CN105582882A - Preparation method of porous geopolymer aerogel - Google Patents
Preparation method of porous geopolymer aerogel Download PDFInfo
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- CN105582882A CN105582882A CN201510995103.0A CN201510995103A CN105582882A CN 105582882 A CN105582882 A CN 105582882A CN 201510995103 A CN201510995103 A CN 201510995103A CN 105582882 A CN105582882 A CN 105582882A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000004964 aerogel Substances 0.000 title abstract description 6
- 229920000876 geopolymer Polymers 0.000 title abstract 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 14
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims description 35
- 239000007788 liquid Substances 0.000 claims description 35
- 239000000843 powder Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 23
- 229920000642 polymer Polymers 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 15
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical class [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 14
- 235000019353 potassium silicate Nutrition 0.000 claims description 13
- 239000012043 crude product Substances 0.000 claims description 10
- -1 20~40 parts Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 238000005352 clarification Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 6
- 239000011148 porous material Substances 0.000 abstract description 6
- 229910021529 ammonia Inorganic materials 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 235000015110 jellies Nutrition 0.000 abstract description 3
- 239000008274 jelly Substances 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000499 gel Substances 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 239000004115 Sodium Silicate Substances 0.000 abstract 3
- 229910052911 sodium silicate Inorganic materials 0.000 abstract 3
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 abstract 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 abstract 2
- 235000019837 monoammonium phosphate Nutrition 0.000 abstract 2
- 239000012190 activator Substances 0.000 abstract 1
- 238000012643 polycondensation polymerization Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- 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
- B01J20/12—Naturally occurring clays or bleaching earth
-
- 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
-
- 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
- B01J20/28047—Gels
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a preparation method of porous geopolymer aerogel and belongs to the field of adsorbing materials. The porous geopolymer aerogel comprises raw materials in parts by weight as follows: 20-40 parts of sodium hydroxide, 20-40 parts of water, 120-200 parts of sodium silicate, 100-200 parts of kaolin and 5-10 parts of ammonium dihydrogen phosphate. The kaolin and sodium silicate are taken as silicon sources, ammonium dihydrogen phosphate is taken as a pore structure control agent, and sodium hydroxide is taken as an activator; sodium silicate, metakaolin and sodium hydroxide are mixed, water is added, the mixture has condensation polymerization, jelly in a gel state is produced through reaction and adopts a three-dimensional structure, a system produces ammonia at a high temperature, larger and more uniform pores are formed in the three-dimensional structure by ammonia, so that the porous geopolymer aerogel has larger surface area, more pores and higher adsorbing capacity, and the use amount of the porous geopolymer aerogel is reduced.
Description
Technical field
The invention belongs to sorbing material field, relate in particular to the system of a kind of porous ground polymers aerogePreparation Method.
Background technology
Aeroge is a kind of Performances of Novel Nano-Porous meter level porosu solid material with continuous three-dimensional net structureMaterial, formed by continuous solid skeletal and connective nanoaperture, wherein porosity up to80%～99.8%, solids content is few, therefore aeroge have low-density (3kg/m3～600kg/m3), high-specific surface area (300kg/m3～1200m2/g), be current apparent densityLittle condensed state material, has the title of " solid smog " or " solid air ". Aeroge uniquenessNano-pore structure make it have excellent performance, as the aperture of aeroge is less than air moleculeMean free path, thereby in aerogel pores, there is no cross-ventilation, and the porosity of aerogeUp to 80%～99.8%, the shared volume ratio of solid is extremely low, makes aeroge become current generationThe minimum solid material of thermal conductivity in boundary, its thermal conductivity can be low to moderate at room temperature atmospheric air0.002W/ (mK), can reach 0.001W/ (mK) in a vacuum. And its three-dimensional networkStructure structure can be controlled and cutting in nanoscale, therefore at necks such as medical science, building, the energyTerritory has vast potential for future development, can be used as superinsulation material, catalyst carrier, adsorbentAnd the electrode of heavy-duty battery etc.
