CN101274265A - Mesoporous medical sorbent material - Google Patents
Mesoporous medical sorbent material Download PDFInfo
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- CN101274265A CN101274265A CNA2007101725408A CN200710172540A CN101274265A CN 101274265 A CN101274265 A CN 101274265A CN A2007101725408 A CNA2007101725408 A CN A2007101725408A CN 200710172540 A CN200710172540 A CN 200710172540A CN 101274265 A CN101274265 A CN 101274265A
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- mesoporous
- sba
- bilirubin
- adsorption capacity
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Abstract
The invention relates to a mesoporous medical adsorption material, belonging to the field of mesporous material. The mesoporous adsorbent material of the invention has orderly mesoporous opening structure and composition of SiO2; amino modification of the surface of the material can be carried out. The adsorbent material of the invention can carry out the medical adsorption on various harmful matters such as bilirubin, cholic acid, uric acid, etc., and has good adsorption effect.
Description
Technical field
The present invention relates to mesoporous medical sorbent material, belong to mesoporous materials field.
Background technology
Poisonous substance roughly is divided into exogenous poisonous substance and endogenous poisonous substance two classes in the human body.The former comes exogenic noxious material (as agricultural chemicals, hypnotic etc.), assembles at inside of human body when them can cause various pathologies when too much; The latter then is that human body self detoxification system, immune system and the caused metabolite of metabolic system fault are too much accumulated and the noxious material (as bilirubin, cholic acid, uric acid etc.) of formation, also can cause various pathologies.Under the normal condition,
Human body can detoxify, remove or the endogenous or exogenous poisonous substance that neutralizes by autoprotection system such as liver detoxification system, human body self immune system and excretory system etc.But for diseases such as acute drugs poisoning, uremia, kidney failure, hepatic failures, human body self has lost detoxification ability substantially, only uses general internal medicine Clinical Processing (comprising gastric lavage, transfusion, diuresis, use antagonism medicine etc.) usually to be difficult to prove effective.So adopt medical adsorbent blood perfusion to purify the blood, remove the purpose that some morbid substance wherein just can reach clinical treatment.The main mechanism of blood perfusion is suction-operated, so be also referred to as blood absorption.
Blood perfusion has important effect with the development of sorbent material in the blood perfusion field, is the key factor of decision perfusion effect.Adsorbent commonly used at present mainly is activated carbon, resin and polysaccharide material.Because mostly the aperture is big, pore-size distribution is inhomogeneous, specific area is low etc. for above-mentioned material, make its in various degree exist deficiencies such as adsorptive selectivity is bad, adsorption capacity is low.Research and develop new and effective, high selectivity, high-adsorption-capacity, can realize that the sorbent material of perfusion device miniaturization is the active demand of blood purification treatment.
Meso pore silicon oxide material is the porous molecular sieve materials of class aperture between 2-50nm, such material have single pore-size distribution, high-sequential pore passage structure, high specific surface, preparation is simple, raw material is easy to get and be easy to carry out advantages such as modification and chemical modification and receive much concern, and is the research focuses of each ambit over nearly 15 years such as physics, chemistry, material, medicine, biology always.Mesoporous material has also been obtained some tremendous developments in the application study in fields such as catalysis, absorption, separation.Mesoporous material is as sorbent material, and the absorption that can be used to pollutants such as heavy metal ion, organic dyestuff at field of environment protection is removed, and in sensor field, can be used for adsorbing NO
xSensitive material Deng all gases molecule.Mesoporous material but rarely has report in the application aspect the medical sorbent material always.
Summary of the invention
The present invention is on to the preparation of mesopore silicon oxide and amino modified basis thereof, obtains a class and can be used as medical sorbent material as blood perfusion.
The preparation of material comprises the steps:
(1) preparation of mesopore silicon oxide SBA-15: every gram triblock copolymer surfactant P123 (BASF AG's product) is dissolved in the hydrochloric acid and 5～10 ml deionized water of 10～40 milliliters of 2mol/L, stir to forming a clear solution, then this solution is placed 37 ℃ water-bath, 0.5～2 gram ethyl orthosilicates are added in this surfactant solution, temperature is remained between 30-45 ℃, stirred 24 hours, and then under 100 ℃ of conditions hydrothermal treatment consists 20～72 hours.With deionized water filtration washing repeatedly, the gained powder is calcined in 400～600 ℃ of following air and was obtained mesoporous material SBA-15 in 2～8 hours after 100 ℃ of dry processing at last.Mesoporous SBA-15 has the orderly pore passage structure of six sides (2-50nm).
