CN2231570Y - Distillation crystallizing apparatus with distillation tower section - Google Patents
Distillation crystallizing apparatus with distillation tower section Download PDFInfo
- Publication number
- CN2231570Y CN2231570Y CN 95207057 CN95207057U CN2231570Y CN 2231570 Y CN2231570 Y CN 2231570Y CN 95207057 CN95207057 CN 95207057 CN 95207057 U CN95207057 U CN 95207057U CN 2231570 Y CN2231570 Y CN 2231570Y
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- solvent
- crystallization apparatus
- rectifying
- crystallization
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Abstract
The utility model belongs to the chemical engineering, particularly a rectifying and crystallizing apparatus in the separating process in medicinal projects. The utility model is combined with a rectifying device and a crystallizing device into a whole body; the utility model can be operated continuously and intermittently. The rectifying and crystallizing process has the advantages of high process yield, little solvent dosage, high productivity, little produced waste solvent in the process of production, low cost, etc.
Description
The invention belongs to Chemical Engineering, pharmaceutical engineering separation rectifying crystallization apparatus.
Obtain high-purity chemical industry, the medicine crystal product, often need material is carried out atmospheric evaporation or reduction vaporization Crystallization Separation, this has report in existing technology, as U.S. Wyeth, Flour Danid company and Italian I.S.F, the penicillin crystallization apparatus of Farmitalia company etc., can obtain high-purity crystalline product, product purity all can reach the standards of pharmacopoeia of respective country, but these devices are not broken through traditional mode yet, solvent-oil ratio is big, the process yield generally≤94%, can't overcome defective [Xu Zhizhong chief editor, " chemical pharmacy technology, " Chemical Industry Press (1980) that conventional reduction vaporization crystallization exists; Wu Hangyan, Xiong Zonggui, Hu Zhang help the chief editor, " antibiotics production technology, " Chemical Industry Press (1982); Jiang makes very to wait volume, pharmaceutical factory consersion unit and workshop technological design, " Chinese Medicine science and technology publishing house (1994)].
The purpose of this invention is to provide a kind of rectifying crystallization apparatus that rectifier unit and crystallization apparatus are combined, reduce solvent consumption, improve the process yield, and use computer-aided control, overcome the problem of prior art existence.
Rectifying crystallization apparatus of the present invention is the conjoined structure that rectifying column section and crystallization kettle combine.Its structure is divided into four sections by function.First section is the separated from solvent district, is high efficiency packing or 1～10 block of column plate in the tower, and loading height is 0.2～4 meter; Second section is the Reaction Separation district, is special filler and tower internals in the tower, and loading height is 0.2～1 meter; The 3rd section is the vapor-liquid separation district, has board-like separator, highly is 0.3～1.5 meter; The 4th section is crystallization kettle, and this crystallization kettle such as has at the bottom of " ω " type at distinctive appearance, is provided with efficient pusher stirrer paddle that fluid flow guiding tube and computer-aided manufacturing go out etc. in the still.For ease of controlling the operation of rectifying crystallization apparatus of the present invention, column plate is provided with the several temperature measurement point, and these control point signals are introduced special-purpose industrial collecting and distributing computer control system, and the rectifying crystallization process is controlled and operated.The material of separated purification enters from device middle part, and the solvent that rectifying is come out is from the cat head extraction, and crystalline product suspension is discharged at the bottom of by still.
Rectifying crystallization apparatus crystallization process yield height of the present invention, solvent load is few, equipment capacity is big, solvent slop that produced is few, helps the recycling of solvent, and production cost is low.But but also intermittently operated of rectifying crystallization apparatus of the present invention continued operation.
Rectifying crystallization apparatus structure of the present invention is shown in the drawings, and 1 is the separated from solvent section among the figure, and 2 is the Reaction Separation section, 3 is the vapor-liquid separation section, and 4 is crystallization kettle, and 5 is the feed(raw material)inlet, 6 is solvent outlet, 7 are the supplementing solvent inlet, and 8 is the medium inlet, and 9 are the magma outlet, 10 is media outlet, 11 is computer control system, and 12 is pusher stirrer paddle, and 13 is condenser.
