CN102557714A - Hole channel amplification method of porous ceramic microballoon sphere - Google Patents
Hole channel amplification method of porous ceramic microballoon sphere Download PDFInfo
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Abstract
The invention discloses a hole channel amplification method of a porous ceramic microballoon sphere for liquid chromatography, which enables silica, zirconium dioxide or titanium dioxide powder to serve as ceramic framework materials, enables nanometer powdered carbon, ammonium chloride, polyving akohol, urea, polyethylene glycol, sodium chloride, sodium sulfate, sodium phosphate, potassium phosphate, potassium chloride, potassium sulfate and the like to serve as porogen, and prepares macropore ceramic microballoon spheres through reversed phase suspension and high temperature sintering. The specific steps are as following: (1) preparing ceramic slurry, enabling the ceramic framework materials, the porogen and sodium alginate solution to be mixed; (2) preparing the porous ceramic microballoon sphere, enabling the ceramic slurry to be conducted reversed phase suspension and dispersion in an oil phase, adding saturation calcium chloride solution in a dropping mode, solidifying to from the sphere, and molding by high temperature sintering; and (3) removing residual porogen, enabling the ceramic microballoon sphere to be soaked in water, hydrochloric acid or sodium hydroxide solution, shaking to dissolve the residual porogen. The microballoon sphere developed by the method has the advantages of having rigidity, and being big in hole diameter and good in spherical degree, and the microballoon sphere can be used for substrates of large biological molecule chromatographic separation media.
Description
Technical field
The present invention relates to a kind of duct amplification method of ceramic foam microballoon
Background technology
Development of biology, for the scale operation of high-value protein medicine provides maybe.The large-scale industrialization purifying of pharmaceutical grade protein, higher purity standard and Financial cost requirement have promoted the very big development of bioseparation technology.The LC technology is a significant element in the bioseparation process, and in biological-pharmacy, has played the part of an important role.Invented based on the ion-exchange type chromatography media of cellulose base and be successfully applied to protein purification in middle period the 1950's from Peterson and Sobers and begin, chromatography media has obtained continuous raising on performances such as mass-producing operation, resolving power, separation efficiency, selectivity, loading capacity.But the development of chromatography media stagnation, the particularly design of substrate material did not still to a certain extent still have great improvement after surplus the experience 50 year.This will cause the development of downstream separation technology to lag behind the upper reaches far away.Therefore, very be necessary to study the chromatography media that preparation has novel texture, the development of the biological downstream industry of advancing by leaps and bounds with reply.
Related patent U.S. Patent No. (publication No. CN101879429A) discloses a kind of novel rigid pottery/agarose composite microsphere that can be used for the protein LC.In this complex media; Hydrogels such as agarose are filled in the porous rigidity ceramic skeleton; Can improve physical strength and chemicalstability and can strengthen the chemically modified ability again, and then can derive chromatography media, to satisfy different chromatography requirements with multiple functional group.The adsorptive power of this complex media is the total amount decision by sepharose in the hole, increases in order to make the sepharose volume that plays the macromole adsorption function, and the porosity of these microballoons should be high as much as possible.And for the mass transfer abilities of macromole in medium such as further raising protein, the aperture that should when reaching high porosity, further improve ceramic microsphere.
Traditional porous ceramic duct amplification method mainly contains and is used to prepare the bigger porous material of volume, and its size of ceramic foam microballoon that is used for the protein LC is 30-200 μ m, and it is bigger directly to use conventional methods the duct limitation that increases.Therefore seeking more effectively, the duct amplification method is only the key of dealing with problems.Just seem more difficult and obtain all better ceramic foam microballoon of profile, aperture, pore volume and pore structure simultaneously, have only through constantly improving technology and come practical requirement.Carbon nano powder, ammonium chloride, Z 150PH, urea, the decomposable material of this type high temp of polyoxyethylene glycol can be mixed and made into stable suspension with ceramic slurry at an easy rate, can decompose through high temperature sintering, reach the purpose in amplification duct.While sodium-chlor, sodium sulfate, sodium phosphate, potassiumphosphate, Repone K, this type of vitriolate of tartar monovalent cation salt, fusing point can reach 800-1400 ℃; In high-temperature sintering process, do not decompose or the part decomposition, through the solution stripping, can reach the purpose in amplification ceramic microsphere duct after the sinter molding.
Summary of the invention
The duct amplification method that the purpose of this invention is to provide the ceramic foam microballoon that a kind of LC uses.