(2) mesopore silicon oxide SBA-15's is amino modified: the mesoporous powder SBA-15 after every gram calcining is dispersed in 50～200 milliliters of toluene, adds 3～10 milliliters of monoamine H again
2N (CH
2)
3Si (OC
2H
5)
3, diamine H
2NCH
2CH
2NH (CH
2)
3Si (OCH
3)
3, triamine silane coupler H
2N (CH
2)
2HN (CH
2)
2NH (CH
2)
3Si (OCH
3)
3, at 120 ℃, N
2Reaction (cooling water backflow) was fully filtered back gained powder with toluene and was obtained amino modified mesoporous material 1N-SBA-15,2N-SBA-15 and 3N-SBA-15 at 80 ℃ of vacuum drying treatment 8-15 hours more than 10 hours in the atmosphere.Mesoporous SBA-15 after amino modified has kept the orderly pore passage structure (2-50nm) of original six sides equally.
(3) preparation of mesopore silicon oxide MCM-41: every gram softex kw and 0.1～0.5 gram NaOH are dissolved in 10～50 ml waters, again 5～10 milliliters of ethyl orthosilicates are splashed into wherein, after hydrolysis 3-5 hour, above-mentioned mixed liquor is transferred in the water heating kettle, 110 ℃ of hydrothermal treatment consists 24～72 hours are filtered and are obtained obtaining mesoporous MCM-41 550 ℃ of calcinings after 500 minutes behind the powder drying.Mesoporous MCM-41 has the orderly pore passage structure of six sides (2-50nm).
(4) preparation of mesopore silicon oxide KIT-6: every gram P123 is dissolved in 20～40g deionized water and the 1～3g concentrated hydrochloric acid, stir to forming clear solution, add 0.5～2g n-butanol then and form homogeneous solution, this solution placed 40 ℃ oil bath, 2～4 gram ethyl orthosilicates slowly are added drop-wise in this surfactant solution, temperature is remained on 40 ℃, stirred 20 hours, and then under 100 ℃ of conditions hydrothermal treatment consists 24 hours.At last with deionized water filtration washing repeatedly, the gained powder 400～600 ℃ of calcinings 6 hours down, obtains mesoporous KIT-6 after 100 ℃ of dry processing.Mesoporous KIT-6 has a cube orderly pore passage structure ((2-50nm)
The carrying out of adsorption experiment:
(1) preparation of bilirubin solution:
Accurately take by weighing 100 milligrams of bilirubin under the lucifuge, with a spot of 0.1mol/lNaOH solution dissolving, again solution is transferred in 100 milliliters of volumetric flasks earlier, be settled to graduation mark with the sodium hydrogen phosphate of PH=7.4 and the cushioning liquid of sodium dihydrogen phosphate (PBS).By dilution, can prepare the bilirubin adsorption liquid of required various concentration at last.
(2) preparation of cholic acid solution:
Accurately take by weighing 0.15 gram cholic acid, be dissolved in the sodium hydrogen phosphate and sodium dihydrogen phosphate buffer of 100 milliliters of pH=7.4.
(3) preparation of uric acid solution:
Accurately take by weighing 0.5 gram uric acid, be dissolved in the NaOH solution of 250 milliliters of 0.02M.
(4) adsorption process and adsorbance are calculated:
Accurately take by weighing 0.2 gram adsorbent of above-mentioned preparation, join respectively in 20 milliliters of bilirubin, cholic acid or the uric acid adsorption liquid.Mixed liquor is stirred (bilirubin solution needs lucifuge) under constant temperature, behind the certain hour, a certain amount of upper strata stillness of night is got in centrifugation, measures the absorbance under bilirubin, cholic acid and the uric acid characteristic absorption wavelength and obtains its concentration.Adsorbance Q (mg/g) and adsorption rate E (%) are calculated by following equation respectively:
Q(mg/g)＝(C
0-C
1)V/1000W；
C in the formula
0, C
1Be respectively the concentration (mg/l) of absorption front and back solution mesobilirubin, cholic acid or uric acid, W is a mesopore silicon oxide powder weight (g), and V is adsorption liquid volume (ml).
