Method for Synthesis of Ordered Mesoporous Silicone Material with Tyrosine Skeleton
A mesoporous organosilicon and tyrosine technology, applied in organic chemistry, chemical instruments and methods, compounds of group 4/14 elements of the periodic table, etc., can solve the problem of poor hydrothermal stability of PMSs, narrow pore size distribution, pore Problems such as low adjustability of surface chemical properties
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Embodiment 1
[0023] Example 1: PMOs material containing 2.5% tyrosine organosilicon compound.
[0024] (1) Synthesis of tyrosine methyl ester: tyrosine (10.86g 60.0mmol) was added to a 250mL three-necked flask, then 120mL of frozen methanol was added, and then SOCl was slowly added dropwise 2 (10.0 g 85 mmol). After stirring overnight at room temperature, the solvent was spin-dried to obtain crude tyrosine methyl ester hydrochloride as a white solid. Crude tyrosine hydrochloride (5 g 21.6 mmol) was dissolved in 75 mL THF to form a white suspension, triethylamine (2.18 g 21.6 mmol) was added thereto, and stirred overnight at room temperature. The reaction solution was filtered, the filter cake was washed 1-2 times with THF, and the filtrate was spin-dried to obtain 4.03 g of yellow oil.
[0025] (2) Coupling of tyrosine methyl ester and hydrazine hydrate: 4.03g tyrosine methyl ester is dissolved in 100mL methanol, then add excess hydrazine hydrate, stir at room temperature for one day, di...
Embodiment 2
[0030] Example 2: PMOs material containing 7.5% tyrosine organosilicon compound.
[0031] Steps (1), (2), and (3) of this embodiment are the same as in Embodiment 1.
[0032] (4) This step is basically the same as step (4) of Example 1, except that the mass of tetraethyl orthosilicate and tyrosine organosilicon compound added are 3.854g and 1.034g.
[0033] From Figure 4 It can be seen in the d 100 There are still obvious diffraction peaks at d 110 place and d 200 Almost no diffraction peaks can be observed, indicating that the material still has a pore structure similar to mesoporous materials.
[0034] Figure 5 The nitrogen adsorption-desorption isotherm is a typical IV type, as can be seen from the figure, in the P / P 0 =0.7-0.9 An obvious H1-type hysteresis loop can be observed, which is caused by the capillary condensation phenomenon of mesoporous channels; in the pore size distribution diagram, the size of the mesoporous pores is about 3.8nm.
Embodiment 3
[0035] Example 3: PMOs material containing 15% tyrosine organosilicon compound.
[0036] Steps (1), (2), and (3) of this embodiment are the same as in Embodiment 1.
[0037](4) This step is basically the same as step (4) of Example 1, except that the mass of tetraethyl orthosilicate and tyrosine organosilicon compound added are 3.333g and 2.067g.
[0038] From Figure 6 It can be seen in the d 100 The diffraction peak at is very weak and can hardly be observed, d 110 place and d 200 Diffraction peaks disappear completely, indicating that with the increase of organosilicon content, the unit cell shrinks, and the silicon wall exhibits lower structural regularity.
[0039] Figure 7 The nitrogen adsorption-desorption isotherm is a typical IV type. It can be seen from the figure that the hysteresis ring changes from H1 type to H3 type, which is caused by the slit-shaped uniform channels; in the pore size distribution diagram, the mesopore diameter The size is around 3.4nm. ...
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