CN104784970B - Chiral chromatogram filler applying device and method - Google Patents
Chiral chromatogram filler applying device and method Download PDFInfo
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- CN104784970B CN104784970B CN201510196885.1A CN201510196885A CN104784970B CN 104784970 B CN104784970 B CN 104784970B CN 201510196885 A CN201510196885 A CN 201510196885A CN 104784970 B CN104784970 B CN 104784970B
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- heating roller
- chiral chromatogram
- scraping blade
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- material mouth
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Abstract
The invention discloses a kind of chiral chromatogram filler applying device and method, including homogenate bucket, stirring paddle, crowded material mouth, coating scraping blade, heat roller, rewinding scraping blade；Being provided with the stirring paddle for being stirred by filler in homogenate bucket, the bottom of homogenate bucket offers crowded material mouth, and heating roller is arranged on below crowded material mouth；Coating scraping blade it is connected with, for making the packing layer thickness on heating roller uniform at crowded material mouth；Also include rewinding scraping blade, for the packing layer being dried on heating roller is scraped collection.Product prepared by chiral chromatogram filler applying device of the present invention and method, output capacity is higher, and separating degree is more preferable, and good product quality reduces production cost simultaneously；Solve existing in the case of containing substantial amounts of solvent and painting dressing, be dried the uneven caking phenomenon caused with agglomerating force, rapidly and efficiently can produce continuously, improve work efficiency.
Description
Technical field
The present invention relates to a kind of chiral chromatogram filler applying device, belong to the filling automatic control technology field of chromatographic column.
Background technology
Business-like chiral chromatogram filler is divided into two kinds according to mode of production difference: coating-type and bonding type.Coating-type hands
The production of property chromatograph packing material is to be dissolved by solvent by many carbohydrates and their derivative with chiral recognition, by polysaccharide and spread out
Biology is coated in the method on silica gel uniformly.Method known to present stage is to be added dropwise in silica gel by coating liquid, along with stirring
Mix, coating liquid is uniformly mixed with silica gel, more slowly solvent is evaporated by the way of heating in vacuum, it is thus achieved that be dried and can load
Filler.Also have been reported that the method acquisition coating-type filler separating out crystallization with solution, but be rarely used in batch production, more have no special
The report used with device.Both the above mode has two big drawbacks:
(1) production efficiency ratio is relatively low: the quantity of primary coating and the size of hermetic container have direct relation, tens kilograms
Above coating produces, and needs the hermetic container of significant volume, and it is long slowly to steam solvent time, is dried the most thorough.
(2) the coating quality of production and productivity are low: because not having special equipment, and the conventional chemosynthesis equipment of single dependence is raw
Producing, concordance is low, often has caking and applies uneven situation generation.
The generation of case above, is primarily due to the filler particles selected by chiral chromatogram filler the least, mostly be 3 μm, 5
μm, 10 μm, 20 μm, many carbohydrates and their derivative absorption affinity itself with chiral Recognition is very strong, and silica gel mixes with the coating liquid of thickness
After conjunction, being difficult to not reunite, even if not stopping stirring, dried some presents powdery, and major part all becomes
Bulk, even needs external force to disperse, and after such filler dress post, separating power is low, and single chiral medicine is presented as post heterodyne.
Summary of the invention
Purpose: in order to overcome the deficiencies in the prior art, solves containing substantial amounts of solvent and the situation of painting dressing
Under, it being dried the uneven caking phenomenon caused with agglomerating force, the present invention provides a kind of chiral chromatogram filler applying device and method,
Rapidly and efficiently can produce continuously, improve work efficiency.
Technical scheme: for solving above-mentioned technical problem, the technical solution used in the present invention is:
A kind of chiral chromatogram filler applying device, it is characterised in that: including being homogenized bucket, stirring paddle, crowded material mouth, coating is scraped
Sheet, heats roller, rewinding scraping blade；
Being provided with the stirring paddle for being stirred by filler in described homogenate bucket, the bottom of homogenate bucket offers material extrusion
Mouthful, heating roller is arranged on below crowded material mouth；Coating scraping blade it is connected with, for making the filler on heating roller at crowded material mouth
Layer thickness is uniform；
Also include rewinding scraping blade, for the packing layer being dried on heating roller is scraped collection.