Description of drawings
Fig. 1 is sample SBA-15, the mesoporous material (1N-SBA-15) of monoamine base modification, the SBA-15 of diamine modification (2N-SBA-15), the small angle X-ray diffraction collection of illustrative plates of the mesoporous material of triamine modification (3N-SBA-15).
Fig. 2 is sample SBA-15,1N-SBA-15,2N-SBA-15, the N of 3N-SBA-15
2Adsorption.
Fig. 3 is sample SBA-15,1N-SBA-15,2N-SBA-15, the pore size distribution curve of 3N-SBA-15.
Fig. 4 is the little angle XRD figure spectrum of mesoporous MCM-41 and KIT-6.
Fig. 5 is the N2 adsorption of mesoporous MCM-41 and KIT-6.
Fig. 6 is the pore size distribution curve of mesoporous MCM-41 and KIT-6.
Fig. 7 for sample SBA-15 and 2N-SBA-15 to bilirubinic adsorption capacity curve (the bilirubin initial concentration is 300mg/l, 37 ℃ of temperature) over time.
Fig. 8 is sample SBA-15, and 1N-SBA-15 and 2N-SBA-15 are to the change curve (adsorption equilibrium time 3 hour, temperature 37 ℃) of bilirubinic adsorption capacity with the bilirubin initial concentration.
Fig. 9 be sample 3N-SBA-15 to bilirubinic adsorption capacity with variation of temperature curve (initial concentration 500mg/l, equilibrium adsorption 2 hours).
The specific embodiment
Be directly used in bilirubinic absorption after surfactant is removed in mesopore silicon oxide SBA-15 calcining, the specific area of mesoporous pure silica SBA-15 is 775m
2/ g, the about 6.8nm of average pore size (being shown in Table 1).Over time as seen be adsorbed on after 2 hours and can reach balance by investigating bilirubin adsorption capacity on mesoporous SBA-15, obtain the equilibrium adsorption capacity (as shown in Figure 5) of material.When the initial concentration of bilirubin solution is 500mg/l, equilibrium adsorption is in the time of 3 hours, and the bilirubin equilibrium adsorption capacity of SBA-15 is 37mg/g (as shown in Figure 6).Along with the increase of bilirubin initial concentration, material also increases bilirubinic equilibrium adsorption capacity thereupon; When bilirubinic initial concentration increased to 1200mg/l, material can reach 100mg/g (as shown in Figure 6) to bilirubinic equilibrium adsorption capacity.
The pore structure parameter of table 1 sample, N content and bilirubin adsorption capacity list
| Sample | Specific area (m 2/g) | Aperture (nm) | Pore volume (ml/ g) | N content (mmol/g) | aBilirubin adsorption capacity (mg/g) |
| MCM-41 | 708 | 2.6 | 0.60 | - | 63 |
| KIT-6 | 684 | 5.8 | 0.79 | - | 52 |
| SBA-15 | 775 | 6.8 | 1.20 | - | 37 |
| 1N-SBA-15 | 373 | 6.0 | 0.76 | 1.41 | 51 |
| 2N-SBA-15 | 336 | 6.1 | 0.74 | 2.59 | 47 |
| 3N-SBA-15 | 256 | 6.1 | 0.57 | 4.00 | 42 |
aThe initial concentration 500mg/l of bilirubin solution, 37 ℃ of temperature.
The specific area of the mesoporous material 1N-SBA-15 of monoamine base modification is compared with pure mesopore silicon oxide SBA-15 to some extent and is descended, and specific area is 373m
2/ g, the about 6.0nm of average pore size (being shown in Table 1).When the initial concentration of bilirubin solution is 500mg/l, equilibrium adsorption is in the time of 3 hours, and the bilirubin equilibrium adsorption capacity of 1N-SBA-15 is 51mg/g, than the adsorption capacity big (as shown in table 1) of pure mesopore silicon oxide.Along with the increase of bilirubin initial concentration, material also increases bilirubinic equilibrium adsorption capacity thereupon; When bilirubinic initial concentration increased to 1200mg/l, material can reach 110mg/g (as shown in Figure 6) to bilirubinic equilibrium adsorption capacity.
