CN106276933A - A kind of method preparing threadiness lithium magnesium silicate powder body - Google Patents

A kind of method preparing threadiness lithium magnesium silicate powder body Download PDF

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Publication number
CN106276933A
CN106276933A CN201610583972.7A CN201610583972A CN106276933A CN 106276933 A CN106276933 A CN 106276933A CN 201610583972 A CN201610583972 A CN 201610583972A CN 106276933 A CN106276933 A CN 106276933A
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lithium
magnesium silicate
powder body
silicate powder
source
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CN106276933B (en
Inventor
海春喜
周园
任秀峰
曾金波
李松
孙艳霞
申月
董欧阳
李翔
张丽娟
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Qinghai Institute of Salt Lakes Research of CAS
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Qinghai Institute of Salt Lakes Research of CAS
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/26Aluminium-containing silicates, i.e. silico-aluminates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The invention discloses a kind of method preparing threadiness lithium magnesium silicate powder body, said method comprising the steps of: 1) 1~5.4g magnesium source is dissolved in deionized water, it is added dropwise over aqueous slkali and generates Mg (OH)2White depositions, stirs under room temperature, filters, washs, collects;2) under agitation 0.03 0.18g lithium source is dissolved in the water, is formed containing lithium ion aqueous solution;3) by step 1) Mg (OH) for preparing2White depositions is added to step 2) prepare containing in lithium ion aqueous solution, add water and be modulated into reaction paste, the solids content in slurry is 2 4wt%;4) after being 11 13 with aqueous slkali regulation pH, continuously stirred 2 4h;5), after putting into 2.16 11.7g solid silicon source in a kettle., the reaction paste stirred, 160 200 DEG C of reaction 4h 360h are poured into;6) products therefrom by centrifugation, washing to after neutrality, add washing with alcohol, then filter, be dried, collect and i.e. obtain fibrous lithium magnesium silicate powder body.The method is simple, and repeatability is high.

