CN106902747B - A kind of amidoxim mesoporous silicon dioxide micro-sphere adsorbent and preparation method thereof - Google Patents
A kind of amidoxim mesoporous silicon dioxide micro-sphere adsorbent and preparation method thereof Download PDFInfo
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- CN106902747B CN106902747B CN201710194885.7A CN201710194885A CN106902747B CN 106902747 B CN106902747 B CN 106902747B CN 201710194885 A CN201710194885 A CN 201710194885A CN 106902747 B CN106902747 B CN 106902747B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
Abstract
A kind of amidoxim mesoporous silicon dioxide micro-sphere adsorbent is synthesized using sodium metasilicate as primary raw material using microwave-hydrothermal method, since sodium metasilicate cost of material is far below ethyl orthosilicate, can effectively reduce production cost;And it can significantly shorten the reaction time to 12~18h using microwave attenuation materials, improve production efficiency, and microwave attenuation materials can promote spontaneous nucleation, make nucleation more evenly, and while microwave-hydrothermal method synthesizing mesoporous silicon dioxide microsphere adsorbent, further functional group (amidoxime group) is introduced using copolycondensation method to be modified adsorbent, gained amidoxim mesoporous silicon dioxide micro-sphere adsorbent has flourishing ordered mesopore structure, good mechanical strength and chemical stability, it rapidly enters in duct and adsorbs convenient for uranium, the separation and recovery of uranium suitable for uranium-containing waste water.
Description
Technical field
The present invention relates to inorganic functional material technical fields more particularly to a kind of amidoxim mesoporous silicon dioxide micro-sphere to inhale
Attached dose and preparation method thereof.
Background technique
Uranium concentration reaches mg/L magnitude in the uranium-containing waste water that uranium generates in process of production, using novel absorption material from uranium-bearing
Separating enriched uranium not only can effectively recycle the uranium resource in waste water in waste water, but also can reduce uranium-containing waste water discharge bring environment dirt
Dye;Mesoporous silicon dioxide micro-sphere not only has good chemical stability and radiation resistance, but also high mechanical strength, specific surface area
Greatly, highly developed orderly pore structure is convenient for uranyl ion quick adsorption, therefore is ideal uranium absorption material.Mesoporous dioxy
SiClx microballoon produces usually using ethyl orthosilicate as raw material, but its production cost is higher, and the reaction time for needing to grow very much
(24~120h), and then cause production efficiency low, while mesoporous silicon dioxide micro-sphere is usually lower to the adsorption capacity of uranium;Cause
How this, be effectively reduced mesoporous silicon dioxide micro-sphere adsorbent production cost, improves production efficiency, and improve meso-porous titanium dioxide
Silicon microballoon to the adsorption capacity of uranium, must be solved using mesoporous silicon dioxide micro-sphere absorption separating enriched uranium from uranium-containing waste water
Major issue.
Summary of the invention
Technical problem solved by the invention be to provide a kind of amidoxim mesoporous silicon dioxide micro-sphere adsorbent and its
Preparation method, to solve the disadvantage in above-mentioned background technique.
Technical problem solved by the invention is realized using following technical scheme:
A kind of amidoxim mesoporous silicon dioxide micro-sphere adsorbent, general formula of molecular structure are as follows: SiO2[O3SiCH2CH2C
(NH2)NOH]x(x=0.06~0.13), molecular structure schematically as follows:
A kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method, the specific steps are as follows:
(1) amidoxim organosilan functionalized reagent is synthesized
120mg (3- cyanogen propyl) triethoxysilane is added in 20mL alcohol-water mixture (ethyl alcohol: water=1.6:5v/v)
(abbreviation CP-TES), 387.2mg azanol (abbreviation AO) and 275mg Na2CO3, reaction 12h is heated at reflux under the conditions of 70 DEG C, then
It is purified through soxhlet extraction, obtains amidoxim organosilan functionalized reagent ((3- amidoxime group propyl) triethoxysilane, abbreviation
AOES), reaction equation is as follows:
(2) amidoxim mesoporous silicon dioxide micro-sphere adsorbent is prepared
60mL dehydrated alcohol, 80mL deionized water, 30mL acetum (25wt.%) and 2.0mL pore template is taken to set
Quickly be stirred in container, side stirring, while be added into the container 50mL sodium silicate solution and (1.0~3.0g) together with amine
Oximate organosilan functionalized reagent mixes well to obtain mixture;Gained mixture is placed in reaction kettle again, in 40 DEG C of conditions
2~3h of lower stirring, then carry out microwave hydrothermal processing 10h under the conditions of being warming up to 90 DEG C and obtain intermediate compound I;Then this intermediate compound I is passed through
It is cooling, be separated by filtration to obtain solid product, while after obtained solid product is alternately washed using deionized water and ethyl alcohol, dividing again
It is dissipated in 80mL acid ethanol solution, 12h is heated at reflux under the conditions of 60 DEG C and sloughs pore template, obtains intermediate II;After
Separation of intermediates II is filtered, after being then separated by filtration the intermediate II finished using deionized water and ethanol washing, in 60 DEG C of items
It is sieved after being dried in vacuo 48h under part, obtains the amidoxim mesoporous silicon dioxide micro-sphere adsorbent that partial size is 90~150 microns.