The specific area of the SBA-15 of diamine modification is 336g, the about 6.1m of average pore size (being shown in Table 1).Over time as seen be adsorbed on after 2 hours and also can reach balance by investigating bilirubin adsorption capacity on mesoporous SBA-15, obtain the equilibrium adsorption capacity (as shown in Figure 5) of material.When the initial concentration of bilirubin solution is 500mg/l, equilibrium adsorption is in the time of 3 hours, and the bilirubin equilibrium adsorption capacity of 2N-SBA-15 is 47mg/g (as shown in table 1).Along with the increase of bilirubin initial concentration, material also increases bilirubinic equilibrium adsorption capacity thereupon; When bilirubinic initial concentration increased to 1200mg/l, material can reach 105mg/g (as shown in Figure 6) to bilirubinic equilibrium adsorption capacity.
The specific area of the mesoporous material 3N-SBA-15 of triamine modification is 256m
2/ g, the about 6.1nm of average pore size (being shown in Table 1).When the initial concentration of bilirubin solution is 500mg/l, equilibrium adsorption is in the time of 3 hours, and the bilirubin equilibrium adsorption capacity of 3N-SBA-15 is 42mg/g, than the adsorption capacity big (as shown in table 1) of pure mesopore silicon oxide.The mesopore silicon oxide of N base modification is all than the bilirubin adsorption capacity height of unmodified pure mesopore silicon oxide, illustrates that modification introduced more active group, carries out hydrogen bond with bilirubin and combines easilier.The raising of N content does not bring increase substantially (as shown in table 1) of bilirubin adsorption capacity, and it is relevant that this has occupied space, duct (specific area reduction) in the long-chain surfactant.Rising along with temperature, material decreases bilirubinic adsorption capacity, and when the bilirubin initial concentration is 500mg/l, 3N-SBA-15 is about 45mg/g to bilirubinic equilibrium adsorption capacity in the time of 15 ℃, when temperature rose to 55 ℃, adsorption capacity was reduced to 41mg/g (as shown in Figure 7).
Be directly used in bilirubinic absorption after surfactant is removed in mesopore silicon oxide MCM-41 calcining, the specific area of mesoporous MCM-41 is 708m
2/ g, the about 2.6nm of average pore size (seeing Table 1).When the initial concentration of bilirubin solution is 500mg/l, equilibrium adsorption is in the time of 3 hours, and MCM-41 is 63mg/g to bilirubinic equilibrium adsorption capacity.
Be directly used in bilirubinic absorption after surfactant is removed in mesopore silicon oxide KIT-6 calcining, the specific area of mesoporous KIT-6 is 684m
2/ g, the about 5.8nm of average pore size (seeing Table 1).When the initial concentration of bilirubin solution is 500mg/l, equilibrium adsorption is in the time of 3 hours, and KIT-6 is 52mg/g to bilirubinic equilibrium adsorption capacity.
The absorption that is directly used in uric acid behind the surfactant is removed in mesopore silicon oxide MCM-41 calcining, and the specific area of mesoporous MCM-41 is 708m
2/ g, the about 2.6nm of average pore size (seeing Table 1).When the uric acid initial concentration of solution is 2000mg/l, equilibrium adsorption is in the time of 6 hours, and MCM-41 is 108mg/g to the equilibrium adsorption capacity of uric acid.
Embodiment 8:
The absorption that is directly used in uric acid behind the surfactant is removed in mesopore silicon oxide SBA-15 calcining, and the specific area of mesoporous pure silica SBA-15 is 775m
2/ g, the about 6.8nm of average pore size (being shown in Table 1).When the uric acid initial concentration of solution is 2000mg/l, equilibrium adsorption is in the time of 6 hours, and SBA-15 is 118mg/g to the equilibrium adsorption capacity of uric acid.
The specific area of the SBA-15 of diamine modification is 336g, the about 6.1m of average pore size (being shown in Table 1).When the uric acid initial concentration of solution is 2000mg/l, equilibrium adsorption is in the time of 6 hours, and 2N-SBA-15 is 104mg/g to the equilibrium adsorption capacity of uric acid.
The absorption that is directly used in cholic acid behind the surfactant is removed in mesopore silicon oxide MCM-41 calcining, and the specific area of mesoporous MCM-41 is 708m
2/ g, the about 2.6nm of average pore size (seeing Table 1).When the cholic acid initial concentration of solution is 1500mg/l, equilibrium adsorption is in the time of 6 hours, and MCM-41 is 70mg/g to the equilibrium adsorption capacity of cholic acid.
