CN1108151C - Fluid energy milling process and apparatus - Google Patents
Fluid energy milling process and apparatus Download PDFInfo
- Publication number
- CN1108151C CN1108151C CN99805243A CN99805243A CN1108151C CN 1108151 C CN1108151 C CN 1108151C CN 99805243 A CN99805243 A CN 99805243A CN 99805243 A CN99805243 A CN 99805243A CN 1108151 C CN1108151 C CN 1108151C
- Authority
- CN
- China
- Prior art keywords
- compressed air
- humidity
- air
- compressed
- dihydrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/06—Jet mills
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C25/00—Control arrangements specially adapted for crushing or disintegrating
Landscapes
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Preparation (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Disintegrating Or Milling (AREA)
- Medicines Containing Plant Substances (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Crushing And Grinding (AREA)
Abstract
The invention provides a fluid energy milling apparatus including means for adjusting humidity of the compressed air used for milling provides improved micronised product, in particular hydrates for use as drug substance in pharmaceutical compositions.
Description
The present invention relates to produce the method and apparatus of fine-powder, particularly drug powder.The present invention relates to the improvement of fluid energy milling particularly.
Fluid energy milling is also referred to as micronization, normally is used to prepare the program of fine-powder.It is specially adapted to the micronization of medicine, because there is not abrasive media to stain product.In fluid energy milling, the reducing of its granularity is that the energy utilize compressed air to produce causes attrition between the grinding charge matter granule.
Compressed-air actuated humidity used in fluid energy milling is very low, and this is owing to increased the condensation ability in compressed air system.After compression, from air, remove dampness, to avoid its condensation in using compressed-air actuated equipment.Normally by condensation, at compression postcooling compressed air with make compressed air realize removing dampness by drying tower before entering the fluid energy milling machine then.Compressed-air actuated pressure used in fluid energy milling is about 6bar usually, and its dew point also can hang down-70 ℃ below-40 ℃.
In process of lapping, method of micronization may destroy the crystal structure of substance to be processed.When grinding crystallohydrate and solvate, the combination of attrition and very dried air can cause additional infringement, and this is because in processing procedure, from crystal structure except that anhydrate/the solvate molecule causes.After grinding, this micronized material after a period of time according to storage requirement its original crystal structure of also can reentrying.Therefore, the medicine that is crystallohydrate may not be in its original specification behind fluid energy milling, and can turn back to its primary specification after the long period of storage of imprevision.In addition, the infringement that is caused by attrition/desolvation can influence institute's predetermined characteristics of product, for example, and surface energy, stability, bioavailability.Under specific circumstances, the powder of grinding is further closing gathering in the processing procedure, rather than homodisperse.
The present invention is based on following discovery, is about in fluid energy milling used compressed-air actuated humidity and is controlled at apparently higher than used scope usually, but be lower than the humidity that condensation takes place in can causing grinding, and just can cause less infringement to the crystallinity of abrasive product.This material desiccation reduces or the degree of crystallinity of its original level of avoiding also helping reentrying after grinding thereupon in process of lapping.Therefore, the invention provides the micronized product that characteristic is more consistent and quality control is more excellent.The variation that this just significantly reduces between the batch process causes less reprocessing to be handled or inefficacy in batches.In addition, the inventive method reduces the granularity that is reached by micronization processes does not have injurious effects.
Most importantly the invention provides a kind of fluid energy milling equipment, this equipment comprises the device of regulating abradant compressed-air actuated humidity.
The present invention also provides a kind of Ginding process, this method comprises compressed air infeeded the grinding chamber that contains particulate matter, and makes this material through fluid energy milling, it is characterized in that, monitor this compressed-air actuated humidity, regulate this humidity when needing to reduce infringement to abrasive product.
The adjusting of being done according to the present invention normally increases humidity.But in case determined optimum, and the equipment adjusted increases to making compressed air produce required humidity, and what then need to do in process of lapping is to calibrate the humidity level up and down, to keep its optimum.
