CN1238285C - Process of high molecular network gel for preparing lithium aluminium silicon series micro-crystal glass superfine perdow - Google Patents
Process of high molecular network gel for preparing lithium aluminium silicon series micro-crystal glass superfine perdow Download PDFInfo
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- CN1238285C CN1238285C CN 200410013562 CN200410013562A CN1238285C CN 1238285 C CN1238285 C CN 1238285C CN 200410013562 CN200410013562 CN 200410013562 CN 200410013562 A CN200410013562 A CN 200410013562A CN 1238285 C CN1238285 C CN 1238285C
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Abstract
The present invention discloses a high molecular network gel method for preparing the microcrystalline glass superfine powder of a lithium aluminium silicon series, which relates to a synthetic method for microcrystalline glass powder. The present invention prepares microcrystalline glass powder according to the following steps: a. TEOS is dissolved in water, and PH is regulated between 2 and 3 by nitric acid; b. a lithium compound and an aluminium compound are respectively dissolved in dilute nitric acid; c. after a TEOS solution is transparent, solutions obtained in the step a and the step b are uniformly mixed; d. organic monomers and a crosslinking agent are added in a mixed solution; e. the mixed solution is heated to 70 to 100 DEG C, and then, an initiating agent is added into the mixed solution to be uniformly stirred in order to obtain a wet gel block after 5 to 30 minutes; f. the wet gel block is dried for 12 hours at 120 DEG C, or is heated for 15 to 30 minutes by high fire in a microwave oven, and a dry gel block is obtained; g. after the dry gel block is ground in a mortar, the dry gel block is placed in a calciner to be heated to 600 to 1200 DEG C, the temperature of the dry gel block is kept 1 to 2 hours, and the microcrystalline glass superfine powder of a lithium aluminium silicon series is obtained. The microcrystalline glass superfine powder of the lithium aluminium silicon series has the advantages of low cost, high synthetic speed, high purity and small particle diameters.
Description
Technical field:
The present invention relates to a kind of synthetic method of devitrified glass powder, be specifically related to a kind of synthetic method of lithium aluminium silicon series devitrified glass ultrafine powder.
Background technology:
The lithium aluminium silicon series devitrified glass has the thermal shock resistance and the higher mechanical properties of extremely low thermal expansivity, excellence, and it is with a wide range of applications at the aspects such as cavity of cooking range panel, large-scale astronomical telescope mirror base, laser tube.The lithium aluminium silica flour body granularity of traditional solid reaction process preparation is big, size distribution broad, calcining temperature height, and raw material reacts with natural accumulation mode, and efficient is lower and volatiles is scattered and disappeared.The most frequently used in the multicomponent system preparation methods is alkoxide sol-gel method and nitrate sol-gel method, and these two kinds of methods all have certain requirement to the selection of raw material.People such as Liu Zhien replace alkoxide to adopt the nitrate sol-gel method to prepare lithium aluminium silicon powder with inorganic salt, and the particle diameter of the micro mist that this method makes is bigger, and the reaction times is longer, and solution generation precipitation, cause being separated, and cause the product component inhomogeneous.The nineties middle and later periods in last century, people such as N.N Ghosh adopt the unit carboxylic acid as complexing agent metal ion-chelant to be become complex compound, make it to become soluble product, form gel through complex compound type colloidal sol process then, though this method has solved the deficiency of inorganic polymer type sol-gel method, preparation time is oversize.
