CN105536285A - Device and method for extracting dihydromyricetin and polysaccharide from ampelopsis grossedentata leftovers - Google Patents
Device and method for extracting dihydromyricetin and polysaccharide from ampelopsis grossedentata leftovers Download PDFInfo
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- CN105536285A CN105536285A CN201610011456.7A CN201610011456A CN105536285A CN 105536285 A CN105536285 A CN 105536285A CN 201610011456 A CN201610011456 A CN 201610011456A CN 105536285 A CN105536285 A CN 105536285A
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- tank body
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- air inlet
- liquid outlet
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/32—2,3-Dihydro derivatives, e.g. flavanones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
Abstract
The invention discloses a device for extracting dihydromyricetin and polysaccharide from ampelopsis grossedentata leftovers. The device comprises a pot body. A pot cover is arranged on the pot body. A filter plate is arranged on the upper portion inside the pot body. A sieve plate where materials are placed is arranged on the lower portion of the pot body. The side wall of the pot body is provided with a liquid outlet located above the filter plate. The bottom of the pot body is provided with a liquid drainage pipeline and communicated with the bottom of a liquid storage pot through a vapor-liquid pipeline, the top of the liquid storage pot is provided with a liquid inlet, and the liquid storage pot is further provided with an air inlet pipe with one end extending to the bottom of the liquid storage pot. The invention further discloses a method for extracting the dihydromyricetin and the polysaccharide from the ampelopsis grossedentata leftovers. The energy utilization rate can be improved by one time or above, and the cost is greatly reduced. The dihydromyricetin and the polysaccharide are extracted, efficient purification is achieved, solvent consumption is small, operation is easy, and the cost is low. Water is recycled, and pollution discharge is avoided.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to the device extracting dibydro myricetrin and polysaccharide from vine tea leftover bits and pieces, also relate to the method extracting dibydro myricetrin and polysaccharide from vine tea leftover bits and pieces, be applicable to extract dibydro myricetrin and polysaccharide in vine tea leftover bits and pieces.
Background technology
Ampelopsin has protecting the liver, relieves the effect of alcohol, hypotensive, antitumor, promote the important medical values such as skin repair, be developed to various medicine, functional food or cosmetics in recent years.Therefore also cause the demand of ampelopsin huge, the industrial high efficiency Isolation and purification technology of ampelopsin is also subject to the extensive concern in industry.At present in the extraction process of natural products, adopt toxic organic solvents degreasing impurity elimination to extract natural drug or food composition is still widely used method.But toxic organic solvents remains and brings a lot of potential safety hazard to medicine or food production.In the extraction purification technology of ampelopsin, current bibliographical information and disclosed patented technology can be summed up as following basic skills: adopt the fat-soluble organic solvent such as benzinum or gasoline to dried material degreasing, then the material water heating after degreasing is boiled and boil extraction, then concentrating and precipitating or column chromatography are carried out to extract, obtain the ampelopsin that purity is higher.There is a fatal weakness in this kind of technique: in skimming processes, have employed toxic organic solvents exactly, makes to remain with toxic solvent in the ampelopsin extracted.Therefore, study a kind of simple effectively, environmental protection and can the ampelopsin extracting method that uses of large-scale low-cost most important for the sound development of the sector.The present invention specifically solves following key technical problem: (1) adopts pure water and food-grade alcohol as Extraction solvent, does not adopt any other solvent in addition; (2) by special heat reusing device and method, extraction cost drop by half is made.
Summary of the invention
The object of the invention is the problems referred to above being to exist for prior art, the device extracting dibydro myricetrin and polysaccharide is provided, the method extracting dibydro myricetrin and polysaccharide from vine tea leftover bits and pieces is also provided from vine tea leftover bits and pieces.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
The device of dibydro myricetrin and polysaccharide is extracted from vine tea leftover bits and pieces, comprise tank body, tank body is provided with cover, top in tank body is provided with filter plate, and the bottom of tank body is provided with the sieve plate for placing material, and tank wall is provided with the liquid outlet be positioned at above filter plate, tank base is provided with fluid pipeline, tank base is also communicated with the bottom of fluid reservoir by vapour-liquid pipeline, and the top of fluid reservoir is provided with inlet, fluid reservoir is also provided with one end and extends to air inlet pipe bottom fluid reservoir.
