CN107416873A - A kind of preparation method of the pillared magnalium hydrotalcite of Stability Analysis of Structures type - Google Patents
A kind of preparation method of the pillared magnalium hydrotalcite of Stability Analysis of Structures type Download PDFInfo
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- CN107416873A CN107416873A CN201710793658.6A CN201710793658A CN107416873A CN 107416873 A CN107416873 A CN 107416873A CN 201710793658 A CN201710793658 A CN 201710793658A CN 107416873 A CN107416873 A CN 107416873A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/063—Polymers comprising a characteristic microstructure
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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Abstract
The invention discloses a kind of preparation method of the pillared magnalium hydrotalcite of Stability Analysis of Structures type, belong to magnalium hydrotalcite preparing technical field.The present invention is raw material by dicyclopentadienyl nickel and dichlorodimethylsilane, high molecular polymer of the synthesis with network structure, pass through the net high-polymer polymer of formation, inter-modification and filling are carried out to pillared magnalium hydrotalcite, improves the inter-layer bonding force of pillared magnalium pillared hydrotalcite, hydrotalcite layered structure is improved by network polymers, pass through the cladding of network structure, hydrotalcite is effectively reduced because the phenomenon that layer structure causes to collapse produces, improves pillared hydrotalcite stability, improves material mechanical performance.
Description
Technical field
The invention discloses a kind of preparation method of the pillared magnalium hydrotalcite of Stability Analysis of Structures type, belongs to magnalium hydrotalcite preparation
Technical field.
Background technology
Hydrotalcite-based compound is a kind of anionic inorganic materials with layer structure, also referred to as layered bi-metal hydrogen
Oxide.Natural hydrotalcite class compound is magnalium hydrotalcite, is found earliest by Sweden in 1840s.With
Afterwards, two kinds of salting liquids of magnalium and sodium hydroxide reaction are prepared into magnalium into twentieth century initial stage, first passage experimental method
Hydrotalcite, while they propose the compound and have the imagination of double-decker by analysis.In the property and knot to hydrotalcite
Structure has carried out research and has found that it can be applied to catalytic field as a kind of acid base catalysator.Existing scholar's research laminate is difference
The crystal structure of the hydrotalcite of metal species, it is proposed that the architectural feature of hydrotalcite.By being heat-treated to hydrotalcite, find
Its roast product has good catalytic activity as catalyst in through sour condensation reaction, illustrates hydrotalcite in base catalysis, oxidation
Certain catalytic action can be played during reduction catalystses.
Under normal circumstances, the cation between the interlayer anion of pillared hydrotalcite and laminate relies primarily on electrostatic, oxygen key etc.
Interaction is stablized, and this interaction force is relatively weak, when being reacted as catalyst, with reaction progress its
Layer structure easily collapses, and can not be recycled so as to cause losing for catalytic activity.Therefore select a kind of layer structure compared with
The stable pillared hydrotalcite for being not easy to cave in is applied to catalytic reaction, will greatly improve the recycling effect of catalyst, saves
Cost, also comply with environmental requirement.
The content of the invention
Present invention mainly solves technical problem：Easily collapsed for existing pillared hydrotalcite layer structure, so as to cause
Losing for catalytic activity and the problem of can not recycle, there is provided a kind of preparation side of the pillared magnalium hydrotalcite of Stability Analysis of Structures type
Method.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）In mass ratio 1:5, dicyclopentadienyl nickel is added in n-hexane, is stirred to obtain matrix liquid, then in mass ratio 1:3, by four
Methyl ethylenediamine is added in matrix liquid, is stirred to obtain mixed liquor, and by volume 1:1, lithium amide hexane solution is added dropwise
Into mixed liquor, after being added dropwise to complete, filter cake is stirred and filtered and to obtain, washing, is dried, intermediate powder of milling to obtain；
（2）Count in parts by weight, weigh 45~50 parts of ether, 45~50 parts of tetramethylethylenediamines, 10~15 parts of intermediates respectively
Powder and 2~3 parts of dichlorodimethylsilane, stirring reaction, standing are warming up to room temperature, ageing, filtering, obtain filter residue；
（3）After rinsing filter residue, drying is placed in sublimator, and distillation crystallizes to obtain crystalline solid, in mass ratio 1:8, by crystalline solid with
Tetrahydrofuran is stirred, then in mass ratio 1:100, lithium amide hexane solution is added dropwise in conical flask, is stirred
It polymerize mixed liquor；
（4）In mass ratio 1:20, polymerization mixed liquor is added dropwise in hexane solution, it is still aging and filter, obtain ageing filter cake
And dry, mill, obtain modified powder；
（5）Count in parts by weight, weigh 10~15 parts of magnesium nitrates, 6~8 parts of aluminum nitrates, 85~90 parts of deionized water stirrings respectively
Mixing, pH to 10 is adjusted, obtains mixed base body fluid, in mass ratio 1：1：10, modification liquid is added dropwise in mixed base body fluid, in nitrogen
Heating water bath under atmosphere, standing are cooled to room temperature, adjust pH to 7.0, filter to obtain filter cake, dry, mill, you can are prepared into one kind
The pillared magnalium hydrotalcite of Stability Analysis of Structures type.