Aeroge kind is a lot, generally can be divided into organic and inorganic and organic/nothing according to its compositionMachine hydridization aeroge three major types. Because the method for hydridization can be controlled material on molecular levelStructure and composition, carries out cutting to aeroge performance, brings into play each component excellent properties and even obtainsNew performance, is therefore widely used in aeroge, becomes a study hotspot in aeroge fieldAnd new growth point.
Summary of the invention
The invention provides a kind of porous ground polymers aeroge. Its raw material comprises following weight portionRaw material: 20～40 parts, NaOH, 20～40 parts, water, 120～200 parts of waterglass, kaolin100～200 parts, 5～10 parts of ammonium hydrogen phosphates.
Further, comprise the raw material of following weight portion: 30 parts, NaOH, 30 parts, water, water150 parts, glass, 160 parts of kaolin, 8 parts of ammonium hydrogen phosphates.
Further, described water is deionized water.
Meanwhile, the present invention also provides the preparation method of a kind of porous ground polymers aeroge, its spyLevy and be to comprise the following steps:
1) metakaolin preparation, makes kaolin at the temperature lower calcination 4～6h of 500～900 DEG CMetakaolin;
2) alkali swashs the configuration of liquid, first the NaOH weighing up is poured in the waterglass weighing up,Then adding the water weighing up, and till being stirred to rapidly solution clarification, then more than standing 1h;
3), by metakaolin, swash the mixing of liquid with alkali, first ammonium hydrogen phosphate is added to metakaolinIn mix and make powder, then the powder of making is added alkali to swash in liquid, addition manner is:First the powder of 1/3 amount being poured into alkali swashs in liquid and rapid stirring reaction 1～3min; And then by 1/3The powder of amount is poured alkali into and is swashed in liquid and rapid stirring reaction 1～3min; Finally again by remaining 1/3Amount powder is poured alkali into and is swashed in liquid and rapid stirring reaction 1～3min; Stir 2～4min, obtain airsettingGlue crude product;
4) by step 3) aeroge crude product ageing 4～8h at the temperature of 65～75 DEG C of obtaining,And then with supercritical fluid drying, obtain this ground polymers aeroge.
Further, the modulus of the sharp liquid of described alkali is 1.0～3.0.
Further, described ammonium hydrogen phosphate before use, grinds granulating in super grinderFootpath is the particle of 100～500 μ m, and when grinding, keeping temperature is 10～20 DEG C.
Beneficial effect of the present invention is: the present invention is taking kaolin and waterglass as silicon source, phosphoric acidHydrogen ammonium is pore structure controlling agent, and NaOH is as exciting agent; Waterglass, metakaolin and hydrogenSodium oxide molybdena mixes and the generation polycondensation reaction that adds water, and generates the jelly of gel state, then adds phosphorusAcid hydrogen ammonium, its phosphate radical has three reactive functionality, and presents three-dimensional structure, can with glueThing is in conjunction with forming tridimensional network, and ammonium radical ion reacts with the hydroxyl of jelly, follow-upHigh temperature aging step in generate ammonia, ammonia tridimensional network form evenHole, make this porous ground polymers aeroge surface area larger, hole is more, its energy of adsorptionPower is stronger, reduces the use amount of this porous ground polymers aeroge. Meanwhile, the present invention is by phosphoric acid hydrogenAmmonium grinds to form the particle that particle diameter is 100～500 μ m, makes it more equal with mixing of jellyEven, the hole of the porous ground polymers aeroge of formation is more even.
Detailed description of the invention
Further describe technical scheme of the present invention below, but claimed scope is not limited toIn described.
Embodiment mono-
1, raw material
NaOH 20kg, deionized water 20kg, waterglass 120kg, kaolin 100kg, phosphorusAcid hydrogen ammonium 5kg.