Inlet as above is provided with inlet valve; Air inlet pipe is provided with air inlet pipe valve; Vapour-liquid pipeline is provided with air intake valve; Fluid pipeline is provided with fluid valve.
From vine tea leftover bits and pieces, extract the method for dibydro myricetrin and polysaccharide, comprise the following steps:
Step 1, using vine tea leftover bits and pieces pulverize as material, be then encased in tank body, cover cover;
Step 2, Boiler Steam outlet to be connected with air inlet pipe, the high-temperature vapor of 100 ~ 300 degrees Celsius slow transits through air inlet pipe, fluid reservoir and vapour-liquid pipeline and enters in tank body, the heating of infiltration limit, limit is carried out, until to be soaked into by whole material and by heating material to 85 ~ 95 degrees Celsius to the material in this tank body;
Step 3, continue the high-temperature water vapor passing into 100 ~ 300 degrees Celsius to air inlet pipe, the aqueous solution in material slowly flows out from liquid outlet through filter plate, collects the aqueous solution flowed out;
Step 4, by liquid outlet flow out the aqueous solution be injected in sedimentation basin, naturally cool precipitation;
The supernatant liquor of step 5, extraction sedimentation basin, fluid reservoir is injected into from inlet, heated by the high-temperature water vapor entering fluid reservoir, then enter in tank body under the high-temperature water vapor pressure effect of steam boiler, material in tank body is extracted again, return step 4, iterative cycles like this extracts 3 ~ 5 times;
Step 6, sedimentation basin extracted the precipitation after supernatant liquor and take out to dry and pulverize, with 80 ~ 100% alcoholic extractions, filtration, the residue leached dries pulverizing, is Thick many candies; Dibydro myricetrin crude product is obtained to after alcoholic extract recovered alcohol;
Step 7, take out the material in tank body, by dibydro myricetrin crude product drying and crushing, then be encased in tank body, then mixed solution is injected by inlet to fluid reservoir, this mixed solution consists of absolute ethyl alcohol and benzinum, the boiling range of benzinum is 30 ~ 90 degrees Celsius, the volume parts of benzinum: the volume parts of absolute ethyl alcohol is 95 ~ 99:1 ~ 5, then by air inlet pipe, fluid reservoir is pressurizeed, force mixed solution in fluid reservoir slowly through the dibydro myricetrin meal in tank body, and flow out from liquid outlet, until the mixed solution that liquid outlet flows out is colourless,
Step 8 and then inject the ethanolic solution of 1 ~ 5%V/V to fluid reservoir by inlet, then by air inlet pipe, fluid reservoir is pressurizeed, force ethanolic solution in fluid reservoir slowly through the dibydro myricetrin meal in tank body, and flow out from liquid outlet, until the ethanolic solution that liquid outlet flows out is faint yellow or colourless, then collect the dibydro myricetrin powder in tank body.
the present invention compared with prior art, has the following advantages and effect:
1, energy utilization rate is enhanced about more than once by the present invention, greatly reduces costs.
2, the present invention extracts dibydro myricetrin and polysaccharide, efficiently purifying, and solvent consumption is few, simple to operate with low cost.
3, skill water circulation use of the present invention, not blowdown.
Accompanying drawing explanation
Fig. 1 extracts the device schematic diagram of dibydro myricetrin and vine tea polysaccharide.
In figure: 0-material; 1-tank body; 2-cover; 3-liquid outlet; 4-fluid valve; 5-air inlet pipe; 6-filter plate; 7-air intake valve; 8-fluid reservoir; 9-steam inlet; 10-inlet; 11-inlet valve; 12-air inlet pipe valve; 13-vapour-liquid pipeline; 14-fluid pipeline; 15-sieve plate.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, invention is further described.
Embodiment 1:
The device of dibydro myricetrin and polysaccharide is extracted from vine tea leftover bits and pieces, comprise tank body 1, tank body 1 is provided with cover 2, top in tank body 1 is provided with filter plate 6, the bottom of tank body 1 is provided with the sieve plate 15 for placing material 0, tank body 1 sidewall is provided with the liquid outlet 3 be positioned at above filter plate 6, fluid pipeline 14 is provided with bottom tank body 1, also be communicated with the bottom of fluid reservoir 8 by vapour-liquid pipeline bottom tank body 1, the top of fluid reservoir 8 is provided with inlet 10, fluid reservoir 8 is also provided with one end and extends to air inlet pipe 5 bottom fluid reservoir 8.