Step（5）Described modification liquid is to count in parts by weight, respectively weigh 45~50 parts of dichloromethane, 25~30 parts
Deionized water, 5~10 parts of modified powders and 2~3 parts of Tween-80s are placed in beaker, it is agitated mixing and ultrasonic disperse prepare and
Into.
Step（1）And step（3）Described lithium amide hexane solution concentration is 2mol/L.
Step（1）Described lithium amide hexane solution time for adding is 55~65min.
Step（2）Described stirring reaction temperature is -40 DEG C~-35 DEG C.
Step（5）Described modification liquid time for adding is 90~120min.
The beneficial effects of the invention are as follows：
The present invention is raw material by dicyclopentadienyl nickel and dichlorodimethylsilane, high molecular polymer of the synthesis with network structure, is led to
The net high-polymer polymer formed is crossed, inter-modification and filling are carried out to pillared magnalium hydrotalcite, it is pillared to improve pillared magnalium
The inter-layer bonding force of hydrotalcite, hydrotalcite layered structure is improved by network polymers, pass through the cladding of network structure, effectively drop
Low hydrotalcite improves pillared hydrotalcite stability, improves material mechanical performance because the phenomenon that layer structure causes to collapse produces.
Embodiment
In mass ratio 1:5, dicyclopentadienyl nickel is added in n-hexane, 10~15min is stirred, obtains matrix liquid, then by matter
Measure ratio 1:3, tetramethylethylenediamine is added in matrix liquid, is stirred to obtain mixed liquor, by volume 1:1, by 2mol/L ammonia
Base lithium hexane solution is added dropwise in mixed liquor, and it is 55~65min to control time for adding, after being added dropwise to complete, then at room temperature
20~24h is stirred, filters to obtain filter cake, after washing 3~5 times with hexane solution, is dried in vacuo intermediate powder of milling to obtain；
Count in parts by weight, weigh 45~50 parts of ether, 45~50 parts of tetramethylethylenediamines, 10~15 parts of intermediate powders and 2 respectively
~3 parts of dichlorodimethylsilane are placed in three-necked flask, are stirred and are placed in reacting 2~3h at -40~-35 DEG C, then quiet
Put and be warming up to room temperature, after being aged 10~12h, filter to obtain filter residue, after washed with ether 3~5 times, vacuum freeze drying is placed in rising
In magnificent device, distillation crystallizes to obtain crystalline solid, in mass ratio 1:8, crystalline solid and tetrahydrofuran are stirred and are placed in conical flask,
Again in mass ratio 1:100,2mol/L lithium amide hexane solutions are added dropwise in conical flask, after being stirred 45~60min, obtained
Polymerization mixed liquor, in mass ratio 1:20, polymerization mixed liquor is added dropwise in hexane solution, it is still aging and filter, it must be aged
Filter cake is placed in being dried in vacuo 6~8h at 45~50 DEG C, mills and is prepared into modified powder；Count in parts by weight, weigh 10 respectively
~15 parts of magnesium nitrates, 6~8 parts of aluminum nitrates, 85~90 parts of deionized waters are stirred, with the sodium hydroxide solution of mass fraction 5%
PH to 10 is adjusted, obtains mixed base body fluid, in mass ratio 1：1：10, modification liquid is added dropwise in mixed base body fluid, when control is added dropwise
Between be 90~120min, after being added dropwise to complete, lead to nitrogen exclude air, at nitrogen atmosphere, 75~80 DEG C heating water bath 20~
24h, standing are cooled to room temperature, and glacial acetic acid is added dropwise to pH value of solution to 7.0, filters to obtain filter cake, vacuum freeze drying is simultaneously milled, you can
It is prepared into a kind of pillared magnalium hydrotalcite of Stability Analysis of Structures type.Described modification liquid is to count in parts by weight, weighs 45~50 respectively
Part dichloromethane, 25~30 parts of deionized waters, 5~10 parts of modified powders and 2~3 parts of Tween-80s are placed in beaker, agitated mixed
Merge ultrasonic disperse to be prepared.
