Meso-porous material containing nano silver granulates and preparing method

Abstract

The present invention relates to a mesopore material containing nano silver granules. It is characterized by that more than 90% of nano silver granules are distributed in the pore channels, their grain size is 2-8n. Its preparation method includes the following steps: (a), nitration treatment of mesopore material: nitridizing mesopore material for 10-80 hr, at 70-1200 deg.C in the atmosphere containing ammonia to obtain nitrided mesopore material; the composition of atmosphere containing ammonia is: inert gas / ammonia=0-99%; (b) immersion: immersing the nitrided mesopore material prepared in step (a) in soluble silver salt aqueous solution whose concentration is 0.001-1 mal / l, under the ultrasonic or water bath condition stirring for 0.5-10 hr, then drying; and (c) calcinations: calcining the immersed sample prepared in step (b) for 3-24 hr at 300-550 deg.C so as to obtain the invented product.

Description

technical field

[0001] The invention relates to a mesoporous material containing nano silver particles and a preparation method thereof. Background technique

[0002] Silver is a good conductor of heat and electricity, and also has good ductility and chemical stability. When the size of silver particles reaches the nanometer range, it will have high activity, and at the same time exhibit unique optical, electrical and catalytic properties, especially breakthroughs have been made in antibacterial and catalytic aspects. Due to its unique antibacterial properties, nanosilver is widely used in medical antibacterial materials such as Chinese patent "Nanosilver Wound Paste" (publication number: CN2489751), Chinese patent "broad-spectrum antibacterial nano ointment" (publication number: CN1480045), etc. . And the nano-silver in the photocatalytic oxidation of gas-phase n-heptane reaction and CH 4 It has good catalytic activity in the selective reduction of NO reaction. It has b...

Examples

Embodiment 1

[0021] Preparation of Mesoporous Materials Containing Nano-Silver Particles Using SBA-15 as a Carrier

[0022] a. Take 1000 mg of SBA-15 sample, put it into a quartz tube furnace, and first purging it with nitrogen for 30 minutes at a flow rate of 80ml / min, then injecting ammonia gas at a flow rate of 100ml / min, while raising the temperature to 1000°C for 20 Hour. It was then cooled to room temperature under a nitrogen atmosphere. The nitrided product SBA-15N1 was obtained with a nitrogen content of 10%.

[0023] b. Take 100 mg of the nitriding sample SBA-15N1 prepared in a above, put it into a small crucible, and then put it into a container. Use a dropper to add silver nitrate solution to the crucible until the sample is just completely wet. Put it in the ultrasonic pool for ultrasonic treatment for 30-120 minutes, take it out and dry it.

[0024] c. Put the dried sample into a muffle furnace, raise the temperature to 300° C., and keep it for 3 hours to finally obtain the...

Embodiment 2

[0026] The sample Ag-SBA-15N1 that obtains in embodiment one is carried out each property test, and test situation and result thereof are as follows:

[0027] Using a transmission electron microscope (TEM) to observe, it can be seen that there are nano-silver particles in the pores of the mesoporous molecular sieve, the shape is spherical or ellipsoidal, the particle size is uniform, and the particle size is 7-8 nanometers. Under the same field of view, the number of silver particles on the outer surface is less than 5% (such as figure 1 and figure 2 shown).

[0028] Using X-ray diffraction analysis (XRD), it can be determined from the diffraction peak that the regular pore structure of the mesoporous material is maintained, and the presence of crystalline silver particles (such as image 3 ).

Embodiment 3

[0030] Preparation of Mesoporous Materials Containing Nano-Silver Particles Using SBA-15 as a Carrier

[0031] a. Take 1000 mg of SBA-15 sample, put it into a quartz tube furnace, and first blow it with nitrogen for 30 minutes at a flow rate of 80ml / min, then introduce ammonia gas at a flow rate of 15ml / min, and simultaneously raise the temperature to 1000°C and keep for 40 Hour. It was then cooled to room temperature under a nitrogen atmosphere. A nitrided mesoporous material SBA-15N2 with a nitrogen content of 15% was obtained.

