CN100569645C - A kind of high length-diameter ratio antifungin whisker synthesis method - Google Patents
A kind of high length-diameter ratio antifungin whisker synthesis method Download PDFInfo
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- CN100569645C CN100569645C CNB2006100084835A CN200610008483A CN100569645C CN 100569645 C CN100569645 C CN 100569645C CN B2006100084835 A CNB2006100084835 A CN B2006100084835A CN 200610008483 A CN200610008483 A CN 200610008483A CN 100569645 C CN100569645 C CN 100569645C
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Abstract
The present invention relates to a kind of high length-diameter ratio antifungin whisker synthesis method, with boric acid, magnesium chloride, caustic soda is reaction generation magnesium borate compound precipitation in the aqueous solution by a certain percentage, filter, be preparation magnesium borate crystal whisker presoma, NaCl or NaCl are mixed with this presoma with the fusing assistant that KCl forms, adding is by methyl alcohol, ethanol, water or their mixing solutions, dipping, stir, mix, then with mixture in 500～900 ℃ of pyroreactions 5～10 hours, cooling, wash with water, drying, obtaining length is 100～150 μ m, the magnesium borate crystal whisker of length-to-diameter ratio＞100.Present method raw material is easy to get, and synthesis technique is simple, and no HCl gas is discharged, product yield 〉=95%.
Description
Technical field
The present invention relates to the magnesium borate crystal whisker synthetic method
Background technology
Magnesium borate crystal whisker is a kind of low-dimensional crystal of height-oriented property of monocrystalline form growth, have and carbon whisker, high strength that silicon carbide whisker is close, high-modulus, high abrasion and excellent erosion resistance, but its price only is their 1/20～1/30, can be widely used as the strongthener of magnalium Base Metal, rubber, plastics, ceramic and other composite material, be one of hi-tech of external at present competitively development.
The synthesis technique of magnesium borate crystal whisker mainly adopts scorification at present, soon raw material boron source boric acid, magnesium source magnesium chloride mix with water by a certain percentage with fusing assistant sodium-chlor, Repone K etc., the spray-dried powder that obtains, again after high-temperature fusion reaction, washing, dry and make.The main drawback of this method is:
1) will emit large quantity of moisture and HCl gas in the high-temperature fusion reaction, big to the corrodibility of high-temperature heater, easily cause environmental pollution, the extensive enforcement of industry difficulty is big;
2) drying process with atomizing complexity, power consumption is high, in the aqueous solution raw material is mixed with fusing assistant, and though mix, the water add-on is big, and also need heat these water evaporations that will add, and energy consumption is very big, and equipment is expensive and complicated, and processing condition are harsh;
3) the product whisker length is shorter, and length-to-diameter ratio is less, and the magnesium borate crystal whisker length that this method makes is generally 20～30 μ m, and length-to-diameter ratio is 20～40.
Summary of the invention
The present invention is directed to the shortcoming of above-mentioned magnesium borate crystal whisker preparation, provide a kind of low temperature to prepare presoma, in the presence of fusing assistant, the novel method of the synthetic high length magnesium borate crystal whisker of high-temperature fusion.The concrete technology of its synthetic is:
1) low temperature system boron magnesium presoma
Is 1: 2.6～5.0: 1.0～2.6 to prepare burden solid boric acid, 6 aqueous magnesium chlorides and sodium hydroxide by mass ratio, adds entry by solid-to-liquid ratio (quality)=1: 1～4, at 10～80 ℃ following the reaction is taken place down:
2MgCl
26H
2O+2H
3BO
3+4NaOH→Mg
2B
2O
5·nH
2O+4NaCl+mH
2O
Stir 30～50min, filter, obtain boron magnesium presoma, the size of the n in the reaction equation is relevant with temperature of reaction, n=3 in this reaction～8, and m is relevant with amount of water.
2) mix
This boron magnesium presoma and fusing assistant are mixed by one or both of boron magnesium presoma and fusing assistant sodium-chlor, Repone K, its mass ratio is a boron magnesium presoma: sodium-chlor=1: 0.4～1.5 or boron magnesium presoma: sodium-chlor: the ratio of Repone K=1: 0.2～0.5: 0.1～0.5 is prepared burden, adding is by the solution of a kind of, two kinds or the three kinds solvent compositions of methyl alcohol, ethanol, water, the solid-liquid mass ratio is 1: 0.5～3.0, dipping, stirring, make boron magnesium presoma and fusing assistant uniform mixing, filter the sintered material that obtains mixing;
3) high-temperature fusion reaction:
Above-mentioned sintered material is placed container, put into High Temperature Furnaces Heating Apparatus and be incubated 5～10h down, obtain thick magnesium borate crystal whisker product at 500 ℃～900 ℃;
4) washing is dry
Above-mentioned thick magnesium borate crystal whisker product is soaked in water, washs, dry under 80 ℃～100 ℃ after the filtration, promptly obtain the magnesium borate crystal whisker product.
