CN106495178A - A kind of method for preparing mesoporous molecular sieve metatitanic acid neodymium surrounding purifying material - Google Patents
A kind of method for preparing mesoporous molecular sieve metatitanic acid neodymium surrounding purifying material Download PDFInfo
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- CN106495178A CN106495178A CN201610829387.0A CN201610829387A CN106495178A CN 106495178 A CN106495178 A CN 106495178A CN 201610829387 A CN201610829387 A CN 201610829387A CN 106495178 A CN106495178 A CN 106495178A
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- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
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Abstract
A kind of method for preparing mesoporous molecular sieve metatitanic acid neodymium surrounding purifying material, preparation raw material solution:Solution includes ethanol, ethylene glycol, acetone, butyl acetate, Cetyltrimethylammonium bromide, stabilizer LW 6, directed agents P32, neodymium nitrate and metatitanic acid dissident's alcohol ester;Synthetic reaction:Material solution is poured in stainless steel cauldron, is incubated 72h at 220 DEG C, is filtered, and with ethanol purge 3 times, obtains solid filter cake;Aperture moditied processing:After filter cake is processed in 0.5mol/L phosphoric acid solutions, 24h is dried at 120 DEG C, calcine 3 ~ 5h at 800 ~ 950 DEG C, obtain final product after grinding.
Description
Technical field:
The invention belongs to environmental purification function Material Field, and in particular to one kind prepares the mesoporous molecular sieve metatitanic acid neodymium depollution of environment
The method of material.
Background technology:
Molecular sieve referred to uniform aperture, its aperture class material suitable with general molecular size.Molecular sieve is powder
Shape crystal, water insoluble.Due to forming well-regulated duct and clear and definite cavity in framework of molecular sieve structure, molecular sieve has very big
Specific surface area, up to 300~1000 m2/ g, interior brilliant apparent height polarization, is a class high-efficiency adsorbent.Molecular sieve is also a class
Solid acid, surface have very high acid concentration and acid strength, can cause the catalytic reaction of carbonium ion type.The hole of adjustable molecular sieve
Footpath size, changes its adsorption property and catalytic property, so as to the molecular sieve catalyst of different performance is obtained.The application of molecular sieve is non-
Often extensively, can be used as efficient drying agent, selective absorbent, catalyst, ion-exchanger etc..
Silicate or aluminosilicate of the conventional molecular sieve for crystalline state, are to pass through oxygen by silicon-oxy tetrahedron or aluminum-oxygen tetrahedron
Bridged bond is connected and the duct of formation molecular dimension size and cavity system.New point is prepared as basic framework composition with metatitanic acid neodymium
Son sieve material, is a kind of new exploration, and prepared material has application prospect widely.In due to ambient air and water
A lot of contaminant molecule amounts larger, it is impossible to adsorbed by pore type material, prepare size 2 ~ 50 nm scopes mesoporous material have
There is very important meaning.This patent discloses a kind of method for preparing New Mesoporous Molecular Sieves type metatitanic acid neodymium surrounding purifying material.
With the stock of metatitanic acid neodymium ingredient sieve skeleton frame, pore size can be used for pollutant absorption in environment de- in macropore range
Remove and photochemical catalytic oxidation decontamination process.
Content of the invention:
For the problem that prior art is present, the present invention is intended to provide one kind prepares mesoporous molecular sieve metatitanic acid neodymium depollution of environment material
The method of material.
