CN104174468B - Toughness medicine zirconium pearl Ginding process - Google Patents
Toughness medicine zirconium pearl Ginding process Download PDFInfo
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- CN104174468B CN104174468B CN201410428007.3A CN201410428007A CN104174468B CN 104174468 B CN104174468 B CN 104174468B CN 201410428007 A CN201410428007 A CN 201410428007A CN 104174468 B CN104174468 B CN 104174468B
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Abstract
The present invention discloses a kind of toughness medicine zirconium pearl Ginding process; Described method comprises the steps: to prepare the circular zirconium pearl that diameter is 1.0～2.0 millimeters; Described zirconium pearl being put into the stainless steel vessel that rotating disk is housed, after adding toughness medicine, starts rotating disk and drive the upper and lower rolling type grinding of zirconium pearl, grinding rotating speed is 800～2800 revs/min. Described zirconium pearl adopts Y2O3-ZrO2Powder body rolling, the micro-pearl of yttria-stabilized zirconia sintered and become. The present invention adopts the relevant art that high rigidity zirconium pearl combines, and solves the grinding distribution problem of toughness medicine, makes medicine reach ultra-fine stable, and guarantees drug safety.
Description
Technical field
The present invention relates to medicine grinding distribution technology, it is specifically related to a kind of toughness medicine zirconium pearl Ginding process.
Background technology
Grinding medium can be divided into granulated glass sphere by the difference of material, and ceramic bead (comprises zirconium silicate pearl, zirconium dioxide pearl, titanium dioxide aluminium pill). Owing to the difference of chemistry composition and manufacturing process determines the crystalline structure of grinding bead, fine and close crystalline structure ensure that the high strength of pearl, high-wearing feature and low oil suction etc. The proportion high specific gravity that the difference of the degree of various composition determines grinding bead provides guarantee for grinding high-level efficiency; The performance of slurry can be had a certain impact by the wear and tear of the chemistry composition of grinding bead in process of lapping, so except considering low wear rate, chemical element is also the factor to be considered. Order is such as grinding tape powder or other electronic component slurries, and the elements such as metal Fe, Cu should be avoided, containing Fe2O3Or CuSO4Deng the grinding bead of composition just not at the row of selections, therefore the general choice of selection zirconium pearl the industry often; As ground agricultural chemicals, medicine and biochemical aspect, heavy metal is scruple element, and PbO is modal composition. The pollution condition of slurry is the factor selecting grinding medium to be considered by some physicalies (hardness, density, wear resistance) that the chemistry composition of pearl determines and the abrasion of itself.
Current common drug Ginding process has impacting with high pressure, homogeneous cutting etc.; But when being applied to toughness medicine, mesh-of-grind is all undesirable, but also affects the stability of medicine. And when adopting grinding bead to grind, when drug slurries is feeding-up, it is easy to cause the heap sum of grinding bead directly to contact the abrasion piece of shredder and accelerate abrasion and the fragmentation of pearl, and then affect the stability of Grinding Quality and medicine.
Summary of the invention
It is an object of the invention to overcome the deficiency of above-mentioned prior art existence, it is provided that a kind of toughness medicine zirconium pearl Ginding process. The present invention adopts the relevant art that high rigidity zirconium pearl combines, and solves the grinding distribution problem of toughness medicine, makes medicine reach ultra-fine stable, and guarantees drug safety.
It is an object of the invention to be achieved through the following technical solutions:
The present invention relates to a kind of toughness medicine zirconium pearl Ginding process, described method comprises the steps:
A, the circular zirconium pearl preparing diameter and be 1.0～2.0 millimeters;
B, described zirconium pearl being put into the stainless steel vessel that rotating disk is housed, after adding toughness medicine, start rotating disk and drive the upper and lower rolling type grinding of zirconium pearl, grinding rotating speed is 800～2800 revs/min.
Preferably, described milling time regulates according to the viscosity of toughness medicine.
Preferably, described zirconium pearl is yttria-stabilized zirconia microballoon.
Preferably, the preparation of described zirconium pearl comprises the steps:
A, employing Y2O3-ZrO2Powder body rolling method prepares yttria-stabilized zirconia green microspheres;
B, described green microspheres being carried out staged sintering, furnace cooling after insulation 1～3h, obtains described zirconium pearl; Described staged sintering process system is: room temperature to 1000 DEG C, and temperature rise rate is 100 DEG C/h; 1000 DEG C to 1500 DEG C, temperature rise rate is 50 DEG C/h.
Preferably, the spray water used in described powder body rolling method contains 0.3wt%PVA binding agent.