Description

A kind of method preparing threadiness lithium magnesium silicate powder body
Technical field
The invention belongs to the preparing technical field of lithium magnesium silicate, in particular it relates to one prepares threadiness silicic acid The method of magnesium powder for lithium.
Background technology
Due to reasons such as the mineralising cycle are longer, mineralising condition harsh, purity is relatively low, although In Natural Silicate magnesium powder for lithium has very Many excellent performances, but its application in different field is subject to many limitations.And the lithium magnesium silicate powder body manually prepared by In can effectively control composition and reaction condition, therefore can successfully solve this puzzlement.So far, except microwave reaction method it Outward, hydro-thermal method, due to reasons such as productivity is high, little, the morphology controllable of diameter of particle of preparation, is to prepare lithium magnesium silicate and other stratiforms One of most common method of silicate mineral.Showing through numerous studies, reaction temperature, response time and pH value are to affect hydro-thermal Method prepares the important parameter of lithium magnesium silicate.It addition, abroad also there are some researches show, different raw materials to the structure of lithium magnesium silicate and Performance also has a significant impact.According to the relevant document preparing lithium magnesium silicate powder body with waterglass for silicon source, waterglass is in reaction system In gradually decompose release silicon dioxide for synthetically prepared the having very important significance of nano-scale lithium magnesium silicate powder body.This It is mainly due to effectively control reaction system nucleation in course of reaction-growth balance.Therefore, raw-material selection for The preparation of lithium magnesium silicate powder body has very important significance.
In the most commonly used hydro-thermal method prepares the method for lithium magnesium silicate powder body, mostly with lithium salts, sodium silicate/silicic acid Potassium, magnesium chloride/magnesium sulfate etc. are prepared for raw material.Verify according to relevant report, use hydro-thermal method to prepare the mistake of lithium magnesium silicate powder body Cheng Zhong, beyond reaction condition, the selection of reaction raw materials is also that success prepares the important decisive of lithium magnesium silicate powder body Factor.It addition, in the hydro-thermal method reported at present prepares the report of lithium magnesium silicate powder body, except reaction cost is high, preparation method Outside complicated, productivity is low, the lowest to the controllability of its pattern.The most prepared lithium magnesium silicate powder body is two-dimensional nano sheet Shape, has not seen the report being related to threadiness lithium magnesium silicate powder body.
Summary of the invention
It is an object of the invention to, it is provided that a kind of method preparing threadiness lithium magnesium silicate powder body, the method is to powder body Nucleation-growth balance has carried out effective control, thus can successfully prepare threadiness lithium magnesium silicate powder body.The method is simple, weight Renaturation is high, and obtained lithium magnesium silicate powder body is shaped as threadiness and specific surface area is higher.
For reaching above-mentioned purpose, present invention employs following technical scheme:
A kind of method preparing threadiness lithium magnesium silicate powder body, said method comprising the steps of:
1) 1~5.4g magnesium source is dissolved in appropriate deionized water, is added dropwise over aqueous slkali and generates Mg (OH)2White is heavy Shallow lake thing, stirs under room temperature, filters, washs, collects;
2) under agitation 0.03-0.18g lithium source is dissolved in suitable quantity of water, is formed containing lithium ion aqueous solution;
3) by step 1) Mg (OH) for preparing2White depositions is added to step 2) prepare containing in lithium ion aqueous solution, add Water is modulated into reaction paste, and the solids content in slurry is 2-4wt%;
4) after being 11-13 with aqueous slkali regulation pH, continuously stirred 2-4h;
5), after putting into 2.16-11.7g solid silicon source in a kettle., the reaction paste stirred is poured into, 160-200 DEG C Reaction 4h-360h;
6) products therefrom by centrifugation, washing to after neutrality, add washing with alcohol, then filter, be dried, collect and i.e. obtain fiber Shape lithium magnesium silicate powder body.
Preferably, described magnesium source is selected from MgCl2·6H2O、MgSO4And MgCO3In one.Preferably, described step 1) In aqueous slkali be ammonia, NaOH solution or KOH solution.
Preferably, described lithium source is selected from LiF, LiOH, Li2CO3With containing the one in lithium salt.
Preferably, described solid silicon source one in sheet glass, glass tubing, quartz ampoule and piezoid.
The present invention uses glass etc. for raw material to prepare bar-shaped magnesium silicate powder for lithium, and the lithium magnesium silicate powder body of preparation is not only Purity is higher, degree of crystallinity is high, productivity is high, also achieves the effective control to its pattern and degree of crystallinity.And it is set in this invention The method of meter is simple, and repeatability is high, is one of effective ways preparing threadiness lithium magnesium silicate nano-powder.
