CN1541770A - Low-temperature ultramicro disintegrating method of Chinese traditional medicinal materials - Google Patents
Low-temperature ultramicro disintegrating method of Chinese traditional medicinal materials Download PDFInfo
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- CN1541770A CN1541770A CNA031397743A CN03139774A CN1541770A CN 1541770 A CN1541770 A CN 1541770A CN A031397743 A CNA031397743 A CN A031397743A CN 03139774 A CN03139774 A CN 03139774A CN 1541770 A CN1541770 A CN 1541770A
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- vibromill
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- 238000000034 method Methods 0.000 title claims abstract description 68
- 239000000463 material Substances 0.000 title abstract description 25
- 239000002826 coolant Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011089 carbon dioxide Nutrition 0.000 claims abstract description 10
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000000919 ceramic Substances 0.000 claims description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 26
- 239000003814 drug Substances 0.000 claims description 25
- 229940079593 drug Drugs 0.000 claims description 23
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 16
- 238000000498 ball milling Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 13
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 10
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 10
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 10
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 9
- 238000000975 co-precipitation Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 7
- 239000000292 calcium oxide Substances 0.000 claims description 7
- 239000000395 magnesium oxide Substances 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 7
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 7
- 238000007710 freezing Methods 0.000 claims description 6
- 230000008014 freezing Effects 0.000 claims description 6
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 16
- 239000012620 biological material Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 12
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 12
- 229910052785 arsenic Inorganic materials 0.000 description 12
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 12
- 229910052793 cadmium Inorganic materials 0.000 description 12
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 12
- 229910052802 copper Inorganic materials 0.000 description 12
- 239000010949 copper Substances 0.000 description 12
- 235000013312 flour Nutrition 0.000 description 12
- 229910052759 nickel Inorganic materials 0.000 description 12
- 229910052719 titanium Inorganic materials 0.000 description 12
- 239000010936 titanium Substances 0.000 description 12
- 229910052725 zinc Inorganic materials 0.000 description 12
- 239000011701 zinc Substances 0.000 description 12
- 239000011133 lead Substances 0.000 description 11
- 230000036760 body temperature Effects 0.000 description 10
- 238000001514 detection method Methods 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 6
- 238000000315 cryotherapy Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000009527 percussion Methods 0.000 description 3
- 230000004071 biological effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 230000008542 thermal sensitivity Effects 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 241000222336 Ganoderma Species 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 238000004137 mechanical activation Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000004531 microgranule Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
- Crushing And Grinding (AREA)
Abstract
The present invention relates to one kind of method suitable for super micro crushing of Chinese medicinal material. Vibrating mill with vibrating mill barrel lining grinding body of high-strength ceramic material is used as the super micro crusher. Before and/or during super micro crushing, the crushed material is freeze treated and/or the NO2 or dry ice as cooling agent is used to cool heating grinding parts. The method of the present invention is suitable for continuous industrial super micro crushing production of heat-sensitive biological material, such as Chinese medicinal material. The crushed Chinese medicinal material has granularity of 0.09-1.5 micron and no pollutant heavy metal detected, and the material temperature during super micro crushing is below 10 deg.c.
Description
Technical field
The present invention relates to a kind of method that is applicable to super micro crushing of Chinese medicinal material.
Background technology
It is heat subject in the internationalization of tcm Modern Manufacturing Technology that the Chinese crude drug ultramicron is pulverized.Be applied to the mechanized equipment in this field, as superfine grinding, micropowder is broken, devices such as micronizing arise at the historic moment, by strong extruding, shear, impact, bump, collision, grind, friction, cut stranding, the hole blast, mechanical activation comminution such as turbulence, though can reach the purpose that makes the material micronizing, but also cause material accepting the fierce impact of metal material percussion and grinding component simultaneously, bump, collision, grind, cut stranding, generate heat in the micronizing processes such as friction, reduce mechanical performance, and influence is by the biological activity of micronizing material, appearance heavy metal break flour microgranule in various degree peels off and disengages simultaneously, as chromium, nickel, cadmium, titanium, ferrum, copper, zinc, plumbous, heavy metals such as arsenic, make micronizing process Chinese medicine raw material be subjected to severe contamination, lose original medical value.
