CN114988444A - Preparation method of nano alumina microspheres special for antibiotic decolorization - Google Patents
Preparation method of nano alumina microspheres special for antibiotic decolorization Download PDFInfo
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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Abstract
The microsphere alumina prepared by the scheme has the particle size of not less than 150 mu m and high porosity, so that the penetrating power and the penetrating speed are high in the process of decolorizing the antibiotics, the production capacity is greatly improved, the pore volume of the microsphere alumina is not less than 0.8 ml/g, the specific surface area is not less than 200 square meters per gram, the adsorption capacity is high in the process of decolorizing the antibiotics, the decolorizing effect is good, and the product quality is greatly improved.
Description
Technical Field
The invention relates to a preparation process technology of an alumina decolorant, in particular to a preparation method of a special nano alumina microsphere for antibiotic decoloration.
Background
The nanometer microsphere is a small sphere with the grain diameter of micron order, can be used as a medicine decoloration, a catalyst carrier, a liquid crystal spacer, an enzyme carrier and the like, and is widely applied to the industries of biological pharmacy, chemical production, food safety detection, medical diagnosis and the like.
China has been imported from Japan mainly before, is monopolized by several Japanese enterprises, and is expensive. At present, the Jiangsu nano micro-technology company in China can also produce high-quality liquid crystal materials used by liquid crystal screens, but the decoloration of medical intermediates mainly uses powder materials with irregular shapes, such as antibiotics such as cefazolin sodium, cefotaxime sodium, cefradine, cefoselis and the like, and the production processes of traditional Chinese medicine flavone, notoginsenoside, matrine and the like need decoloration and chromatography, and the particle size of the decolorant used is mainly concentrated at 50-75 mu m; the specific surface area is 120-150 m2/g, and the pore volume is 0.22-0.25 ml/g. The decoloring agent has low transmission rate and weak adsorption capacity in the decoloring process of medicines due to small particle size, small pore volume and low specific surface, and the production capacity and the product quality are seriously influenced. The requirements of manufacturers on the decolorization of the drug intermediate are higher and higher, and correspondingly, higher requirements are put forward on various technical indexes of alumina for decolorization. This necessitates the preparation of higher performance bleached alumina.
Application No. 201410347664.5, App. 20140722, discloses a preparation method of large-pore-volume and high-viscosity pseudo-boehmite, and the pseudo-boehmite with the peptization index of more than or equal to 99%, the pore volume of more than or equal to 0.80mL/g and the specific surface area of more than or equal to 200 m2/g can be prepared by the preparation method.
Disclosure of Invention
The invention mainly solves the technical problem of providing a preparation method of nano alumina microspheres special for decoloring antibiotics, and the alumina microspheres have the characteristics of high porosity, large pore volume, high specific surface area, high permeation rate and strong adsorption capacity in the adsorption and decoloring processes of cefazolin sodium, cefotaxime sodium, ceftazidime and cefoselis.
In order to solve the technical problems, the invention provides a preparation method of nano alumina microspheres special for antibiotic decoloration, which comprises the following steps:
the pore volume is selected to be more than or equal to 0.8 ml/g and the specific surface area is selected to be more than or equal to 200 m in the step (1) 2 (ii)/g of trabeconite with peptization index of more than or equal to 99 percent;
placing the pseudo-boehmite into a distilled water containing batching tank to start stirring, and controlling the mass concentration of the alumina in the liquid to be 50 g/L;
adding 1-10% of dilute nitric acid into a batching tank, then adding steam, heating to 90 ℃, continuing stirring for 2 hours to change liquid into glue solution, and controlling the kinematic viscosity of the glue solution to be 70-80 mm 2 /s；
The glue solution prepared in the step (4) is stored in a storage trough through a bottom series valve, and the storage trough keeps the temperature of 80-85 ℃;
step (5), pumping the glue solution in the storage material tank to a material turntable rotating at a high speed by using a hose for granulation to obtain microspheres;
dropping the microspheres into a drying tower through a distributor, and drying the microspheres by hot air at 350-400 ℃ from a hot air furnace to remove surface adsorbed water;
roasting the dried microspheres in a rotary kiln at the temperature of 500-800 ℃ for 3h for crystal form conversion to gamma-Al 2 O 3 ；
And (8) naturally cooling to room temperature, and then screening and packaging by using a multilayer vibrating screen to obtain the nano alumina microspheres special for antibiotic decoloration.
In the step (3), the concentration of the dilute nitric acid is 1-10%, preferably 2-8%, and more preferably 3-5%.
In the step (5), the rotating speed of the material rotating disc is 10000/min.
In the step (7), the roasting temperature is 500-800 ℃, preferably 550-750 ℃, and more preferably 600-700 ℃.