Described chiral chromatogram filler applying device, it is characterised in that: the lower section of described heating roller is provided with rewinding tank,
For collecting the packing layer being dried scraped on heating roller.
Described chiral chromatogram filler applying device, it is characterised in that: being provided with stirring sheet in described rewinding tank, being used for will
The packing layer being dried scraped stirs to powdery.
The present invention also provides for the coating method of a kind of chiral chromatogram filler, uses above-mentioned chiral chromatogram filler coating dress
Put, comprise the following steps:
1) in homogenate bucket, use volatile solvent to be dissolved by many carbohydrates and their derivative, and be sufficiently stirred for silica gel
To mixture；
2) the flowable mixture that will be stirred, by certain extruding, is laid on the heating roller of rotation formation
Mixture thin layer, solvent is heated volatilization at ambient pressure, and mixture thin layer becomes the packing layer of relatively dry on heating runner；
3) by rewinding scraping blade, the packing layer of relatively dry is collected, be stirred for powdery obtaining fleut；
4) by the fleut convection drying after stirring, get product dress column packing.
Preferably, the coating method of described chiral chromatogram filler, it is characterised in that: described solvent is tetrahydrochysene furan
Mutter, one or more in dichloromethane, acetone, chloroform.
Preferably, the coating method of described chiral chromatogram filler, it is characterised in that: mixed on described heating roller
Compound thin layer tiling thickness is 0.1-2mm.
Preferably, the coating method of described chiral chromatogram filler, it is characterised in that: adding of described heating roller
Hot temperature is 40-65 degrees Celsius.
Beneficial effect: the chiral chromatogram filler coating method that the present invention provides, uses the chiral chromatogram filler of the present invention to be coated with
Coating apparatus, first passes through thin layer volatile dry, obtains the mixture of relatively dry, then obtains product by stirring and redrying.
Solve existing in the case of containing substantial amounts of solvent and painting dressing, be dried uneven and that agglomerating force causes caking existing
As, rapidly and efficiently can produce continuously, improve work efficiency；Product prepared by chiral chromatogram filler applying device of the present invention and method
Product, output capacity is higher, and separating degree is more preferable, and good product quality reduces production cost simultaneously.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention；
In figure: homogenate bucket 1, stirring paddle 2, crowded material mouth 3, coating scraping blade 4, heat roller 5, rewinding scraping blade 6, rewinding tank 7, stir
Mix sheet 8.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described.
As it is shown in figure 1, a kind of chiral chromatogram filler applying device, including homogenate bucket 1, stirring paddle 2, crowded material mouth 3, coating is scraped
Sheet 4, heats roller 5, rewinding scraping blade 6, rewinding tank 7, stirs sheet 8；It is provided with for stirring that filler is stirred in homogenate bucket 1
Mixing oar 2, the bottom of homogenate bucket 1 offers crowded material mouth 3, and heating roller 5 is arranged on below crowded material mouth 3；Connect at crowded material mouth 3 and arrange
There is coating scraping blade 4, for making the packing layer thickness on heating roller 5 uniform；Also include rewinding scraping blade 6, for roller 5 will be heated
The upper packing layer being dried scrapes collection.The lower section of heating roller 5 is provided with rewinding tank 7, scrapes on heating roller 5 for collecting
The packing layer being dried.Rewinding tank 7 is provided with stirring sheet 8, for stirring the packing layer being dried scraped to powdery.
The coating method of a kind of chiral chromatogram filler, uses above-mentioned chiral chromatogram filler applying device, including following step
Rapid:
1) in homogenate bucket, use volatile solvent to be dissolved by many carbohydrates and their derivative, and be sufficiently stirred for silica gel
To mixture；
2) the flowable mixture that will be stirred, by certain extruding, is laid on the heating roller 5 of rotation formation
Mixture thin layer, solvent is heated volatilization at ambient pressure, and mixture thin layer becomes the packing layer of relatively dry on heating runner；
3) by rewinding scraping blade 6, the packing layer of relatively dry is collected, be stirred for powdery obtaining fleut；
4) by the fleut convection drying after stirring, get product dress column packing.
Preferably, the coating method of described chiral chromatogram filler, it is characterised in that: described solvent is tetrahydrochysene furan
Mutter, one or more in dichloromethane, acetone, chloroform.