Accompanying drawing explanation
Fig. 1 is the XRD diffraction pattern of embodiment 1 products therefrom;
Fig. 2 is the TEM figure of embodiment 1 products therefrom;
Fig. 3 is the XRD diffraction pattern of embodiment 2 products therefrom;
Fig. 4 is the XRD diffraction pattern of embodiment 3 products therefrom.
Detailed description of the invention
With the drawings and specific embodiments, the present invention is further detailed explanation below.
Embodiment 1
1. by 5.4g MgCl2·6H2O is dissolved in deionized water, is added dropwise over 2ml 9mol/L NH3·H2O generates Mg (OH)2White depositions, after stirring 1h, filters, washs, collects under room temperature;
The most under agitation 0.18g LiF is dissolved in 20ml water, forms LiF aqueous solution;
3. by the white Mg (OH) of preparation in 12Precipitation is added in step 2 in the LiF aqueous solution of preparation, adds water and is modulated into 150ml reaction paste, the solid content in slurry is 3wt%;
4. after being 12 with NaOH solution regulation pH, continuously stirred 3h;
After putting into the sheet glass that 11.6933g cleans the most in a kettle., pour the reaction paste stirred into, install anti- Answer 180 DEG C of reaction 120h after still;
6. products therefrom by centrifugation, washing to after neutrality, add washing with alcohol, then filter, be dried, collect and i.e. obtain fiber Shape lithium magnesium silicate powder body.
Gained lithium magnesium silicate powder body carries out XRD and transmission electron microanalysis, and result is the most as depicted in figs. 1 and 2.From Fig. 1 is it can be seen that the present invention is successfully prepared lithium magnesium silicate powder body, and has one (001) the strongest about 2 θ=6.8 ° Peak occurs, shows that this kind of lithium magnesium silicate powder body has layer structure, and the growth that has superiority along 001 direction.Can from Fig. 2 Going out, it is bar-shaped for using this lithium magnesium silicate powder body prepared, and lithium magnesium silicate rod length, footpath be respectively micron and nanoscale.
Embodiment 2
1. by 1g MgSO4It is dissolved in deionized water, is added dropwise over 2ml 9mol/L KOH and generates Mg (OH)2White precipitate Thing, after stirring 1h, filters, washs, collects under room temperature;
The most under agitation 0.03g LiOH is dissolved in 20ml water, forms LiOH aqueous solution;
3. by the white Mg (OH) of preparation in 12Precipitation is added in step 2 in the LiOH aqueous solution of preparation, adds water and is modulated into 150ml reaction paste, the solid content in slurry is 2wt%;
4. after being 11 with KOH solution regulation pH, continuously stirred 4h;
After putting into the glass tubing that 2.16g cleans the most in a kettle., pour the reaction paste stirred into, install reactor Later 200 DEG C of reaction 4h;
6. products therefrom by centrifugation, washing to after neutrality, add washing with alcohol, then filter, be dried, collect.
Gained lithium magnesium silicate powder body is carried out XRD, and result is as shown in Figure 3.From figure 3, it can be seen that the present invention is successfully prepared Lithium magnesium silicate powder body, and have (001) peak the strongest to occur about 2 θ=6.8 °, show this kind of lithium magnesium silicate powder body There are layer structure, and the growth that has superiority along 001 direction.
Embodiment 3
1. by 5.4g MgCO3It is dissolved in deionized water, is added dropwise over 2ml 9mol/L NH3·H2O generates Mg (OH)2 White depositions, after stirring 1h, filters, washs, collects under room temperature;
The most under agitation by 0.18g LiCO3It is dissolved in 20ml water, forms Li CO3Aqueous solution;
3. by the white Mg (OH) of preparation in 12Precipitation is added in step 2 LiCO of preparation3In aqueous solution, add water and be modulated into 150ml reaction paste, the solid content in slurry is 4wt%;
4. after being 13 with NaOH solution regulation pH, continuously stirred 2h;
After putting into the sheet glass that 11.6933g cleans the most in a kettle., pour the reaction paste stirred into, install anti- Answer 160 DEG C of reaction 360h after still;
6. products therefrom by centrifugation, washing to after neutrality, add washing with alcohol, then filter, be dried, collect.
Gained lithium magnesium silicate powder body is carried out XRD, and result is as shown in Figure 4.From fig. 4, it can be seen that the present invention is successfully prepared Lithium magnesium silicate powder body, and have (001) peak the strongest to occur about 2 θ=7.1 °, show this kind of lithium magnesium silicate powder body There are layer structure, and the growth that has superiority along 001 direction, present preferable crystalline structure.This also indicates that this magnesium silicate simultaneously Interlamellar spacing in powder for lithium changes.It follows that by controlling reaction condition, the shape of prepared lithium magnesium silicate powder body Looks, interlamellar spacing etc. can be carried out regulation and control.
It should be noted last that, above example is only in order to illustrate technical scheme and unrestricted.Although ginseng According to embodiment, the present invention is described in detail, it will be apparent to an ordinarily skilled person in the art that the technical side to the present invention Case is modified or equivalent, and without departure from the spirit and scope of technical solution of the present invention, it all should be contained in the present invention Right in the middle of.