The nano-alumina microspheres prepared by the technical scheme of the invention have the following advantages:
1. the particle size of the nano alumina microspheres is more than or equal to 150 mu m, the porosity is high, the penetration capacity is strong in the process of decoloring the antibiotic, the penetration rate is high, and the production capacity is greatly improved;
2. the pore volume of the nano alumina microspheres is more than or equal to 0.8 ml/g, and the specific surface area is more than or equal to 200 m 2 The/g, the adsorption capacity is strong in the process of decoloring the antibiotics, the decoloring effect is good, and the product quality is greatly improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) The pore volume is not less than 0.8 ml/g, the specific surface area is not less than 200 m 2 (ii)/g of trabeconite with peptization index of more than or equal to 99 percent;
(2) placing pseudo-boehmite into a distilled water containing batching tank to start stirring, and controlling the mass concentration of alumina in liquid to be 50 g/L;
(3) adding 1% dilute nitric acid into a batching tank, then adding steam, heating to 90 ℃, continuing stirring for 2 hours to change liquid into glue solution, and controlling the kinematic viscosity of the glue solution to be 70-80 mm 2 /s；
(4) The prepared glue solution is stored in a storage trough through a bottom series valve, and the storage trough keeps the temperature at 80-85 ℃;
(5) pumping the glue solution in the storage material tank to a material turntable rotating at a high speed (10000/min) by using a hose for granulation to obtain microspheres;
(6) dropping the microspheres into a drying tower through a distributor, and drying the microspheres by hot air at 350 ℃ from a hot air furnace to remove surface adsorbed water;
(7) roasting the dried microspheres in a rotary kiln at the temperature of 500 ℃ for 3h for carrying out crystal form conversion to convert the microspheres into gamma-Al 2 O 3 ；
(8) And naturally cooling to room temperature, and then screening and packaging by using a multilayer vibrating screen to obtain the nano alumina microspheres special for antibiotic decoloration.
The results of various performance tests on the obtained nano-alumina microspheres are shown in table 1.
Example 2
(1) The pore volume is not less than 0.8 ml/g, the specific surface area is not less than 200 m 2 (ii)/g of trabeconite with peptization index of more than or equal to 99 percent;
(2) placing pseudo-boehmite into a distilled water containing batching tank to start stirring, and controlling the mass concentration of alumina in liquid to be 50 g/L;
(3) adding 10% dilute nitric acid into a dosing tank, then adding steam, heating to 90 ℃, continuing stirring for 2 hours to change liquid into glue solution, and controlling the kinematic viscosity of the glue solution to be 70-80 mm 2 /s；
(4) The prepared glue solution is stored in a storage trough through a bottom series valve, and the storage trough keeps the temperature at 80-85 ℃;
(5) pumping the glue solution in the storage material tank to a material turntable rotating at a high speed (10000/min) by using a hose for granulation to obtain microspheres;
(6) the microspheres fall into a drying tower through a distributor and are dried by hot air at 400 ℃ from a hot air furnace to remove surface adsorbed water;
(7) roasting the dried microspheres in a rotary kiln at 800 ℃ for 3h for crystal form conversion to gamma-Al 2 O 3 ；
(8) And naturally cooling to room temperature, and then screening and packaging by using a multilayer vibrating screen to obtain the nano alumina microspheres special for antibiotic decoloration.
The results of various performance tests on the obtained nano-alumina microspheres are shown in table 1.
Example 3
(1) The selected pore volume is more than or equal to 0.8 ml/g, and the specific surface area is more than or equal to 200 m 2 (ii)/g of trabeconite with peptization index of more than or equal to 99 percent;
(2) placing pseudo-boehmite into a distilled water containing batching tank to start stirring, and controlling the mass concentration of alumina in liquid to be 50 g/L;
(3) adding 2% dilute nitric acid into a batching tank, then adding steam, heating to 90 ℃, continuing stirring for 2 hours to change liquid into glue solution, and controlling the kinematic viscosity of the glue solution to be 70-80 mm 2 /s；
(4) The prepared glue solution is stored in a storage trough through a bottom series valve, and the storage trough keeps the temperature at 80-85 ℃;
(5) pumping the glue solution in the storage material tank to a material turntable rotating at a high speed (10000/min) by a hose for granulation to obtain microspheres;
(6) dropping the microspheres into a drying tower through a distributor, and drying the microspheres by hot air at 350 ℃ from a hot air furnace to remove surface adsorbed water;
(7) roasting the dried microspheres in a rotary kiln at 550 ℃ for 3h for crystal form conversion to gamma-Al 2 O 3 ；
(8) And naturally cooling to room temperature, and then screening and packaging by using a multilayer vibrating screen to obtain the nano alumina microspheres special for antibiotic decoloration.
The results of various performance tests of the obtained nano-alumina microspheres are shown in table 1.
