pores of the modified diatomite; according to the method, different process conditions such as strong acid type, strong acid concentration, oscillation time and the like in the step (1) are adjusted to finally obtain strong acid selective hydrochloric acid, the strong acid concentration is selected to be 3mol/L, and when the oscillation time is selected to be 50min, the modified diatomite has the best adsorption effect on the solanesol.
The adsorption capacity of the solanesol molecules in the modified diatomite can be known through the quantification of the concentration of the solanesol, and experimental results prove that the separation efficiency of the solanesol molecules is effectively improved, and the purification cost is greatly reduced. The method has the advantages of good stability, accuracy, reliability, simple and quick operation and good repeatability, and is very suitable for separating and purifying the solanesol in the tobacco extract.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (4)
1. A new process for purifying solanesol based on chemically modified diatomite is characterized in that: the method comprises the following steps:
(1) grinding 3.0g of diatomite into fine powder with the particle size of 500-800 meshes, adding 8-12ml of any strong acid except hydrofluoric acid into the fine powder to form a solution, filling the solution into a first closed container, placing the first closed container in a constant-temperature water bath, oscillating for 45-55min at normal temperature, washing the oscillated solution to be neutral, filtering by using a screen with the aperture of 20-25 mu m, and drying the obtained filtrate to constant weight to obtain modified diatomite;
(2) adding 0.3-0.8g of modified diatomite obtained in the step (1) into 50ml of an extract containing solanesol to form a mixed solution, filling the mixed solution into a third closed container, placing the third closed container into a constant-temperature water bath, shaking for 45-55min at normal temperature, filtering the mixed solution after shaking to obtain filter residues, wherein the aperture of a mesh screen for filtering is 10-15 mu m;
(3) and washing the filter residue by using a washing solution to obtain the solanesol, wherein the washing solution is a solution in which the solanesol is easy to dissolve.
2. The new process for purifying solanesol based on chemically modified diatomite as claimed in claim 1, wherein: the strong acid added into the fine powder in the step (1) is hydrochloric acid with the concentration of 3 mol/L.
3. The new process for purifying solanesol based on chemically modified diatomite as claimed in claim 1, wherein: the washing liquid in the step (3) is hexane.
4. The new process for purifying solanesol based on chemically modified diatomite as claimed in claim 1, 2 or 3, wherein: the constant temperature water bath device is a constant temperature water bath oscillator.
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| CN202111561624.7A CN114249632A (en) | 2021-12-20 | 2021-12-20 | Novel process for purifying solanesol based on chemically modified diatomite |
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| CN202111561624.7A CN114249632A (en) | 2021-12-20 | 2021-12-20 | Novel process for purifying solanesol based on chemically modified diatomite |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686988A (en) * | 2005-04-05 | 2005-10-26 | 杨雪峰 | Method for preparing high pure solanesol |
| WO2007029264A2 (en) * | 2005-09-05 | 2007-03-15 | Jonnalagadda Raghunath Rao | Method of isolating solanesol extract from tobacco utilizing super critical co2 fluid extraction processing |
| CN104072336A (en) * | 2014-06-06 | 2014-10-01 | 山东中烟工业有限责任公司 | Process for extracting solanesol |
| CN104310411A (en) * | 2014-10-16 | 2015-01-28 | 桂林新竹大自然生物材料有限公司 | Method for preparing high-quality diatomite by oscillation-based hydrochloric acid process |
| CN105646150A (en) * | 2016-02-03 | 2016-06-08 | 河西学院 | Method for extracting high-purity solanesol from tobacco leaves |
| CN208990286U (en) * | 2018-09-14 | 2019-06-18 | 湖南省烟草公司郴州市公司 | A kind of device extracting Salanesol from tobacco |
| CN111233630A (en) * | 2019-12-31 | 2020-06-05 | 常德市正阳生物科技股份有限公司 | Separation method of solanesol-containing eluent |
| CN111732498A (en) * | 2020-07-02 | 2020-10-02 | 贵州省烟草公司遵义市公司 | Mixed solvent for extracting solanesol and method for extracting solanesol by using same |
| CN113264812A (en) * | 2021-05-15 | 2021-08-17 | 昆明理工大学 | Method for extracting and purifying solanesol |
-
2021
- 2021-12-20 CN CN202111561624.7A patent/CN114249632A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686988A (en) * | 2005-04-05 | 2005-10-26 | 杨雪峰 | Method for preparing high pure solanesol |
| WO2007029264A2 (en) * | 2005-09-05 | 2007-03-15 | Jonnalagadda Raghunath Rao | Method of isolating solanesol extract from tobacco utilizing super critical co2 fluid extraction processing |
| CN104072336A (en) * | 2014-06-06 | 2014-10-01 | 山东中烟工业有限责任公司 | Process for extracting solanesol |
| CN104310411A (en) * | 2014-10-16 | 2015-01-28 | 桂林新竹大自然生物材料有限公司 | Method for preparing high-quality diatomite by oscillation-based hydrochloric acid process |
| CN105646150A (en) * | 2016-02-03 | 2016-06-08 | 河西学院 | Method for extracting high-purity solanesol from tobacco leaves |
| CN208990286U (en) * | 2018-09-14 | 2019-06-18 | 湖南省烟草公司郴州市公司 | A kind of device extracting Salanesol from tobacco |
| CN111233630A (en) * | 2019-12-31 | 2020-06-05 | 常德市正阳生物科技股份有限公司 | Separation method of solanesol-containing eluent |
| CN111732498A (en) * | 2020-07-02 | 2020-10-02 | 贵州省烟草公司遵义市公司 | Mixed solvent for extracting solanesol and method for extracting solanesol by using same |
| CN113264812A (en) * | 2021-05-15 | 2021-08-17 | 昆明理工大学 | Method for extracting and purifying solanesol |
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