Claims (5)

1. the method preparing threadiness lithium magnesium silicate powder body, said method comprising the steps of:
1) 1~5.4g magnesium source is dissolved in deionized water, is added dropwise over aqueous slkali and generates Mg (OH)2White depositions, under room temperature Stirring, filters, washs, collects;
2) under agitation 0.03-0.18g lithium source is dissolved in the water, is formed containing lithium ion aqueous solution;
3) by step 1) Mg (OH) for preparing2White depositions is added to step 2) prepare containing in lithium ion aqueous solution, add water modulation Becoming reaction paste, the solids content in slurry is 2-4wt%;
4) after being 11-13 with aqueous slkali regulation pH, continuously stirred 2-4h;
5), after putting into 2.16-11.7g solid silicon source in a kettle., the reaction paste stirred, 160-200 DEG C of reaction are poured into 4h-360h;
6) products therefrom by centrifugation, washing to after neutrality, add washing with alcohol, then filter, be dried, collect and i.e. obtain fibrous silicon Acid magnesium powder for lithium.
A kind of method preparing threadiness lithium magnesium silicate powder body the most according to claim 1, it is characterised in that described magnesium source Selected from MgCl2·6H2O、MgSO4And MgCO3In one.
A kind of method preparing threadiness lithium magnesium silicate powder body the most according to claim 1, it is characterised in that described step 1) aqueous slkali in is ammonia, NaOH solution or KOH solution.
A kind of method preparing threadiness lithium magnesium silicate powder body the most according to claim 1, it is characterised in that described lithium source Selected from LiF, LiOH, Li2CO3With containing the one in lithium salt.
A kind of method preparing lithium magnesium silicate powder body for silicon source with glass the most according to claim 1, it is characterised in that institute State solid silicon source one in sheet glass, glass tubing, quartz ampoule and piezoid.
CN201610583972.7A 2016-07-22 2016-07-22 A method of preparing fibrous lithium magnesium silicate powder Expired - Fee Related CN106276933B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108671883A (en) * 2018-05-30 2018-10-19 贾玉臻 A kind of method in the miscellaneous hectorite material processing pharmacy waste water containing arylamine of manganese

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4687653A (en) * 1982-10-08 1987-08-18 Toyo Soda Manufacturing Co., Ltd. Process for preparation of zeolite OE having an offretite type structure
CN101798095A (en) * 2010-03-10 2010-08-11 昊青薪材(北京)技术有限公司 Process for preparing sodium potassium silicate solution by predesiliconizing potassium-rich rock
CN105645419A (en) * 2015-12-30 2016-06-08 威远县大禾陶瓷原料有限公司 Industrialized production method of cordierite structure material with ultralow heat expansion coefficient

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4687653A (en) * 1982-10-08 1987-08-18 Toyo Soda Manufacturing Co., Ltd. Process for preparation of zeolite OE having an offretite type structure
CN101798095A (en) * 2010-03-10 2010-08-11 昊青薪材(北京)技术有限公司 Process for preparing sodium potassium silicate solution by predesiliconizing potassium-rich rock
CN105645419A (en) * 2015-12-30 2016-06-08 威远县大禾陶瓷原料有限公司 Industrialized production method of cordierite structure material with ultralow heat expansion coefficient

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
周春晖等: "水热体系合成锂皂石结构的演化和影响规律研究", 《无机化学学报》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108671883A (en) * 2018-05-30 2018-10-19 贾玉臻 A kind of method in the miscellaneous hectorite material processing pharmacy waste water containing arylamine of manganese
CN108671883B (en) * 2018-05-30 2021-04-13 贾玉臻 Method for treating arylamine-containing pharmaceutical wastewater by using manganese heterophyllite material

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