Typical fluid energy milling system comprises compressed air source, drying tower and contains grinding chamber and the grinder of gathering-device.This gathering-device can be filter bag or the expanding chamber in the outlet air logistics, and the energy of air logistics is dissipated so that under the electrodeposition substance that grinds in this expanding chamber.The humidity of the plant air in grinder increases by the layout of bypass drying tower, so that compressed air directly enters grinder from empty source.But, this system's preferred design becomes controlled, and its method is to be provided with to walk around the bypass circulation of drying tower, and has the control valve air that commutate between bypass circulation and drying tower mobile, thus, be changeable by compressed-air actuated relative scale bypass and by tower.By the humidity that monitoring enters the air of grinder, utilize the control valve scalable by bypass and the air capacity by drying tower, to reach humidity required in the grinding chamber.
In another embodiment, the air of undried can mix at a specific compressed air outlet with the air of drying, only the plant air of supplying with project equipment is carried out humidity regulation.
In the embodiment outside not, humidity can be regulated by water spray, preferably water is fed in the compressed air piping of upstream position with vaporific or spray shape, and it can be dispersed in the whole air logistics moisture before entering grinder.
Humidity is preferably come valuation with the dew point measurement.The present invention includes any process of regulating humidity, so that the dew point of the plant air in the grinder is higher than the compressed-air actuated dew point that is produced.Common humidity is increased to dew point and is-30 ℃-5 ℃, preferably is about-15 ℃-0 ℃.Optimum to predetermined substance can be by routine test to change dew point and to assess product quality and determine.
Humidity is measured by cold-spot hygrometer usually.For example can carry out continuous measurement by probe being placed in the air logistics that enters before the grinding chamber; Or utilize air logistics sampling to be interrupted mensuration to entering before the grinding chamber.
The present invention can be applicable to any fluid energy milling process, for example be applied to reach the system that pre-sizing is discharged this particulate system by the internal classification device or is applied to be provided with clasfficiator when granule, in this system, product is required particle size range by grinder up to granule repeatedly.
The present invention is except that the advantageous effects to the micronization product, and its another advantage is to have improved of micronization process itself, makes to keep feed rate and the air pressure balance is more easy.In addition, the inventive method has been improved concordance and the quality at continuous production micronized drug products in the cycle.
In addition, the present invention is effective especially to the fine powder medicine that preparation is used for Pharmaceutical composition.Therefore, the invention provides a kind of Pharmaceutical composition that contains by the medicine of said method gained on the other hand.
The present invention will improve the quality of the micronization product of most of material, but be applied in the course of processing crystallization be damaged the micronization of responsive material especially.Because the removal of the water of crystallization (if existence) itself can make the crystal structure instability, in traditional micronization processes process of crystallohydrate, the probability of crystalline damage is a serious problem, and the present invention will overcome this problem.
In a preferred embodiment, program of the present invention is to be used to prepare micronized mupirocin (mupirocin) calcium dihydrate (EPO167856-A2, BEECHAM Group plc).Can form undesirable aggregation when in the past, the micronization product of the fluid energy milling of this material generation is in sneaking into ointment base.Supposed that this is by grinding the loss cause water of crystallization and the change of the surface energy that infringement produced of crystal structure is caused in very dried air.The humidity of plant air is controlled to the atmospheric pressure dew point overcome this problem for-15 ℃-0 ℃.The moisture of the micronized Calcium mupirocin dihydrate. that produces by program of the present invention is preferably 3.0-4.0%, and 3.4-3.7% more preferably, and after crystallinity is recovered low amorphous content is arranged is preferably 5% or still less.
Therefore, the invention provides a kind of Pharmaceutical composition on the other hand, it comprises the micronized Calcium mupirocin dihydrate. that is obtained by said method.The advantage of this based composition is the medicine that comprises more consistent mass property, and avoids forming in ointment for example the aggregation of Calcium mupirocin dihydrate..
Preferably, this based composition comprises ointment, Emulsion and nasal spray, described at EPO231621-A2 (Beecham Group plc), EP0251434-A2 (Beecham Group plc), WO95/10999 (Smithkline Beecham Corp) and WO98/14189 (Smithkline Beecham).A kind of preferred compositions is a kind of unguentum of the mupirocin calcium dihydrate in containing the white freestone cerul material of glyceride, can be bought with product B actroban Nasal by Smithkline Beecham company.Another kind of preferred compositions is a kind of Emulsion of the mupirocin calcium dihydrate in the base material that contains mineral oil, the single cetyl ether of Polyethylene Glycol (1000), cetyl alcohol, octadecanol, Xanthan gum and water, can be buied with product B ectroban Cream by Smithkline Beecham company.