The technical solution used in the present invention is:
A kind of method for preparing mesoporous molecular sieve metatitanic acid neodymium surrounding purifying material, including following processing steps:
Step 1:Preparation raw material solution
Step 1.1:Be separately added in 200 mL beakers 36 ~ 43 mL ethanol, 33 ~ 38 mL ethylene glycol, 26 ~ 35 mL acetone,
12 ~ 15 mL butyl acetates, 6.3 ~ 7.2 g Cetyltrimethylammonium bromides, 1.5 ~ 1.6 g stabilizer LW-6,1.2 ~ 1.3 g
Directed agents P32;Beaker is placed in constant temperature electric heating water-bath, bath temperature is controlled for 30 DEG C, with 200 r/min speed magnetic force
Stir 30 min;
Step 1.2:5.1 ~ 5.3 g neodymium nitrates and 15 ~ 17 mL metatitanic acid dissident's alcohol esters are added in the solution in beaker, with 200
R/min speed continues 30 min of stirring;Material solution is obtained after cooling, standby;
Step 2:Synthetic reaction
Step 2.1:The material solution for preparing is poured in the stainless steel cauldron that volume is 200 mL, reactor is put in perseverance
Warm electrically heated drying cabinet, is incubated 72 h at 220 DEG C;
Step 2.2:Gained solid-liquid mix products are filtered, with ethanol purge 3 times in filter process, solid filter cake is obtained;
Step 3:Aperture moditied processing
Step 3.1:Solid matter obtained in step 2.2 is put in 500 mL three neck round bottom flask, and 300 are added in flask
ML concentration is the phosphoric acid solution of 0.5 mol/L, be respectively mounted on 3 interfaces of flask electric blender, straight cold finger and
Thermometric thermoelectricity corner;
Step 3.2:Flask is placed in constant temperature electrical heating bag, it is 75 DEG C to adjust solution temperature in flask, and motor stirrer is stirred
Speed is mixed for 200 r/min, 60 min is kept, is then cooled to room temperature;
Step 3.3:The product that step 3.2 is obtained is poured in centrifuge tube, in the high speed centrifuge with 8000 r/min rotating speeds from
30 min of the heart, gained solidliquid mixture is filtered, and in filter process, deionized water is cleaned 3 times, obtains solid filter cake;
Step 3.4:Solid filter cake is placed 24 h in 120 DEG C of constant temperature electric heating drying baker;
Step 3.5:Dried solid matter is put in porcelain crucible and is transferred in program control cabinet-type electric furnace, with 5 DEG C/min's
Calcining heat is risen to 800 ~ 950 DEG C by heating rate, is kept 3 ~ 5 h of this temperature, is cooled to room temperature, then fills in porcelain mortar
Divide grinding, that is, material requested is obtained.
Compared with prior art, it is an advantage of the current invention that:
The key technology of the present invention is the optimized choice to preparation technology and composition of raw materials.Optimally allocate in material solution
Solvent and the ratio of key component, are conducive to generating the high metatitanic acid neodymium material of purity, and can be in rational allocation material aperture chi
Very little.Thermal synthesis reaction and follow-up aperture moditied processing process are the weights for generating metatitanic acid neodymium material and constructing framework of molecular sieve structure
Want process.The materials synthesis processing step that the present invention is provided is clear, and product purity is high, and in material, table is compared in macropore range in aperture
Area is big.