Example 1
In mass ratio 1:5, dicyclopentadienyl nickel is added in n-hexane, 10min is stirred, obtains matrix liquid, then in mass ratio 1:3,
Tetramethylethylenediamine is added in matrix liquid, is stirred to obtain mixed liquor, by volume 1:1, by 2mol/L lithium amides just oneself
Alkane solution is added dropwise in mixed liquor, and it is 55min to control time for adding, after being added dropwise to complete, then mixing 20h is stirred at room temperature,
Filter cake is filtered to obtain, after washing 3 times with hexane solution, is dried in vacuo intermediate powder of milling to obtain；Count, claim respectively in parts by weight
45 parts of ether of amount, 45 parts of tetramethylethylenediamines, 10 parts of intermediate powders and 2 parts of dichlorodimethylsilane are placed in three-necked flask,
It is stirred and is placed in reacting 2h at -40 DEG C, then stands and be warming up to room temperature, after being aged 10h, filter to obtain filter residue, rushed with ether
After washing 3 times, vacuum freeze drying is placed in sublimator, and distillation crystallizes to obtain crystalline solid, in mass ratio 1:8, by crystalline solid and four
Hydrogen furans, which is stirred, to be placed in conical flask, then in mass ratio 1:100,2mol/L lithium amide hexane solutions are added dropwise to cone
In shape bottle, after being stirred 45min, polymerization mixed liquor, in mass ratio 1 are obtained:20, polymerization mixed liquor is added dropwise to hexane solution
In, it is still aging and filter, filter cake must be aged and be placed in being dried in vacuo 6h at 45 DEG C, mill and be prepared into modified powder；By weight
Number meter, 10 parts of magnesium nitrates, 6 parts of aluminum nitrates, 85 parts of deionized waters are weighed respectively and are stirred, with the hydroxide of mass fraction 5%
Sodium solution adjusts pH to 10, obtains mixed base body fluid, in mass ratio 1：1：10, modification liquid is added dropwise in mixed base body fluid, controlled
Time for adding is 90min, after being added dropwise to complete, leads to nitrogen and excludes air, the heating water bath 20h at nitrogen atmosphere, 75 DEG C, stand
Room temperature is cooled to, glacial acetic acid is added dropwise to pH value of solution to 7.0, filters to obtain filter cake, vacuum freeze drying is simultaneously milled, you can is prepared into one
The kind pillared magnalium hydrotalcite of Stability Analysis of Structures type.Described modification liquid is to count in parts by weight, respectively weigh 45 parts of dichloromethane,
25 parts of deionized waters, 5 parts of modified powders and 2 parts of Tween-80s are placed in beaker, and simultaneously ultrasonic disperse is prepared for agitated mixing.
Example 2
In mass ratio 1:5, dicyclopentadienyl nickel is added in n-hexane, 12min is stirred, obtains matrix liquid, then in mass ratio 1:3,
Tetramethylethylenediamine is added in matrix liquid, is stirred to obtain mixed liquor, by volume 1:1, by 2mol/L lithium amides just oneself
Alkane solution is added dropwise in mixed liquor, and it is 60min to control time for adding, after being added dropwise to complete, then mixing 22h is stirred at room temperature,
Filter cake is filtered to obtain, after washing 4 times with hexane solution, is dried in vacuo intermediate powder of milling to obtain；Count, claim respectively in parts by weight
47 parts of ether of amount, 47 parts of tetramethylethylenediamines, 12 parts of intermediate powders and 3 parts of dichlorodimethylsilane are placed in three-necked flask,
It is stirred and is placed in reacting 3h at -37 DEG C, then stands and be warming up to room temperature, after being aged 11h, filter to obtain filter residue, rushed with ether
After washing 4 times, vacuum freeze drying is placed in sublimator, and distillation crystallizes to obtain crystalline solid, in mass ratio 1:8, by crystalline solid and four
Hydrogen furans, which is stirred, to be placed in conical flask, then in mass ratio 1:100,2mol/L lithium amide hexane solutions are added dropwise to cone
In shape bottle, after being stirred 47min, polymerization mixed liquor, in mass ratio 1 are obtained:20, polymerization mixed liquor is added dropwise to hexane solution
In, it is still aging and filter, filter cake must be aged and be placed in being dried in vacuo 7h at 47 DEG C, mill and be prepared into modified powder；By weight
Number meter, 12 parts of magnesium nitrates, 7 parts of aluminum nitrates, 87 parts of deionized waters are weighed respectively and are stirred, with the hydroxide of mass fraction 5%
Sodium solution adjusts pH to 10, obtains mixed base body fluid, in mass ratio 1：1：10, modification liquid is added dropwise in mixed base body fluid, controlled
Time for adding is 100min, after being added dropwise to complete, leads to nitrogen and excludes air, heating water bath 22h, quiet at nitrogen atmosphere, 77 DEG C
Put and be cooled to room temperature, glacial acetic acid is added dropwise to pH value of solution to 7.0, filters to obtain filter cake, vacuum freeze drying is simultaneously milled, you can is prepared into
A kind of pillared magnalium hydrotalcite of Stability Analysis of Structures type.Described modification liquid is to count in parts by weight, weighs 47 parts of dichloromethanes respectively
Alkane, 27 parts of deionized waters, 8 parts of modified powders and 2 parts of Tween-80s are placed in beaker, it is agitated mixing and ultrasonic disperse prepare and
Into.