Preferably, described Y2O3-ZrO2The preparation of powder body comprises the steps:
A, by Y2O3Content is the ratio of 3mol%, configuration ZrO (NO3)2.2H2O and Y (NO3)3.6H2O mixing solutions is mother liquor; ZrO (NO in described mixing mother liquor3)2Concentration be 0.25～1.5mol/L;
B, at 80 DEG C, adding chitosan and pectin, adjust ph is 1～3, and ageing polymerization forms gel, dry, obtains presoma;
C, presoma is heat-treated, obtain described Y2O3-ZrO2Powder body.
Preferably, described thermal treatment temp is 600～800 DEG C, and heat treatment time is 1～3h.
Compared with prior art, the present invention has following useful effect:
1, the zirconium pearl hardness of the present invention is superpower, with during medicament contact without abrasive conditions, drug safety can be guaranteed.
2, medicine can be ground to form ultra tiny degree by the zirconium pearl of the present invention in high speed rotating, the stability of toughness medicine is improved, and is conducive to absorption of human body.
3, yttria-stabilized zirconia micro-pearl proportion is 1.6 times of common zirconium oxide bead, has higher mill efficiency under equal conditions.
4, the micro-pearl good toughness of yttria-stabilized zirconia, abrasion only have the 1/2 of zirconium silicate pearl.
5, adopting powder body rolling method directly to prepare yttria-stabilized zirconia microballoon, facility investment is little, and production cost is low.
Accompanying drawing explanation
By reading with reference to the detailed description that non-limiting example is done by the following drawings, the other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is the infared spectrum of yttria-stabilized zirconia presoma; Wherein, 1 is the infared spectrum of presoma, and 2 is the infared spectrum of pectin, and 3 is the infared spectrum of chitosan;
The XRD figure of the yttria-stabilized zirconia powder of preparation when Fig. 2 is different concns;
Fig. 3 be nifedipine bulk drug, two kinds of grinding mixture XRD compare schematic diagram; Wherein, 4 is the mixture after 95 zirconium pearls are ground, and 5 is the mixture after the grinding of yttria-stabilized zirconia pearl, and 6 is nifedipine bulk drug.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail. The technician contributing to this area is understood the present invention by following examples further, but does not limit the present invention in any form. It should be appreciated that to those skilled in the art, without departing from the inventive concept of the premise, it is also possible to make some distortion and improvement. These all belong to protection scope of the present invention.
Embodiment 1
The present embodiment relates in toughness medicine zirconium pearl Ginding process the preparation of the zirconium pearl yttria-stabilized zirconia microballoon of 1.0～2.0 millimeters (diameter be) used; Described method specifically comprises the steps:
A, by Y2O3Content is the ratio of 3mol%, configuration ZrO (NO3)2.2H2O and Y (NO3)3.6H2O mixing solutions is mother liquor; Get ZrO (NO in mixing mother liquor3)2Concentration be respectively 0.25mol/L, 0.75mol/L, 1.5mol/L;
B, at 80 DEG C, adding chitosan and pectin, adjust ph is 1, and ageing polymerization forms gel, dry, obtains presoma;
ZrO(NO3)2The presoma corresponding when being 0.75mol/L of concentration infrared spectra as shown in Figure 1, at the stretching vibration peak that wave number 3410/cm annex is O-H in gelinite, the stretching vibration peak of-the COOH at 1630/cm place and chitosan are compared with pectin and are strengthened to some extent, and at 1422cm-1Stretching vibration peak and the chitosan at place is compared with pectin and be there occurs frequency displacement, illustrates that Zr, Y-ion and chitosan and pectin define stable polymkeric substance.
C, presoma is heat-treated, obtain 3mol%Y2O3-ZrO2Powder body; Thermal treatment temp is 600～800 DEG C, and heat treatment time is 1～3h.
The XRD figure of the yttria-stabilized zirconia powder of preparation when Fig. 2 is different concns, as shown in Figure 2, the sample obtained under 0.25～1.5mol/L concentration conditions is obtained for obvious cube of phase character collection of illustrative plates in XRD characterizes, and illustrates that the method can obtain cube phase of stable yttria-stabilized zirconia.
Y obtained when research zirconates concentration is 2.0mol/L, 3.0mol/L further2O3-ZrO2Powder body, it has been found that still can obtain stable cube phase at 2.0mol/L, 3.0mol/L, but transmission electron microscope finds, and strength of solution is more big, and the reunion of generation is more many. This is owing to zirconates concentration is greater than 1.5mol/L, and the production concentration causing hydrolysis to obtain increases, and causes aggregation of particles or precipitation. Reunion is many, will be unfavorable for follow-up powder body rolling technique; The Y that zirconates concentration 2mol/L, 3mol/L are obtained2O3-ZrO2Below, powder body rolling operation fails powder body.