In the present invention, in step (2), the pore template is polyethylene oxide-polypropylene oxide-polyethylene oxide
Triblock copolymer, abbreviation P123.
In the present invention, in step (2), silicic acid sodium content is 10.0g in the 50mL sodium silicate solution.
In the present invention, in step (2), the mass ratio of the amidoxim organosilan functionalized reagent and sodium metasilicate is
10wt.%~30wt.%.
The utility model has the advantages that
1) present invention uses sodium metasilicate substitution ethyl orthosilicate for primary raw material, since sodium metasilicate cost of material only has positive silicon
The 1/10 of acetoacetic ester cost of material, therefore can effectively reduce production cost;And utilize microwave-hydrothermal method synthesis amidoximization mesoporous
Silicon dioxide microsphere adsorbent can shorten the reaction time to 12~18h, significantly improve production efficiency;In addition, microwave-hydrothermal method is closed
At can promote spontaneous nucleation, gained amidoxim mesoporous silicon dioxide micro-sphere adsorbent granularity is more evenly;
2) present invention further utilizes copolycondensation while microwave-hydrothermal method synthesizing mesoporous silicon dioxide microsphere adsorbent
Method introduces functional group (amidoxime group) and is modified to adsorbent, therefore can significantly improve mesoporous silicon dioxide micro-sphere to uranium
Adsorption capacity;
3) amidoxim mesoporous silicon dioxide micro-sphere adsorbent prepared by the present invention has good mechanical strength and chemistry
Stability, can be from uranium-containing waste water quick adsorption uranium, and time of equilibrium adsorption is short, and uranium absorption capacity is high, and can reuse 6 times with
On, the separation and recovery of uranium suitable for uranium-containing waste water.
Detailed description of the invention
Fig. 1 is the preparation flow figure of presently preferred embodiments of the present invention.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Conjunction is specifically illustrating, and the present invention is further explained.
Embodiment 1
A kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method, the specific steps are as follows:
(1) amidoxim organosilan functionalized reagent (AOES) is synthesized
120mg (3- cyanogen propyl) triethoxysilane is added in 20mL alcohol-water mixture (ethyl alcohol: water=1.6:5v/v)
(CP-TES), 387.2mg azanol (AO) and 275mg Na2CO3, reaction 12h is heated at reflux under the conditions of 70 DEG C, then extract through Soxhlet
Purification is taken, obtains amidoxim organosilan functionalized reagent ((3- amidoxime group propyl) triethoxysilane), reaction equation is as follows:
(2) amidoxim mesoporous silicon dioxide micro-sphere adsorbent is prepared (by AOES/Na2SiO3Mass ratio 10wt.% is implemented)
60mL dehydrated alcohol, 80mL deionized water, 30mL acetum (25wt.%) and 2.0mL P123 is taken to be placed in appearance
It is quickly stirred in device, side stirring, while 50mL sodium silicate solution (sodium metasilicate containing 10.0g) and 1.0g are added into the container
AOES mixes well to obtain mixture;Gained mixture is placed in reaction kettle again, the stir about 2.5h under the conditions of 40 DEG C, then heated up
Microwave hydrothermal processing 10h is carried out under the conditions of to 90 DEG C obtains intermediate compound I;Then by this intermediate compound I through cooling, be separated by filtration to obtain solid
Product, while after obtained solid product is alternately washed using deionized water and ethyl alcohol, it is molten that it is dispersed to 80mL acidic ethanol again
In liquid, it is heated at reflux 12h under the conditions of 60 DEG C, to slough pore template (P123), obtains intermediate II;It is intermediate to refilter separation
Body II after being then separated by filtration the use deionized water and ethanol washing that finish, is sieved after being dried in vacuo 48h under the conditions of 60 DEG C
Point, obtain the amidoxim mesoporous silicon dioxide micro-sphere adsorbent that partial size is 90-150 microns.