Example 3
In mass ratio 1:5, dicyclopentadienyl nickel is added in n-hexane, 15min is stirred, obtains matrix liquid, then in mass ratio 1:3,
Tetramethylethylenediamine is added in matrix liquid, is stirred to obtain mixed liquor, by volume 1:1, by 2mol/L lithium amides just oneself
Alkane solution is added dropwise in mixed liquor, and it is 65min to control time for adding, after being added dropwise to complete, then mixing 24h is stirred at room temperature,
Filter cake is filtered to obtain, after washing 5 times with hexane solution, is dried in vacuo intermediate powder of milling to obtain；Count, claim respectively in parts by weight
50 parts of ether of amount, 50 parts of tetramethylethylenediamines, 15 parts of intermediate powders and 3 parts of dichlorodimethylsilane are placed in three-necked flask,
It is stirred and is placed in reacting 3h at -35 DEG C, then stands and be warming up to room temperature, after being aged 12h, filter to obtain filter residue, rushed with ether
After washing 4 times, vacuum freeze drying is placed in sublimator, and distillation crystallizes to obtain crystalline solid, in mass ratio 1:8, by crystalline solid and four
Hydrogen furans, which is stirred, to be placed in conical flask, then in mass ratio 1:100,2mol/L lithium amide hexane solutions are added dropwise to cone
In shape bottle, after being stirred 60min, polymerization mixed liquor, in mass ratio 1 are obtained:20, polymerization mixed liquor is added dropwise to hexane solution
In, it is still aging and filter, filter cake must be aged and be placed in being dried in vacuo 8h at 50 DEG C, mill and be prepared into modified powder；By weight
Number meter, 15 parts of magnesium nitrates, 8 parts of aluminum nitrates, 90 parts of deionized waters are weighed respectively and are stirred, with the hydroxide of mass fraction 5%
Sodium solution adjusts pH to 10, obtains mixed base body fluid, in mass ratio 1：1：10, modification liquid is added dropwise in mixed base body fluid, controlled
Time for adding is 120min, after being added dropwise to complete, leads to nitrogen and excludes air, heating water bath 24h, quiet at nitrogen atmosphere, 80 DEG C
Put and be cooled to room temperature, glacial acetic acid is added dropwise to pH value of solution to 7.0, filters to obtain filter cake, vacuum freeze drying is simultaneously milled, you can is prepared into
A kind of pillared magnalium hydrotalcite of Stability Analysis of Structures type.Described modification liquid is to count in parts by weight, weighs 50 parts of dichloromethanes respectively
Alkane, 30 parts of deionized waters, 10 parts of modified powders and 3 parts of Tween-80s are placed in beaker, it is agitated mixing and ultrasonic disperse prepare and
Into.
Example 1,2,3 and control group prepared by the present invention（The hydrotalcite FM300 of Jiangsu Jingjiang company production）Carry out
Performance comparison, performance comparison is as shown in following table table 1：
Again by carrying out powder x ray diffraction sign to example 1,2,3 and control group hydrotalcite（XRD）Carry out exterior syndrome discovery, example
The hydrotalcite layers that 1,2,3 interlamellar spacing is successively decreased step by step and prepared by the present invention are away from respectively less than control group, so water prepared by the present invention
Talcum and control group contrast illustrate the effective intercalation of modified powder of the present invention and improve material with less interlamellar spacing
Stability.