Inlet 10 is provided with inlet valve 11; Air inlet pipe 5 is provided with air inlet pipe valve 12; Vapour-liquid pipeline 13 is provided with air intake valve 7; Fluid pipeline 14 is provided with fluid valve 4.
From vine tea leftover bits and pieces, extract the method for dibydro myricetrin and polysaccharide, comprise the following steps:
Step 1, using vine tea leftover bits and pieces pulverize as material 0, be then encased in tank body 1, cover cover 2;
Step 2, Boiler Steam outlet to be connected with air inlet pipe 5, the high-temperature vapor of 100 degrees Celsius slow transits through air inlet pipe 5, fluid reservoir 8 and vapour-liquid pipeline 13 and enters in tank body 1, the heating of infiltration limit, limit is carried out, until soaked into by whole material 0 and material 0 is heated to 85 degrees Celsius to the material 0 in this tank body 1;
Step 3, continue the high-temperature water vapor passing into 100 degrees Celsius to air inlet pipe 5, the aqueous solution in material slowly flows out from liquid outlet 3 through filter plate 6, collects the aqueous solution flowed out;
Step 4, the aqueous solution that liquid outlet 3 flows out is injected in sedimentation basin, naturally cools precipitation;
The supernatant liquor of step 5, extraction sedimentation basin, fluid reservoir 8 is injected into from inlet 10, heated by the high-temperature water vapor entering fluid reservoir, then enter in tank body 1 under the high-temperature water vapor pressure effect of steam boiler, material 0 in tank body 1 is extracted again, return step 4, iterative cycles like this extracts 3 times;
Step 6, sedimentation basin extracted the precipitation after supernatant liquor and takes out to dry and pulverize, use 80%(mass percent) alcoholic extraction, filtration, the residue leached is dried and is pulverized, and is Thick many candies; Dibydro myricetrin crude product is obtained to after alcoholic extract recovered alcohol;
Step 7, take out the material in tank body 1, by dibydro myricetrin crude product drying and crushing, then be encased in tank body 1, then mixed solution is injected by inlet 10 to fluid reservoir 8, this mixed solution consists of absolute ethyl alcohol and benzinum, the boiling range of benzinum is 30 degrees Celsius, the volume parts of benzinum: the volume parts of absolute ethyl alcohol is 95:5, then pressurizeed by air inlet pipe 5 pairs of fluid reservoirs 8, force mixed solution in fluid reservoir 8 slowly through the dibydro myricetrin meal in tank body 1, and flow out from liquid outlet 3, until the mixed solution that liquid outlet 3 flows out is colourless,
Step 8 and then injected the ethanolic solution of 1%V/V by inlet 10 to fluid reservoir 8, then pressurizeed by air inlet pipe 5 pairs of fluid reservoirs 8, force ethanolic solution in fluid reservoir 8 slowly through the dibydro myricetrin meal in tank body 1, and flow out from liquid outlet 3, until the ethanolic solution that liquid outlet 3 flows out is faint yellow or colourless, then collect the dibydro myricetrin powder in tank body 1, purity can reach more than 98%.
embodiment 2:
The device of dibydro myricetrin and polysaccharide is extracted from vine tea leftover bits and pieces, comprise tank body 1, tank body 1 is provided with cover 2, top in tank body 1 is provided with filter plate 6, the bottom of tank body 1 is provided with the sieve plate 15 for placing material 0, tank body 1 sidewall is provided with the liquid outlet 3 be positioned at above filter plate 6, fluid pipeline 14 is provided with bottom tank body 1, also be communicated with the bottom of fluid reservoir 8 by vapour-liquid pipeline bottom tank body 1, the top of fluid reservoir 8 is provided with inlet 10, fluid reservoir 8 is also provided with one end and extends to air inlet pipe 5 bottom fluid reservoir 8.
Inlet 10) be provided with inlet valve 11; Air inlet pipe 5 is provided with air inlet pipe valve 12; Vapour-liquid pipeline 13 is provided with air intake valve 7; Fluid pipeline 14 is provided with fluid valve 4.