Summary of the invention:
The present invention is big for the particle diameter that solves the prior art existence, the shortcoming of long reaction time, has developed a kind of polymer-network gel method of lithium aluminium silicon series devitrified glass superfine powder.The present invention is prepared as follows: a, tetraethoxy (TEOS) is soluble in water, regulate pH=2～3 with nitric acid, and stirred 30～60 minutes, make TEOS prehydrolysis; B, respectively lithium-containing compound and aluminum contained compound are dissolved in rare nitric acid, described lithium-containing compound is Lithium Oxide 98min or the inorganic salt that contain lithium, and aluminum contained compound is aluminum oxide or aluminiferous inorganic salt; C, treat that TEOS solution is transparent after, the solution that above-mentioned a step and b step are obtained is Li with the stoichiometric ratio
+: Al
3+: Si
4+=1: 1: the mixed of (1～4) is even; D, add organic monomer and linking agent in mixed solution, described organic monomer is acrylamide or Methacrylamide, and linking agent is N, N '-methylene-bisacrylamide; E, be warming up to 70～100 ℃, add initiator then, stir, solution begins gel after 5～30 minutes, obtains the wet gel piece; F, with the wet gel piece 120 ℃ dry 12 hours or in microwave oven, heat and removed moisture in 15～30 minutes down with high fire, obtain the xerogel piece; G, the xerogel piece ground in mortar after, place calcining furnace to be heated to 600～1200 ℃, be incubated 1～2 hour, obtaining grain size is the lithium aluminium silicon series devitrified glass ultrafine powder of 30～50nm.
The present invention also can be prepared as follows: a, TEOS is soluble in water, regulate pH=2～3 with nitric acid, and stirred 30～60 minutes, make TEOS prehydrolysis; B, respectively lithium-containing compound and aluminum contained compound are dissolved in rare nitric acid, described lithium-containing compound is Lithium Oxide 98min or the inorganic salt that contain lithium, and aluminum contained compound is aluminum oxide or aluminiferous inorganic salt; C, treat that TEOS solution is transparent after, the solution that above-mentioned a step and b step are obtained is Li with the stoichiometric ratio
+: Al
3+: Si
4+=1: 1: the mixed of (1～4) is even; D, add organic monomer and linking agent in mixed solution, described organic monomer is acrylamide or Methacrylamide, and linking agent is N, N '-methylene-bisacrylamide; E, be warming up to 70～100 ℃, add initiator then, stir, solution begins gel after 5～30 minutes, obtains the wet gel piece; F, directly the wet gel piece is placed calcining furnace be heated to 600～1200 ℃, be incubated 1～2 hour, obtain the xerogel piece; G, the xerogel piece ground in mortar after, obtaining grain size is the lithium aluminium silicon series devitrified glass ultrafine powder of 30～50nm.
The present invention is simple to the requirement of raw material, can avoid using expensive alkoxide, has reduced cost; This method resultant velocity is fast, has overcome the shortcoming of traditional sol-gel method long reaction time; In polymer-network gel method, the macromolecule micelle that the organic monomer polymerization forms has three-dimensional net structure, can tightly be wrapped in the raw material particle wherein, make its position keep relative fixed, improved the reaction efficiency of raw material, reduced scattering and disappearing of volatiles, reduced the generation of reuniting, can make high-purity powder, help getting rid of the interference of dephasign, it has the advantage that cost is low, resultant velocity is fast, purity is high and particle diameter is little.
Embodiment:
Embodiment one: present embodiment is prepared as follows: a, TEOS is soluble in water, regulate pH=2～3 with nitric acid, and stirred 30～60 minutes, make TEOS prehydrolysis; B, respectively lithium-containing compound and aluminum contained compound are dissolved in rare nitric acid; C, treat that TEOS solution is transparent after, the solution that above-mentioned a step and b step are obtained is Li with the stoichiometric ratio
+: Al
3+: Si
4+=1: 1: the mixed of (1～4) is even; D, in mixed solution, add organic monomer and linking agent; E, be warming up to 70～100 ℃, add initiator then, stir, solution begins gel after 5～30 minutes, obtains the wet gel piece; F, with the wet gel piece 120 ℃ dry 12 hours or in microwave oven, heat and removed moisture in 15～30 minutes down with high fire, obtain the xerogel piece; G, the xerogel piece ground in mortar after, place calcining furnace to be heated to 600～1200 ℃, be incubated 1～2 hour, obtaining grain size is the lithium aluminium silicon series devitrified glass ultrafine powder of 30～50nm.Described lithium-containing compound is Lithium Oxide 98min or the inorganic salt that contain lithium; Aluminum contained compound is aluminum oxide or aluminiferous inorganic salt; Organic monomer is acrylamide or Methacrylamide; Linking agent is N, N '-methylene-bisacrylamide or ethyleneglycol dimethacrylate; The add-on of organic monomer is 5～10% of a raw material gross weight; The weight ratio of organic monomer and linking agent is (3～30): 1; Initiator is Ammonium Persulfate 98.5, Diisopropyl azodicarboxylate or Tetramethyl Ethylene Diamine; The add-on of initiator is 0.1～0.5% of an organic monomer weight; The weight concentration of initiator is 5～20%.