The present invention compares with existing magnesium borate crystal whisker synthetic technology, has the following advantages:
1) product quality better
The magnesium borate crystal whisker length that the present invention synthesizes can reach 150～200 μ m, diameter 1.0～2.0, and length-to-diameter ratio reaches more than 100, product yield can reach 95%, and the magnesium borate crystal whisker length that prior art synthesizes is generally 20～30 μ m, and length-to-diameter ratio is 20～40, and product yield can be only 90%;
2) no HCl gaseous emission has significantly reduced the corrosion to High Temperature Furnaces Heating Apparatus, has avoided gas contamination
Existing preparation technology magnesium chloride in pyroprocess can decomposes produce a large amount of HCl gases and moisture content discharging inevitably, not only stronger corrosion to the material production of High Temperature Furnaces Heating Apparatus, reduce the work-ing life of High Temperature Furnaces Heating Apparatus greatly, also will cause polluting than serious environmental.The present invention makes raw material MgCl owing to adopt the presoma synthetic technology in the aqueous solution
2In Cl
-Be converted into NaCl, and NaCl is very stable under this temperature of reaction, no HCl produces in the high temperature building-up reactions.So the present invention is a green synthesis techniques.
3) technology is simple, and energy consumption is low, and production cost is low
Because in water at normal temperature solution, form the reactant presoma, reduced the spraying drying operation in the existing synthesis technique, and owing to adopt the organic solvent dipping to mix, start material is mixed, the mass transfer process of the high-temperature fusion reaction that is highly advantageous to follow-up, and the pyroreaction temperature is carried out under 500 ℃～900 ℃, reduce by 100 ℃ than existing method, energy consumption reduces greatly, and production cost is low;
Description of drawings
Fig. 1 is the Photomicrograph of embodiment 1,
Fig. 2 is the Photomicrograph of embodiment 2,
Fig. 3 is the Photomicrograph of embodiment 3,
Embodiment
Embodiment 1
With the industrial one-level MgCl of 233.3 grams
26H
2O and the industrial one-level boric acid of 65 grams are incorporated in the H of 1560ml
2Among the O, add 92 gram NaOH again, stirred 50 minutes down in 40 ℃, still aging 2 hours, filter, obtain magnesium borate crystal whisker presoma 160 grams, with this presoma and 32 industrial one-level NaCl of gram and the industrial one-level KCl solid phase mixing of 80 grams, add entry again, solid-to-liquid ratio (mass ratio) is 1: 0.5, stir under the normal temperature, filter, filtering mixing initiator thing is placed crucible, put into High Temperature Furnaces Heating Apparatus 850 ℃ of pyroreactions 5 hours, take out the cooling back, with 200 gram water logging bubbles, washing is filtered, in 80 ℃ of loft drier dry 10 hours again, obtain the magnesium borate crystal whisker product.Its analytical results sees Table 1, Fig. 1.
Embodiment 2
With the industrial one-level MgCl of 169 grams
26H
2O and the industrial one-level boric acid of 65 grams are incorporated in the H of 400ml
2Among the O, add 169 gram NaOH again, stirred 30 minutes down in 40 ℃, still aging 1 hour, filter, obtain magnesium borate crystal whisker presoma 144 grams, with this presoma and the industrial one-level NaCl solid phase mixing of 120 grams, add again by methyl alcohol, ethanol, the organic solvent that water is formed, its proportioning is a methyl alcohol: ethanol: water=4: 3: 3 (mass ratio), to mix, and solid-to-liquid ratio (mass ratio) is 1: 3, stir under the normal temperature, filter, filtering mixing initiator is placed crucible, put into High Temperature Furnaces Heating Apparatus 900 ℃ of pyroreactions 10 hours, cooling, with 200g water logging bubble, washing is filtered, in 100 ℃ of following loft drier dry 3 hours again, obtain the magnesium borate crystal whisker product.Its analytical results sees Table 1, Fig. 2.
Embodiment 3
With the industrial one-level MgCl of 325 grams
26H
2O and the industrial one-level boric acid of 65 grams are incorporated in the H of 500ml
2Among the O, add 65 gram NaOH again, stirred 30 minutes down in 40 ℃, still aging 1 hour, filter, obtain magnesium borate crystal whisker presoma 130 grams, with this presoma and 65 industrial one-level NaCl of gram and the industrial one-level KCl solid phase mixing of 13 grams, add again by methyl alcohol, ethanol, the organic solvent that water is formed, its proportioning is a methyl alcohol: ethanol water=4: 3 (mass ratio), to mix, and solid-to-liquid ratio (mass ratio) is 1: 0.5, stir under the normal temperature, filter, filtering mixing initiator is placed crucible, put into High Temperature Furnaces Heating Apparatus 500 ℃ of pyroreactions 10 hours, cooling, with 200g water logging bubble, washing is filtered, in 100 ℃ of following loft drier dry 3 hours again, obtain the magnesium borate crystal whisker product.Its analytical results sees Table 1, Fig. 2.