Embodiment: concrete tower section size is as follows: 0.25 meter of tower body diameter, the separated from solvent section is high 1.0 meters, in adorn 0.5 meter high stainless steel ripple filler; The Reaction Separation section is high 0.5 meter, and the vapor-liquid separation section is high 1.2 meters, in adorn two sieve plates; 1.6 meters of crystallization kettle diameters, 3.8 meters of height overalls are " ω " type at the bottom of the crystallization kettle, also having diameter in the still is that 1.0 meters, height are 0.8 meter guide shell; Screw is the pusher blade that is gone out by computer-aided manufacturing, 0.95 meter of diameter of propeller blade; Used computer control system is U.S. CIM-PAC2000 type Distributed Control System.
Use rectifying crystallization apparatus of the present invention to be used for potassium penicillin G production, elder generation's crystal solution that---n-butanol---water is formed with potassium penicillin G is packed in the crystallization kettle, and the rectifying crystal system is under the 720mmHg vacuum, in the crystallization kettle chuck, feed low pressure water vapor to crystallization kettle in material heat, stir tremble rotating speed be 40 (rev/min), solvent slop and water distillate from cat head, by the heating rate of fluid temperature and the evaporation rate of system in the computer aided control system crystallization control still, the water overwhelming majority in system distillates, thereby obtain evenly complete crystal of potassium penicillin G in crystallization kettle, product purity meets or exceeds the related standards in the nineteen ninety version Chinese Pharmacopoeia.
Adopt rectifying crystallization apparatus of the present invention, its Crystallization Separation index is compared with external similar simple crystallization apparatus during data are listed in the table below.
| Country origin, company's project | U.S. Wyeth | U.S. Flour Danid | Italy I.S.F. | Italy Farmitalia | Apparatus of the present invention |
| Yield | ≤94％ | 90～94％ | ≤94％ | ～93％ | ≥94％ |
| Solvent load | High by 100 | High～100 | High～100 | High～100 | Low 50～70 |
| Equipment capacity | Medium 1.0 | Medium～1.0 | Medium～1.0 | Medium～1.0 | (height) 1.7～2.0 greatly |
| The solvent slop treating capacity | Greatly | Greatly | Greatly | Greatly | Little |
| Cost | Lower | Medium | Lower | Medium | Low |
Claims (5)
1. the rectifying crystallization apparatus that separation process is used the invention is characterized in rectifier unit and crystallization apparatus are combined that its structure is by separated from solvent district 1, Reaction Separation district 2, vapor-liquid separation district 3, crystallization kettle 4, feed(raw material)inlet 5, solvent outlet 6, supplementing solvent inlet 7, medium inlet 8, magma outlet 9, media outlet 10, computer control system 11, pusher stirrer paddle 12, condenser 13 constitutes.
2. described rectifying crystallization apparatus of claim 1 is characterized in that in the tower in separated from solvent district 1 constituting for high efficiency packing or 1～10 block of column plate, and loading height is 0.2～4 meter.
3. described rectifying crystallization apparatus of claim 1 is characterized in that being filler and tower internals in the tower in Reaction Separation district 2 that loading height is 0.2～1 meter.
4. the described rectifying crystallization apparatus of claim 1 is characterized in that vapor-liquid separation district 3 is board-like separators, highly is 0.3～1.5 meter.
5. the described rectifying crystallization apparatus of claim 1 is characterized in that crystallization kettle 4 has " ω " type base profile, is provided with the efficient stirrer paddle of guide shell and particular design in the still.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95207057 CN2231570Y (en) | 1995-04-12 | 1995-04-12 | Distillation crystallizing apparatus with distillation tower section |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95207057 CN2231570Y (en) | 1995-04-12 | 1995-04-12 | Distillation crystallizing apparatus with distillation tower section |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2231570Y true CN2231570Y (en) | 1996-07-24 |
Family
ID=33858810
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 95207057 Expired - Lifetime CN2231570Y (en) | 1995-04-12 | 1995-04-12 | Distillation crystallizing apparatus with distillation tower section |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN2231570Y (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104289005A (en) * | 2013-10-24 | 2015-01-21 | 高邮市助剂厂 | Liquid-sealed distillation equipment |
| CN105435482A (en) * | 2015-11-27 | 2016-03-30 | 天津大学 | Multi-stage vacuum adiabatic flash continuous crystallization method and equipment |
-
1995
- 1995-04-12 CN CN 95207057 patent/CN2231570Y/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104289005A (en) * | 2013-10-24 | 2015-01-21 | 高邮市助剂厂 | Liquid-sealed distillation equipment |
| CN105435482A (en) * | 2015-11-27 | 2016-03-30 | 天津大学 | Multi-stage vacuum adiabatic flash continuous crystallization method and equipment |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CX01 | Expiry of patent term |