CN1289199C - 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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- CN1289199C CN1289199C CN 03139774 CN03139774A CN1289199C CN 1289199 C CN1289199 C CN 1289199C CN 03139774 CN03139774 CN 03139774 CN 03139774 A CN03139774 A CN 03139774A CN 1289199 C CN1289199 C CN 1289199C
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Abstract
The present invention relates to a method which is suitable for the super fine crushing of Chinese medicinal herbs. A vibration mill super fine crushing device is composed of a vibration mill barrel lining and a grinding element which are made of ceramic materials of high strength; crushed raw materials (the Chinese medical herbs) are frozen before super fine crushing or/and the super fine crushing process; or/and nitrogen oxide is sprayed into the raw materials in the super fine process, or dry ice is added as a coolant for cooling in time and heating the grinding element, and then the Chinese medicinal herbs are processed by super fine crushing at low temperature. The method of the present invention is suitable for the super fine crushing industrialization continuous production of thermal sensitivity biological materials, such as Chinese medicinal herbs. The super fineness of the Chinese medicinal herbs in the super fine crushing is 0.09 to 1.5 mu m, material temperature in the super fine process is lower than 10 DEG C, and no heavy metal pollution is measured in the super fine crushing materials.
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 medicine ultramicron is pulverized.Be applied to the mechanized equipment in this field, as ultra-fine grinding, micro mist is broken, devices such as ultramicro grinding arise at the historic moment, by strong extruding, shear, impact, bump, collision, grind, friction, cut stranding, the hole blast, mechanical crushing such as turbulence, though can reach the purpose that makes the material ultramicro grinding, 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 ultramicro grinding processes such as friction, reduce mechanical performance, and influence is by the biologically active of ultramicro grinding material, appearance heavy metal break flour particulate in various degree peels off and disengages simultaneously, as chromium, nickel, cadmium, titanium, iron, copper, zinc, plumbous, heavy metals such as arsenic, make ultramicro grinding process Chinese traditional 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 low temperature superfine grinding method of Chinese medicine, adopt this method, by fine Du Keda 0.09～1.5 μ m of the Chinese medicine of ultramicro grinding, ultramicro grinding process temperature of charge is lower than 10 ℃; Chinese medicine ultra micro powder after ultramicro grinding, pollution-free, heavy metal break flour particulates such as Chrome-free, nickel, cadmium, titanium, iron, copper, zinc, lead, arsenic peel off and disengage; Can the medical value of Chinese medicine after ultramicro grinding 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 ultramicro grinding or/and the ultramicro grinding process will be pulverized raw material (Chinese medicine) through freezing processing, in time cool off the heating grinding component or/and in the ultramicro grinding process, spray into nitrogen dioxide or add dry ice as cooling agent, Chinese medicine is carried out the low temperature ultramicro grinding.
The inventive method described before ultramicro grinding or the ultramicro grinding process will be pulverized raw material through freezing preliminary treatment, 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 cooling agent in the ultramicro grinding process, its straying quatity or addition are generally 0.05～2 times by comminuting matter weight, are generally 0.2～0.4 times.
The industrialization that low temperature superfine grinding method of the present invention is suitable for the ultramicro grinding of thermal sensitivity biomaterial such as Chinese medicine is produced continuously.
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 zirconia (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 zirconia (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 magnesia (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 control zirconia (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), magnesia (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 ultramicro grinding effect that requires ultramicro grinding 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 ultramicro grinding thermal sensitivity biomaterial, before pulverizing or crushing process will be by the ultramicro grinding raw material through freezing preliminary treatment, or in cylindrical shell, spray into nitrogen dioxide, or dry ice is as cooling agent, abrasive body can obtain effective cooling at the utmost point in the short time, makes pulverized Chinese medicine reach the effect of ultramicro grinding in the short time and keep high biologically active at the utmost point.The inventive method is applicable to Chinese medicine low temperature ultramicro grinding, 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 medicine micro mist of ultramicro grinding.
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 cooling agent nitrogen dioxide at crushing process in cylindrical shell, straying quatity is 0.3 times by comminuting matter weight.
7, according to detection, ultramicro grinding process abrasive body temperature is lower than 5 ℃, and Chinese medicine micro mist after crushed, fine degree reach 0.1 μ m, and be pollution-free, and heavy metal break flour particulates such as Chrome-free, nickel, cadmium, titanium, iron, 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 cooling agent dry ice at crushing process in cylindrical shell, straying quatity is 0.25 times by comminuting matter weight.
7, according to detection, ultramicro grinding process abrasive body temperature is lower than 6 ℃, and Chinese medicine micro mist after crushed, fine degree reach 0.2 μ m, and be pollution-free, and heavy metal break flour particulates such as Chrome-free, nickel, cadmium, titanium, iron, copper, zinc, lead, arsenic peel off and disengage.
Embodiment three:
1, chemical co-precipitation method technology zirconia 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 superfreeze to-60 ℃.
7, according to detection, ultramicro grinding process abrasive body temperature is lower than 3 ℃, and Chinese medicine micro mist after crushed, fine degree reach 0.15 μ m, and be pollution-free, and heavy metal break flour particulates such as Chrome-free, nickel, cadmium, titanium, iron, copper, zinc, lead, arsenic peel off and disengage.
Embodiment four:
1, chemical co-precipitation method technology zirconia 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%, magnesia 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 cooling agent nitrogen dioxide before pulverizing in cylindrical shell, straying quatity is 0.35 times by comminuting matter weight.
