CN107201542A - A kind of preparation method of alkali magnesium sulfate crystal whisker - Google Patents
A kind of preparation method of alkali magnesium sulfate crystal whisker Download PDFInfo
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- CN107201542A CN107201542A CN201710426865.8A CN201710426865A CN107201542A CN 107201542 A CN107201542 A CN 107201542A CN 201710426865 A CN201710426865 A CN 201710426865A CN 107201542 A CN107201542 A CN 107201542A
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- Prior art keywords
- magnesium sulfate
- preparation
- crystal whisker
- sulfate crystal
- alkali
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of preparation method of alkali magnesium sulfate crystal whisker, the preparation method comprises the following steps：1) crystalline sulfuric acid magnesium is configured to Adlerika, stirring adds light magnesium oxide and auxiliary agent, obtains slurry；2) by step 1) obtained slurry moved into hydrothermal reaction kettle, adds crystal seed, the addition of crystal seed is the 0.1%~10% of light magnesium oxide quality, stirs, is reacted 1~12 hour at 100 DEG C~150 DEG C；3) cooled down after reaction terminates, obtained suspension obtains alkali magnesium sulfate crystal whisker after filtering, drying.The present invention with the addition of crystal seed in reaction slurry, and alkali magnesium sulfate is easy to nucleating growth, therefore can reduce temperature and the reaction time of Hydrothermal Synthesiss, and greatly reduces energy consumption.
Description
Technical field
The invention belongs to technical field of preparation for inorganic material, in particular it relates to a kind of alkali magnesium sulfate crystal whisker
Preparation method.
Background technology
Its chemical formula of alkali magnesium sulfate crystal whisker is (5Mg (OH)2·MgSO4·3H2O or 5Mg (OH)2·MgSO4·2H2O),
It is a kind of performance more excellent inorganic reinforcement, can the product such as excellent reinforced plastics, rubber, and with excellent resistance extensively
Fire performance.The method of synthesis alkali magnesium sulfate crystal whisker is main using sodium hydroxide (or ammoniacal liquor) and magnesium sulfate as raw material at present, passes through
Hydrothermal Synthesiss.But because preparation process is complicated, and the temperature range of hydro-thermal is narrow, and required time is long, therefore hardly results in high major diameter
The alkali magnesium sulfate crystal whisker of ratio.As Lu can just exist《Study in salt lake》Magnesium sulfate and hydrogen-oxygen are used in (the 3rd phase of volume 19 in 2011)
Change sodium is raw material, and adds EDTA improvement whisker morphologies, and discovery, which can form only reasonable control temperature, can just obtain single
Fibrous whisker.There is substantial amounts of oxidation magnesium resource in China, and the magnesium system of high added value how is directly prepared by raw material of magnesia
Product have great importance.But when using the magnesia to prepare magnesium sulfate crystal whisker for raw material, due to by raw material particle size, crystallization degree
Influence, so being difficult to ensure that the magnesium sulfate crystal whisker uniformity of synthesis.Therefore, if magnesia can be used for raw material, using compared with
Low energy consumption prepares the whisker of high length-diameter ratio, significant for its popularization and application.
The content of the invention
It is an object of the present invention to provide a kind of preparation method of alkali magnesium sulfate crystal whisker.This method is in reaction slurry
Crystal seed is with the addition of, alkali magnesium sulfate is easy to nucleating growth, therefore can reduce temperature and the reaction time of Hydrothermal Synthesiss, and significantly
Reduce energy consumption.
To reach above-mentioned purpose, present invention employs following technical scheme：
A kind of preparation method of alkali magnesium sulfate crystal whisker, the preparation method comprises the following steps：
1) crystalline sulfuric acid magnesium is configured to Adlerika, stirring adds light magnesium oxide and auxiliary agent, obtains slurry；
2) by step 1) obtained slurry moved into hydrothermal reaction kettle, adds crystal seed, the addition of crystal seed is lightweight oxidation
The 0.1%~10% of magnesia amount, stirs, and is reacted 1~12 hour at 100 DEG C~150 DEG C；
3) cooled down after reaction terminates, obtained suspension obtains alkali magnesium sulfate crystal whisker after filtering, drying.