Specific embodiment:
Embodiment 1
A kind of method for preparing mesoporous molecular sieve metatitanic acid neodymium surrounding purifying material, including following processing steps:
Step 1:Preparation raw material solution
Step 1.1:36 mL ethanol, 33 mL ethylene glycol, 26 mL acetone, 12 mL acetic acid are separately added in 200 mL beakers
Butyl ester, 6.3 g Cetyltrimethylammonium bromides, 1.5 g stabilizer LW-6,1.2 g directed agents P32;Beaker is placed in constant temperature
In electric hot water bath, bath temperature is controlled for 30 DEG C, with 200 r/min speed magnetic agitation, 30 min;
Step 1.2:5.1 g neodymium nitrates and 15 mL metatitanic acid dissident's alcohol esters are added in the solution in beaker, with 200 r/min speed
Rate continues 30 min of stirring;Material solution is obtained after cooling, standby;
Step 2:Synthetic reaction
Step 2.1:The material solution for preparing is poured in the stainless steel cauldron that volume is 200 mL, reactor is put in perseverance
Warm electrically heated drying cabinet, is incubated 72 h at 220 DEG C;
Step 2.2:Gained solid-liquid mix products are filtered, with ethanol purge 3 times in filter process, solid filter cake is obtained;
Step 3:Aperture moditied processing
Step 3.1:Solid matter obtained in step 2.2 is put in 500 mL three neck round bottom flask, and 300 are added in flask
ML concentration is the phosphoric acid solution of 0.5 mol/L, be respectively mounted on 3 interfaces of flask electric blender, straight cold finger and
Thermometric thermoelectricity corner;
Step 3.2:Flask is placed in constant temperature electrical heating bag, it is 75 DEG C to adjust solution temperature in flask, and motor stirrer is stirred
Speed is mixed for 200 r/min, 60 min is kept, is then cooled to room temperature;
Step 3.3:Product is poured in centrifuge tube, 30 min is centrifuged with 8000 r/min rotating speeds in high speed centrifuge, by institute
Obtain solidliquid mixture to filter, in filter process, deionized water is cleaned 3 times, obtains solid filter cake;
Step 3.4:Solid filter cake is placed 24 h in 120 DEG C of constant temperature electric heating drying baker;
Step 3.5 is put into dried solid matter in porcelain crucible and is transferred in program control cabinet-type electric furnace, with 5 DEG C/min's
Calcining heat is risen to 800 DEG C by heating rate, is kept 5 h of this temperature, is cooled to room temperature, is then fully ground in porcelain mortar,
Material requested is obtained.
Embodiment 2
A kind of method for preparing mesoporous molecular sieve metatitanic acid neodymium surrounding purifying material, including following processing steps:
Step 1:Preparation raw material solution
Step 1.1:39 mL ethanol, 36 mL ethylene glycol, 30 mL acetone, 13 mL acetic acid are separately added in 200 mL beakers
Butyl ester, 6.7 g Cetyltrimethylammonium bromides, 1.55 g stabilizer LW-6,1.25 g directed agents P32;Beaker is placed in perseverance
In warm electric hot water bath, bath temperature is controlled for 30 DEG C, with 200 r/min speed magnetic agitation, 30 min;
Step 1.2:5.2 g neodymium nitrates and 16 mL metatitanic acid dissident's alcohol esters are added in the solution in beaker, with 200 r/min speed
Rate continues 30 min of stirring;Material solution is obtained after cooling, standby;
Step 2:Synthetic reaction
Step 2.1:The material solution for preparing is poured in the stainless steel cauldron that volume is 200 mL, reactor is put in perseverance
Warm electrically heated drying cabinet, is incubated 72 h at 220 DEG C;
Step 2.2:Gained solid-liquid mix products are filtered, with ethanol purge 3 times in filter process, solid filter cake is obtained;
Step 3:Aperture moditied processing
Step 3.1:Solid matter obtained in step 2.2 is put in 500 mL three neck round bottom flask, and 300 are added in flask
ML concentration is the phosphoric acid solution of 0.5 mol/L, be respectively mounted on 3 interfaces of flask electric blender, straight cold finger and
Thermometric thermoelectricity corner;
Step 3.2:Flask is placed in constant temperature electrical heating bag, it is 75 DEG C to adjust solution temperature in flask, and motor stirrer is stirred
Speed is mixed for 200 r/min, 60 min is kept, is then cooled to room temperature;
Step 3.3:Product is poured in centrifuge tube, 30 min is centrifuged with 8000 r/min rotating speeds in high speed centrifuge, by institute
Obtain solidliquid mixture to filter, in filter process, deionized water is cleaned 3 times, obtains solid filter cake;
Step 3.4:Solid filter cake is placed 24 h in 120 DEG C of constant temperature electric heating drying baker;
Step 3.5:Dried solid matter is put in porcelain crucible and is transferred in program control cabinet-type electric furnace, with 5 DEG C/min
Heating rate calcining heat is risen to 900 DEG C, keep 4 h of this temperature, be cooled to room temperature, then fully grind in porcelain mortar
Mill, that is, be obtained material requested.