Embodiment 11
The absorption that is directly used in cholic acid behind the surfactant is removed in mesopore silicon oxide SBA-15 calcining, and the specific area of mesoporous pure silica SBA-15 is 775m
2/ g, the about 6.8nm of average pore size (being shown in Table 1).When the cholic acid initial concentration of solution is 1500mg/l, equilibrium adsorption is in the time of 6 hours, and SBA-15 is 52mg/g to the equilibrium adsorption capacity of cholic acid.
The absorption that is directly used in cholic acid behind the surfactant is removed in mesopore silicon oxide KIT-6 calcining, and the specific area of mesoporous KIT-6 is 684m
2/ g, the about 5.8nm of average pore size (seeing Table 1).When the cholic acid initial concentration of solution is 1500mg/l, equilibrium adsorption is in the time of 6 hours, and KIT-6 is 29mg/g to the equilibrium adsorption capacity of cholic acid.
Claims (5)
1, mesoporous medical sorbent material is characterized in that having the ordered mesoporous pore canals structure of 2-50nm, and constituent is a silica.
2,, it is characterized in that the ordered mesoporous pore canals surface carried out amino modified by the described mesoporous medical sorbent material of claim 1.
3,, it is characterized in that the ordered mesoporous pore canals surface carried out monoamine modification, diamine modification or triamine modification by the described mesoporous medical sorbent material of claim 2.
4, be used for medical adsorbing domain by claim 1 or 2 or 3 described mesoporous medical sorbent materials.
5, be used for absorption by claim 1 or 2 or 3 described mesoporous medical sorbent materials to bilirubin or cholic acid or uric acid.
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| CNA2007101725408A CN101274265A (en) | 2007-12-19 | 2007-12-19 | Mesoporous medical sorbent material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973558A (en) * | 2010-09-30 | 2011-02-16 | 南京工业大学 | Amino modified SiO2 aerogel material and application thereof |
| CN103303938A (en) * | 2012-03-15 | 2013-09-18 | 上海中科高等研究院 | Amino-methyl dual-functionalized SBA-15 material as well as preparation method and application thereof |
| CN103655207A (en) * | 2013-12-04 | 2014-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Drug-loaded mesoporous-silica-reinforced dental binder and preparation method thereof |
| CN110523387A (en) * | 2019-09-25 | 2019-12-03 | 桂林电子科技大学 | Bilirubin high-efficiency adsorbent and preparation method thereof |
| CN111701575A (en) * | 2020-05-26 | 2020-09-25 | 武汉瑞法医疗器械有限公司 | Coated modified mesoporous titanium dioxide bilirubin adsorption material and preparation method thereof |
| CN112221474A (en) * | 2020-09-23 | 2021-01-15 | 重庆天外天生物技术有限公司 | Bilirubin adsorbent with high mechanical strength and good biocompatibility and preparation method thereof |
-
2007
- 2007-12-19 CN CNA2007101725408A patent/CN101274265A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973558A (en) * | 2010-09-30 | 2011-02-16 | 南京工业大学 | Amino modified SiO2 aerogel material and application thereof |
| CN103303938A (en) * | 2012-03-15 | 2013-09-18 | 上海中科高等研究院 | Amino-methyl dual-functionalized SBA-15 material as well as preparation method and application thereof |
| CN103655207A (en) * | 2013-12-04 | 2014-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Drug-loaded mesoporous-silica-reinforced dental binder and preparation method thereof |
| CN110523387A (en) * | 2019-09-25 | 2019-12-03 | 桂林电子科技大学 | Bilirubin high-efficiency adsorbent and preparation method thereof |
| CN110523387B (en) * | 2019-09-25 | 2022-06-10 | 桂林电子科技大学 | Bilirubin high-efficiency adsorbent and preparation method thereof |
| CN111701575A (en) * | 2020-05-26 | 2020-09-25 | 武汉瑞法医疗器械有限公司 | Coated modified mesoporous titanium dioxide bilirubin adsorption material and preparation method thereof |
| CN111701575B (en) * | 2020-05-26 | 2022-09-23 | 武汉瑞法医疗器械有限公司 | Coated modified mesoporous titanium dioxide bilirubin adsorption material and preparation method thereof |
| CN112221474A (en) * | 2020-09-23 | 2021-01-15 | 重庆天外天生物技术有限公司 | Bilirubin adsorbent with high mechanical strength and good biocompatibility and preparation method thereof |
| CN112221474B (en) * | 2020-09-23 | 2023-04-07 | 重庆天外天生物技术有限公司 | Bilirubin adsorbent with high mechanical strength and good biocompatibility and preparation method thereof |
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