Summary of the invention
The purpose of this invention is to provide a kind of superfine comminution at low temperature method of Chinese crude drug, adopt this method, by fine Du Keda 0.09～1.5 μ m of the Chinese crude drug of micronizing, micronizing process temperature of charge is lower than 10 ℃; Chinese crude drug superfine powder after micronizing, pollution-free, heavy metal break flour microgranules such as Chrome-free, nickel, cadmium, titanium, ferrum, copper, zinc, lead, arsenic peel off and disengage; Can the medical value of Chinese crude drug after micronizing be more widely used through further being processed into medicine, health food.
The inventive method is to adopt to have the vibromill cylindrical shell lining that makes with high-strength ceramic material and the vibromill micron ultra shifter of abrasive body, before micronizing or/and the micronizing process will be pulverized raw material (Chinese crude drug) through freezing processing, in time cool off the heating grinding component or/and in the micronizing process, spray into nitrogen dioxide or add dry ice as coolant, Chinese crude drug is carried out superfine comminution at low temperature.
The inventive method described before micronizing or the micronizing process will be pulverized raw material through freezing pretreatment, its cryogenic temperature is generally-98～-5 ℃, is generally-78～-18 ℃.Describedly spray into nitrogen dioxide in (in cylindrical shell) or add dry ice as coolant in the micronizing process, its straying quatity or addition are generally 0.05～2 times by comminuting matter weight, are generally 0.2～0.4 times.
Superfine comminution at low temperature method of the present invention is suitable for the industrialization continuous production of the micronizing of thermal sensitivity biomaterial such as Chinese crude drug.
The basic structure of the micron ultra shifter that the inventive method is used is similar to common industrial micron ultra shifter vibromill, it is characterized in that having employing ZrO
2Material, perhaps ZrO
2Material adds nanometer Al
2O
3Or Y
2O
3, MgO, CaO the dusty material high-strength ceramic vibromill cylindrical shell lining and the abrasive body that make.
Described high-strength ceramic material cylindrical shell lining and abrasive body are to be that 90～99.6% (being generally 91～99.4%), granularity are monocline pure zirconia or the chemical co-precipitation method technology zirconium oxide (ZrO mutually of 0.5～1.6 μ m (being generally 0.7～1 μ m) with purity
2) raw material, according to required specification prefabricated molds base, form at 1200～1620 ℃ of (being generally 1400～1600 ℃) temperature sintering; Also can be at zirconium oxide (ZrO
2) to add purity in the raw material be the flexibilizer nano aluminium oxide (Al of 95～99.6% (being generally 96～99.4%)
2O
3) or yittrium oxide (Y
2O
3), in the magnesium oxide (MgO), calcium oxide (CaO) one or more, addition is that 0.2～20%wt (is generally 0.5～5%wt).
The specification of the high-strength pottery of described vibromill or high tenacity ceramic cylinder lining: the different model specification according to cylindrical shell determines that ceramic cylinder lining gauge thickness generally is 20～100mm, is generally 35～70mm;
The high-strength pottery of described vibromill or high tenacity ceramic grinding body can be ball milling body, short column body or cylinder; Ball milling body format diameter is 10～70mm, is generally 18～42mm; Short column body format diameter is 10～40mm, is generally 18～32mm, and length is 20～120mm, is generally 25～70mm; The cylinder format diameter is 10～45mm, is generally 18～32mm, and length is 120～850mm, is generally 150～500mm.
The placement amount of the high-strength pottery of described vibromill or high tenacity ceramic grinding body is decided on its cylindrical shell model specification and abrasive body size specification, is generally 180～800, is generally 250～500.
The common industrial vibration mill that the present invention relates to can be the inertial oscillation mill and revolve vibromill partially.