[0032] b. Take 100 mg of the nitriding sample SBA-15N2 prepared in a above, put it into a small crucible, and then use a dropper to drop the silver nitrate solution into the crucible until the sample is just completely wetted. Put the crucible in a water bath and heat it to 50-80°C, keep it for 5-10 hours, then take it out and dry it.

[0033] c. Put the dried sample into a muffle furnace, raise the temperature to 300°C, and keep it for 6 hours t...

technical field

[0001] The invention relates to a mesoporous material containing nano silver particles and a preparation method thereof. Background technique

[0002] Silver is a good conductor of heat and electricity, and also has good ductility and chemical stability. When the size of silver particles reaches the nanometer range, it will have high activity, and at the same time exhibit unique optical, electrical and catalytic properties, especially breakthroughs have been made in antibacterial and catalytic aspects. Due to its unique antibacterial properties, nanosilver is widely used in medical antibacterial materials such as Chinese patent "Nanosilver Wound Paste" (publication number: CN2489751), Chinese patent "broad-spectrum antibacterial nano ointment" (publication number: CN1480045), etc. . And the nano-silver in the photocatalytic oxidation of gas-phase n-heptane reaction and CH 4 It has good catalytic activity in the selective reduction of NO reaction. It has b...

Examples

Embodiment 1

[0021] Preparation of Mesoporous Materials Containing Nano-Silver Particles Using SBA-15 as a Carrier

[0022] a. Take 1000 mg of SBA-15 sample, put it into a quartz tube furnace, and first purging it with nitrogen for 30 minutes at a flow rate of 80ml / min, then injecting ammonia gas at a flow rate of 100ml / min, while raising the temperature to 1000°C for 20 Hour. It was then cooled to room temperature under a nitrogen atmosphere. The nitrided product SBA-15N1 was obtained with a nitrogen content of 10%.

[0023] b. Take 100 mg of the nitriding sample SBA-15N1 prepared in a above, put it into a small crucible, and then put it into a container. Use a dropper to add silver nitrate solution to the crucible until the sample is just completely wet. Put it in the ultrasonic pool for ultrasonic treatment for 30-120 minutes, take it out and dry it.

[0024] c. Put the dried sample into a muffle furnace, raise the temperature to 300° C., and keep it for 3 hours to finally obtain the...

Embodiment 2

[0026] The sample Ag-SBA-15N1 that obtains in embodiment one is carried out each property test, and test situation and result thereof are as follows:

[0027] Using a transmission electron microscope (TEM) to observe, it can be seen that there are nano-silver particles in the pores of the mesoporous molecular sieve, the shape is spherical or ellipsoidal, the particle size is uniform, and the particle size is 7-8 nanometers. Under the same field of view, the number of silver particles on the outer surface is less than 5% (such as figure 1 and figure 2 shown).

[0028] Using X-ray diffraction analysis (XRD), it can be determined from the diffraction peak that the regular pore structure of the mesoporous material is maintained, and the presence of crystalline silver particles (such as image 3 ).

Embodiment 3

[0030] Preparation of Mesoporous Materials Containing Nano-Silver Particles Using SBA-15 as a Carrier

[0031] a. Take 1000 mg of SBA-15 sample, put it into a quartz tube furnace, and first blow it with nitrogen for 30 minutes at a flow rate of 80ml / min, then introduce ammonia gas at a flow rate of 15ml / min, and simultaneously raise the temperature to 1000°C and keep for 40 Hour. It was then cooled to room temperature under a nitrogen atmosphere. A nitrided mesoporous material SBA-15N2 with a nitrogen content of 15% was obtained.

[0032] b. Take 100 mg of the nitriding sample SBA-15N2 prepared in a above, put it into a small crucible, and then use a dropper to drop the silver nitrate solution into the crucible until the sample is just completely wetted. Put the crucible in a water bath and heat it to 50-80°C, keep it for 5-10 hours, then take it out and dry it.

[0033] c. Put the dried sample into a muffle furnace, raise the temperature to 300°C, and keep it for 6 hours t...

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