The present invention illustrates with the following example.
Embodiment 1
A plant-scale factory that is used for micronization mupirocin calcium dihydrate thing sends into the micronization grinder with compressed air through silicagel column.In the loop that supplies to be provided with in the plant air bypass silica dehydrator post to grinder.Utilize the ratio of the air of the dry post of valve change bypass, so that the humidity in the plant air can be controlled.
Get single mupirocin calcium in batches, and be divided into three parts to carry out independent micronization three times.Micronization (son crowd A) is to use factory's compressor plant air of supply usually for the first time.The dew point of air is-58 ℃.In addition the micronization of two parts of chargings is: once (son crowd B) is to use the air that dew point is controlled at-10 ℃, and once (son crowd C) is to use the air (the available humidity higher limit of this factory) that dew point is controlled at 0 ℃.Each run produces the micronization product of about 5kg.Under each situation, dew point is all measured by near the upstream air sampling of the grinder the air admission mouth, and evaluates with dew point under atmospheric pressure.
All three micronized sons are criticized and are all met required granularity specification.This product is evaluated its crystallinity with solution calorimeter, and with its moisture of CALVER Xie Er (Karl Fischer) assay determination.The micronization that son under dew point-58 ℃ is criticized A shows the amorphous content (is 2%) of its desiccation (moisture: 3.1-3.2% (w/w)) and about 15% in micronization dihydrate not.Son crowd B and son crowd C are respectively in dew point-10 ℃ and 0 ℃ generation down, show that (moisture: 3.6% (w/w)), its amorphous content is about 9% to no desiccation.The continuous monitoring that each son is criticized shows, criticizes B and son crowd C for son, and in several weeks thereafter, its amorphous content constantly reduces, and because sub crowd A has desiccation, so it can not recover its crystalline damage.
Son is criticized A and B mixes with ointment base.Being criticized in the ointment that A makes by son has a large amount of aggregations; Criticize in the ointment that B makes by son and not find aggregation.
Embodiment 2
In another experiment, test for each part of-50 ℃ the micronized a collection of mupirocin calcium of air with the dew point that uses compressed air system to produce usually for-15 ℃ to-5 ℃ air micronization using the control dew point, with relatively its influence, also change the stress state of other micronization parameter in the process simultaneously with simulation process to moisture and crystalline damage (amorphous medicine content).Experiment to each part of the micronized batch of material of air that uses control dew point (15 ℃ to-5 ℃) shows that its average moisture is 3.5% (w/w), and average amorphous medicine content is 16.5%.Experiment to each part of using the micronized batch of material of standard compressed air shows that its average moisture is 2.9% (w/w), and average amorphous medicine content is 38.3%.When adopting the technology of controlled humidity, to compare with adopting common compressed-air actuated situation, its product medicine has more consistent quality, and the present invention of this proof has improved the stability of micronization process.
Claims (10)
1. micronized Calcium mupirocin dihydrate., its moisture are 3.0-4.0%, and its amorphous content is 5% or lower.
2. according to the micronized Calcium mupirocin dihydrate. of claim 1, its moisture is 3.4-3.7%.
3. be used to prepare the Ginding process of the micronized Calcium mupirocin dihydrate. of claim 1, it comprises the grinding chamber that compressed air is infeeded mupirocin calcium dihydrate particulate matter, and make this material through fluid energy milling, it is characterized in that, monitor this compressed-air actuated humidity, regulate this humidity when needing to reduce infringement to abrasive product.
4. according to the method for claim 3, wherein grinding is to carry out in the system that comprises compressed air source, drying tower, grinding chamber and gathering-device.
5. according to the method for claim 3 or 4, the device of wherein monitoring humidity is to be in and the contacted drimeter probe of compressed air stream.
6. according to the method for claim 3 or 4, the device of wherein monitoring humidity comprises the device of the compressed air stream sampling of grinding chamber upstream and the drimeter that off-line is provided with.
7. according to the method for claim 3 or 4, the device of wherein regulating compressed air humidity is a kind of syringe, and it is introduced water, water smoke or spray quinoline water in the compressed air line.