The inventive method is by controlled oxidation zirconium (ZrO
2) material purity, granularity and sintering temperature, also can select flexibilizer nano aluminium oxide (Al for use
2O
3) or high purity yttria (Y
2O
3), magnesium oxide (MgO), in the calcium oxide (CaO) one or more, obtain the high tenacity ceramic material grinding component of anti-percussion of high rigidity, fine and close tough and tensile, wear-resistant, erosion resistance, anti-thermal shock, be embedded in vibromill cylindrical shell lining and as abrasive body, very good to the biomaterial micronizing effect that requires micronizing process heavy metal free to pollute.Fierce high impact forces percussion of vibromill and abrasive action cause very easily frictional heating of abrasive body, because high tenacity ceramic material conductivity of heat is poor, the cooling-cycle device that is equipped with is not obvious to the high tenacity ceramic grinding body cooling effect of heating, therefore, the inventive method proposes for micronizing thermal sensitivity biomaterial, before pulverizing or crushing process will be by the micronizing raw material through freezing pretreatment, or in cylindrical shell, spray into nitrogen dioxide, or dry ice is as coolant, abrasive body can obtain effective cooling at the utmost point in the short time, makes pulverized Chinese crude drug reach the effect of micronizing in the short time and keep high biological activity at the utmost point.The inventive method is applicable to the Chinese crude drug superfine comminution at low temperature, because contact vibromill cylindrical shell of material and abrasive body are the high-strength pottery or the high tenacity ceramic material of high rigidity, wear-resistant, erosion resistance, anti-thermal shock, are not detected heavy metal pollution in the Chinese crude drug micropowder of micronizing.
The specific embodiment
Below in conjunction with embodiment the present invention is described in further detail.
The structure of the vibromill device that each embodiment superfine grinding method adopts and the preparation method of ceramic material cylindrical shell lining and abrasive body thereof as previously described, actual conditions and characteristic parameter are respectively as described in each embodiment.
Embodiment one:
1, monocline phase pure zirconia raw material 98.7%, purity 92%, granularity 0.5～0.8 μ m.
2, select nano aluminium oxide 0.9% for use, yittrium oxide 0.2%, calcium oxide 0.2%, flexibilizer material purity are 95～96%.
3, vibromill cylindrical shell lining and abrasive body specification are with reference to cylindrical shell model specification prefabricated molds base, and cylindrical shell lining gauge thickness is 56mm; Ball milling body format diameter is 29mm.
4, the blank sintering temperature of high-strength ceramic cylinder lining and abrasive body is 1610 ℃.
The high-strength ceramic cylinder lining that 5, will prepare is embedded in the vibromill cylindrical shell, is placed into 420 of high tenacity pottery ball milling bodies.
6, during comminuting matter, spray into coolant nitrogen dioxide at crushing process in cylindrical shell, straying quatity is 0.3 times by comminuting matter weight.
7, according to detection, micronizing process abrasive body temperature is lower than 5 ℃, and Chinese crude drug micropowder after crushed, fine degree reach 0.1 μ m, and be pollution-free, and heavy metal break flour microgranules such as Chrome-free, nickel, cadmium, titanium, ferrum, copper, zinc, lead, arsenic peel off and disengage.
Embodiment two:
1, monocline phase pure zirconia raw material 95%, purity 95%, granularity 0.6～0.7 μ m.
2, select flexibilizer nano aluminium oxide 4% for use, yittrium oxide 1%, flexibilizer material purity are 99.2%.
3, vibromill cylindrical shell lining and abrasive body specification are with reference to cylindrical shell model specification prefabricated molds base, and cylindrical shell lining gauge thickness is 63mm; Ball milling body format diameter is 38mm.
4, the blank sintering temperature of high tenacity ceramic cylinder lining and abrasive body is 1570 ℃.
5, the high tenacity ceramic cylinder lining with preparation is embedded in the vibromill cylindrical shell, is placed into 350 of high tenacity pottery ball milling bodies.
6, during comminuting matter, spray into coolant dry ice at crushing process in cylindrical shell, straying quatity is 0.25 times by comminuting matter weight.
7, according to detection, micronizing process abrasive body temperature is lower than 6 ℃, and Chinese crude drug micropowder after crushed, fine degree reach 0.2 μ m, and be pollution-free, and heavy metal break flour microgranules such as Chrome-free, nickel, cadmium, titanium, ferrum, copper, zinc, lead, arsenic peel off and disengage.
Embodiment three:
1, chemical co-precipitation method technology zirconium oxide raw material 91%, purity 99.5%, granularity 0.7～0.9 μ m.
2, select flexibilizer nano aluminium oxide 6%, yittrium oxide 3% for use, the flexibilizer material purity is 99.3%.
3, vibromill cylindrical shell lining and abrasive body specification are with reference to cylindrical shell model specification prefabricated molds base, and cylindrical shell lining gauge thickness is 41mm; Short column body format diameter 33mm, length is 50mm.
4, the blank sintering temperature of high-strength ceramic cylinder lining and abrasive body is 1598 ℃.