Table 1 embodiment result
| Embodiment | Whisker length μ m | Length-to-diameter ratio | Whisker productive rate % | Whisker purity % |
| Embodiment 1 | 20～30 | 20～40 | 85 | 99.1 |
| Embodiment 2 | 70～200 | ≥100 | 95 | 99.0 |
| Embodiment 3 | 70～150 | 50～100 | 94 | 99.3 |
Claims (1)
1, a kind of high length-diameter ratio antifungin whisker synthesis method, the length-to-diameter ratio that it is characterized in that whisker reaches more than 100, the concrete technology of synthetic is: a low temperature system boron magnesium presoma, b mixes, the reaction of c high-temperature fusion, dry four technological processs of d washing are formed, wherein, the processing condition of low temperature system boron magnesium presoma process are for being 1: 2.6～5.0: 1.0～2.6 to prepare burden solid boric acid, magnesium chloride hexahydrate and sodium hydroxide by mass ratio, add entry by solid-to-liquid ratio (quality)=1: 1～4, react below the generation down at 10～80 ℃:
2MgCl
2+2H
3BO
3+4NaOH→Mg
2B
2O
5·n H
2O+4NaCl+m H
2O
Stirred 30～50 minutes, still aging 1～3 hour, filter, obtain boron magnesium presoma; The processing condition of mixing process are that one or both of boron magnesium presoma and fusing assistant sodium-chlor, Repone K are mixed, its mass ratio is a boron magnesium presoma: sodium-chlor=1: 0.4～1.5, or boron magnesium presoma: sodium-chlor: the ratio batching of Repone K=1: 0.2～0.5: 0.1～0.5, composition mixture, adding is by the solution of a kind of, two kinds or the three kinds solvent compositions of methyl alcohol, ethanol, water, its solid-liquid mass ratio is 1: 0.5～3.0, dipping, stirring, make boron magnesium presoma and fusing assistant uniform mixing, filter the sintered material that obtains mixing; The processing condition of high-temperature fusion reaction are put into High Temperature Furnaces Heating Apparatus and are incubated 5～10h down at 500 ℃～900 ℃ for above-mentioned sintered material is placed container, obtain thick magnesium borate crystal whisker product; The processing condition of washing drying process are for to be soaked in water above-mentioned thick magnesium borate crystal whisker product, wash, and are dry under 80 ℃～100 ℃ after the filtration, promptly obtain the magnesium borate crystal whisker product.
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100375795C (en) * | 2006-09-08 | 2008-03-19 | 清华大学 | Magnesium borate whisker hydrothermal synthesis preparation method |
| CN101311372B (en) * | 2008-03-24 | 2010-09-01 | 清华大学 | Low-temperature molten salt thermal inversion preparation method of aporate-crystal antifungin whiskers |
| CN101928986B (en) * | 2010-04-30 | 2012-07-04 | 中国科学院青海盐湖研究所 | Process for preparing magnesium borate whiskers with high aspect ratio by utilizing carnallite |
| CN102206860B (en) * | 2011-05-23 | 2013-07-10 | 华东理工大学 | Method for preparing magnesium borate whisker with high length-to-diameter ratio by pelletization |
| CN103132146B (en) * | 2012-10-29 | 2015-11-18 | 厦门三荣陶瓷开发有限公司 | A kind of preparation method of magnesium borate crystal whisker |
| CN103626510B (en) * | 2013-11-29 | 2014-12-17 | 成都理工大学 | Method for preparing magnesium borate whisker porous ceramic by employing in-situ growth |
| CN104562210A (en) * | 2015-01-14 | 2015-04-29 | 黄冈师范学院 | Preparation method of magnesium borate whisker with controllable size and morphology |
| CN105568378B (en) * | 2016-01-07 | 2017-10-17 | 西南科技大学 | A kind of preparation method for possessing multi-functional and compound with regular structure lead borate whisker |
| CN109265640A (en) * | 2018-08-16 | 2019-01-25 | 德清舒华泡沫座椅有限公司 | A kind of high-damping high-strength polyurethane foam |
| CN109161209A (en) * | 2018-08-16 | 2019-01-08 | 德清舒华泡沫座椅有限公司 | A kind of preparation method of high-damping antidetonation silicon foams |
| CN109021201A (en) * | 2018-08-16 | 2018-12-18 | 德清舒华泡沫座椅有限公司 | A kind of preparation method of high-damping high-strength polyurethane foam |
| CN108912694A (en) * | 2018-08-16 | 2018-11-30 | 德清舒华泡沫座椅有限公司 | A kind of high-damping antidetonation silicon foams |
| CN112897991A (en) * | 2021-03-12 | 2021-06-04 | 武汉科技大学 | Magnesium borate whisker porous ceramic material based on molten salt growth method and preparation method thereof |
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| CN1552958A (en) * | 2003-05-30 | 2004-12-08 | 青海海兴科技开发有限公司 | Preparing process for antifungin crystal whisker |
| CN1556259A (en) * | 2003-12-31 | 2004-12-22 | 国家海洋局天津海水淡化与综合利用研 | Preparation method of magnesium borate whisker |
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| CN1552958A (en) * | 2003-05-30 | 2004-12-08 | 青海海兴科技开发有限公司 | Preparing process for antifungin crystal whisker |
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