The amidoxim mesoporous silicon dioxide micro-sphere adsorbent is detected to uranium absorption capacity upto 97mg/g, can be used
The separation and recovery of uranium in uranium-containing waste water, for time of equilibrium adsorption in 1h, amidoxim mesoporous silicon dioxide micro-sphere adsorbent can
Reuse 6 times or more, uranium absorption capacity decline 11.6%.
Embodiment 2
A kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method, the specific steps are as follows:
(1) amidoxim organosilan functionalized reagent (AOES) is synthesized
120mg (3- cyanogen propyl) triethoxysilane is added in 20mL alcohol-water mixture (ethyl alcohol: water=1.6:5v/v)
(CP-TES), 387.2mg azanol (AO) and 275mg Na2CO3, reaction 12h is heated at reflux under the conditions of 70 DEG C, then extract through Soxhlet
Purification is taken, obtains amidoxim organosilan functionalized reagent ((3- amidoxime group propyl) triethoxysilane), reaction equation is as follows:
(2) amidoxim mesoporous silicon dioxide micro-sphere adsorbent is prepared (by AOES/Na2SiO3Mass ratio 20wt.% is implemented)
60mL dehydrated alcohol, 80mL deionized water, 30mL acetum (25wt.%) and 2.0mL P123 is taken to be placed in appearance
It is quickly stirred in device;Side stirring, while 50mL sodium silicate solution (sodium metasilicate containing 10.0g) and 2.0g are added into the container
AOES mixes well to obtain mixture;Gained mixture is placed in reaction kettle again, the stir about 2.5h under the conditions of 40 DEG C, then heated up
Microwave hydrothermal processing 10h is carried out under the conditions of to 90 DEG C obtains intermediate compound I;Then by this intermediate compound I through cooling, be separated by filtration to obtain solid
Product, while after obtained solid product is alternately washed using deionized water and ethyl alcohol, it is molten that it is dispersed to 80mL acidic ethanol again
In liquid, it is heated at reflux 12h under the conditions of 60 DEG C, to slough pore template (P123), obtains intermediate II;It is intermediate to refilter separation
Body II, after being then separated by filtration the intermediate II finished using deionized water and ethanol washing, vacuum is dry under the conditions of 60 DEG C
It is sieved after dry 48h, obtains the amidoxim mesoporous silicon dioxide micro-sphere adsorbent that partial size is 90-150 microns.
The amidoxim mesoporous silicon dioxide micro-sphere adsorbent is detected to uranium absorption capacity upto 160mg/g, can be used
The separation and recovery of uranium in uranium-containing waste water, for time of equilibrium adsorption in 1h, amidoxim mesoporous silicon dioxide micro-sphere adsorbent can
Reuse 6 times or more, uranium absorption capacity decline 9.5%.
Embodiment 3
A kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method, the specific steps are as follows:
(1) amidoxim organosilan functionalized reagent (AOES) is synthesized
120mg (3- cyanogen propyl) triethoxysilane is added in 20mL alcohol-water mixture (ethyl alcohol: water=1.6:5v/v)
(CP-TES), 387.2mg azanol (AO) and 275mg Na2CO3, reaction 12h is heated at reflux under the conditions of 70 DEG C, then extract through Soxhlet
Purification is taken, obtains amidoxim organosilan functionalized reagent ((3- amidoxime group propyl) triethoxysilane), reaction equation is as follows:
(2) amidoxim mesoporous silicon dioxide micro-sphere adsorbent is prepared (by AOES/Na2SiO3Mass ratio 30wt.% is implemented)
60mL dehydrated alcohol, 80mL deionized water, 30mL acetum (25wt.%) and 2.0mL P123 is taken to be placed in appearance
It is quickly stirred in device, side stirring, while 50mL sodium silicate solution (sodium metasilicate containing 10.0g) and 3.0g are added into the container
AOES mixes well to obtain mixture;Gained mixture is placed in reaction kettle again, the stir about 2.5h under the conditions of 40 DEG C, then heated up
Microwave hydrothermal processing 10h is carried out under the conditions of to 90 DEG C obtains intermediate compound I;Then by this intermediate compound I through cooling, be separated by filtration to obtain solid
Product, while after obtained solid product is alternately washed using deionized water and ethyl alcohol, it is molten that it is dispersed to 80mL acidic ethanol again
In liquid, it is heated at reflux 12h under the conditions of 60 DEG C, to slough pore template (P123), obtains intermediate II;It is intermediate to refilter separation
Body II, after being then separated by filtration the intermediate II finished using deionized water and ethanol washing, vacuum is dry under the conditions of 60 DEG C
It is sieved after dry 48h, obtains the amidoxim mesoporous silicon dioxide micro-sphere adsorbent that partial size is 90-150 microns.