7, according to detection, ultramicro grinding process abrasive body temperature is lower than 2 ℃, and Chinese medicine micro mist after crushed, fine degree reach 0.4 μ m, and be pollution-free, and heavy metal break flour particulates such as Chrome-free, nickel, cadmium, titanium, iron, 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 cooling agent dry ice at crushing process in cylindrical shell, straying quatity is 0.4 times by comminuting matter weight.
7, according to detection, ultramicro grinding process abrasive body temperature is lower than 10 ℃, and Chinese medicine micro mist after crushed, fine degree reach 0.3 μ m, and be pollution-free, and heavy metal break flour particulates such as Chrome-free, nickel, cadmium, titanium, iron, copper, zinc, lead, arsenic peel off and disengage.
Embodiment six:
1, chemical co-precipitation method technology zirconia 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 superfreeze to-35 ℃.
6, according to detection, ultramicro grinding process abrasive body temperature is lower than 7 ℃, and Chinese medicine micro mist after crushed, fine degree reach 0.5 μ m, and be pollution-free, and heavy metal break flour particulates such as Chrome-free, nickel, cadmium, titanium, iron, 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 cooling agent nitrogen dioxide at crushing process in cylindrical shell, straying quatity is 0.6 times by comminuting matter weight.
7, according to detection, ultramicro grinding 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 particulates such as Chrome-free, nickel, cadmium, titanium, iron, copper, zinc, lead, arsenic peel off and disengage.
Embodiment eight:
1, chemical co-precipitation method technology zirconia 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 superfreeze to-58 ℃.
7, according to detection, ultramicro grinding process abrasive body temperature is lower than 3 ℃, and Chinese medicine micro mist after crushed, fine degree reach 1 μ m, and be pollution-free, and heavy metal break flour particulates such as Chrome-free, nickel, cadmium, titanium, iron, 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 cooling agent nitrogen dioxide at crushing process in cylindrical shell, straying quatity is 0.18 times by comminuting matter weight.
7, according to detection, ultramicro grinding process abrasive body temperature is lower than 8 ℃, and Chinese medicine micro mist after crushed, fine degree reach 1.5 μ m, and be pollution-free, and heavy metal break flour particulates such as Chrome-free, nickel, cadmium, titanium, iron, copper, zinc, lead, arsenic peel off and disengage.
Embodiment ten:
1, chemical co-precipitation method technology zirconia 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 superfreeze; During comminuting matter, spray into cooling agent 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, ultramicro grinding process abrasive body temperature is lower than 6 ℃, and Chinese medicine micro mist after crushed, fine degree reach 1.4 μ m, and be pollution-free, and heavy metal break flour particulates such as Chrome-free, nickel, cadmium, titanium, iron, copper, zinc, lead, arsenic peel off and disengage.
Claims (12)
1. the low temperature superfine grinding method of a Chinese medicine, 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 ultramicro grinding or/and the ultramicro grinding process will be pulverized raw material through freezing processing, in time cool off the heating grinding component or/and in the ultramicro grinding process, spray into nitrogen dioxide or add dry ice as cooling agent, Chinese medicine is carried out the low temperature ultramicro grinding; Described before ultramicro grinding or the ultramicro grinding process will be pulverized raw material through freezing preliminary treatment, its cryogenic temperature is-78～-18 ℃; Describedly spray into nitrogen dioxide or add dry ice as cooling agent in the ultramicro grinding process, its straying quatity or addition are 0.2～0.4 times by comminuting matter weight.
2. in accordance with the method for claim 1, 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 zirconia raw material mutually, according to required specification prefabricated molds base, form at 1200～1620 ℃ of temperature sintering.
3. in accordance with the method for claim 2, 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 zirconia raw material mutually, according to required specification prefabricated molds base, form at 1400～1600 ℃ of temperature sintering.
4. according to claim 2 or 3 described methods, it is characterized in that in the zirconia raw material, also being added with purity and be in 95～99.6% flexibilizer nano aluminium oxide or yittrium oxide, magnesia, the calcium oxide one or more, addition is 0.2～20%wt.
5. in accordance with the method for claim 4, it is characterized in that the purity of the flexibilizer that added is 96～99.4%, addition is 0.5～5%wt.
6. in accordance with the method for claim 1, it is characterized in that the high-strength pottery of described vibromill or high tenacity ceramic cylinder lining gauge thickness are 20～100mm.
7. in accordance with the method for claim 6, the ceramic cylinder lining gauge thickness that it is characterized in that described vibromill is 35～70mm.
8. in accordance with the method for claim 1, 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.
9. in accordance with the method for claim 8, 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.
10. in accordance with the method for claim 9, 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.
11. it is characterized in that in accordance with the method for claim 1, the high-strength pottery of described vibromill or high tenacity ceramic grinding body placement amount are 180～800.
12. it is characterized in that in accordance with the method for claim 11, the high-strength pottery of described vibromill or high tenacity ceramic grinding body placement amount are 250～500.
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| CN100577134C (en) * | 2006-12-30 | 2010-01-06 | 中国人民解放军第三军医大学第一附属医院 | Super micronization method for botanical medicinal, product obtained thereby and use thereof |
| US20120289559A1 (en) * | 2009-11-13 | 2012-11-15 | Toshiyuki Niwa | Method for producing fine powder and the fine powder produced by the same |
| US9044758B2 (en) * | 2009-11-13 | 2015-06-02 | Moriroku Chemicals Company, Ltd. | Method for producing fine powder and the fine powder produced by the same |
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| CN1541770A (en) | 2004-11-03 |
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