The high-strength ceramic cylinder lining that 5, will prepare is embedded in the vibromill cylindrical shell, is placed into 410 of high tenacity pottery short column bodies.
6, during comminuting matter, will be pulverized raw material through cryotherapy to-60 ℃.
7, according to detection, micronizing process abrasive body temperature is lower than 3 ℃, and Chinese crude drug micropowder after crushed, fine degree reach 0.15 μ m, and be pollution-free, and heavy metal break flour microgranules such as Chrome-free, nickel, cadmium, titanium, ferrum, copper, zinc, lead, arsenic peel off and disengage.
Embodiment four:
1, chemical co-precipitation method technology zirconium oxide raw material 96.8%, purity 98%, granularity 0.9～1.1 μ m.
2, select flexibilizer nano aluminium oxide 0.2% for use, yittrium oxide 1%, magnesium oxide 2%, the flexibilizer material purity is respectively 97%, 94% and 98%.
3, vibromill cylindrical shell lining and abrasive body specification are with reference to cylindrical shell model specification prefabricated molds base, and cylindrical shell lining gauge thickness is 48mm; Short column body format diameter 28mm, length is 58mm.
4, the blank sintering temperature of high tenacity ceramic cylinder lining and abrasive body is 1495 ℃.
5, the high tenacity ceramic cylinder lining with preparation is embedded in the vibromill cylindrical shell, is placed into 420 of high tenacity pottery short column bodies.
6, during comminuting matter, spray into coolant nitrogen dioxide before pulverizing in cylindrical shell, straying quatity is 0.35 times by comminuting matter weight.
7, according to detection, micronizing process abrasive body temperature is lower than 2 ℃, and Chinese crude drug micropowder after crushed, fine degree reach 0.4 μ m, and be pollution-free, and heavy metal break flour microgranules such as Chrome-free, nickel, cadmium, titanium, ferrum, copper, zinc, lead, arsenic peel off and disengage.
Embodiment five:
1, monocline phase pure zirconia raw material 99.6%, purity 95%, granularity 0.7～0.9 μ m.
2, select yittrium oxide 0.2% for use, calcium oxide 0.2%, flexibilizer material purity are 97～98.2%.
3, vibromill cylindrical shell lining and abrasive body specification are with reference to cylindrical shell model specification prefabricated molds base, and cylindrical shell lining gauge thickness is 68mm; The cylinder format diameter is 32mm, and length is 360mm.
4, the blank sintering temperature of high-strength ceramic cylinder lining and abrasive body is 1618 ℃.
The high-strength ceramic cylinder lining that 5, will prepare is embedded in the vibromill cylindrical shell, is placed into 390 of high tenacity pottery ball milling bodies.
6, during comminuting matter, spray into coolant dry ice at crushing process in cylindrical shell, straying quatity is 0.4 times by comminuting matter weight.
7, according to detection, micronizing process abrasive body temperature is lower than 10 ℃, and Chinese crude drug micropowder after crushed, fine degree reach 0.3 μ m, and be pollution-free, and heavy metal break flour microgranules such as Chrome-free, nickel, cadmium, titanium, ferrum, copper, zinc, lead, arsenic peel off and disengage.
Embodiment six:
1, chemical co-precipitation method technology zirconium oxide raw material 100%, purity 99%, granularity 0.7～0.8 μ m.
2, vibromill cylindrical shell lining and abrasive body specification are with reference to cylindrical shell model specification prefabricated molds base, and cylindrical shell lining gauge thickness is 60mm; Ball milling body format diameter is 38mm.
3, the blank sintering temperature of high-strength ceramic cylinder lining and abrasive body is 1610 ℃.
The high-strength ceramic cylinder lining that 4, will prepare is embedded in the vibromill cylindrical shell, is placed into 350 of high-strength ceramic ball milling bodies.
5, during comminuting matter, will be pulverized raw material through cryotherapy to-35 ℃.
6, according to detection, micronizing process abrasive body temperature is lower than 7 ℃, and Chinese crude drug micropowder after crushed, fine degree reach 0.5 μ m, and be pollution-free, and heavy metal break flour microgranules such as Chrome-free, nickel, cadmium, titanium, ferrum, copper, zinc, lead, arsenic peel off and disengage.
Embodiment seven:
1, monocline phase pure zirconia raw material 96.3%, purity 98%, granularity 0.75～0.95 μ m.