The amidoxim mesoporous silicon dioxide micro-sphere adsorbent is detected to uranium absorption capacity upto 135mg/g, can be used
The separation and recovery of uranium in uranium-containing waste water, for time of equilibrium adsorption in 1h, amidoxim mesoporous silicon dioxide micro-sphere adsorbent can
Reuse 6 times or more, uranium absorption capacity decline 10.4%.
It is detected by the amidoxim mesoporous silicon dioxide micro-sphere adsorbent prepared to 1~embodiment of embodiment 3 it is found that most
Good adsorption conditions are as follows: AOES/Na2SiO330 DEG C, Optimal pH 5.0-5.5 of mass ratio 20wt.%, adsorption temp, adsorbent amount
1.0g/L。
Basic principles and main features and major advantage of the invention have been shown and described above.The technical staff of the industry
It should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe the present invention
Principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these variation and
Improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent
Object defines.
Claims (8)
1. a kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method, which is characterized in that specific step is as follows:
(1) amidoxim organosilan functionalized reagent is synthesized
120mg (3- cyanogen propyl) triethoxysilane, 387.2mg azanol and 275mg is added in 20mL alcohol-water mixture
Na2CO3, it is heated at reflux reaction 12h under the conditions of 70 DEG C, then purify through soxhlet extraction, obtains the examination of amidoxim organosilan functionalization
Agent, reaction equation are as follows:
(2) amidoxim mesoporous silicon dioxide micro-sphere adsorbent is prepared
60mL dehydrated alcohol, 80mL deionized water, 30mL acetum and 2.0mL pore template is taken to be placed in container and quickly stir
Mixing, side stirring are mixed, while 50mL sodium silicate solution and quantitative amidoxim organosilan functionalization examination are added into the container
Agent is sufficiently mixed to obtain mixture;Gained mixture is placed in reaction kettle again, 2~3h is stirred under the conditions of 40 DEG C, then be warming up to
Microwave hydrothermal processing 10h is carried out under the conditions of 90 DEG C obtains intermediate compound I;Then by this intermediate compound I through cooling, be separated by filtration to obtain solid produce
Object, while after obtained solid product is alternately washed using deionized water and ethyl alcohol, it is dispersed to 80mL acid ethanol solution again
In, it is heated at reflux 12h under the conditions of 60 DEG C and sloughs pore template, obtains intermediate II;Separation of intermediates II is refiltered, then will
After the intermediate II finished is separated by filtration using deionized water and ethanol washing, sieved after being dried in vacuo 48h under the conditions of 60 DEG C,
Obtain the amidoxim mesoporous silicon dioxide micro-sphere adsorbent that partial size is 90~150 microns.
2. a kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method according to claim 1, feature exist
In in step (1), the volume ratio of ethyl alcohol and water is 1.6:5 in the alcohol-water mixture.
3. a kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method according to claim 1, feature exist
In in step (2), acetic acid quality divides rate to be 25% in the acetum.
4. a kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method according to claim 1, feature exist
In in step (2), the pore template is polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer.
5. a kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method according to claim 1, feature exist
In in step (2), silicic acid sodium content is 10.0g in the 50mL sodium silicate solution.
6. a kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method according to claim 1, feature exist
In in step (2), the mass ratio of the amidoxim organosilan functionalized reagent and sodium metasilicate is 10~30%.
7. a kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method according to claim 1, feature exist
In in step (2), the amidoxim organosilan functionalized reagent being added in the container is 1.0~3.0g.
8. a kind of amidoxim mesoporous silicon dioxide micro-sphere sorbent preparation method according to claim 1, feature exist
In the amidoxim mesoporous silicon dioxide micro-sphere sorbent molecule general structure of preparation are as follows: SiO2[O3SiCH2CH2C(NH2)
NOH]x, wherein the range of x is 0.06~0.13.
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CN109954484B (en) * | 2019-04-04 | 2022-03-18 | 哈尔滨工程大学 | Uranium adsorbing material of mesoporous silica gel particle loaded amidoxime polymer and preparation method |
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CN102765727A (en) * | 2012-07-09 | 2012-11-07 | 陕西科技大学 | Method for preparing SiO2 microsphere |
CN104525130A (en) * | 2014-12-31 | 2015-04-22 | 南华大学 | Method for preparing amidoxime-group ethane bridged bond mesoporous silica |
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CN102765727A (en) * | 2012-07-09 | 2012-11-07 | 陕西科技大学 | Method for preparing SiO2 microsphere |
CN104525130A (en) * | 2014-12-31 | 2015-04-22 | 南华大学 | Method for preparing amidoxime-group ethane bridged bond mesoporous silica |
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