Example 4
(1) The selected pore volume is more than or equal to 0.8 ml/g, and the specific surface area is more than or equal to 200 m 2 (ii)/g of trabeconite with peptization index of more than or equal to 99 percent;
(2) placing pseudo-boehmite into a distilled water containing batching tank to start stirring, and controlling the mass concentration of alumina in liquid to be 50 g/L;
(3) adding 8% dilute nitric acid into a batching tank, then adding steam, heating to 90 ℃, continuing stirring for 2 hours to change liquid into glue solution, and controlling the kinematic viscosity of the glue solution to be 70-80 mm 2 /s；
(4) The prepared glue solution is stored in a storage trough through a bottom series valve, and the storage trough keeps the temperature at 80-85 ℃;
(5) pumping the glue solution in the storage material tank to a material turntable rotating at a high speed (10000/min) by using a hose for granulation to obtain microspheres;
(6) the microspheres fall into a drying tower through a distributor and are dried by hot air at 400 ℃ from a hot air furnace to remove surface adsorbed water;
(7) roasting the dried microspheres in a rotary kiln at 750 ℃ for 3h for crystal form conversion to gamma-Al 2 O 3 ；
(8) And naturally cooling to room temperature, and then screening and packaging by using a multilayer vibrating screen to obtain the nano alumina microspheres special for antibiotic decoloration.
The results of various performance tests on the obtained nano-alumina microspheres are shown in table 1.
Example 5
(1) The selected pore volume is more than or equal to 0.8 ml/g, and the specific surface area is more than or equal to 200 m 2 (ii)/g of trabeconite with peptization index of more than or equal to 99 percent;
(2) placing pseudo-boehmite into a distilled water containing batching tank to start stirring, and controlling the mass concentration of alumina in liquid to be 50 g/L;
(3) adding 3% dilute nitric acid into a batching tank, then adding steam, heating to 90 ℃, continuing stirring for 2 hours to change liquid into glue solution, and controlling the kinematic viscosity of the glue solution to be 70-80 mm 2 /s；
(4) The prepared glue solution is stored in a storage trough through a bottom series valve, and the storage trough keeps the temperature at 80-85 ℃;
(5) pumping the glue solution in the storage material tank to a material turntable rotating at a high speed (10000/min) by using a hose for granulation to obtain microspheres;
(6) dropping the microspheres into a drying tower through a distributor, and drying the microspheres by hot air at 350 ℃ from a hot air furnace to remove surface adsorbed water;
(7) roasting the dried microspheres in a rotary kiln at the temperature of 600 ℃ for 3h for carrying out crystal form conversion to convert the microspheres into gamma-Al 2 O 3 ；
(8) Naturally cooling to room temperature, and then screening and packaging by using a multilayer vibrating screen to obtain the nano alumina microspheres special for the antibiotic decoloration.
The results of various performance tests of the obtained nano-alumina microspheres are shown in table 1.
Example 6
(1) The selected pore volume is more than or equal to 0.8 ml/g, and the specific surface area is more than or equal to 200 m 2 (ii)/g of trabeconite with peptization index of more than or equal to 99 percent;
(2) placing pseudo-boehmite into a distilled water containing batching tank to start stirring, and controlling the mass concentration of alumina in liquid to be 50 g/L;
(3) adding 5% dilute nitric acid into a batching tank, then adding steam, heating to 90 ℃, continuing stirring for 2 hours to change liquid into glue solution, and controlling the kinematic viscosity of the glue solution to be 70-80 mm 2 /s；
(4) The prepared glue solution is stored in a storage trough through a bottom series valve, and the storage trough keeps the temperature at 80-85 ℃;
(5) pumping the glue solution in the storage material tank to a material turntable rotating at a high speed (10000/min) by a hose for granulation to obtain microspheres;
(6) the microspheres fall into a drying tower through a distributor and are dried by hot air at 400 ℃ from a hot air furnace to remove surface adsorbed water;
(7) roasting the dried microspheres in a rotary kiln at the temperature of 700 ℃ for 3h for carrying out crystal form conversion to convert the microspheres into gamma-Al 2 O 3 ；
(8) And naturally cooling to room temperature, and then screening and packaging by using a multilayer vibrating screen to obtain the nano alumina microspheres special for antibiotic decoloration.
Through the tests of the products of the above embodiments, the particle size of the nano alumina microspheres prepared by the technical scheme of the invention is more than or equal to 150 μm, the porosity is high, the penetration capacity in the decolorization process of antibiotics is strong, the penetration rate is high, and the production capacity is greatly improved; the pore volume of the nano alumina microspheres is more than or equal to 0.8 ml/g, and the specific surface area is more than or equal to 200 m 2 The/g, the adsorption capacity is strong in the process of decoloring the antibiotics, the decoloring effect is good, and the product quality is greatly improved.