Preferably, the coating method of described chiral chromatogram filler, it is characterised in that: mixed on described heating roller
Compound thin layer tiling thickness is 0.1-2mm.
Preferably, the coating method of described chiral chromatogram filler, it is characterised in that: adding of described heating roller
Hot temperature is 40-65 degrees Celsius.
Embodiment:
By 6 kilograms of silica gel (5 μm particle diameter) of a collection of purchase, being divided into 6 parts, 1 kilogram every part, wherein three parts according to evaporated in vacuo
Mode, three parts use methods and apparatus of the present invention.
Example 1:
1, the painting dressing of 90g is dissolved in 100ml oxolane, is then added in coating machine, then by weight be
The silica gel (particle diameter is 5 μm) of 500g, adds in coating machine, starts coating.
2, the most semiarid product during collecting device coating reclaims bucket, puts in vacuum drying oven 65 degrees Celsius, directly
It is vacuum dried 2 hours, it is thus achieved that powder.
3, by the electric sieve in 10 μm apertures, powder being removed block, obtain 560g product, productivity is 94.9%.
4, after being homogenized by powder with homogenate, capo is dressed up into the automatic packing column machine controlled with automatic controller
(4.6mm*250mm), medicine test separating degree (with flavanone as comparative), comparative result are used.
Example 2:
1, the painting dressing of 180g is dissolved in 200ml oxolane, is then added in coating machine, then by weight be
The silica gel (particle diameter is 5 μm) of 1000g, adds in coating machine, starts coating.
2, the method for procedure below such as example 1, it is thus achieved that finished product 1155g powder, productivity 97.5%, dress post compares separating degree.
Example 3:
1, the painting dressing of 360g is dissolved in 400ml oxolane, is then added in coating machine, then by weight be
The silica gel (particle diameter is 5 μm) of 2000g, adds in coating machine, starts coating.
2, other process such as example 1, it is thus achieved that finished product 2337g powder, productivity 99.0%, dress post compares separating degree.
Comparative example 1:
1, the painting dressing of 90g is dissolved in 100ml oxolane, then adds and drop to the silica gel of 500g (particle diameter is 5 μ
M) in, stirring.
2, after stirring, it is heated to 40 degrees Celsius, is evacuated to 400hPa and slowly solvent is evaporated, 90 points
Zhong Houzai adjusting vacuum to 150hPa, obtains product after 12 hours.
3, by the electric sieve in 10 μm apertures, powder being removed block, obtain 470g product, productivity is 79.7%.
4, after powder being homogenized with homogenate, with the automatic packing column machine that with automatic controller control identical with example 1
Dress up into capo (4.6mm*250mm), use medicine test separating degree on medicine (flavanone), comparative result.
Comparative example 2:
1, the painting dressing of 180g is dissolved in 200ml oxolane, then adds and drop to the silica gel of 1000g (particle diameter is 5
μm) in, stirring.
2, process is identical with comparative example 1.
3, by the electric sieve in 10 μm apertures, powder being removed block, obtain 730g product, productivity is 61.9%.
4, after powder being homogenized with homogenate, with the automatic packing column machine that with automatic controller control identical with example 1
Dressing up into capo (4.6mm*250mm), use medicine test separating degree (with flavanone as comparative), comparative result see table:
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| Output capacity | 94.9% | 97.5% | 99.0% | 79.7% | 61.9% |
| Separating degree | 5.7 | 5.8 | 5.7 | 4.2 | 4.0 |
As can be seen from the table, product prepared by chiral chromatogram filler applying device of the present invention and method, output capacity is higher,
Separating degree is more preferable, and good product quality reduces production cost simultaneously.