D, by 3mol%Y2O3-ZrO2Powder body rolling method prepares yttria-stabilized zirconia green microspheres;
The principle of powder body rolling method is with alumina-ceramic rolling, using simple rotatable ball machine, first add prefabricated ball base crystal seed, then ceramic powder is added on limit rotary water jet mist limit, powder body constantly adheres to seed surface and grows up gradually, finally obtains the ball base of desired size. Concrete technique is: isostatic cool pressing powder body blank, and--broken--sieve prefabricated crystal seed, and------------roll atomized water spray atomized water spray--rolling surface finish--drying--ball base of growing up to predetermined size to add powder to add powder to add bowling machine rolling. The spray water used in the present embodiment contains 0.3wt%PVA binding agent. It has been generally acknowledged that zirconia ball is difficult to rolling at present shaping, its major cause be the requirement to powder body unclear caused by; Zirconium powder prepared by hydrothermal co-precipitation, its powder body is too bulk, and specific surface area is very big, is not thus suitable for powder body rolling method and prepares ball base; The present invention can be applicable to the shaping reason of powder body rolling may be that the yttria-stabilized zirconia powder obtained has stable cube phase, reunites few.
E, described green microspheres being carried out staged sintering, furnace cooling after insulation 1～3h, obtains described zirconium pearl; Described staged sintering process system is: room temperature to 1000 DEG C, and temperature rise rate is 100 DEG C/h; 1000 DEG C to 1500 DEG C, temperature rise rate is 50 DEG C/h.
The micro-pearl of yttria-stabilized zirconia of obtained diameter 3mm is carried out performance test, and the performance recorded is such as table 1:
Volume density measures: the micro-pearl after sintering is measured at ten thousand/precision sky chessboard its dry weight and the weight in water respectively, calculates the volume density of micro-pearl by Archimedes's method.
Measure from wear rate: get micro-pearl 1kg, it is designated as ml (precision 0.01g), load 1L ball-aluminium oxide ceramic pot, add 500ml deionized water, vibration 5h on vibrating ball mill, takes out sample clean clean, weighs in 80 DEG C of oven dry, it is designated as m2, from wear rate=1000 (m1-m2)/5ml.
Crushing strength measures: at the alumina ceramic plate that the upper push-down head place liner 10mm of 100kN universal testing machine is thick, to treat that micrometer pearl is placed therebetween, pressure is applied until fragmentation with the loading rate of 0.5mm/min, record peak pressure is crushing strength, each survey three samples, average as average crush strength.
Table 1
Embodiment 2
The present embodiment relates to toughness medicine zirconium pearl Ginding process, it is specially and adopts the obtained diameter of embodiment 1 to be that the micro-pearl of 2mm yttria-stabilized zirconia is ground, it is specially: described zirconium pearl is put into the stainless steel vessel that rotating disk is housed, after adding toughness medicine, starting rotating disk and drive the upper and lower rolling type grinding of zirconium pearl, grinding rotating speed is 800～2800 revs/min; Milling time regulates according to the viscosity of toughness medicine.
For nifedipine, carry out grinding experiment. Nifedipine belongs to insoluble drug, limits by dissolution characteristics, there is dissolution rate low, the problem that bioavailability is low. For improving bioavailability, by adopting grinding to reduce particle diameter, increase effective stripping area of medicine, and then improve the dissolution rate of medicine. The stability of mill efficiency and the rear medicine of grinding weighs the important evidence of sticky thick medicine grinding scheme. The micro-pearl of the yttria-stabilized zirconia of the present invention lower compared with 95 zirconium pearls from wear rate and better hardness, thus mill efficiency is better.
Being the 95 zirconium pearls of 2mm respectively taking diameter, zirconates concentration is that nifedipine is ground by the micro-pearl of yttria-stabilized zirconia that 0.75mol/L obtains. It is specially: get nifedipine bulk drug 50g, adds the HPMC auxiliary material solution 100g that massfraction is 20%, all mixed; Micro-to zirconium pearl or yttria-stabilized zirconia pearl being put into the stainless steel vessel that rotating disk is housed, adds mixed equal toughness medicine, start rotating disk and drive the upper and lower rolling type grinding of zirconium pearl, grinding rotating speed is 2000 revs/min; Milling time 1h.
