CN1398604A - Technological process and plant for extracting effective component from fine animal and plant powder - Google Patents
Technological process and plant for extracting effective component from fine animal and plant powder Download PDFInfo
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- CN1398604A CN1398604A CN 01123488 CN01123488A CN1398604A CN 1398604 A CN1398604 A CN 1398604A CN 01123488 CN01123488 CN 01123488 CN 01123488 A CN01123488 A CN 01123488A CN 1398604 A CN1398604 A CN 1398604A
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Abstract
In the present invention the extraction process is making the coarse material powder pass the following units successively; crushing unit; stage I extracting unit; stage II extracting unit comprising two stages of slurry mixing tank, extractor and solid-liquid separator; and liquid returning unit to return partial extracting liquid from the stage II extracting unit to the front one. More stages extracting units can be set.
Description
Technology and device that the active ingredient of a kind of animals and plants micropowder of the present invention is extracted belong to animals and plants micropowder active ingredient extractive technique.
When animals and plants are used as medicine and health product,, often adopt extraction process, its active ingredient is extracted in order to reduce dose.In extracting method, the most frequently used is lixiviate, even solvent such as water, ethanol, through soaking, hot digestion dissolves in the solvent active ingredient in the animals and plants, again through solid-liquid separation, as adopt methods such as filtration, filter pressing, sedimentation that recrement is removed, again to extracting solution take purification, concentrate, processing such as drying finally obtains concentrated extracting solution or dry extract.The time-consuming length of this leach extraction method is extracted temperature height (80 ℃-100 ℃), uses the solvent amount big, also must use expensive solvent under many situations, as: ethanol.Thereby make extraction efficiency low, the cost height destroys the thermal sensitivity active ingredient.Particularly, make the composition of proposition not thorough, incomplete, cause the waste of resource because this method makes active ingredient move to the interior out from animal and plant body by the concentration difference diffusion principle.Specify as follows:
In this conventional extracting technology, the animal and plant body that enters leaching process is a former material or through the granule of coarse crushing.The cell overwhelming majority of animal and plant body is complete, and becomes the cluster shape to exist.Must at first material be soaked (heating, the pressurization of still needing sometimes) during extraction in solvent solvent is entered in the animal and plant body, in cell, solvent is dissolved in active ingredient.At this moment intracellular active ingredient concentration is greater than extracellular active ingredient concentration.Set up the condition of active ingredient to the diffusion of extracellular solvent.Diffusion is from the granule okioplast, carrying out along with diffusion motion, components and concentration in the okioplast reduces gradually, form concentration difference with the concentration of composition in the interior confluent monolayer cells, the intercellular composition diffusion of ectonexine begins thereupon, and active ingredient enters the outer solvent of born of the same parents must pass through a cell wall or film (okioplast) or several cell wall (film) even tens of, up to a hundred cell wall (film).The macromole composition is subjected to the influence of cell wall (film) penetrance may may not arrive the outer solvent of born of the same parents, for the micromolecule composition, passes through cell wall (film) and also will be subjected to drag effect, and the cell wall that passes (film) the more resistance is bigger.Be to have diffusional resistance inside and outside the cell, also there is diffusional resistance in iuntercellular.The existence of this resistance must influence composition moving out in the animal and plant body, makes the one-tenth deal of extraction not thorough, and kind is incomplete.
For overcoming the shortcoming that the said extracted method exists, purpose of the present invention is for providing a kind of " animals and plants micropowder active ingredient extraction process and device ", reach and remove the resistance of intact cell wall (film) the composition stripping, with raising composition extraction ratio, and the purpose of realization suitability for industrialized production.
Technology and device that the active ingredient of a kind of animals and plants micropowder of the present invention is extracted, its technological process is as follows:
(1), the coarse powder raw material enters the pulverizing unit: the raw material coarse powder is crushed to the cell breakage level;
(2), I level extraction unit: first extraction unit enters this extraction unit by pulverizing the animals and plants micropowder that comes out the unit; By two-stage size mixing jar, extraction element and equipment for separating liquid from solid form;
(3), II level extraction unit: the second extraction unit also adds inlet for solvent; By two-stage size mixing jar, extraction element and equipment for separating liquid from solid form;
(4), return liquid device: the extracting solution ratio that II level extraction unit is discharged returns to the prime extraction unit;
Extraction unit optionally can be arranged to multistage; As adding III, IV again ... level.Its method of attachment and I, the connection between II level extraction element is identical.