Embodiment 3
A kind of method for preparing mesoporous molecular sieve metatitanic acid neodymium surrounding purifying material, including following processing steps:
Step 1:Preparation raw material solution
Step 1.1:43 mL ethanol, 38 mL ethylene glycol, 35 mL acetone, 15 mL acetic acid are separately added in 200 mL beakers
Butyl ester, 7.2 g Cetyltrimethylammonium bromides, 1.6 g stabilizer LW-6,1.3 g directed agents P32;Beaker is placed in constant temperature
In electric hot water bath, bath temperature is controlled for 30 DEG C, with 200 r/min speed magnetic agitation, 30 min;
Step 1.2:5.3 g neodymium nitrates and 17 mL metatitanic acid dissident's alcohol esters are added in the solution in beaker, with 200 r/min speed
Rate continues 30 min of stirring;Material solution is obtained after cooling, standby;
Step 2:Synthetic reaction
Step 2.1:The material solution for preparing is poured in the stainless steel cauldron that volume is 200 mL, reactor is put in perseverance
Warm electrically heated drying cabinet, is incubated 72 h at 220 DEG C;
Step 2.2:Gained solid-liquid mix products are filtered, with ethanol purge 3 times in filter process, solid filter cake is obtained;
Step 3:Aperture moditied processing
Step 3.1:Solid matter obtained in step 2.2 is put in 500 mL three neck round bottom flask, and 300 are added in flask
ML concentration is the phosphoric acid solution of 0.5 mol/L, be respectively mounted on 3 interfaces of flask electric blender, straight cold finger and
Thermometric thermoelectricity corner;
Step 3.2:Flask is placed in constant temperature electrical heating bag, it is 75 DEG C to adjust solution temperature in flask, and motor stirrer is stirred
Speed is mixed for 200 r/min, 60 min is kept, is then cooled to room temperature;
Step 3.3:Product is poured in centrifuge tube, 30 min is centrifuged with 8000 r/min rotating speeds in high speed centrifuge, by institute
Obtain solidliquid mixture to filter, in filter process, deionized water is cleaned 3 times, obtains solid filter cake;
Step 3.4:Solid filter cake is placed 24 h in 120 DEG C of constant temperature electric heating drying baker;
Step 3.5:Dried solid matter is put in porcelain crucible and is transferred in program control cabinet-type electric furnace, with 5 DEG C/min's
Calcining heat is risen to 950 DEG C by heating rate, is kept 3 h of this temperature, is cooled to room temperature, is then fully ground in porcelain mortar,
Material requested is obtained.