From vine tea leftover bits and pieces, extract the method for dibydro myricetrin and polysaccharide, comprise the following steps:
Step 1, using vine tea leftover bits and pieces pulverize as material 0, be then encased in tank body 1, cover cover 2;
Step 2, Boiler Steam outlet to be connected with air inlet pipe 5, the high-temperature vapor of 300 degrees Celsius slow transits through air inlet pipe 5, fluid reservoir 8 and vapour-liquid pipeline 13 and enters in tank body 1, the heating of infiltration limit, limit is carried out, until soaked into by whole material 0 and material 0 is heated to 95 degrees Celsius to the material 0 in this tank body 1;
Step 3, continue the high-temperature water vapor passing into 300 degrees Celsius to air inlet pipe 5, the aqueous solution in material slowly flows out from liquid outlet 3 through filter plate 6, collects the aqueous solution flowed out;
Step 4, the aqueous solution that liquid outlet 3 flows out is injected in sedimentation basin, naturally cools precipitation;
The supernatant liquor of step 5, extraction sedimentation basin, fluid reservoir 8 is injected into from inlet 10, heated by the high-temperature water vapor entering fluid reservoir, then enter in tank body 1 under the high-temperature water vapor pressure effect of steam boiler, material 0 in tank body 1 is extracted again, return step 4, iterative cycles like this extracts 5 times;
Step 6, sedimentation basin extracted the precipitation after supernatant liquor and take out to dry and pulverize, extract with 100% alcohol (absolute ethyl alcohol), filter, the residue leached dries pulverizing, is Thick many candies; Dibydro myricetrin crude product is obtained to after alcoholic extract recovered alcohol;
Step 7, take out the material in tank body 1, by dibydro myricetrin crude product drying and crushing, then be encased in tank body 1, then mixed solution is injected by inlet 10 to fluid reservoir 8, this mixed solution consists of absolute ethyl alcohol and benzinum, the boiling range of benzinum is 90 degrees Celsius, the volume parts of benzinum: the volume parts of absolute ethyl alcohol is 99:1, then pressurizeed by air inlet pipe 5 pairs of fluid reservoirs 8, force mixed solution in fluid reservoir 8 slowly through the dibydro myricetrin meal in tank body 1, and flow out from liquid outlet 3, until the mixed solution that liquid outlet 3 flows out is colourless,
Step 8 and then injected the ethanolic solution of 5%V/V by inlet 10 to fluid reservoir 8, then pressurizeed by air inlet pipe 5 pairs of fluid reservoirs 8, force ethanolic solution in fluid reservoir 8 slowly through the dibydro myricetrin meal in tank body 1, and flow out from liquid outlet 3, until the ethanolic solution that liquid outlet 3 flows out is faint yellow or colourless, then collect the dibydro myricetrin powder in tank body 1, purity can reach more than 99.5%.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Claims (3)
1. from vine tea leftover bits and pieces, extract the device of dibydro myricetrin and polysaccharide, comprise tank body (1), it is characterized in that, tank body (1) is provided with cover (2), top in tank body (1) is provided with filter plate (6), the bottom of tank body (1) is provided with the sieve plate (15) for placing material (0), tank body (1) sidewall is provided with the liquid outlet (3) being positioned at filter plate (6) top, tank body (1) bottom is provided with fluid pipeline (14), tank body (1) bottom is also communicated with the bottom of fluid reservoir (8) by vapour-liquid pipeline (13), the top of fluid reservoir (8) is provided with inlet (10), fluid reservoir (8) is also provided with the air inlet pipe (5) that one end extends to fluid reservoir (8) bottom.
2. the device extracting dibydro myricetrin and polysaccharide from vine tea leftover bits and pieces as requested described in 1, is characterized in that: inlet (10) is provided with inlet valve (11); Air inlet pipe (5) is provided with air inlet pipe valve (12); Vapour-liquid pipeline (13) is provided with air intake valve (7); Fluid pipeline (14) is provided with fluid valve (4).