2, manufacture craft
1) metakaolin preparation, makes kaolin at the temperature lower calcination 4～6h of 500～900 DEG CMetakaolin;
2) alkali swashs the configuration of liquid, first the NaOH weighing up is poured in the waterglass weighing up,Then adding the water weighing up, and till being stirred to rapidly solution clarification, stir speed (S.S.) is300r/min, then more than standing 1h, the modulus that alkali swashs liquid is controlled at 1.0～3.0;
3) ammonium hydrogen phosphate grinds, and in super grinder, grinding to form particle diameter is 100～500 μ m'sParticle, when grinding, keeping temperature is 10 DEG C;
4), by metakaolin, swash the mixing of liquid with alkali, first ammonium hydrogen phosphate is added to metakaolinIn mix and make powder, then the powder of making is added alkali to swash in liquid, addition manner is:First the powder of 1/3 amount being poured into alkali swashs in liquid and rapid stirring reaction 1～3min; And then by 1/3The powder of amount is poured alkali into and is swashed in liquid and rapid stirring reaction 1～3min; Finally again by remaining 1/3Amount powder is poured alkali into and is swashed in liquid and rapid stirring reaction 1～3min; Stir 2～4min, obtain airsettingGlue crude product;
5) by step 4) aeroge crude product ageing 4～8h at the temperature of 65 DEG C of obtaining, thenUse again supercritical fluid drying, obtain this ground polymers aeroge.
Embodiment bis-
1, raw material
NaOH 40kg, deionized water 40kg, waterglass 200kg, kaolin 200kg, phosphorusAcid hydrogen ammonium 10kg.
2, manufacture craft
1) metakaolin preparation, makes kaolin at the temperature lower calcination 4～6h of 500～900 DEG CMetakaolin;
2) alkali swashs the configuration of liquid, first the NaOH weighing up is poured in the waterglass weighing up,Then adding the water weighing up, and till being stirred to rapidly solution clarification, stir speed (S.S.) is500r/min, then more than standing 1h, the modulus that alkali swashs liquid is controlled at 1.0～3.0;
3) ammonium hydrogen phosphate grinds, and in super grinder, grinding to form particle diameter is 100～500 μ m'sParticle, when grinding, keeping temperature is 20 DEG C
4), by metakaolin, swash the mixing of liquid with alkali, first ammonium hydrogen phosphate is added to metakaolinIn mix and make powder, then the powder of making is added alkali to swash in liquid, addition manner is:First the powder of 1/3 amount being poured into alkali swashs in liquid and rapid stirring reaction 1～3min; And then by 1/3The powder of amount is poured alkali into and is swashed in liquid and rapid stirring reaction 1～3min; Finally again by remaining 1/3Amount powder is poured alkali into and is swashed in liquid and rapid stirring reaction 1～3min; Stir 2～4min, obtain airsettingGlue crude product;
5) by step 4) aeroge crude product ageing 4～8h at the temperature of 75 DEG C of obtaining, thenUse again supercritical fluid drying, obtain this ground polymers aeroge.
Embodiment tri-
1, raw material
NaOH 30kg, water 30kg, waterglass 150kg, kaolin 160kg, ammonium hydrogen phosphate8kg。
2, manufacture craft
1) metakaolin preparation, makes kaolin at the temperature lower calcination 4～6h of 500～900 DEG CMetakaolin;
2) alkali swashs the configuration of liquid, first the NaOH weighing up is poured in the waterglass weighing up,Then adding the water weighing up, and till being stirred to rapidly solution clarification, stir speed (S.S.) is400r/min, then more than standing 1h, the modulus that alkali swashs liquid is controlled at 1.0～3.0;
3) ammonium hydrogen phosphate grinds, and in super grinder, grinding to form particle diameter is 100～500 μ m'sParticle, when grinding, keeping temperature is 15 DEG C;
4), by metakaolin, swash the mixing of liquid with alkali, first ammonium hydrogen phosphate is added to metakaolinIn mix and make powder, then the powder of making is added alkali to swash in liquid, addition manner is:First the powder of 1/3 amount being poured into alkali swashs in liquid and rapid stirring reaction 1～3min; And then by 1/3The powder of amount is poured alkali into and is swashed in liquid and rapid stirring reaction 1～3min; Finally again by remaining 1/3Amount powder is poured alkali into and is swashed in liquid and rapid stirring reaction 1～3min; Stir 2～4min, obtain airsettingGlue crude product;
5) by step 4) aeroge crude product ageing 4～8h at the temperature of 70 DEG C of obtaining, thenUse again supercritical fluid drying, obtain this ground polymers aeroge.