Technology and device that the active ingredient of a kind of animals and plants micropowder of the present invention is extracted, the composition and the workflow of its device are as follows:
With sending into pulverizing mill after the coarse crushing of animals and plants material, material is crushed to the cell breakage level by pulverizing mill; Micropowder behind the cell breakage is sent into jar I that sizes mixing, add rework solution and solvent, the adjusting solid-liquid ratio reaches to give decides level, to adapt to the requirement of extraction element (micropowder extractor I), the serosity that mixes up is delivered to extraction element (micropowder extractor I) and is extracted operation, extract and after operation is finished slip is sent into jar I ' that sizes mixing, add rework solution and solvent, requirement by the later separation operation transfers to suitable solid-liquid ratio with slip, after adjusting solid-liquid ratio, feed liquid enters equipment for separating liquid from solid (centrifugal sedimentation seperator I), carries out the feed liquid detached job under certain separation factor; Isolated liquid is the product that this technological process will be obtained.Send into jar II that sizes mixing by the isolated solid material of equipment for separating liquid from solid (centrifugal sedimentation seperator I) and add solvent adjustment slurry ratio simultaneously, to adapt to the requirement of subsequent extracted device (micropowder extractor); The slip that mixes up is sent into extraction element (micropowder extractor II) and is extracted operation once more, after operation is finished slip is sent into jar II ' that sizes mixing, and adds solvent simultaneously, adjusts pulp density, to adapt to the needs of equipment for separating liquid from solid (centrifugal sedimentation seperator); The slip that mixes up is sent into equipment for separating liquid from solid (centrifugal sedimentation seperator II), feed liquid is separated, recrement after the separation is pending, and the surplus liquid after the separation is through rework solution connecting line and rework solution control distributing valve, and ratio is on demand sent into size mixing jar I and jar I ' that sizes mixing;
Extraction unit optionally can be arranged to multistage; As adding III, IV again ... level.Its method of attachment and I, the connection between II level extraction element is identical.
Technology and device that the active ingredient of a kind of animals and plants micropowder of the present invention is extracted, its topmost characteristics and advantage are:
Entering the animals and plants of extracting operation has reached or be crushed to cytoclastic level in leaching process.This moment, cellular content directly was exposed in the solvent, did not exist because of there is the diffusional resistance that forms in cell wall (multilamellar or monolayer).The micropowder extractor that adopts is in the intensive relative ballistic movement material and solvent, thereby active ingredient is eluted rapidly from animal vegetable tissue, when particularly adopting the dynamic extraction machine, the liquid material is fully stirred, when making feed liquid be in intensive relative ballistic movement, material is also by intensive forward extrusion and tangential the shearing, extruding force forces the active ingredient of granule interior, extrude with solvent, shearing force is quickened active ingredient and is eluted from particle surface, a material is ground into littler granule again at the same time, has more quickened active ingredient and has extruded process with eluting.
Extract operation and adopted sedimentation-separation technology, the melt cinder of extraction is separated into may and reaches optimum efficiency.
Take secondary extraction or more multistage method to make extraction more thorough more complete, have more following advantages:
1, extraction ratio height of the present invention: as puerarin, its coarse powder extraction ratio is 1.53%, and the fine powder extraction ratio is respectively 2.46% (10 ℃) 3.04% (40 ℃)
2, the extraction temperature is low: as puerarin, its coarse powder room temperature-100 ℃ fine powder is 10 ℃-100 ℃
3, accumulation solvent consumption is few: as puerarin, its coarse powder is 1300ml for the 2600ml fine powder
4, extraction group number is few: as puerarin, and 3 fine powders of its coarse powder 2 times
5, extraction time is short: as puerarin, and 1-2h/ total time 3-6 of its coarse powder hour
Fine powder 5 minutes for the first time 3 minutes for the second time amounts to 8 minutes
6, solvent is required to reduce: as puerarin, 10 ℃ of fine powder extraction rate reached 91.5% of its ethanol; Water is carried 40 ℃ of fine powder extraction ratios can reach 95%; Water carry 40 ℃ better than 10 ℃ of effects of alcohol extraction.
The present invention has following accompanying drawing:
Fig. 1 process chart of the present invention.
Technology that Fig. 2 active ingredient of the present invention is extracted and device sketch map.
Technology that the active ingredient of Fig. 3 another embodiment of the present invention is extracted and device sketch map.