8. according to the method for claim 3 or 4, bypass circulation is set wherein, makes compressed air walk around drying tower, and it is mobile with commutation air between drying tower and bypass circulation that control valve is set.
9. method according to Claim 8, wherein control valve is adjustable, so that be variable by the compressed-air actuated ratio of drying tower and bypass circulation.
10. Pharmaceutical composition, it comprises the micronized Calcium mupirocin dihydrate. of claim 1, and this medicine is dispersed in the pharmaceutical carrier.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB9808470.0 | 1998-04-22 | ||
| GBGB9808470.0A GB9808470D0 (en) | 1998-04-22 | 1998-04-22 | Novel process and apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1297378A CN1297378A (en) | 2001-05-30 |
| CN1108151C true CN1108151C (en) | 2003-05-14 |
Family
ID=10830710
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99805243A Expired - Fee Related CN1108151C (en) | 1998-04-22 | 1999-04-19 | Fluid energy milling process and apparatus |
Country Status (24)
| Country | Link |
|---|---|
| EP (1) | EP1073524B1 (en) |
| JP (1) | JP2002512117A (en) |
| KR (1) | KR20010042863A (en) |
| CN (1) | CN1108151C (en) |
| AR (3) | AR015000A1 (en) |
| AT (1) | ATE255466T1 (en) |
| AU (1) | AU748262B2 (en) |
| BR (1) | BR9909806A (en) |
| CA (1) | CA2329732A1 (en) |
| CO (1) | CO4820444A1 (en) |
| CZ (1) | CZ292385B6 (en) |
| DE (1) | DE69913331T2 (en) |
| ES (1) | ES2211073T3 (en) |
| GB (1) | GB9808470D0 (en) |
| HK (1) | HK1034216A1 (en) |
| HU (1) | HUP0102244A3 (en) |
| IL (1) | IL138874A0 (en) |
| NO (1) | NO20005235D0 (en) |
| NZ (1) | NZ507489A (en) |
| PL (1) | PL343563A1 (en) |
| TR (1) | TR200003035T2 (en) |
| TW (1) | TW558453B (en) |
| WO (1) | WO1999054048A1 (en) |
| ZA (1) | ZA200005739B (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9826284D0 (en) * | 1998-12-01 | 1999-01-20 | Rhone Poulence Rorer Limited | Process |
| AR022695A1 (en) * | 1999-01-28 | 2002-09-04 | Schering Corp | SOLID PARTICULATE CARRIER AND METHOD TO PROVIDE PARTICULATE CONTROL FOR THE DISTRIBUTION OF SIZE OF PARTICLES AND CONVERTIBLE AMORPH CONTENT DURING PREPARATION |
| US6623760B1 (en) | 1999-01-28 | 2003-09-23 | Schering Corporation | Method of preparing particles for agglomeration |
| GB0409703D0 (en) | 2004-04-30 | 2004-06-02 | Vectura Ltd | Pharmaceutical compositions |
| WO2007144901A1 (en) * | 2006-06-12 | 2007-12-21 | Jubilant Organosys Limited | Process for stabilization of olanzapine polymorphic form i |
| US8235314B2 (en) * | 2009-02-12 | 2012-08-07 | Linde Aktiengesellschaft | Nonequilibrium humidity control for jet milling |
| JO3510B1 (en) | 2011-03-04 | 2020-07-05 | Heptares Therapeutics Ltd | Use of glycopyrrolate for treating tachycardia |
| DE102012215511A1 (en) | 2012-08-31 | 2014-06-12 | Schülke & Mayr GmbH | Process for the preparation of a semi-solid preparation containing bispyridiniumalkane |
| SG11201507286QA (en) | 2013-03-15 | 2015-10-29 | Pearl Therapeutics Inc | Methods and systems for conditioning of particulate crystalline materials |
| LT3191081T (en) | 2014-09-09 | 2020-07-10 | Vectura Limited | Formulation comprising glycopyrrolate, method and apparatus |
| CN108135851B (en) | 2015-09-09 | 2022-03-15 | 维克多瑞有限公司 | Jet milling method |
| US10967345B2 (en) | 2016-04-18 | 2021-04-06 | Premex S.A.S. | Multiple modular system for the formation of particles in powder and microcapsule form for different processes |