Claims (6)
1. a kind of preparation method of the pillared magnalium hydrotalcite of Stability Analysis of Structures type, it is characterised in that specifically preparation process is：
（1）In mass ratio 1:5, dicyclopentadienyl nickel is added in n-hexane, is stirred to obtain matrix liquid, then in mass ratio 1:3, by four
Methyl ethylenediamine is added in matrix liquid, is stirred to obtain mixed liquor, and by volume 1:1, lithium amide hexane solution is added dropwise
Into mixed liquor, after being added dropwise to complete, filter cake is stirred and filtered and to obtain, washing, is dried, intermediate powder of milling to obtain；
（2）Count in parts by weight, weigh 45~50 parts of ether, 45~50 parts of tetramethylethylenediamines, 10~15 parts of intermediates respectively
Powder and 2~3 parts of dichlorodimethylsilane, stirring reaction, standing are warming up to room temperature, ageing, filtering, obtain filter residue；
（3）After rinsing filter residue, drying is placed in sublimator, and distillation crystallizes to obtain crystalline solid, in mass ratio 1:8, by crystalline solid with
Tetrahydrofuran is stirred, then in mass ratio 1:100, lithium amide hexane solution is added dropwise in conical flask, is stirred
It polymerize mixed liquor；
（4）In mass ratio 1:20, polymerization mixed liquor is added dropwise in hexane solution, it is still aging and filter, obtain ageing filter cake
And dry, mill, obtain modified powder；
（5）Count in parts by weight, weigh 10~15 parts of magnesium nitrates, 6~8 parts of aluminum nitrates, 85~90 parts of deionized water stirrings respectively
Mixing, pH to 10 is adjusted, obtains mixed base body fluid, in mass ratio 1：1：10, modification liquid is added dropwise in mixed base body fluid, in nitrogen
Heating water bath under atmosphere, standing are cooled to room temperature, adjust pH to 7.0, filter to obtain filter cake, dry, mill, you can are prepared into one kind
The pillared magnalium hydrotalcite of Stability Analysis of Structures type.
A kind of 2. preparation method of pillared magnalium hydrotalcite of Stability Analysis of Structures type according to claim 1, it is characterised in that：Step
Suddenly（5）Described modification liquid is to count in parts by weight, weighs 45~50 parts of dichloromethane, 25~30 parts of deionized waters, 5 respectively
~10 parts of modified powders and 2~3 parts of Tween-80s are placed in beaker, and simultaneously ultrasonic disperse is prepared for agitated mixing.
A kind of 3. preparation method of pillared magnalium hydrotalcite of Stability Analysis of Structures type according to claim 1, it is characterised in that：Step
Suddenly（1）And step（3）Described lithium amide hexane solution concentration is 2mol/L.
A kind of 4. preparation method of pillared magnalium hydrotalcite of Stability Analysis of Structures type according to claim 1, it is characterised in that：Step
Suddenly（1）Described lithium amide hexane solution time for adding is 55~65min.
A kind of 5. preparation method of pillared magnalium hydrotalcite of Stability Analysis of Structures type according to claim 1, it is characterised in that：Step
Suddenly（2）Described stirring reaction temperature is -40 DEG C~-35 DEG C.
A kind of 6. preparation method of pillared magnalium hydrotalcite of Stability Analysis of Structures type according to claim 1, it is characterised in that：Step
Suddenly（5）Described modification liquid time for adding is 90~120min.
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| CN104893136A (en) * | 2014-03-03 | 2015-09-09 | 南通艾德旺化工有限公司 | Preparation method for modified composite magnesium aluminum hydrotalcite heat stabilizer |
| CN106076357A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of preparation method of magnetic loading manganese dioxide-catalyst |
| CN106076348A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of Fe-Al-Ce ternary metal oxide method for preparing catalyst |
| CN107099104A (en) * | 2017-05-23 | 2017-08-29 | 南通艾德旺化工有限公司 | Magnalium hydrotalcite composite thermal stabilizer and preparation method thereof, application |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102093654A (en) * | 2011-01-06 | 2011-06-15 | 中南大学 | Zinc-aluminium terres rares hydrotalcite compound heat stabilizer for polyvinyl chloride (PVC) as well as preparation and application of compound heat stabilizer |
| CN102617979A (en) * | 2012-04-17 | 2012-08-01 | 苏州科技学院 | Intercalation hydrotalcite fire retardant and preparation method thereof |
| CN102795649A (en) * | 2012-08-02 | 2012-11-28 | 浙江工业大学 | Preparation method for magnesium-aluminium hydrotalcite |
| CN103601750A (en) * | 2013-10-28 | 2014-02-26 | 南京大学 | Tetrakis(ethylmethylamino)hafnium synthesis method |
| CN104893136A (en) * | 2014-03-03 | 2015-09-09 | 南通艾德旺化工有限公司 | Preparation method for modified composite magnesium aluminum hydrotalcite heat stabilizer |
| CN106076357A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of preparation method of magnetic loading manganese dioxide-catalyst |
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Application publication date: 20171201 |