Number in the figure is as follows:
1 pulverizes unit 2 I level extraction units, 3 II level extraction units
4 return liquid device 5 pulverizing mills 6,16 size mixing jar (a jar I sizes mixing)
7,17 extraction elements (micropowder extractor I) 8,18 size mixing jar (a jar I ' sizes mixing)
9,19 equipment for separating liquid from solid (centrifugal sedimentation seperator I)
10,20 size mixing jar (a jar II sizes mixing) 11,21 extraction elements (micropowder extractor II)
12,22 size mixing jar (a jar II ' sizes mixing)
13 equipment for separating liquid from solid (centrifugal sedimentation seperator II), 14 rework solutions control distributing valve, 15 rework solution connecting lines
23 coarse powder, 24 solvents, 25 products, 26 slags
Now be described in detail as follows for embodiment and conjunction with figs.:
Technology and device that the active ingredient of a kind of animals and plants micropowder of the present invention is extracted see also Fig. 1, shown in Figure 2, and whole process flow is made of 4 parts:
(1), raw material coarse powder 23 enters and pulverize unit 1: its equipment that uses is ground into fine powder as pulverizing mill 5 (as select the patent No. for use be 95234942.6 pulverizing mill) with raw material coarse powder 23, is crushed to the cell breakage level, is generally 200 order to 300 orders;
(2), I level extraction unit 2: first extraction unit, the animals and plants micropowder adds inlet, also is provided with solvent and returns liquid to add inlet, sizes mixing jars 6,8 by two-stage, extraction element 7 (micropowder extractor I) and equipment for separating liquid from solid 9 (centrifugal sedimentation seperator I) composition;
(3), II level extraction unit 3: secondary extraction unit 3, be provided with solvent 24 and rework solution and add inlet, size mixing jars 10,12 by two-stage, extraction element 11 (micropowder extractor II) and equipment for separating liquid from solid 13 (centrifugal sedimentation seperator II) composition;
(4), return liquid device 4: the extracting solution (being rework solution) that II level extraction unit 3 is discharged returns to the prime extraction unit in proportion;
Specifically, its technical process is: enter pulverizing unit 1-material after 23 coarse crushings of raw material coarse powder and be crushed to cell grade micropowder level, it is the cell wall breaking level, sporoderm-broken rate is generally greater than 80-95%, powder fineness according to different cell controlled amount built in 100 orders, 200 orders, fineness levels such as 300 orders, material after the cell grade micropowder is broken is sent into I level extraction unit 2, meanwhile extraction solvent 24 (is selected according to different materials, water, ethanol, water, the alcohol blend solvent) also enters I level extraction unit 2, also enter simultaneously through returning the final stage extracting solution (rework solution) that liquid device 4 returns, carry out extracting operation for the I time, this unitary equipment for separating liquid from solid 9 was with liquid after operation was finished, solid separates, and liquid is discharged as product 25, solid slag 26 is sent into II level extraction unit 3, meanwhile, solvent 24 adds simultaneously, carries out second extraction; After operation was finished, the equipment for separating liquid from solid 13 in the II level extraction unit 3 separated the solid, liquid body, and the foldback after returning liquid device 4 distribution of the liquid after the separation returns the I except that the final stage extraction unit, II ... the level extraction unit; Solid slag 26 after the separation is discharged as waste residue.Extraction unit optionally can be arranged to multistage; As adding III, IV again ... level.Its method of attachment and I, the connection between II level extraction element is identical.
Be described as follows for embodiment 1 according to above-mentioned technological process coupling apparatus: see shown in Figure 2;
Also can take embodiment illustrated in fig. 32 methods that show in the enforcement, be that extraction element can be selected dynamic extraction machine (being that application number that the inventor invents is 01215813.5 dynamic extraction machine) for use, broken two combine into one with vibration extraction with the material micropowder for this dynamic extraction function, carries out simultaneously.Extraction element 17 in embodiment illustrated in fig. 32 adopts the dynamic extraction machine, and removes the pulverizing mill 5 in embodiment illustrated in fig. 21, and coarse powder 23 is directly added jar 16 (shown in Figure 3) of sizing mixing, the same example I of all the other technological processes.
Made the Chinese medicine puerarin according to foregoing invention and extracted the contrast experiment, situation is as follows.
Radix Puerariae sample 50% ethanol extraction effect relatively
Sample 1: get coarse powder 100g, with 50% ethanol 80-90 ℃ reflux, extract, 1h, totally three times, quantity of solvent is 800ml for the first time, and the 2nd, 3 each 500ml filters, and filtrate merges.