Claims (2)
1. a kind of method for preparing mesoporous molecular sieve metatitanic acid neodymium surrounding purifying material, it is characterised in that walk including following techniques
Suddenly:
Step 1:Preparation raw material solution
Step 1.1:Be separately added in 200 mL beakers 36 ~ 43 mL ethanol, 33 ~ 38 mL ethylene glycol, 26 ~ 35 mL acetone,
12 ~ 15 mL butyl acetates, 6.3 ~ 7.2 g Cetyltrimethylammonium bromides, 1.5 ~ 1.6 g stabilizer LW-6,1.2 ~ 1.3 g
Directed agents P32;Beaker is placed in constant temperature electric heating water-bath, bath temperature is controlled for 30 DEG C, with 200 r/min speed magnetic force
Stir 30 min;
Step 1.2:5.1 ~ 5.3 g neodymium nitrates and 15 ~ 17 mL metatitanic acid dissident's alcohol esters are added in the solution in beaker, continues to stir
Mix 30 min;Material solution is obtained after cooling, standby;
Step 2:Synthetic reaction
Step 2.1:The material solution for preparing is poured in the stainless steel cauldron that volume is 200 mL, reactor is put in perseverance
Warm electrically heated drying cabinet, is incubated 72 h at 220 DEG C;
Step 2.2:Step 2.2 gained solid-liquid mix products are filtered, with ethanol purge 3 times in filter process, solid is obtained
Filter cake;
Step 3:Aperture moditied processing
Step 3.1:Solid matter obtained in step 2.2 is put in 500 mL three neck round bottom flask, and 300 are added in flask
ML concentration is the phosphoric acid solution of 0.5 mol/L, be respectively mounted on 3 interfaces of flask electric blender, straight cold finger and
Thermometric thermoelectricity corner;
Step 3.2:Flask is placed in constant temperature electrical heating bag, it is 75 DEG C to adjust solution temperature in flask, and motor stirrer is stirred
Speed is mixed for 200 r/min, 60 min is kept, is then cooled to room temperature;
Step 3.3:Product obtained in step 3.3 is poured in centrifuge tube, in the high speed centrifuge with 8000 r/min rotating speeds from
30 min of the heart, gained solidliquid mixture is filtered, and in filter process, deionized water is cleaned 3 times, obtains solid filter cake;
Step 3.4:Solid filter cake is placed 24 h in 120 DEG C of constant temperature electric heating drying baker;
Step 3.5:Dried solid matter is put in porcelain crucible and is transferred in program control cabinet-type electric furnace, with 5 DEG C/min's
Calcining heat is risen to 800 ~ 950 DEG C by heating rate, is kept 3 ~ 5 h of this temperature, is cooled to room temperature, then fills in porcelain mortar
Divide grinding, that is, material requested is obtained.
2. the method for preparing mesoporous molecular sieve metatitanic acid neodymium surrounding purifying material according to claim 1, it is characterised in that
The speed of agitator of the step 1.2 is 200 r/min.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107961776A (en) * | 2017-12-15 | 2018-04-27 | 沈阳理工大学 | A kind of preparation method of the structure mesoporous material of three-dimensional Ti-Sr oxide frameworks |
CN108246361A (en) * | 2018-01-08 | 2018-07-06 | 沈阳理工大学 | A kind of method for preparing molecular sieve type titanium cerium oxide catalysis material |
CN108502898A (en) * | 2018-06-28 | 2018-09-07 | 沈阳理工大学 | A method of preparing titanium germanium molecular sieve |
CN109399726A (en) * | 2018-11-15 | 2019-03-01 | 沈阳理工大学 | A kind of preparation method of iron lanthanum-oxides molecular sieve type scavenging material |
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CN105797707A (en) * | 2016-04-14 | 2016-07-27 | 沈阳理工大学 | Method for preparing mesoporous titanic acid lanthanum zinc photocatalyst |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107961776A (en) * | 2017-12-15 | 2018-04-27 | 沈阳理工大学 | A kind of preparation method of the structure mesoporous material of three-dimensional Ti-Sr oxide frameworks |
CN108246361A (en) * | 2018-01-08 | 2018-07-06 | 沈阳理工大学 | A kind of method for preparing molecular sieve type titanium cerium oxide catalysis material |
CN108246361B (en) * | 2018-01-08 | 2020-10-30 | 沈阳理工大学 | Method for preparing molecular sieve type titanium cerium oxide photocatalytic material |
CN108502898A (en) * | 2018-06-28 | 2018-09-07 | 沈阳理工大学 | A method of preparing titanium germanium molecular sieve |
CN108502898B (en) * | 2018-06-28 | 2019-10-25 | 沈阳理工大学 | A method of preparing titanium germanium molecular sieve |
CN109399726A (en) * | 2018-11-15 | 2019-03-01 | 沈阳理工大学 | A kind of preparation method of iron lanthanum-oxides molecular sieve type scavenging material |
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