Claims (6)
1. a porous ground polymers aeroge, is characterized in that, it comprises the raw material of following weight portion: 20～40 parts, NaOH, 20～40 parts, water, 120～200 parts of waterglass, 100～200 parts of kaolin, 5～10 parts of ammonium hydrogen phosphates.
2. a porous ground polymers aeroge, is characterized in that, it comprises the raw material of following weight portion: 30 parts, NaOH, 30 parts, water, 150 parts of waterglass, 160 parts of kaolin, 8 parts of ammonium hydrogen phosphates.
3. porous as claimed in claim 1 or 2 ground polymers aeroge, is characterized in that: described water is deionized water.
Porous as described in claim 1～3 the preparation method of polymers aeroge, it is characterized in that comprising the following steps:
1) metakaolin preparation, makes metakaolin by kaolin at the temperature lower calcination 4～6h of 500～900 DEG C;
2) alkali swashs the configuration of liquid, first the NaOH weighing up is poured in the waterglass weighing up, and is then adding the water weighing up, and till being stirred to rapidly solution clarification, then more than standing 1h;
3) by metakaolin, swash the mixing of liquid with alkali, first ammonium hydrogen phosphate is added in metakaolin and mixes and make powder, then the powder of making is added alkali to swash in liquid, addition manner is: first the powder of 1/3 amount is poured into alkali and swashed in liquid and rapid stirring reaction 1～3min; And then pour the powder of 1/3 amount into alkali and swash in liquid and rapid stirring reaction 1～3min; Finally more remaining 1/3 amount powder being poured into alkali swashs in liquid and rapid stirring reaction 1～3min; Stir 2～4min, obtain aeroge crude product;
4) by step 3) aeroge crude product ageing 4～8h at the temperature of 65～75 DEG C of obtaining, and then with supercritical fluid drying, obtain this ground polymers aeroge.
5. the preparation method of porous as claimed in claim 4 ground polymers aeroge, is characterized in that: the modulus that described alkali swashs liquid is 1.0～3.0.
6. the preparation method of porous as claimed in claim 4 ground polymers aeroge, is characterized in that: described ammonium hydrogen phosphate before use, grinds to form the particle that particle diameter is 100～500 μ m in super grinder, and when grinding, keeping temperature is 10～20 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510995103.0A CN105582882A (en) | 2015-12-25 | 2015-12-25 | Preparation method of porous geopolymer aerogel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510995103.0A CN105582882A (en) | 2015-12-25 | 2015-12-25 | Preparation method of porous geopolymer aerogel |
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| CN105582882A true CN105582882A (en) | 2016-05-18 |
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| CN201510995103.0A Pending CN105582882A (en) | 2015-12-25 | 2015-12-25 | Preparation method of porous geopolymer aerogel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114933448A (en) * | 2022-06-24 | 2022-08-23 | 陈鹏飞 | High-strength heat-insulating material not easy to peel and preparation method thereof |
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|---|---|---|---|---|
| CN101560071A (en) * | 2009-05-26 | 2009-10-21 | 广西大学 | Porous material of phosphate-based geopolymer and preparation method thereof |
| WO2011071687A1 (en) * | 2009-12-08 | 2011-06-16 | Dow Global Technologies Llc | Geopolymer precursor dry mixture, package, processes and methods |
| CN103864322A (en) * | 2014-01-17 | 2014-06-18 | 广西大学 | Synthetic method of geopolymer |
-
2015
- 2015-12-25 CN CN201510995103.0A patent/CN105582882A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101560071A (en) * | 2009-05-26 | 2009-10-21 | 广西大学 | Porous material of phosphate-based geopolymer and preparation method thereof |
| WO2011071687A1 (en) * | 2009-12-08 | 2011-06-16 | Dow Global Technologies Llc | Geopolymer precursor dry mixture, package, processes and methods |
| CN103864322A (en) * | 2014-01-17 | 2014-06-18 | 广西大学 | Synthetic method of geopolymer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114933448A (en) * | 2022-06-24 | 2022-08-23 | 陈鹏飞 | High-strength heat-insulating material not easy to peel and preparation method thereof |
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Application publication date: 20160518 |