Preferably, the crystalline sulfuric acid magnesium is epsom salt or magnesium sulfate monohydrate.
Preferably, the step 1) MgSO in the Adlerika4Mass fraction be 10%~25%.
Preferably, the auxiliary agent is one or more mixtures in tartaric acid, citric acid or citric acid trisodium.
Preferably, the mass ratio of the light magnesium oxide and auxiliary agent is 4~10：0.1~2.
Preferably, the step 2) in crystal seed be made by the following method：
The Adlerika for being 10%~25% by light magnesium oxide, mass fraction and tartaric acid are 100 according to mass ratio:
240~480:0.1~5 hybrid reaction is ground obtained by 80 DEG C~150 DEG C drying after 1~7 day.
Compared with prior art, the advantage of the invention is that：
1) by adding crystal seed, help to reduce the potential barrier to form alkali magnesium sulfate crystal whisker formation, therefore production can be improved
Required energy consumption in rate or water-heat process.
2) by adding auxiliary agent, help to control the hydration rate of magnesia in water-heat process, the hydroxyl for producing it
Concentration be unlikely to excessive, reduce its degree of supersaturation, and enable the hydroxyl of generation to be almost fully able to added
Seed surface carries out growth in situ, so as to be readily obtained the alkali magnesium sulfate crystal whisker of high length-diameter ratio.
3) can be to improve the avtive spot of growth during Hydrothermal Synthesiss due to the crystal seed of use.Prepared by therefore
The pattern of alkali magnesium sulfate crystal whisker, will not be influenceed by the particle diameter or crystallization degree of raw materials of magnesium oxide, and the mainly crystalline substance with addition
The amount planted is relevant with initial pattern.
Brief description of the drawings
Fig. 1 is the flow chart of preparation method of the present invention.
Fig. 2 is the XRD diffraction patterns of the gained crystal seed of embodiment 1.
Fig. 3 is the electron microscope of the gained whisker of embodiment 1.
Fig. 4 is the electron microscope of whisker obtained by comparative example.
Embodiment
With the drawings and specific embodiments, the present invention is further detailed explanation below.
Embodiment 1：
As shown in figure 1, a kind of preparation method of alkali magnesium sulfate crystal whisker, the synthetic method of the crystal seed used is by 100g
Light magnesium oxide is mixed with the 25% of 240g Adlerika and 0.1g tartaric acid, after sclerous reaction 7 days, is ground to
200 mesh, are dried at 150 DEG C.The XRD diffracting spectrums of resulting crystal seed are shown in Fig. 2, and analysis understands that main product is alkali formula
Magnesium sulfate crystals (5Mg (OH)2·MgSO4·3H2O)；And there is figure to understand that its each diffraction maximum is wider, illustrate that crystallization degree is low, defect
Content is high, therefore helps to play crystal seed effect in Hydrothermal Synthesiss alkali magnesium sulfate crystal whisker.
100g epsom salts dissolution of crystals is formed in 95g water 25% Adlerika, and it is anti-to be transferred to hydro-thermal
Answer in kettle.0.1g tartaric acid (auxiliary agent), 0.1g crystal seeds, 4g light magnesium oxides are added in Adlerika, after being well mixed
Obtain slurry.Slurry reacts 1h at 150 DEG C.After reaction terminates and cooled down, length is obtained for 30~50 μm through filtration washing, it is long
Spend for 0.5~1 μm, draw ratio is 60~100 (such as Fig. 3) alkali magnesium sulfate crystal whisker.
Embodiment 2：
The synthetic method of the crystal seed used for by 10% Adlerika of 100g light magnesium oxides and 480g and
5g tartaric acid mixing, after sclerous reaction 7 days, is ground to 200 mesh, is dried at 80 DEG C, obtain crystal seed.