Prepare the ceramic foam microballoon through this method and have tangible macroporous structure, mean pore size has reached
The maximum diameter of hole can reach
Porosity is 50-90%, and specific surface area is 20-45m
2/ cm
3, the grain size scope is 30-200 μ m.
Preparing method's step is following:
1) preparation ceramic slurry
With pore-creating agent mixings such as nano zirconium dioxide, titanium oxide or SiO 2 powder, Hydrocerol A, sodium alginate soln and carbon nano powder, Z 150PH, polyoxyethylene glycol, ammonium chloride, urea, sodium-chlor, sodium sulfate, sodium phosphate, Repone K, vitriolate of tartar, potassiumphosphates to gel.
2) ceramic foam microballoon preparation
Ceramic slurry anti-phase suspension in oil phase is disperseed, drip saturated calcium chloride solution and solidify balling-up, collect microballoon, cleaning, oven dry, the high temperature sintering moulding.
3) place to go of remaining pore-creating agent
Ceramic microsphere is immersed in water, hydrochloric acid or the sodium hydroxide solution, with remaining pore-creating agent stripping, collects microballoon and clean and dry behind the concussion certain hour.
The present invention takes the method for anti-phase suspension balling-up, interpolation pore-creating agent amplification duct, high temperature sintering to prepare the ceramic foam microballoon that possesses macropore on preparation technology.Therefore, the agarose spheroidal particle of being developed is through further chemically derived sorbent material and the chromatography media with multiple functional group that make.The invention has the advantages that: 1) rigidity ceramic skeleton structure, Stability Analysis of Structures, intensity are big, are adapted to the chromatographic separation operational requirement under high flow rate, the high pressure; 2) the inner aperture of microballoon increases, can improve biomacromolecule mass-transfer efficiency, help the chromatographic separation operation; 3) pore size of microballoon and size can be regulated, and can satisfy the needs of different application environment; 4) preparation technology is simple, is easy to control and amplification; 5) with low cost, environmental pollution is little.
Description of drawings
Fig. 1 is the overall appearance stereoscan photograph of ceramic foam microballoon of the present invention.
Fig. 2 is the surface tissue stereoscan photograph of ceramic foam microballoon of the present invention.
Fig. 3 is the internal structure stereoscan photograph of ceramic foam microballoon of the present invention.
Embodiment
Below through embodiment the present invention is done further description:
Embodiment 1
The sodium alginate soln of 30g nano zirconium dioxide, 2g Hydrocerol A, 30mL water mixing, 5g nano-carbon powder and 20mL 5% is stirred to gel.Above-mentioned ceramic slurry is transferred in the 500mL there-necked flask, added 200mL pump oil, class of 10mL department 80,700r/min stirs 30min, drips the saturated calcium chloride of 10mL, continues to stir 10min.After reaction finishes, filter and collect microballoon, totally dry in back 50 ℃ of baking ovens with alcohol and washed with de-ionized water, be incubated 20min after in retort furnace, being warming up to 1450 ℃, naturally cooling can obtain the ceramic foam microballoon.The ceramic foam microballoon that obtains, mean pore size has reached
The maximum diameter of hole does
Porosity is 60%, and specific surface area is 22m
2/ cm
3, median size is 120 μ m.
Embodiment 2
The sodium alginate soln of 28g nano titanium oxide, 1g Hydrocerol A, 30mL water mixing, 5g polyoxyethylene glycol and 20mL 5% is stirred to gel.Above-mentioned ceramic slurry is transferred in the 500mL there-necked flask, added 200mL pump oil, class of 10mL department 80,600r/min stirs 30min, drips the saturated calcium chloride of 10mL, continues to stir 10min.After reaction finishes, filter and collect microballoon, totally dry in back 50 ℃ of baking ovens with alcohol and washed with de-ionized water, be incubated 20min after in retort furnace, being warming up to 1300 ℃, naturally cooling can obtain the ceramic foam microballoon.The ceramic foam microballoon that obtains, mean pore size has reached
The maximum diameter of hole does
Porosity is 62%, and specific surface area is 22.6m
2/ cm
3, median size is 98 μ m.