Embodiment two: what present embodiment and embodiment one were different is f and g two steps, promptly directly the wet gel piece is placed calcining furnace to be heated to 600～1200 ℃, be incubated 1～2 hour, obtain the xerogel piece, after the xerogel piece ground in mortar, obtaining grain size was the lithium aluminium silicon series devitrified glass ultrafine powder of 30～50nm.Other preparation processes and processing parameter are with embodiment one.
Embodiment three: what present embodiment and embodiment one, two were different is, has also increased zirconium nitrate solution in the mixing solutions in the c step, and the add-on of zirconium nitrate solution is 0.1～4% of a reactant gross weight.Other preparation processes and processing parameter are with embodiment one, two.The adding of zirconium nitrate solution can reduce the recrystallization temperature of lithium aluminium silicon series devitrified glass, and can delay the transformation of β-quartz solid solution to β-triphane sosoloid.
Embodiment four: present embodiment is prepared as follows: a, TEOS is dissolved in the distilled water, regulates pH=2～3 with nitric acid, stirred 30～60 minutes, make TEOS prehydrolysis; B, Quilonum Retard is dissolved in the nitric acid, makes lithium nitrate solution; C, treat that TEOS solution is transparent after, with itself and Al (NO
3)
39H
2O and lithium nitrate solution are Li with the stoichiometric ratio
+: Al
3+: Si
4+=1: 1: 2 proportioning is mixed, and under induction stirring solution is mixed; D, to add weight in mixed solution be that the acrylamide and the weight of raw material gross weight 8% is the N of raw material gross weight 3%, and N '-methylene-bisacrylamide regulates pH=1～2 with nitric acid, evenly stirs; E, be warming up to 70 ℃, add weight then and be acrylamide weight 0.1～0.5%, weight concentration is 5～20% the Ammonium Persulfate 98.5 aqueous solution, solution gel after 5 minutes obtains the wet gel piece; F, the wet gel piece that obtains is put into the polytetrafluoroethylplastic plastic cup rapidly, place microwave oven, obtain xerogel with high fire heating 15 minutes; G, the xerogel piece is put into mortar grind, make dry gel powder, place calcining furnace to be heated to 600～1200 ℃ the dry gel powder that makes, be incubated 2 hours, obtaining grain size is the lithium aluminium silicon series devitrified glass ultrafine powder of 30～50nm.
Claims (8)
1, a kind of polymer-network gel method for preparing lithium aluminium silicon series devitrified glass ultrafine powder, it is characterized in that the present invention is prepared as follows: a, tetraethoxy is soluble in water, regulate pH=2～3 with nitric acid, stirred 30～60 minutes, make tetraethoxy prehydrolysis; B, respectively lithium-containing compound and aluminum contained compound are dissolved in rare nitric acid, described lithium-containing compound is Lithium Oxide 98min or the inorganic salt that contain lithium, and aluminum contained compound is aluminum oxide or aluminiferous inorganic salt; C, treat that teos solution is transparent after, the solution that above-mentioned a step and b step are obtained is Li with the stoichiometric ratio
+: Al
3+: Si
4+=1: 1: the mixed of (1～4) is even; D, add organic monomer and linking agent in mixed solution, described organic monomer is acrylamide or Methacrylamide, and linking agent is N, N '-methylene-bisacrylamide; E, be warming up to 70～100 ℃, add initiator then, stir, solution begins gel after 5～30 minutes, obtains the wet gel piece; F, with the wet gel piece 120 ℃ dry 12 hours or in microwave oven, heat and removed moisture in 15～30 minutes down with high fire, obtain the xerogel piece; G, the xerogel piece ground in mortar after, place calcining furnace to be heated to 600～1200 ℃, be incubated 1～2 hour, obtaining grain size is the lithium aluminium silicon series devitrified glass ultrafine powder of 30～50nm.