Respectively nifedipine bulk drug, two kinds of grinding mixture being carried out XRD determining, experiment condition: CuKa target graphite monochromator device diffracted beam monochromeization, high pressure 40KV, single current 40mA, scanning 2 θ angles is 5～60 °, and sweep velocity is 2 ° of min-1Unit. Scanning result is such as Fig. 3. As seen from the figure, nifedipine is typical crystalline compounds, all there is obvious crystalline diffraction peak at 8.086 °, 10.392 °, 11.746 °, 14.637 °, 16.208 °, 17.010 °, 19.550 °, 24.597 ° places. The peak crystallization of two kinds of grinding mixture Chinese traditional medicines all exists, and consistent with untreated bulk drug, therefore can determine that process of lapping does not cause brilliant type to transform. In 95 zirconium pearl abrasive materials, the diffraction peak of medicine is weakened; Thus can think that the stability of the rear medicine of the yttria-stabilized zirconia of the present invention micro-pearl grinding is better.
Above specific embodiments of the invention are described. It is understood that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect the flesh and blood of the present invention.
Claims (3)
1. a toughness medicine zirconium pearl Ginding process, it is characterised in that, described method comprises the steps:
A, the circular zirconium pearl preparing diameter and be 1.0～2.0 millimeters;
B, described zirconium pearl being put into the stainless steel vessel that rotating disk is housed, after adding toughness medicine, start rotating disk and drive the upper and lower rolling type grinding of zirconium pearl, grinding rotating speed is 800～2800 revs/min;
Described zirconium pearl is yttria-stabilized zirconia microballoon;
The preparation of described zirconium pearl comprises the steps:
A, employing Y2O3-ZrO2Powder body rolling method prepares yttria-stabilized zirconia green microspheres;
B, described green microspheres being carried out staged sintering, furnace cooling after insulation 1～3h, obtains described zirconium pearl; Described staged sintering process system is: room temperature to 1000 DEG C, and temperature rise rate is 100 DEG C/h; 1000 DEG C to 1500 DEG C, temperature rise rate is 50 DEG C/h;
The spray water used in described powder body rolling method contains 0.3wt%PVA binding agent;
Described Y2O3-ZrO2The preparation of powder body comprises the steps:
A, by Y2O3Content is the ratio of 3mol%, configuration ZrO (NO3)22H2O and Y (NO3)36H2O mixing solutions is mother liquor; ZrO (NO in described mixing mother liquor3)2Concentration be 0.25～1.5mol/L;
B, at 80 DEG C, adding chitosan and pectin, adjust ph is 1～3, and ageing polymerization forms gel, dry, obtains presoma;
C, presoma is heat-treated, obtain described Y2O3-ZrO2Powder body.
2. toughness medicine zirconium pearl Ginding process according to claim 1, it is characterised in that, described milling time regulates according to the viscosity of toughness medicine.
3. toughness medicine zirconium pearl Ginding process according to claim 1, it is characterised in that, described thermal treatment temp is 600～800 DEG C, and heat treatment time is 1～3h.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4430279A (en) * | 1981-08-28 | 1984-02-07 | Nippon Tungsten Co., Ltd. | Process for producing zirconia yttria grinding media used for grinding magnetic coating powder |
| CN1441704A (en) * | 2000-05-10 | 2003-09-10 | 斯凯伊药品加拿大公司 | Medium milling |
| CN101209926A (en) * | 2007-12-22 | 2008-07-02 | 淄博华创精细陶瓷有限公司 | Method for preparing low cost zirconium oxide ceramic grinding medium |
| CN101252914A (en) * | 2005-05-05 | 2008-08-27 | 塞诺菲-安万特美国有限责任公司 | Stable nanoparticle formulations |
| CN102438593A (en) * | 2009-04-24 | 2012-05-02 | 伊休蒂卡有限公司 | Production of encapsulated nanoparticles at high volume fractions |
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- 2014-08-27 CN CN201410428007.3A patent/CN104174468B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4430279A (en) * | 1981-08-28 | 1984-02-07 | Nippon Tungsten Co., Ltd. | Process for producing zirconia yttria grinding media used for grinding magnetic coating powder |
| CN1441704A (en) * | 2000-05-10 | 2003-09-10 | 斯凯伊药品加拿大公司 | Medium milling |
| CN101252914A (en) * | 2005-05-05 | 2008-08-27 | 塞诺菲-安万特美国有限责任公司 | Stable nanoparticle formulations |
| CN101209926A (en) * | 2007-12-22 | 2008-07-02 | 淄博华创精细陶瓷有限公司 | Method for preparing low cost zirconium oxide ceramic grinding medium |
| CN102438593A (en) * | 2009-04-24 | 2012-05-02 | 伊休蒂卡有限公司 | Production of encapsulated nanoparticles at high volume fractions |
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