Embodiment 3
The sodium alginate soln of 12g nano titanium oxide, 2g Hydrocerol A, 30mL water mixing, 4g Z 150PH and 20mL 5% is stirred to gel.Above-mentioned ceramic slurry is transferred in the 500mL there-necked flask, added 200mL pump oil, class of 10mL department 80,800r/min stirs 40min, drips the saturated calcium chloride of 10mL, continues to stir 10min.After reaction finishes, filter and collect microballoon, totally dry in back 60 ℃ of baking ovens with alcohol and washed with de-ionized water, be incubated 20min after in retort furnace, being warming up to 1000 ℃, naturally cooling can obtain the ceramic foam microballoon.The ceramic foam microballoon that obtains, mean pore size has reached
The maximum diameter of hole does
Porosity is 58%, and specific surface area is 20.7m
2/ cm
3, median size is 118 μ m.
Embodiment 4
The sodium alginate soln of 12g nano silicon, 2g Hydrocerol A, 30mL water mixing, 2g ammonium chloride, 3g urea and 20mL 5% is stirred to gel.Above-mentioned ceramic slurry is transferred in the 500mL there-necked flask, added 200mL pump oil, class of 10mL department 80,800r/min stirs 40min, drips the saturated calcium chloride of 10mL, continues to stir 10min.After reaction finishes, filter and collect microballoon, totally dry in back 60 ℃ of baking ovens with alcohol and washed with de-ionized water, be incubated 20min after in retort furnace, being warming up to 1000 ℃, naturally cooling can obtain the ceramic foam microballoon.Above-mentioned ceramic foam microballoon is transferred in the 250mL tool plug Erlenmeyer flask, adds the hydrochloric acid 100mL of 2mol/L, 140r/min concussion 3h collects microballoon, water cleaning and oven dry afterwards in shaking table.The ceramic foam microballoon that obtains, mean pore size has reached
The maximum diameter of hole does
Porosity is 62%, and specific surface area is 20.9m
2/ cm
3, median size is 122 μ m.
Embodiment 5
The sodium alginate soln of 32g nano zirconium dioxide, 1g Hydrocerol A, 30mL water mixing, 2g potassiumphosphate, 5g sodium phosphate and 20mL 5% is stirred to gel.Above-mentioned ceramic slurry is transferred in the 500mL there-necked flask, added 200mL pump oil, class of 12mL department 80,750r/min stirs 30min, drips the saturated calcium chloride of 10mL, continues to stir 10min.After reaction finishes, filter and collect microballoon, totally dry in back 50 ℃ of baking ovens with alcohol and washed with de-ionized water, be incubated 30min after in retort furnace, being warming up to 1450 ℃, naturally cooling can obtain the ceramic foam microballoon.Above-mentioned ceramic foam microballoon is transferred in the 250mL tool plug Erlenmeyer flask, adds the sodium hydroxide 100mL of 3mol/L, 140r/min concussion 2h collects microballoon, water cleaning and oven dry afterwards in shaking table.The ceramic foam microballoon that obtains, mean pore size has reached
The maximum diameter of hole does
Porosity is 59%, and specific surface area is 22.7m
2/Cm
3, median size is 81 μ m.
Embodiment 6
The sodium alginate soln of 12g nano silicon, 2g Hydrocerol A, 30mL water mixing, 8g sodium-chlor and 20mL 5% is stirred to gel.Above-mentioned ceramic slurry is transferred in the 500mL there-necked flask, added 200mL pump oil, class of 15mL department 80,850r/min stirs 30min, drips the saturated calcium chloride of 10mL, continues to stir 10min.After reaction finishes, filter and collect microballoon, totally dry in back 50 ℃ of baking ovens with alcohol and washed with de-ionized water, be incubated 25min after in retort furnace, being warming up to 1000 ℃, naturally cooling can obtain the ceramic foam microballoon.Above-mentioned ceramic foam microballoon is transferred in the 250mL tool plug Erlenmeyer flask, adds the 100mL deionized water, 140r/min concussion 4h collects microballoon, water cleaning and oven dry afterwards in shaking table.The ceramic foam microballoon that obtains, mean pore size has reached
The maximum diameter of hole does
Porosity is 58%, and specific surface area is 23.7m
2/ cm
3, median size is 79 μ m.
Embodiment 7
The sodium alginate soln of 12g nano zirconium dioxide, 6g nano silicon, 10g titanium oxide, 2g Hydrocerol A, 30mL water, 8g sodium-chlor, 3g sodium sulfate 5g nano-carbon powder, 2g polyoxyethylene glycol and 20mL 5% is stirred to gel.Above-mentioned ceramic slurry is transferred in the 500mL there-necked flask, added 200mL pump oil, class of 15mL department 80,860r/min stirs 30min, drips the saturated calcium chloride of 10mL, continues to stir 10min.After reaction finishes, filter and collect microballoon, totally dry in back 60 ℃ of baking ovens with alcohol and washed with de-ionized water, be incubated 30min after in retort furnace, being warming up to 1300 ℃, naturally cooling can obtain the ceramic foam microballoon.Above-mentioned ceramic foam microballoon is transferred in the 250mL tool plug Erlenmeyer flask, adds the hydrochloric acid 100mL of 3mol/L, 140r/min concussion 4h collects microballoon, water cleaning and oven dry afterwards in shaking table.The ceramic foam microballoon that obtains, mean pore size has reached
The maximum diameter of hole does
Porosity is 80%, and specific surface area is 23.7m
2/ cm
3, median size is 76 μ m.
Embodiment 8
The sodium alginate soln of 12g nano zirconium dioxide, 6g nano silicon, 10g titanium oxide, 2g Hydrocerol A, 30mL water, 8g sodium-chlor, 3g sodium sulfate 5g nano-carbon powder, 2g polyoxyethylene glycol and 20mL 5% is stirred to gel.Above-mentioned ceramic slurry is transferred in the 500mL there-necked flask, added 200mL pump oil, class of 15mL department 80,860r/min stirs 30min, drips the saturated calcium chloride of 10mL, continues to stir 10min.After reaction finishes, filter and collect microballoon, totally dry in back 60 ℃ of baking ovens with alcohol and washed with de-ionized water, be incubated 30min after in retort furnace, being warming up to 1300 ℃, naturally cooling can obtain the ceramic foam microballoon.Above-mentioned ceramic foam microballoon is transferred in the 250mL tool plug Erlenmeyer flask, adds the hydrochloric acid 100mL of 3mol/L, 140r/min concussion 4h collects microballoon, water cleaning and oven dry afterwards in shaking table.The ceramic foam microballoon that obtains, mean pore size has reached
The maximum diameter of hole does
Porosity is 80%, and specific surface area is 23.7m
2/ cm
3, median size is 76 μ m.
Embodiment 9
The sodium alginate soln of 10g nano zirconium dioxide, 5g nano silicon, 15g titanium oxide, 2g Hydrocerol A, 30mL water, 2g sodium-chlor, 3g sodium sulfate 5g nano-carbon powder, 2g sodium phosphate, 2g vitriolate of tartar, 2g polyoxyethylene glycol and 20mL 5% is stirred to gel.Above-mentioned ceramic slurry is transferred in the 500mL there-necked flask, added 200mL pump oil, class of 10mL department 80,700r/min stirs 30min, drips the saturated calcium chloride of 10mL, continues to stir 10min.After reaction finishes, filter and collect microballoon, totally dry in back 60 ℃ of baking ovens with alcohol and washed with de-ionized water, be incubated 30min after in retort furnace, being warming up to 1300 ℃, naturally cooling can obtain the ceramic foam microballoon.Above-mentioned ceramic foam microballoon is transferred in the 250mL tool plug Erlenmeyer flask, adds the hydrochloric acid 100mL of 3mol/L, 140r/min concussion 4h collects microballoon, water cleaning and oven dry afterwards in shaking table.The ceramic foam microballoon that obtains, mean pore size has reached
The maximum diameter of hole does
Porosity is 82%, and specific surface area is 23.4m
2/Cm
3, median size is 150 μ m.
Specific form based on spirit of the present invention or principal character is not limited in the foregoing description; Also multiple combination or variation can be arranged; All can adjust to a certain extent like various times, reagent type and addition etc.; Therefore, no matter from which point, above-mentioned embodiment of the present invention all can only be thought can not limit the present invention to explanation of the present invention; In implication suitable and any variation in the scope, all should think to be included in the scope of claims with claims of the present invention.
Claims (7)
1. the duct amplification method of a ceramic foam microballoon; It is characterized in that with ZIRCONIUM DIOXIDE 99.5, titanium oxide or SiO 2 powder be the ceramic skeleton material, is pore-creating agent with carbon nano powder, Z 150PH, polyoxyethylene glycol, ammonium chloride, urea, sodium-chlor, sodium sulfate, sodium phosphate, Repone K, vitriolate of tartar, potassiumphosphate etc.; Prepare the macropore ceramic microsphere through anti-phase suspension and high-temperature sintering process; The mean pore size of microballoon has reached
The maximum diameter of hole can reach
Porosity is 50-90%, and specific surface area is 20-45m
2/ cm
3, the grain size scope is 30-200 μ m.
2. according to the duct amplification method of the described a kind of ceramic foam microballoon of claim 1, it is characterized in that said ceramic skeleton material is that oxide compounds such as 50-500nm silicon-dioxide, ZIRCONIUM DIOXIDE 99.5, titanium oxide are prepared from particle diameter.
3. according to the duct amplification method of the described a kind of ceramic foam microballoon of claim 1, it is characterized in that said pore-creating agent is the soluble monovalent cation salt of this type such as carbon nano powder, Z 150PH, polyoxyethylene glycol, ammonium chloride, the decomposable material of this type high temp of urea and sodium-chlor, sodium sulfate, sodium phosphate, Repone K, vitriolate of tartar, potassiumphosphate.
4. according to the duct amplification method of the described a kind of ceramic foam microballoon of claim 1, it is characterized in that the step of method is following:
1) preparation ceramic slurry
With pore-creating agent mixing to gels such as nano silicon, ZIRCONIUM DIOXIDE 99.5 or titania powder, Hydrocerol A, sodium alginate soln and carbon nano powder, Z 150PH, polyoxyethylene glycol, ammonium chloride, urea, sodium-chlor, sodium sulfate, sodium phosphate, Repone K, vitriolate of tartar, potassiumphosphates;
2) ceramic foam microballoon preparation
Ceramic slurry anti-phase suspension in oil phase is disperseed, drip saturated calcium chloride solution and solidify balling-up, ceramic microsphere is filtered out from oil phase, with alcohol and washed with de-ionized water, oven dry, high temperature sintering, naturally cooling obtain the ceramic foam microballoon;
3) place to go of remaining pore-creating agent
Ceramic microsphere is immersed in water, hydrochloric acid or the sodium hydroxide solution, with remaining pore-creating agent stripping, collects microballoon and clean and dry behind the concussion certain hour.
5. according to the duct amplification method of the described a kind of ceramic foam microballoon of claim 4, the interpolation kind that it is characterized in that pore-creating agent in the said ceramic slurry for wherein one or more, addition is 1-40%.
6. according to the duct amplification method of the described a kind of ceramic foam microballoon of claim 4, it is characterized in that the bake out temperature of the plain embryo of said ceramic microsphere is 60-100 ℃, ceramic sintering temperature is 800-1500 ℃.
7. according to the duct amplification method of the described a kind of ceramic foam microballoon of claim 4, the solubility that it is characterized in that said hydrochloric acid and sodium hydroxide is 1-3mol/L.
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| CN106660889A (en) * | 2014-04-24 | 2017-05-10 | 奥斯设计公司 | Methods of forming a porous ceramic shaped article and porous ceramic products |
| CN108585918A (en) * | 2018-05-28 | 2018-09-28 | 江苏东浦精细陶瓷科技股份有限公司 | porous silicon nitride ceramic and preparation method thereof |
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| CN111380994A (en) * | 2020-05-15 | 2020-07-07 | 淄博山分分析仪器有限公司 | Preparation method of chromatographic rod for rod-shaped thin-layer chromatography |
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| CN103274704B (en) * | 2013-05-07 | 2014-09-24 | 清华大学 | Micron-order honeycomb ceramic and method for adjusting and controlling pore diameter and size of pore wall of micron-order honeycomb ceramic |
| CN103274704A (en) * | 2013-05-07 | 2013-09-04 | 清华大学 | Micron-order honeycomb ceramic and method for adjusting and controlling pore diameter and size of pore wall of micron-order honeycomb ceramic |
| CN106660889B (en) * | 2014-04-24 | 2020-05-15 | 奥斯设计公司 | Method for forming porous ceramic shaped article and porous ceramic product |
| CN106660889A (en) * | 2014-04-24 | 2017-05-10 | 奥斯设计公司 | Methods of forming a porous ceramic shaped article and porous ceramic products |
| CN108585918A (en) * | 2018-05-28 | 2018-09-28 | 江苏东浦精细陶瓷科技股份有限公司 | porous silicon nitride ceramic and preparation method thereof |
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| CN110112352A (en) * | 2019-06-17 | 2019-08-09 | 合肥国轩高科动力能源有限公司 | Polyimide diaphragm and preparation method and application thereof |
| CN110559956A (en) * | 2019-09-06 | 2019-12-13 | 广东省生物工程研究所（广州甘蔗糖业研究所） | Hollow porous cellulose microsphere and preparation method and application thereof |
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| CN111073627A (en) * | 2019-12-31 | 2020-04-28 | 西南石油大学 | Lightweight porous proppant, preparation method and application thereof |
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