2, select flexibilizer nano aluminium oxide 0.8% for use, yittrium oxide 0.9%, calcium oxide 2%, flexibilizer material purity are 98.6%.
3, vibromill cylindrical shell lining and abrasive body specification are with reference to cylindrical shell model specification prefabricated molds base, and cylindrical shell lining gauge thickness is 56mm; The cylinder format diameter is 19mm, and length is 300mm.
4, the blank sintering temperature of high tenacity ceramic cylinder lining and abrasive body is 1600 ℃.
5, the high tenacity ceramic cylinder lining with preparation is embedded in the vibromill cylindrical shell, is placed into 410 of high tenacity pottery cylinders.
6, during comminuting matter, spray into coolant nitrogen dioxide at crushing process in cylindrical shell, straying quatity is 0.6 times by comminuting matter weight.
7, according to detection, micronizing process abrasive body temperature is lower than 5 ℃, and sporoderm-broken rate reaches 99.8% Ganoderma spore micropowder after crushed, and fine degree reaches 0.1 μ m, pollution-free, heavy metal break flour microgranules such as Chrome-free, nickel, cadmium, titanium, ferrum, copper, zinc, lead, arsenic peel off and disengage.
Embodiment eight:
1, chemical co-precipitation method technology zirconium oxide raw material 96%, purity 96.5%, granularity 0.7～0.75 μ m.
2, select flexibilizer nano yttrium oxide 2%, calcium oxide 2% for use, the flexibilizer material purity is 98.3%.
3, vibromill cylindrical shell lining and abrasive body specification are with reference to cylindrical shell model specification prefabricated molds base, and cylindrical shell lining gauge thickness is 60mm; Short column body format diameter 20m, length is 65mm.
4, the blank sintering temperature of high-strength ceramic cylinder lining and abrasive body is 1568 ℃.
The high-strength ceramic cylinder lining that 5, will prepare is embedded in the vibromill cylindrical shell, is placed into 380 of high tenacity pottery short column bodies.
6, during comminuting matter, will be pulverized raw material through cryotherapy to-58 ℃.
7, according to detection, micronizing process abrasive body temperature is lower than 3 ℃, and Chinese crude drug micropowder after crushed, fine degree reach 1 μ m, and be pollution-free, and heavy metal break flour microgranules such as Chrome-free, nickel, cadmium, titanium, ferrum, copper, zinc, lead, arsenic peel off and disengage.
Embodiment nine:
1, monocline phase pure zirconia raw material 98.7%, purity 99%, granularity 0.5～0.6 μ m.
2, select nano aluminium oxide 0.9% for use, yittrium oxide 0.2%, calcium oxide 0.2%, flexibilizer material purity are 97～98.5%.
3, vibromill cylindrical shell lining and abrasive body specification are with reference to cylindrical shell model specification prefabricated molds base, and cylindrical shell lining gauge thickness is 62mm; Ball milling body format diameter is 35mm.
4, the blank sintering temperature of high tenacity ceramic cylinder lining and abrasive body is 1480 ℃.
5, the high tenacity ceramic cylinder lining with preparation is embedded in the vibromill cylindrical shell, is placed into 280 of high tenacity pottery ball milling bodies.
6, during comminuting matter, spray into coolant nitrogen dioxide at crushing process in cylindrical shell, straying quatity is 0.18 times by comminuting matter weight.
7, according to detection, micronizing process abrasive body temperature is lower than 8 ℃, and Chinese crude drug micropowder after crushed, fine degree reach 1.5 μ m, and be pollution-free, and heavy metal break flour microgranules such as Chrome-free, nickel, cadmium, titanium, ferrum, copper, zinc, lead, arsenic peel off and disengage.
Embodiment ten:
1, chemical co-precipitation method technology zirconium oxide raw material 90%, purity 99%, granularity 0.75～0.9 μ m.
2, select flexibilizer nano aluminium oxide 10% for use, the flexibilizer material purity is 99.2%.
3, vibromill cylindrical shell lining and abrasive body specification are with reference to cylindrical shell model specification prefabricated molds base, and cylindrical shell lining gauge thickness is 65mm; Short column body format diameter 19mm, length is 100mm.
4, the blank sintering temperature of high tenacity ceramic cylinder lining and abrasive body is 1240 ℃.