Sample 2: get superfine powder 100g,, in the Baily extractor, extract 5min with 50% ethanol 800ml, centrifugalize (20000rpm) 15min, residue carries out second extraction 3min, adds water 500ml, centrifugalize (20000rpm) 15min, filtrate merges.
Get each sample filtrate, content of puerarin is measured with reference to the Wang Baoqin chief editor, Chinese medicine medical sci-tech publishing house, " Chinese patent medicine quality standard and standard substance research " the 314th page, tlc scanning determination.The results are shown in Table 1:
Table 1 Radix Puerariae sample 50% ethanol extraction effect
| Sample | Medical material puerarin content (%) | Puerarin yield (%) | Puerarin extraction ratio (%) | Accumulative total solvent total amount (ml) | Extraction time (min) | Extraction time | The extraction temperature (℃) |
| Sample 1 | ????3.2 | ????2.32 | ????72.5 | ????1800 | ??180 | ??3 | ??80-90 |
| | ????3.2 | ????2.93 | ????91.5 | ????1300 | ??8 | ??2 | ??10 |
Radix Puerariae sample water leaching effect
Sample 1: get coarse powder 100g, decoct with water and extract 2h, totally 3 times, the 1st amount of water 1000ml respectively adds water 800ml the 2nd, 3 time, and immersion merges and filters.
Sample 2: get superfine powder 100g, add 10 ℃ water 800ml, in the Baily extractor, extract 5min, centrifugalize (20000rpm) 15min, residue carries out second extraction 3min, adds water 500ml, centrifugalize (20000rpm) 15min, filtrate merges.
Sample 3: get superfine powder 100g, add 40 ℃ water 800ml, in the Baily extractor, extract 5min, centrifugalize (20000rpm) 15min, residue carries out second extraction 3min, adds water 500ml, centrifugalize (20000rpm) 15min, filtrate merges.
Get each sample filtrate, content of puerarin is measured with reference to the Wang Baoqin chief editor, Chinese medicine medical sci-tech publishing house, " Chinese patent medicine quality standard and standard substance research " the 314th page.Tlc scanning determination the results are shown in Table 2:
Table 2 Radix Puerariae sample water extraction effect
| Sample | Medical material puerarin content (%) | Puerarin yield (%) | Puerarin extraction ratio (%) | Accumulative total solvent total amount (ml) | Extraction time (min) | Extraction time | The extraction temperature (℃) |
| Sample 1 | ????3.2 | ????1.53 | ????47.8 | ????2600 | ???360 | ????3 | ??90-100 |
| | ????3.2 | ????2.46 | ????77 | ????1300 | ???8 | ????2 | ??10 |
| | ????3.2 | ????3.04 | ????95 | ????1300 | ???8 | ????2 | ??40 |
Claims (2)
1, a kind of technology and device of animals and plants micropowder active ingredient extraction, it is characterized in that: the step of its technological process is as follows:
(1), the coarse powder raw material enters the pulverizing unit: the raw material coarse powder is crushed to the cell breakage level;
(2), I level extraction unit: first extraction unit enters this extraction unit by pulverizing the animals and plants micropowder that comes out the unit; By two-stage size mixing jar, extraction element and equipment for separating liquid from solid form;
(3), II level extraction unit: the second extraction unit also adds inlet for solvent; By two-stage size mixing jar, extraction element and equipment for separating liquid from solid form;
(4), return liquid device: the extracting solution ratio that II level extraction unit is discharged returns to the prime extraction unit;
Extraction unit optionally can be arranged to multistage; As adding III, IV again ... level.Its method of attachment and I, the connection between II level extraction element is identical.