100g magnesium sulfate monohydrates dissolution of crystals is formed in 95g water 10% Adlerika, and it is anti-to be transferred to hydro-thermal
Answer in kettle.2g citric acids (auxiliary agent), 0.05g crystal seeds, 5g light magnesium oxides are added in Adlerika, after being well mixed
To slurry.Slurry reacts 1h at 150 DEG C.After reaction terminates and cooled down, it is 20~30 μm, length to obtain length through filtration washing
For 0.2~0.5 μm, draw ratio is 60~100 alkali magnesium sulfate crystal whisker.
Embodiment 3：
The synthetic method of the crystal seed used for by 15% Adlerika of 100g light magnesium oxides and 300g and
3g tartaric acid mixing, after sclerous reaction 5 days, is ground to 200 mesh, is dried at 100 DEG C, obtain crystal seed.
100g epsom salts dissolution of crystals is formed in 388g water 10% Adlerika, and it is anti-to be transferred to hydro-thermal
Answer in kettle.2g auxiliary agents (1g tartaric acid and 1g citric acids), 1g crystal seeds, 10g light magnesium oxides are added in Adlerika, mixed
Slurry is obtained after closing uniformly.Slurry reacts 3h at 120 DEG C.After reaction terminates and cooled down, it is 20 to obtain length through filtration washing
~40 μm, length is 0.3~0.5 μm, and draw ratio is 50~100 alkali magnesium sulfate crystal whisker.
Embodiment 4：
The preparation method of crystal seed is with example 2.
100g epsom salts dissolution of crystals is formed in 200g water 16% Adlerika, and it is anti-to be transferred to hydro-thermal
Answer in kettle.By 1g auxiliary agents (0.5g tartaric acid, 0.2g trisodium citrates and 0.3g citric acids), 0.7g crystal seeds, 8g light magnesium oxides
It is added in Adlerika, slurry is obtained after being well mixed.Slurry reacts 3h at 120 DEG C.After reaction terminates and cooled down, warp
It is 20~40 μm that filtration washing, which obtains length, and length is 0.3~0.5 μm, and draw ratio is 40~100 alkali magnesium sulfate crystal whisker.
Comparative example：
100g epsom salts dissolution of crystals is formed in 95g water 25% Adlerika, and it is anti-to be transferred to hydro-thermal
Answer in kettle.Slurry reacts 1h at 150 DEG C.After reaction terminates and cooled down, through product obtained by filtration washing in electric Microscopic observation
Such as Fig. 4, its length is shorter less than 10 μm, and draw ratio is less than 10.
It should be noted last that, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted.Although ginseng
The present invention is described in detail according to embodiment, it will be apparent to an ordinarily skilled person in the art that to the technical side of the present invention
Case is modified or equivalent substitution, and without departure from the spirit and scope of technical solution of the present invention, it all should cover in the present invention
Right among.
Claims (6)
1. a kind of preparation method of alkali magnesium sulfate crystal whisker, the preparation method comprises the following steps：
1) crystalline sulfuric acid magnesium is configured to Adlerika, stirring adds light magnesium oxide and auxiliary agent, obtains slurry；
2) by step 1) obtained slurry moved into hydrothermal reaction kettle, adds crystal seed, the addition of crystal seed is light magnesium oxide matter
The 0.1%~10% of amount, stirs, and is reacted 1~12 hour at 100 DEG C~150 DEG C；
3) cooled down after reaction terminates, obtained suspension obtains alkali magnesium sulfate crystal whisker after filtering, drying.
2. the preparation method of alkali magnesium sulfate crystal whisker according to claim 1, it is characterised in that the crystalline sulfuric acid magnesium is seven
Water magnesium sulfate or magnesium sulfate monohydrate.
3. the preparation method of alkali magnesium sulfate crystal whisker according to claim 1, it is characterised in that the step 1) sulfuric acid
MgSO in magnesium solution4Mass fraction be 10%~25%.
4. the preparation method of alkali magnesium sulfate crystal whisker according to claim 1, it is characterised in that the auxiliary agent be tartaric acid,
One or more in citric acid, trisodium citrate.
5. the preparation method of alkali magnesium sulfate crystal whisker according to claim 1, it is characterised in that the light magnesium oxide with
The mass ratio of auxiliary agent is 4~10：0.1~2.