The results of various performance tests of the obtained nano-alumina microspheres are shown in table 1.
TABLE 1 physicochemical Properties of Nano alumina microspheres for antibiotic decolorization
Claims (4)
1. A preparation method of nano alumina microspheres special for decolorizing antibiotics comprises the following steps:
in the step (1), the selected pore volume is more than or equal to 0.8 ml/g, and the specific surface area is more than or equal to 200 m 2 (ii)/g of trabeconite with peptization index of more than or equal to 99 percent;
placing the pseudo-boehmite into a distilled water containing batching tank to start stirring, and controlling the mass concentration of the alumina in the liquid to be 50 g/L;
adding 1-10% of dilute nitric acid into a batching tank, then adding steam, heating to 90 ℃, continuing stirring for 2 hours,the liquid is changed into glue solution, and the kinematic viscosity of the glue solution is controlled to be 70-80 mm 2 /s；
The glue solution prepared in the step (4) is stored in a storage trough through a bottom series valve, and the storage trough keeps the temperature of 80-85 ℃;
step (5), pumping the glue solution in the storage material tank to a material turntable rotating at a high speed by using a hose for granulation to obtain microspheres;
dropping the microspheres into a drying tower through a distributor, and drying the microspheres by hot air at 350-400 ℃ from a hot air furnace to remove surface adsorbed water;
roasting the dried microspheres in a rotary kiln at the temperature of 500-800 ℃ for 3h for crystal form conversion to gamma-Al 2 O 3 ；
And (8) naturally cooling to room temperature, and screening and packaging by using a multilayer vibrating screen to obtain the nano alumina microspheres special for antibiotic decoloration.
2. The preparation method of the nano alumina microspheres specially used for decolorizing antibiotics according to claim 1, characterized by comprising the following steps: in the step (3), the concentration of the dilute nitric acid is 1-10%, preferably 2-8%, and more preferably 3-5%.
3. The preparation method of the nano alumina microspheres specially used for decolorizing antibiotics according to claim 1, characterized by comprising the following steps: in the step (5), the rotating speed of the material rotating disc is 10000/min.
4. The preparation method of the nano alumina microspheres special for antibiotic decoloration according to claim 1, which is characterized in that: in the step (7), the roasting temperature is 500-800 ℃, preferably 550-750 ℃, and more preferably 600-700 ℃.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1097351A (en) * | 1993-07-16 | 1995-01-18 | 中国石油化工总公司 | The preparation method of microspheroidal gama-alumina |
| JPH1017321A (en) * | 1996-06-27 | 1998-01-20 | Catalysts & Chem Ind Co Ltd | Small alumna sphere and its production |
| CN1631787A (en) * | 2004-11-26 | 2005-06-29 | 山东铝业股份有限公司 | Process for producing gama-alumina microsphere |
| CN104085907A (en) * | 2014-07-22 | 2014-10-08 | 温州精晶氧化铝有限公司 | Method for preparing large-pore-volume high-viscosity pseudo bohemite |
| CN106475023A (en) * | 2016-11-15 | 2017-03-08 | 中国海洋石油总公司 | A kind of preparation method of big pore volume aluminum oxide micro-sphere |
| CN107162030A (en) * | 2017-06-28 | 2017-09-15 | 江苏晶晶新材料有限公司 | A kind of preparation method of decolouring special-purpose nanometer aluminum oxide |
| CN111468048A (en) * | 2020-04-13 | 2020-07-31 | 邹凌峰 | Preparation method of high-strength gamma-alumina microspheres |
-
2022
- 2022-04-29 CN CN202210463945.1A patent/CN114988444A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1097351A (en) * | 1993-07-16 | 1995-01-18 | 中国石油化工总公司 | The preparation method of microspheroidal gama-alumina |
| JPH1017321A (en) * | 1996-06-27 | 1998-01-20 | Catalysts & Chem Ind Co Ltd | Small alumna sphere and its production |
| CN1631787A (en) * | 2004-11-26 | 2005-06-29 | 山东铝业股份有限公司 | Process for producing gama-alumina microsphere |
| CN104085907A (en) * | 2014-07-22 | 2014-10-08 | 温州精晶氧化铝有限公司 | Method for preparing large-pore-volume high-viscosity pseudo bohemite |
| CN106475023A (en) * | 2016-11-15 | 2017-03-08 | 中国海洋石油总公司 | A kind of preparation method of big pore volume aluminum oxide micro-sphere |
| CN107162030A (en) * | 2017-06-28 | 2017-09-15 | 江苏晶晶新材料有限公司 | A kind of preparation method of decolouring special-purpose nanometer aluminum oxide |
| CN111468048A (en) * | 2020-04-13 | 2020-07-31 | 邹凌峰 | Preparation method of high-strength gamma-alumina microspheres |
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