| CN115737610B (en) * | 2021-12-13 | 2024-02-27 | 苏州欧米尼医药有限公司 | Air flow crushing method for tiotropium bromide inhalation powder fog agent and active ingredient thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0167856A2 (en) * | 1984-06-19 | 1986-01-15 | Beecham Group Plc | Crystalline calcium pseudomonate and use |
| EP0697254A2 (en) * | 1994-08-18 | 1996-02-21 | Chichibu Onoda Co., Ltd. | Electrostatic powder coating method and apparatus |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2704635A (en) * | 1951-06-02 | 1955-03-22 | Conrad M Trost | Pulverizing mill having opposed jets and circulatory classification |
| GB8530796D0 (en) | 1985-12-13 | 1986-01-22 | Beecham Group Plc | Pharmaceutical composition |
| IE59628B1 (en) | 1986-06-26 | 1994-03-09 | Beecham Group Plc | Treatment of fungal infections |
| JPH02251535A (en) * | 1989-03-27 | 1990-10-09 | Asahi Chem Ind Co Ltd | Pulverization of poly-beta-alanine copolymer |
| PL177592B1 (en) | 1993-10-22 | 1999-12-31 | Smithkline Beecham Corp | Novel composition |
| JP2001504091A (en) | 1996-10-01 | 2001-03-27 | スミスクライン・ビーチャム・コーポレイション | Use of mupirocin for the manufacture of a medicament for the treatment of bacterial infections associated with nasopharyngeal colonization by pathogenic organisms |
-
1998
- 1998-04-22 GB GBGB9808470.0A patent/GB9808470D0/en not_active Ceased
-
1999
- 1999-04-19 ES ES99918105T patent/ES2211073T3/en not_active Expired - Lifetime
- 1999-04-19 DE DE1999613331 patent/DE69913331T2/en not_active Expired - Fee Related
- 1999-04-19 AU AU36149/99A patent/AU748262B2/en not_active Ceased
- 1999-04-19 CN CN99805243A patent/CN1108151C/en not_active Expired - Fee Related
- 1999-04-19 PL PL99343563A patent/PL343563A1/en unknown
- 1999-04-19 CZ CZ20003895A patent/CZ292385B6/en not_active IP Right Cessation
- 1999-04-19 EP EP99918105A patent/EP1073524B1/en not_active Expired - Lifetime
- 1999-04-19 TR TR2000/03035T patent/TR200003035T2/en unknown
- 1999-04-19 HU HU0102244A patent/HUP0102244A3/en unknown
- 1999-04-19 BR BR9909806-7A patent/BR9909806A/en not_active IP Right Cessation
- 1999-04-19 JP JP2000544437A patent/JP2002512117A/en active Pending
- 1999-04-19 AR ARP990101808A patent/AR015000A1/en not_active Application Discontinuation
- 1999-04-19 AT AT99918105T patent/ATE255466T1/en not_active IP Right Cessation
- 1999-04-19 KR KR1020007011637A patent/KR20010042863A/en not_active Application Discontinuation
- 1999-04-19 IL IL13887499A patent/IL138874A0/en unknown
- 1999-04-19 CA CA002329732A patent/CA2329732A1/en not_active Abandoned
- 1999-04-19 WO PCT/GB1999/001189 patent/WO1999054048A1/en not_active Application Discontinuation
- 1999-04-19 NZ NZ507489A patent/NZ507489A/en unknown
- 1999-04-20 CO CO99023658A patent/CO4820444A1/en unknown
- 1999-04-23 TW TW088106573A patent/TW558453B/en active
-
2000
- 2000-03-08 AR ARP000101026A patent/AR022868A2/en not_active Application Discontinuation
- 2000-03-08 AR ARP000101027A patent/AR022869A2/en unknown
- 2000-10-17 ZA ZA200005739A patent/ZA200005739B/en unknown
- 2000-10-18 NO NO20005235A patent/NO20005235D0/en not_active Application Discontinuation
-
2001
- 2001-07-12 HK HK01104886A patent/HK1034216A1/en not_active IP Right Cessation
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0167856A2 (en) * | 1984-06-19 | 1986-01-15 | Beecham Group Plc | Crystalline calcium pseudomonate and use |