6. the preparation method of alkali magnesium sulfate crystal whisker according to claim 1, it is characterised in that the step 2) in crystalline substance
Plant and be made by the following method：
The Adlerika for being 10%~25% by light magnesium oxide, mass fraction and tartaric acid are 100 according to mass ratio:240
~480:0.1~5 hybrid reaction is ground obtained by 80 DEG C~150 DEG C drying after 1~7 day.
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| CN201710426865.8A CN107201542A (en) | 2017-06-08 | 2017-06-08 | A kind of preparation method of alkali magnesium sulfate crystal whisker |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115595666A (en) * | 2022-09-09 | 2023-01-13 | 中国科学院青海盐湖研究所（Cn） | Monodisperse 517 type basic magnesium sulfate whisker and preparation method thereof |
| CN117166062A (en) * | 2023-08-23 | 2023-12-05 | 山东蓝海晶体科技有限公司 | Preparation method of magnesium sulfate whisker |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0474709A (en) * | 1990-07-09 | 1992-03-10 | Nippon Chem Ind Co Ltd | Fibrous basic magnesium sulfate and production thereof |
| CN1288860A (en) * | 1999-09-22 | 2001-03-28 | 中国科学院金属研究所 | Preparation of magnesium salt whisker |
| CN1482287A (en) * | 2003-04-15 | 2004-03-17 | 清华大学 | New method of rapid synthesis of basic bitter salt |
| CN101348937A (en) * | 2008-09-05 | 2009-01-21 | 清华大学 | Preparation of high length-diameter ratio magnesium hydroxide sulfate hydrate whisker |
| CN103789819A (en) * | 2014-02-19 | 2014-05-14 | 中国科学院青海盐湖研究所 | Preparation method of fibrous alkali magnesium sulfate whisker |
| CN104073870A (en) * | 2014-06-20 | 2014-10-01 | 沈阳理工大学 | Method for preparing submicron basic magnesium sulfate whisker with magnesite and prepared products |
| CN104988576A (en) * | 2015-07-14 | 2015-10-21 | 中国科学院青海盐湖研究所 | Preparation method of basic magnesium sulfate whiskers |
-
2017
- 2017-06-08 CN CN201710426865.8A patent/CN107201542A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0474709A (en) * | 1990-07-09 | 1992-03-10 | Nippon Chem Ind Co Ltd | Fibrous basic magnesium sulfate and production thereof |
| CN1288860A (en) * | 1999-09-22 | 2001-03-28 | 中国科学院金属研究所 | Preparation of magnesium salt whisker |
| CN1482287A (en) * | 2003-04-15 | 2004-03-17 | 清华大学 | New method of rapid synthesis of basic bitter salt |
| CN101348937A (en) * | 2008-09-05 | 2009-01-21 | 清华大学 | Preparation of high length-diameter ratio magnesium hydroxide sulfate hydrate whisker |
| CN103789819A (en) * | 2014-02-19 | 2014-05-14 | 中国科学院青海盐湖研究所 | Preparation method of fibrous alkali magnesium sulfate whisker |
| CN104073870A (en) * | 2014-06-20 | 2014-10-01 | 沈阳理工大学 | Method for preparing submicron basic magnesium sulfate whisker with magnesite and prepared products |
| CN104988576A (en) * | 2015-07-14 | 2015-10-21 | 中国科学院青海盐湖研究所 | Preparation method of basic magnesium sulfate whiskers |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115595666A (en) * | 2022-09-09 | 2023-01-13 | 中国科学院青海盐湖研究所（Cn） | Monodisperse 517 type basic magnesium sulfate whisker and preparation method thereof |
| CN117166062A (en) * | 2023-08-23 | 2023-12-05 | 山东蓝海晶体科技有限公司 | Preparation method of magnesium sulfate whisker |
| CN117166062B (en) * | 2023-08-23 | 2024-02-06 | 山东蓝海晶体科技有限公司 | Preparation method of magnesium sulfate whisker |
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Application publication date: 20170926 |