5, the high tenacity ceramic cylinder lining with preparation is embedded in the vibromill cylindrical shell, is placed into 380 of high tenacity pottery short column bodies.
6, will be pulverized raw material through extremely-18 ℃ of cryotherapy; During comminuting matter, spray into coolant dry ice at crushing process in cylindrical shell, straying quatity is 0.59 times by the pulverize and break cellular wall weight of material.
7, according to detection, micronizing process abrasive body temperature is lower than 6 ℃, and Chinese crude drug micropowder after crushed, fine degree reach 1.4 μ m, and be pollution-free, and heavy metal break flour microgranules such as Chrome-free, nickel, cadmium, titanium, ferrum, copper, zinc, lead, arsenic peel off and disengage.
Claims (14)
1. the superfine comminution at low temperature method of a Chinese crude drug, it is characterized in that adopting and have the vibromill cylindrical shell lining that makes with high-strength ceramic material and the vibromill micron ultra shifter of abrasive body, before micronizing or/and the micronizing process will be pulverized raw material through freezing processing, in time cool off the heating grinding component or/and in the micronizing process, spray into nitrogen dioxide or add dry ice as coolant, Chinese crude drug is carried out superfine comminution at low temperature.
2. in accordance with the method for claim 1, it is characterized in that described before micronizing or the micronizing process will be pulverized raw material through freezing pretreatment, its cryogenic temperature is-98～-5 ℃; Describedly spray into nitrogen dioxide in the micronizing process or add dry ice as coolant, its straying quatity or addition are 0.05～2 times by comminuting matter weight.
3. in accordance with the method for claim 2, it is characterized in that described before micronizing or the micronizing process will be pulverized raw material through freezing pretreatment, its cryogenic temperature is-78～-18 ℃; Describedly spray into nitrogen dioxide in the micronizing process or add dry ice as coolant, its straying quatity or addition are 0.2～0.4 times.
4. according to claim 1,2 or 3 described methods, the high-strength ceramic material cylindrical shell lining that it is characterized in that used micron ultra shifter and abrasive body are with purity is 90～99.6%, granularity is 0.5～1.6 μ m monocline pure zirconia or chemical co-precipitation method technology zirconium oxide raw material mutually, according to required specification prefabricated molds base, form at 1200～1620 ℃ of temperature sintering.
5. in accordance with the method for claim 4, the high-strength ceramic material cylindrical shell lining that it is characterized in that used micron ultra shifter and abrasive body are with purity is 91～99.4%, granularity is 0.7～1 μ m monocline pure zirconia or chemical co-precipitation method technology zirconium oxide raw material mutually, according to required specification prefabricated molds base, form at 1400～1600 ℃ of temperature sintering.
6. in accordance with the method for claim 4, it is characterized in that also being added with purity and be in 95～99.6% flexibilizer nano aluminium oxide or yittrium oxide, magnesium oxide, the calcium oxide one or more in the zirconium oxide raw material, addition is 0.2～20%wt.
7. in accordance with the method for claim 6, it is characterized in that the purity of the flexibilizer that added is 96～99.4%, addition is 0.5～5%wt.
8. according to the described method of claim 1,2 or 3, it is characterized in that the high-strength pottery of described vibromill or high tenacity ceramic cylinder lining gauge thickness are 20～100mm.
9. in accordance with the method for claim 8, the ceramic cylinder lining gauge thickness that it is characterized in that described vibromill is 35～70mm.
10. according to the described method of claim 1,2 or 3, it is characterized in that the high-strength pottery of described vibromill or high tenacity ceramic grinding body are ball milling body, short column body or cylinder.
11. in accordance with the method for claim 10, it is characterized in that described ball milling body format diameter is 10～70mm; Short column body format diameter is 10～40mm, and length is 20～120mm; The cylinder format diameter is 10～45mm, and length is 120～850mm.
12. in accordance with the method for claim 11, it is characterized in that described ball milling body format diameter is 18～42mm; Short column body format diameter is 18～32mm, and length is 25～70mm; The cylinder format diameter is 18～32mm, and length is 150～500mm.
13., it is characterized in that the high-strength pottery of described vibromill or high tenacity ceramic grinding body placement amount are 180～800 according to the described method of claim 1,2 or 3.
14. it is characterized in that in accordance with the method for claim 13, the high-strength pottery of described vibromill or high tenacity ceramic grinding body placement amount are 250～500.
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