| EP0697254A2 (en) * | 1994-08-18 | 1996-02-21 | Chichibu Onoda Co., Ltd. | Electrostatic powder coating method and apparatus |
Also Published As
| Publication number | Publication date |
|---|---|
| HUP0102244A3 (en) | 2002-08-28 |
| NO20005235L (en) | 2000-10-18 |
| CZ292385B6 (en) | 2003-09-17 |
| ZA200005739B (en) | 2002-03-25 |
| KR20010042863A (en) | 2001-05-25 |
| PL343563A1 (en) | 2001-08-27 |
| JP2002512117A (en) | 2002-04-23 |
| TR200003035T2 (en) | 2001-02-21 |
| CZ20003895A3 (en) | 2001-08-15 |
| DE69913331T2 (en) | 2004-11-18 |
| AR022869A2 (en) | 2002-09-04 |
| NZ507489A (en) | 2003-06-30 |
| HK1034216A1 (en) | 2001-10-19 |
| AR015000A1 (en) | 2001-04-11 |
| CA2329732A1 (en) | 1999-10-28 |
| ES2211073T3 (en) | 2004-07-01 |
| EP1073524B1 (en) | 2003-12-03 |
| GB9808470D0 (en) | 1998-06-17 |
| EP1073524A1 (en) | 2001-02-07 |
| TW558453B (en) | 2003-10-21 |
| WO1999054048A1 (en) | 1999-10-28 |
| NO20005235D0 (en) | 2000-10-18 |
| HUP0102244A2 (en) | 2001-10-28 |
| CO4820444A1 (en) | 1999-07-28 |
| IL138874A0 (en) | 2001-11-25 |
| DE69913331D1 (en) | 2004-01-15 |
| AU3614999A (en) | 1999-11-08 |
| CN1297378A (en) | 2001-05-30 |
| AR022868A2 (en) | 2002-09-04 |
| BR9909806A (en) | 2000-12-26 |
| ATE255466T1 (en) | 2003-12-15 |
| AU748262B2 (en) | 2002-05-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1108151C (en) | Fluid energy milling process and apparatus | |
| KR100838200B1 (en) | Animal feed additive based on fermentation broth and production process thereof by granulation | |
| CN104970186B (en) | Fluidized bed granulation method for amino acid-containing fermentation liquor | |
| GB1498464A (en) | Process and an apparatus for converting a solution or suspension into a dried particulate granulate product | |
| EP3541765A1 (en) | Process and apparatus for calcination of gypsum | |
| CN1354652A (en) | Milling process for production of finely milled medicinal substances | |
| CN106135644A (en) | The feedstuff production method of composite particles carrier | |
| CN107805410A (en) | A kind of titanium white production method improved in resin system dispersiveness | |
| AU681651B2 (en) | Spray drying device | |
| JP2006520765A (en) | Amoxicillin trihydrate | |
| US5021554A (en) | Process for protein particle size reduction using a fluid-energy mill | |
| JPH11511454A (en) | Solid sucralose | |
| RU54931U1 (en) | PLANT FOR PRODUCING GRANULATED SODIUM PERCARBONATE | |
| MXPA00010306A (en) | Fluid energy milling process and apparatus | |
| US6242006B1 (en) | β-lactam granules free of organic solvents | |
| JPH01284455A (en) | Production of spheroidal molding sand | |
| CN213314860U (en) | Feeding device for powdery medical intermediate | |
| CN210449884U (en) | Adipic acid granularity screening device | |
| CN214210409U (en) | System for regulating and controlling granularity of crystal sugar alcohol product | |
| CA2177814C (en) | Process for producing agglomerates from dusts | |
| EP3765438A1 (en) | Process for drying n,n-dimethyl glycinate salt | |
| CN117602669A (en) | Preparation method of hafnium tetrachloride | |
| CN117379553A (en) | Production process for preparing direct-compression anhydrous calcium hydrophosphate porous spherical particles | |
| CN104742219A (en) | Fiberboard forming system with drying and purifying units | |
| SU1398908A1 (en) | Method of automatic regulation of charging of the ball tumbling mill |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |