CN204564161U - A kind of nucleocapsid particles of filling for chromatogram - Google Patents

A kind of nucleocapsid particles of filling for chromatogram Download PDF

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CN204564161U
CN204564161U CN201520148651.5U CN201520148651U CN204564161U CN 204564161 U CN204564161 U CN 204564161U CN 201520148651 U CN201520148651 U CN 201520148651U CN 204564161 U CN204564161 U CN 204564161U
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sio
nucleocapsid particles
particle
shell
atresia
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阎超
瞿其曙
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Shanghai Tong Micro Analysis Technology Co ltd
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Shanghai Tong Micro Analysis Technology Co ltd
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Abstract

The utility model discloses a kind of nucleocapsid particles of filling for chromatogram, and it adopts atresia SiO 2particle, as core, adopts two phase process at its finishing porous SiO 2shell, and SiO 2shell has radial pore structure, the SiO modified 2the aperture on nucleocapsid particles surface, shell thickness and specific area are that controlled, shell thickness can regulate between 10-500nm.

Description

A kind of nucleocapsid particles of filling for chromatogram
Technical field
The utility model belongs to chromatographic stationary phases field, is specifically related to a kind of nucleocapsid particles of filling for chromatogram.
Background technology
Silica (SiO 2) the micron-size spherical monodisperse particles of matrix applies maximum a kind of Stationary liquid in current chromatographic isolation.The synthetic method of this particle is mainly silica bead method of piling up [Kirkland J J.USP.3782075,1974], sol-gel process [von Hohenesche C.du F., Ehwald V., UngerK.K.J.Chromatogr.A 2004,1025,177-187.] and template [Kresge C.T., Leonowicz M.E., Roth W.J., Vartul i J.C., Beck, J.S.Nature 1992,359:710-712].Adopt the silica gel particle piled up silica bead method and can prepare different-grain diameter, but there is the shortcoming of radius particle pore distribution wide ranges in the particle prepared.Sol-gal process can prepare the particle of narrow diameter distribution, but gained particle is substantially non-porous particle and particle diameter is less than 1 micron.Template can prepare particle diameter at micron-sized particle, but the particle prepared exists more serious adhesion.
Nucleocapsid particles is that a kind of new chromatographic just grown up gradually afterwards for 2008 fills Stationary liquid.At present, the preparation of this particle adopts layer assembly method substantially, namely first prepares the silica core of atresia, and then by the method for nano level silica gel particle by layer assembly, modification in layer, to non-porous particle surface, controls the thickness of shell by the number of plies of controlled modification.The preparation technology of this nucleocapsid particles reaches 100 multisteps, and each step all strictly must control synthesis technique, thus prepares difficulty higher.
In addition, adopt sol-gal process also can prepare nucleocapsid particles, and step is simple.But adopt current existing sol-gal process to prepare nucleocapsid particles, there is the easy adhesion of particle for preparing and shell thickness and the shortcoming such as aperture is wayward.
Utility model content
Technical problem to be solved in the utility model is to provide a kind of nucleocapsid particles of filling for chromatogram, to overcome the deficiency that prior art exists.
In order to solve the problems of the technologies described above, the utility model adopts following technical scheme:
On the one hand, a kind of nucleocapsid particles of filling for chromatogram, comprises atresia SiO 2core and modifying in atresia SiO 2the porous SiO on core surface 2shell, is characterized in that: described atresia SiO 2core is the atresia SiO of 100nm-10 μm 2particle; Described porous SiO 2shell is modified in atresia SiO by two phase process 2core surface, porous SiO 2the thickness of shell is 10-500nm, and surface has radial pore structure, and its aperture is 2-100nm, and the specific area of nucleocapsid particles is 10-600m 2/ g.
Described atresia SiO 2core is the atresia SiO of 0.5-3 μm 2particle.
Described porous SiO 2the thickness of shell is 10-200nm.
The aperture on described whole nucleocapsid particles surface is 3-30nm, and specific area is 15-300m 2/ g.
On the other hand, 0.5-6g diameter is the atresia SiO of 100nm-10 μm by a kind of preparation method of the nucleocapsid particles for chromatogram filling 2particle is as atresia SiO 2core is distributed to the H of 15-18mL 2in O, add the isopropyl alcohol of 0.46-5.52mL, the urea of 0.3-3.6g, the template reagent of 0.5-6g, the tetraethyl orthosilicate of 0.5-6mL, the non-polar solven of 15-180mL, by stirring, being warming up to 60-150 DEG C, react under inactive state, wherein, mixing speed during intensification controls at 0-1500rpm; The product obtained after reaction is filtered, with washed with de-ionized water number time; Remove the template reagent in the rear filter cake of filter.
The mode of above-mentioned removal template reagent can adopt in an oven dry, be cooled to room temperature again after put into crucible, be warming up to 550-1000 DEG C with 0.5-2 DEG C/min, keep 2-12h, then cool to room temperature with the furnace; Or adopt HCl ethanolic solution or aqueous ammonium nitrate solution, react 6-24h at reflux.
Above-mentioned isopropyl alcohol can adopt carbon number to substitute, as methyl alcohol, ethanol, n-butanol, n-amyl alcohol etc. from any one alcohol reagent of 1 to 10.
Described urea can produce ammonia a class reagent such as formamide, DMF or carbonic hydroammonium after can adopting other hydrolysis substitute.
Described tetraethyl orthosilicate (TEOS) can adopt sodium metasilicate to substitute.
Described non-polar solven is any one in cyclohexane, n-hexane, ether, benzene, toluene, carbon tetrachloride.
Described template reagent is any one in softex kw (CTAB), hexadecylamino pyridine, myristyl aminopyridine, octadecylamino pyridine, TTAB, Cetyltrimethylammonium bromide, hexadecyltrimethylammonium chloride, tetradecyl trimethyl ammonium chloride, Cetyltrimethylammonium bromide, the trimethyl ammonium chloride of other carbon number between 8-20, ammonium bromide class surfactant, aminopyridines surfactant.
Adopt technique scheme, nucleocapsid particles for chromatogram filling of the present utility model and preparation method thereof, has following advantage:
1, the SiO modified 2nucleocapsid thickness can regulate between 10-500nm, SiO 2the specific area of nucleocapsid particles can at 10-600m 2adjust between/g;
2, the controlled decorative layer of shell structurre can be obtained on particle diameter 100nm-10 μm of non-porous particle surface;
3, processing step is few, technology of preparing is simple.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the utility model is described in detail:
Fig. 1-0 is structural representation of the present utility model.
Fig. 1 is the SiO that embodiment 1 of the present utility model obtains 2nucleocapsid particles TEM photo.
Fig. 2 is the SiO that embodiment 2 of the present utility model obtains 2nucleocapsid particles TEM photo.
Fig. 3 is the SiO that embodiment 3 of the present utility model obtains 2nucleocapsid particles TEM photo.
Fig. 4 is the SiO that embodiment 4 of the present utility model obtains 2nucleocapsid particles TEM photo.
Fig. 5 is the SiO that embodiment 5 of the present utility model obtains 2nucleocapsid particles TEM photo.
Fig. 6 is the SiO that embodiment 6 of the present utility model obtains 2nucleocapsid particles TEM photo.
Fig. 7 is the SiO that embodiment 7 of the present utility model obtains 2nucleocapsid particles TEM photo.
Fig. 8 is the SiO that embodiment 8 of the present utility model obtains 2nucleocapsid particles TEM photo.
Fig. 9 is the SiO that embodiment 9 of the present utility model obtains 2nucleocapsid particles TEM photo.
Figure 10 is the SiO that embodiment 10 of the present utility model obtains 2nucleocapsid particles TEM photo.
Figure 11 is the SiO that embodiment 11 of the present utility model obtains 2nucleocapsid particles TEM photo.
Figure 12 is the SiO that embodiment 12 of the present utility model obtains 2nucleocapsid particles TEM photo.
Figure 13 is the SiO that embodiment 7 of the present utility model obtains 2the phase chromatographic fractionation figure of nucleocapsid particles.
Detailed description of the invention
The preparation method of the nucleocapsid particles for chromatogram filling of the present utility model is specially: the atresia SiO by 0.5-6g diameter being first 100nm-10 μm 2particle is as atresia SiO 2core is distributed to the H of 15-18mL 2in O, add the isopropyl alcohol of 0.46-5.52mL, the urea of 0.3-3.6g, the template reagent of 0.5-6g, the tetraethyl orthosilicate of 0.5-6mL, the non-polar solven of 15-180mL again, by stirring, being warming up to 60-150 DEG C, react under inactive state, wherein, mixing speed during intensification controls at 0-1500rpm; The product obtained after reaction is filtered, with washed with de-ionized water number time; Remove the template reagent in the filter cake after filter.
The mode of described removal template reagent adopt in an oven dry, be cooled to room temperature again after put into crucible, be warming up to 550-1000 DEG C with 0.5-2 DEG C/min, keep 2-12h, then cool to room temperature with the furnace; Or adopt HCl ethanolic solution or aqueous ammonium nitrate solution, react 6-24h at reflux.
Described isopropyl alcohol adopts carbon number to substitute from any one alcohol reagent of 1 to 10.
Described urea can adopt formamide, DMF or carbonic hydroammonium to substitute.
Described tetraethyl orthosilicate (TEOS) can adopt sodium metasilicate or other can provide silicon source reagent substitute.
Described non-polar solven is any one in cyclohexane, n-hexane, ether, benzene, toluene, carbon tetrachloride.
Described template reagent is any one in softex kw, hexadecylamino pyridine, myristyl aminopyridine, octadecylamino pyridine, TTAB, Cetyltrimethylammonium bromide, hexadecyltrimethylammonium chloride, tetradecyl trimethyl ammonium chloride, Cetyltrimethylammonium bromide, the trimethyl ammonium chloride of other carbon number between 8-20, ammonium bromide class surfactant, aminopyridines surfactant.
As shown in Fig. 1-0, the nucleocapsid particles of filling for chromatogram that said method obtains, comprises atresia SiO 2core 100 and modifying in atresia SiO 2the porous SiO on core 100 surface 2shell 200, atresia SiO 2core is the atresia SiO of 100nm-10 μm 2particle; Porous SiO 2shell is modified in atresia SiO by two phase process 2core surface, porous SiO 2the thickness of shell is 10-500nm, and surface has radial pore structure 300, and its aperture is 2-100nm, and the specific area of nucleocapsid particles is 10-600m 2/ g.
Below in conjunction with accompanying drawing, concrete example explanation is carried out to the utility model:
Embodiment 1
By the SiO that 0.5g diameter is 1 μm 2nucleocapsid particles non-porous particle is distributed to the H of 15mL 2in O, add the isopropyl alcohol of 0.46mL, the urea of 0.3g, the cyclohexane of the TEOS of the CTAB of 0.5g, 0.5mL, 15mL, 150rpm stirs 0.5h, stops stirring, and is warming up to 70 DEG C, reacts 16h under inactive state.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in Figure 1, its shell thickness is about 11nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 43.4m 2/ g, particle aperture is about 4nm.
Embodiment 2
By the SiO that 0.5g diameter is 1 μm 2nucleocapsid particles non-porous particle is distributed to the H of 15mL 2in O, add the isopropyl alcohol of 0.46mL, the formamide of 0.3g, the cyclohexane of the TEOS of the CTAB of 0.5g, 0.5mL, 15mL, 150rpm stirs 0.5h, keeps 150rpm mixing speed, is warming up to 70 DEG C, reacts 16h under inactive state.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in Figure 2, its shell thickness is about 71nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 127.8m 2/ g, particle aperture is about 10nm.
Embodiment 3
By the SiO that 0.5g diameter is 1 μm 2nucleocapsid particles non-porous particle is distributed to the H of 15mL 2in O, add the isopropyl alcohol of 0.46mL, the formamide of 0.3g, the cyclohexane of the TEOS of the CTAB of 0.5g, 0.5mL, 15mL, 500rpm stirs 0.5h, keeps 500rpm mixing speed, is warming up to 70 DEG C, reacts 16h under inactive state.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in Figure 3, its shell thickness is about 45nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 122.6m 2/ g, particle aperture is about 14nm.
Embodiment 4
By the SiO that 0.5g diameter is 1 μm 2nucleocapsid particles non-porous particle is distributed to the H of 90mL 2in O, add the isopropyl alcohol of 2.76mL, the urea of 1.8g, the cyclohexane of the TEOS of the CTAB of 3g, 0.5mL, 90mL, 150rpm stirs 0.5h, keeps 150rpm mixing speed, is warming up to 70 DEG C, reaction 16h.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in Figure 4, its shell thickness is about 80nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 114.9m 2/ g, particle aperture is about 26nm.
Embodiment 5
By the SiO that 0.5g diameter is 1 μm 2nucleocapsid particles non-porous particle is distributed to the H of 15mL 2in O, add the isopropyl alcohol of 0.46mL, the urea of 0.3g, the cyclohexane of the TEOS of the CTAB of 0.5g, 0.5mL, 15mL, 150rpm stirs 0.5h, stirs and stops, being warming up to 70 DEG C, reaction 16h.Adjustment mixing speed is 800rpm, adds the TEOS of 0.5mL, continues reaction 16h.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in Figure 5, its shell thickness is about 160nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 233.6m 2/ g, particle aperture is about 21nm.
Embodiment 6
By the SiO that 0.5g diameter is 1 μm 2nucleocapsid particles non-porous particle is distributed to the H of 15mL 2in O, add the isopropyl alcohol of 0.46mL, the urea of 0.3g, the cyclohexane of the TEOS of the CTAB of 0.5g, 0.5mL, 15mL, 150rpm stirs 0.5h, keeps the mixing speed of 150rpm, is warming up to 70 DEG C, reaction 16h.Adjustment mixing speed is 300rpm, adds the TEOS of 0.5mL, continues reaction 16h.Adjustment mixing speed is 800rpm, adds the TEOS of 0.5mL, continues reaction 16h.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in Figure 6, its shell thickness is about 200nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 241.8m 2/ g, particle aperture is about 20nm.
Embodiment 7
By the SiO that 0.5g diameter is 2.3 μm 2nucleocapsid particles non-porous particle is distributed to the H of 15mL 2in O, add the isopropyl alcohol of 0.46mL, the urea of 0.3g, the cyclohexane of the TEOS of the CTAB of 0.5g, 0.5mL, 15mL, 200rpm stirs 0.5h, keeps 150rpm mixing speed, is warming up to 70 DEG C, reaction 16h.Adjustment mixing speed is 600rpm, adds the TEOS of 0.5mL, continues reaction 16h.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in Figure 7, its shell thickness is about 180nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 137.5m 2/ g, particle aperture is about 14nm.
Embodiment 8
By the SiO that 0.5g diameter is 1 μm 2nucleocapsid particles non-porous particle is distributed to the H of 15mL 2in O, add the isopropyl alcohol of 0.46mL, the urea of 0.3g, the cyclohexane of the TEOS of the CTAC of 0.56g, 0.5mL, 15mL, 150rpm stirs 0.5h, keeps the mixing speed of 150rpm, is warming up to 70 DEG C, reaction 16h.Adjustment mixing speed is 300rpm, adds the TEOS of 0.5mL, continues reaction 16h.Maintenance mixing speed is 150rpm, adds the TEOS of 0.5mL, continues reaction 16h.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in Figure 8, its shell thickness is about 80nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 174.7m 2/ g, particle aperture is about 9nm.
Embodiment 9
By the SiO that 0.5g diameter is 1 μm 2nucleocapsid particles non-porous particle is distributed to the H of 15mL 2in O, add the isopropyl alcohol of 0.46mL, the urea of 0.3g, the carbon tetrachloride of the TEOS of the CTAB of 0.5g, 0.5mL, 15mL, 150rpm stirs 0.5h, keeps the mixing speed of 150rpm, is warming up to 70 DEG C, reaction 16h.Maintenance mixing speed is 300rpm, adds the TEOS of 0.5mL, continues reaction 16h.Maintenance mixing speed is 150rpm, adds the TEOS of 0.5mL, continues reaction 16h.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in Figure 9, its shell thickness is about 100nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 189.1m 2/ g, particle aperture is about 17nm.
Embodiment 10
By the SiO that 0.5g diameter is 1 μm 2nucleocapsid particles non-porous particle is distributed to the H of 15mL 2in O, add the n-butanol of 0.50mL, the urea of 0.3g, the cyclohexane of the TEOS of the CTAB of 0.5g, 0.5mL, 15mL, 150rpm stirs 0.5h, keeps the mixing speed of 150rpm, is warming up to 70 DEG C, reaction 16h.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in Figure 10, its shell thickness is about 60nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 82.4m 2/ g, particle aperture is about 12nm.
Embodiment 11
By the SiO that 0.5g diameter is 1 μm 2nucleocapsid particles non-porous particle is distributed to the H of 15mL 2in O, add the n-amyl alcohol of 0.50mL, the urea of 0.3g, the cyclohexane of the TEOS of the CTAB of 0.5g, 0.5mL, 15mL, 150rpm stirs 0.5h, keeps the mixing speed of 150rpm, is warming up to 70 DEG C, reaction 16h.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in figure 11, its shell thickness is about 20nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 33.2m 2/ g, particle aperture is about 21nm.
Embodiment 12
By the SiO that 0.5g diameter is 1 μm 2nucleocapsid particles non-porous particle is distributed to the H of 15mL 2in O, add the isopropyl alcohol of 0.46mL, 0.73g DMF, the cyclohexane of the TEOS of the CTAB of 0.5g, 0.5mL, 15mL, 150rpm stirs 0.5h, keeps the mixing speed of 150rpm, is warming up to 70 DEG C, reaction 16h.The product that obtains is filtered, by washed with de-ionized water 3 times.Filter cake is dry 3h in 110 DEG C of baking ovens.Put into crucible after being cooled to room temperature, be warming up to 550 DEG C with 1 DEG C/min, keep 2h, then cool to room temperature with the furnace.Adopt the SiO that this method obtains 2as shown in figure 12, its shell thickness is about 25nm to nucleocapsid particles TEM photo, SiO 2the BET of nucleocapsid particles is about 40.0m 2/ g, particle aperture is about 4.2nm.
The particle that embodiment 7 obtained adopts C18 to derive, and be then packed in stainless-steel tubing pillar that diameter is 2.1mm, filling length is 10cm.Adopt Agilent 1290 Ultra Performance Liquid Chromatography to be separated, separation condition is: mobile phase is 50/50: acetonitrile/water, and flow velocity is 0.1mL/min, and sample size is 1 μ L.Separating pressure is 64bar, and the high performance liquid chromatography separation graph of its five kinds of neutral substances as shown in figure 13.Chromatographic peak theoretical cam curve (every meter): uracil (22890), acetophenone (86900), benzene (117440), toluene (141060), naphthalene (151350).Can obviously draw from Figure 13, the particle that the method prepares has good chromatographic isolation effect.
But; those skilled in the art will recognize that; above-mentioned detailed description of the invention is exemplary; to better enable those skilled in the art understand this patent; can not be interpreted as it is restriction to this patent protection domain; as long as according to this patent disclose any equivalent change done or the modification of spirit, all fall into the scope of this patent protection.

Claims (4)

1., for the nucleocapsid particles that chromatogram is filled, comprise atresia SiO 2core and modifying in atresia SiO 2the porous SiO on core surface 2shell, is characterized in that: described atresia SiO 2core is the atresia SiO of 100nm-10 μm 2particle; Described porous SiO 2shell is modified in atresia SiO by two phase process 2core surface, porous SiO 2the thickness of shell is 10-500nm, and surface has radial pore structure, and its aperture is 2-100nm, and the specific area of nucleocapsid particles is 10-600m 2/ g.
2. nucleocapsid particles of filling for chromatogram according to claim 1, is characterized in that: described atresia SiO 2core is the atresia SiO of 0.5-3 μm 2particle.
3. nucleocapsid particles of filling for chromatogram according to claim 1, is characterized in that: described porous SiO 2the thickness of shell is 10-200nm.
4. nucleocapsid particles of filling for chromatogram according to claim 1, is characterized in that: the aperture on described whole nucleocapsid particles surface is 3-30nm, and specific area is 15-300m 2/ g.
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