2, a kind of polymer-network gel method for preparing lithium aluminium silicon series devitrified glass ultrafine powder according to claim 1 is characterized in that the solution that a step and b step obtain preferably is Li with the stoichiometric ratio
+: Al
3+: Si
4+=1: 1: 2 mixed.
3, a kind of polymer-network gel method for preparing lithium aluminium silicon series devitrified glass ultrafine powder according to claim 1, the add-on that it is characterized in that organic monomer is 5～10% of a raw material gross weight; The weight ratio of organic monomer and linking agent is (3～30): 1.
4, a kind of polymer-network gel method for preparing lithium aluminium silicon series devitrified glass ultrafine powder according to claim 1 is characterized in that initiator is Ammonium Persulfate 98.5, Diisopropyl azodicarboxylate or Tetramethyl Ethylene Diamine.
5, a kind of polymer-network gel method for preparing lithium aluminium silicon series devitrified glass ultrafine powder according to claim 1, the add-on that it is characterized in that initiator is 0.1～0.5% of an organic monomer weight.
6, a kind of polymer-network gel method for preparing lithium aluminium silicon series devitrified glass ultrafine powder according to claim 1, the weight concentration that it is characterized in that initiator is 5～20%.
7, a kind of polymer-network gel method for preparing lithium aluminium silicon series devitrified glass ultrafine powder according to claim 1, it is characterized in that also having increased in the mixing solutions in the c step zirconium nitrate solution, the add-on of zirconium nitrate solution is 0.1～4% of a reactant gross weight.
8, a kind of polymer-network gel method for preparing lithium aluminium silicon series devitrified glass ultrafine powder, it is characterized in that the present invention is prepared as follows: a, tetraethoxy is soluble in water, regulate pH=2～3 with nitric acid, stirred 30～60 minutes, make tetraethoxy prehydrolysis; B, respectively lithium-containing compound and aluminum contained compound are dissolved in rare nitric acid, described lithium-containing compound is Lithium Oxide 98min or the inorganic salt that contain lithium, and aluminum contained compound is aluminum oxide or aluminiferous inorganic salt; C, treat that teos solution is transparent after, the solution that above-mentioned a step and b step are obtained is Li with the stoichiometric ratio
+: Al
3+: Si
4+=1: 1: the mixed of (1～4) is even; D, add organic monomer and linking agent in mixed solution, described organic monomer is acrylamide or Methacrylamide, and linking agent is N, N '-methylene-bisacrylamide; E, be warming up to 70～100 ℃, add initiator then, stir, solution begins gel after 5～30 minutes, obtains the wet gel piece; F, directly the wet gel piece is placed calcining furnace be heated to 600～1200 ℃, be incubated 1～2 hour, obtain the xerogel piece; G, the xerogel piece ground in mortar after, obtaining grain size is the lithium aluminium silicon series devitrified glass ultrafine powder of 30～50nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107986630A (en) * | 2017-11-30 | 2018-05-04 | 华南协同创新研究院 | A kind of preparation method of nano-bioactive glass powder |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219386B (en) * | 2011-05-16 | 2013-04-24 | 武汉理工大学 | Preparation method for ultrafine powder body of SiO2-based composite oxide system glass |
| CN112185642A (en) * | 2020-09-23 | 2021-01-05 | 江西艾特磁材有限公司 | Method for coating magnetic powder core with ball milling modified sol-gel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107986630A (en) * | 2017-11-30 | 2018-05-04 | 华南协同创新研究院 | A kind of preparation method of nano-bioactive glass powder |
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