2, a kind of technology and device of animals and plants micropowder active ingredient extraction, it is characterized in that: the composition and the work process of this device are as follows:
With sending into pulverizing mill after the coarse crushing of animals and plants material, material is crushed to the cell breakage level by pulverizing mill; Micropowder behind the cell breakage is sent into jar I that sizes mixing, add rework solution and solvent, the adjusting solid-liquid ratio reaches to give decides level, to adapt to the requirement that extraction element is micropowder extractor I, it is that micropowder extractor I extracts operation that the serosity that mixes up is delivered to extraction element, extract and after operation is finished slip is sent into jar I ' that sizes mixing, add rework solution and solvent, requirement by the later separation operation transfers to suitable solid-liquid ratio with slip, after adjusting solid-liquid ratio, it is centrifugal sedimentation seperator I that feed liquid enters equipment for separating liquid from solid, carries out the feed liquid detached job under certain separation factor; Isolated liquid is the product that this technological process will be obtained.By equipment for separating liquid from solid is that the isolated solid material of centrifugal sedimentation seperator I is sent into jar II that sizes mixing and added solvent simultaneously and adjust the slurry ratio, to adapt to the requirement that the subsequent extracted device is the micropowder extractor; It is that micropowder extractor II extracts operation once more that the slip that mixes up is sent into extraction element, after operation is finished slip is sent into jar II ' that sizes mixing, and adds solvent simultaneously, adjusts pulp density, to adapt to the needs that equipment for separating liquid from solid is the centrifugal sedimentation seperator; It is centrifugal sedimentation seperator II that the slip that mixes up is sent into equipment for separating liquid from solid, feed liquid is separated, recrement after the separation is pending, and the surplus liquid after the separation is through rework solution connecting line and rework solution control distributing valve, and ratio is on demand sent into size mixing jar I and jar I ' that sizes mixing;
Extraction unit optionally can be arranged to multistage; As adding III, IV again ... level, its method of attachment and I, the connection between II level extraction element is identical.
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| CN 01123488 CN1284614C (en) | 2001-07-27 | 2001-07-27 | Technological process and plant for extracting effective component from fine animal and plant powder |
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| CN 01123488 CN1284614C (en) | 2001-07-27 | 2001-07-27 | Technological process and plant for extracting effective component from fine animal and plant powder |
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| CN1284614C CN1284614C (en) | 2006-11-15 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108211511A (en) * | 2018-02-05 | 2018-06-29 | 横县东糖糖业有限公司 | The centrifugal filtration automatic control system of cane sugar factory mud juice |
| CN108295554A (en) * | 2018-02-05 | 2018-07-20 | 横县东糖糖业有限公司 | A kind of centrifugal filtration system of cane sugar factory mud juice |
| CN110215734A (en) * | 2019-06-17 | 2019-09-10 | 安徽紫山农业科技有限公司 | A kind of extract equipment and its extracting method of biological medicine |
| CN110732159A (en) * | 2019-11-05 | 2020-01-31 | 大连大学 | continuous grading type high-efficiency extraction device |
| CN111093791A (en) * | 2017-08-08 | 2020-05-01 | 库尔特瓦特股份有限公司 | System and method for continuous stirred tank solvent extraction using feed |
| US11230613B2 (en) | 2017-08-08 | 2022-01-25 | Kultevat, Inc. | Rubber and by-product extraction systems and methods |
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2001
- 2001-07-27 CN CN 01123488 patent/CN1284614C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111093791A (en) * | 2017-08-08 | 2020-05-01 | 库尔特瓦特股份有限公司 | System and method for continuous stirred tank solvent extraction using feed |
| US11230613B2 (en) | 2017-08-08 | 2022-01-25 | Kultevat, Inc. | Rubber and by-product extraction systems and methods |
| CN111093791B (en) * | 2017-08-08 | 2022-04-01 | 库尔特瓦特股份有限公司 | System and method for continuous stirred tank solvent extraction using feed |
| US11566086B2 (en) | 2017-08-08 | 2023-01-31 | Kultevat, Inc. | Rubber and by-product extraction systems and methods |
| US11565195B2 (en) | 2017-08-08 | 2023-01-31 | Kultevat, Inc. | System and method for continuous stirred tank solvent extraction using feedstock |
| US11833448B2 (en) | 2017-08-08 | 2023-12-05 | Kultevat, Inc. | System and method for continuous stirred tank solvent extraction using feedstock |
| CN108211511A (en) * | 2018-02-05 | 2018-06-29 | 横县东糖糖业有限公司 | The centrifugal filtration automatic control system of cane sugar factory mud juice |
| CN108295554A (en) * | 2018-02-05 | 2018-07-20 | 横县东糖糖业有限公司 | A kind of centrifugal filtration system of cane sugar factory mud juice |
| CN108295554B (en) * | 2018-02-05 | 2020-09-22 | 横县东糖糖业有限公司 | Centrifugal filtration system of cane sugar factory mud juice |
| CN110215734A (en) * | 2019-06-17 | 2019-09-10 | 安徽紫山农业科技有限公司 | A kind of extract equipment and its extracting method of biological medicine |
| CN110215734B (en) * | 2019-06-17 | 2021-11-23 | 安徽紫山农业科技有限公司 | Extraction equipment and extraction method of biological medicine |
| CN110732159A (en) * | 2019-11-05 | 2020-01-31 | 大连大学 | continuous grading type high-efficiency extraction device |
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