3. the device as requested described in 2 carries out the method extracting dibydro myricetrin and polysaccharide from vine tea leftover bits and pieces, it is characterized in that, comprises the following steps:
Step 1, using vine tea leftover bits and pieces pulverize as material (0), be then encased in tank body (1), cover cover (2);
Step 2, Boiler Steam outlet to be connected with air inlet pipe (5), the high-temperature vapor of 100 ~ 300 degrees Celsius slow transits through air inlet pipe (5), fluid reservoir (8) and vapour-liquid pipeline (13) and enters in tank body (1), the heating of infiltration limit, limit is carried out, until soaked into by whole material (0) and material (0) is heated to 85 ~ 95 degrees Celsius to the material (0) in this tank body (1);
Step 3, continue the high-temperature water vapor passing into 100 ~ 300 degrees Celsius to air inlet pipe (5), the aqueous solution in material slowly flows out from liquid outlet (3) through filter plate (6), collects the aqueous solution flowed out;
Step 4, the aqueous solution that liquid outlet (3) flows out is injected in sedimentation basin, naturally cools precipitation;
The supernatant liquor of step 5, extraction sedimentation basin, fluid reservoir (8) is injected into from inlet (10), heated by the high-temperature water vapor entering fluid reservoir, then enter in tank body (1) under the high-temperature water vapor pressure effect of steam boiler, material (0) in tank body (1) is extracted again, return step 4, iterative cycles like this extracts 3 ~ 5 times;
Step 6, sedimentation basin extracted the precipitation after supernatant liquor and take out to dry and pulverize, with 80 ~ 100% alcoholic extractions, filtration, the residue leached dries pulverizing, is Thick many candies; Dibydro myricetrin crude product is obtained to after alcoholic extract recovered alcohol;
Step 7, take out the material in tank body (1), by dibydro myricetrin crude product drying and crushing, then be encased in tank body (1), then mixed solution is injected by inlet (10) to fluid reservoir (8), this mixed solution consists of absolute ethyl alcohol and benzinum, the boiling range of benzinum is 30 ~ 90 degrees Celsius, the volume parts of benzinum: the volume parts of absolute ethyl alcohol is 95 ~ 99:1 ~ 5, then by air inlet pipe (5), fluid reservoir (8) is pressurizeed, force mixed solution in fluid reservoir (8) slowly through the dibydro myricetrin meal in tank body (1), and flow out from liquid outlet (3), until the mixed solution that liquid outlet (3) flows out is colourless,
Step 8 and then inject the ethanolic solution of 1 ~ 5%V/V to fluid reservoir (8) by inlet (10), then by air inlet pipe (5), fluid reservoir (8) is pressurizeed, force ethanolic solution in fluid reservoir (8) slowly through the dibydro myricetrin meal in tank body (1), and flow out from liquid outlet (3), until the ethanolic solution that liquid outlet (3) flows out is faint yellow or colourless, then collect the dibydro myricetrin powder in tank body (1).
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| CN109011680A (en) * | 2017-06-11 | 2018-12-18 | 吴浪 | The efficiently purifying device of one Plant Extracts and the method for purifying plant extracts |
| CN111821720A (en) * | 2020-09-05 | 2020-10-27 | 广州鑫泽化工科技有限公司 | Preparation and processing technology of natural plant essence extract |
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Effective date of registration: 20171106 Address after: 445700 Hubei Province, Enshi Tujia and Miao Autonomous Prefecture of osmanthus tree Laifeng County Economic Development Zone Industrial Park Applicant after: LAIFENG JINQI VINE TEA BIOLOGY Co.,Ltd. Address before: 445000 Xueyuan Road, Enshi Tujia and Miao Autonomous Prefecture, Hubei, China, No. 39 Applicant before: Hubei Institute for Nationalities |
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Effective date of registration: 20220817 Address after: Building 8, Industrial Park, Guihuashu Economic Development Zone, Xiangfeng Town, Laifeng County, Enshi Tujia and Miao Autonomous Prefecture, Hubei Province 445700 Patentee after: Laifeng jinqiteng tea agricultural development Co.,Ltd. Address before: 445700 guihuashu Industrial Park, Laifeng Economic Development Zone, Enshi Tujia and Miao Autonomous Prefecture, Hubei Province Patentee before: LAIFENG JINQI VINE TEA BIOLOGY Co.,Ltd. |
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| CP01 | Change in the name or title of a patent holder |
Address after: Building 8, Industrial Park, Guihuashu Economic Development Zone, Xiangfeng Town, Laifeng County, Enshi Tujia and Miao Autonomous Prefecture, Hubei Province 445700 Patentee after: Hubei Jinrui Biotechnology Co.,Ltd. Address before: Building 8, Industrial Park, Guihuashu Economic Development Zone, Xiangfeng Town, Laifeng County, Enshi Tujia and Miao Autonomous Prefecture, Hubei Province 445700 Patentee before: Laifeng jinqiteng tea agricultural development Co.,Ltd. |