The above is only the preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (6)
1. a coating method for chiral chromatogram filler, uses chiral chromatogram filler applying device, and described chiral chromatogram filler is coated with
Coating apparatus includes being homogenized bucket, stirring paddle, crowded material mouth, coating scraping blade, heats roller, rewinding scraping blade；It is provided with in described homogenate bucket
For the stirring paddle stirred by filler, the bottom of homogenate bucket offers crowded material mouth, and heating roller is arranged on below crowded material mouth；
Coating scraping blade it is connected with, for making the packing layer thickness on heating roller uniform at crowded material mouth；Also include rewinding scraping blade, use
In the packing layer being dried on heating roller is scraped collection；Coating method comprises the following steps:
1) in homogenate bucket, use volatile solvent to be dissolved by many carbohydrates and their derivative, and be sufficiently stirred for being mixed with silica gel
Compound；
2) the flowable mixture that will be stirred, by certain extruding, is laid on the heating roller of rotation formation mixing
Thing thin layer, solvent is heated volatilization at ambient pressure, and mixture thin layer becomes the packing layer of relatively dry on heating roller；
3) by rewinding scraping blade, the packing layer of relatively dry is collected, be stirred for powdery obtaining fleut；
4) by the fleut convection drying after stirring, get product dress column packing.
The coating method of chiral chromatogram filler the most according to claim 1, it is characterised in that: described solvent is tetrahydrochysene furan
Mutter, one or more in dichloromethane, acetone, chloroform.
The coating method of chiral chromatogram filler the most according to claim 1, it is characterised in that: mix on described heating roller
Thing thin layer tiling thickness is 0.1-2mm.
The coating method of chiral chromatogram filler the most according to claim 1, it is characterised in that: the heating of described heating roller
Temperature is 40-65 degrees Celsius.
The coating method of chiral chromatogram filler the most according to claim 1, it is characterised in that: the lower section of described heating roller
It is provided with rewinding tank, for collecting the packing layer being dried scraped on heating roller.
The coating method of chiral chromatogram filler the most according to claim 5, it is characterised in that: described rewinding tank is provided with
Stirring sheet, for stirring the packing layer being dried scraped to powdery.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510196885.1A CN104784970B (en) | 2015-04-23 | 2015-04-23 | Chiral chromatogram filler applying device and method |
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|---|---|---|---|
| CN201510196885.1A CN104784970B (en) | 2015-04-23 | 2015-04-23 | Chiral chromatogram filler applying device and method |
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| Publication Number | Publication Date |
|---|---|
| CN104784970A CN104784970A (en) | 2015-07-22 |
| CN104784970B true CN104784970B (en) | 2016-08-31 |
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| CN201510196885.1A Expired - Fee Related CN104784970B (en) | 2015-04-23 | 2015-04-23 | Chiral chromatogram filler applying device and method |
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Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0002040B1 (en) * | 1977-11-21 | 1981-12-30 | Ciba-Geigy Ag | Process for the application of soldering masks to printed circuits with through holes for contacting |
| ATE99746T1 (en) * | 1988-10-28 | 1994-01-15 | Kufner Textilwerke Gmbh | METHOD AND DEVICE FOR THE RASTERFORM COATING OF FLEXIBLE FLAT STRUCTURES AND THEIR MANUFACTURE PRODUCTS. |
| JP3990467B2 (en) * | 1995-09-26 | 2007-10-10 | 住友電気工業株式会社 | Tubular product manufacturing method and tubular product |
| DE10325140B4 (en) * | 2003-06-04 | 2014-12-31 | Lts Lohmann Therapie-Systeme Ag | Direct coating method and apparatus |
| CN1988103B (en) * | 2005-12-23 | 2010-05-05 | 上海广电电子股份有限公司 | Device and its method for producing coating of flat plate display fluorescence screen |
| JP5520074B2 (en) * | 2010-02-15 | 2014-06-11 | デクセリアルズ株式会社 | Coating resin liquid coating method and coating apparatus |
| CN204563677U (en) * | 2015-04-23 | 2015-08-19 | 南京隆特森化学科技有限公司 | Chiral chromatogram filler applying device |
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| C14 | Grant of patent or utility model | ||
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| CB03 | Change of inventor or designer information |
Inventor after: Wang Zhifa Inventor before: Wu Ying Inventor before: Wang Huanhuan |
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| TR01 | Transfer of patent right |
Effective date of registration: 20170911 Address after: 210000 room 1-0523, No. 36 Sheng Dong Road, Jiangning District, Nanjing, Jiangsu Patentee after: Nanjing Huiheng Scientific Instrument Co. Ltd. Address before: 210000, No. 18, LAN Lu, Jiangning District, Jiangsu, Nanjing Patentee before: Nanjing Long Tesen chemistry Science and Technology Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
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Granted publication date: 20160831 Termination date: 20180423 |