CN104760966B - A kind of method of Mechano-chemical Synthesizing lithium magnesium silicate - Google Patents
A kind of method of Mechano-chemical Synthesizing lithium magnesium silicate Download PDFInfo
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Abstract
The invention discloses a kind of method of Mechano-chemical Synthesizing lithium magnesium silicate.1) synthetic magnesium silicate lithium presoma, and by the temperature control of presoma at 30 DEG C 99 DEG C；2) presoma is input into wet method super-fine equipment, under conditions of being 90 DEG C 99 DEG C in temperature of charge, grinds 5min to 90min, the drying of gained slurries obtains target product lithium magnesium silicate；A diameter of 0.1mm to 5mm of the abrasive media ball that the wet method super-fine equipment is used；Abrasive media ball linear velocity is 8m/s 20m/s.The HTHP synthetic magnesium silicate lithium that the present invention is produced by abrasive media moment, it is low to the requirement of equipment high temperature high voltage resistant, because of the peculiar structure of ultra-fine equipment, continous way production can be carried out, conventional hydrothermal reactor batch production can be solved the problems, such as；Cost is lower compared with conventional hydrothermal synthesizes, safer, it is easy to accomplish industrialization.
Description
Technical field
The present invention relates to a kind of method of Mechano-chemical Synthesizing lithium magnesium silicate.
Background technology
Lithium magnesium silicate, also known as hectorite, hectorite, hectorite, Hectorite (Hectorite), is trioctahedron stratiform
Silicate mineral, category smectite race.Observe under an electron microscope, crystal grain is in irregular sheet, length of a film and wide about 0.3 μm~
2.5 μm, piece thickness about 15nm~230nm, is typical two-dimensional nano mineral material.Because of its special crystal structure and chemical group
Into, there is great gel-forming property in water, can expand quickly, under compared with low-solid content, you can formed and include a large amount of Water Networks
Structure, high viscosity, water white transparency thixotropy gel.With very excellent colloidal dispersion, thickening property, thixotropy, steady
Qualitative, adsorptivity and suspension, be widely used in coating, paint, papermaking, cosmetics, daily chemicals, lithium battery, printing and dyeing assistant,
Medicine and other fields.
But because the mineralising cycle is long, the reason such as mineralising condition harshness, natural hectorite is extremely rare in nature, the world
On possess a small number of areas such as Hunk support of the mineral products and the only California, USA that can be exploited for a long time；And the hectorite of natural output
Impurity content is higher, it is difficult to purify, it is impossible to meet the requirement of special industry.And artificial synthesized lithium magnesium silicate purity is high, composition
Stabilization, can replace natural hectorite.
The traditional approach of artificial synthesized lithium magnesium silicate is hydrothermal synthesis method.Such as patent US3586478 and patent
WO2004096708, is that various materials first are made into precursor slurry in certain calculating ratio, then is added into hydrothermal device, temperature
200 DEG C of degree, at least reacts 10 to 20 hours under 16 atmospheric pressure of pressure, and the product for obtaining has the crystal structure of lithium magnesium silicate.
It is huge and time-consuming permanent, it is necessary to the high pressure resistant equipment of big volume that conventional hydrothermal is synthesized lithium magnesium silicate energy consumption, input cost and
Operation cost is huge；Further, since hydrothermal reaction kettle equipment limit, can only carry out batch production；And as reaction is carried out,
Material viscosity rises in kettle, causes stirring homogenizing difficult, product quality can be caused irregular and yielded poorly down.These problems are all silicon
The large-scale production of sour magnesium lithium brings difficulty.
On this basis, Japan Patent JP06345419 proposes a kind of method of continuous hydrothermal reaction.It is in the patent
Using a kind of 14.3 millimeters of internal diameter, long 100 meters, it is anti-that the tubular reactor equipped with stirring vane carries out hydro-thermal instead of hydrothermal reaction kettle
Should.The precursor slurry prepared in patent is admitted in reaction tube by high-pressure installation, is passed through under conditions of 200~400 DEG C
A few to tens of minutes are lithium magnesium silicate by reaction tube, products therefrom.This method can solve conventional hydrothermal reactor
Batch production and the problems such as uneven product quality, be adapted to produce in enormous quantities.
Another synthetic method is microwave process for synthesizing.Patent US20100098614 is 330W~3800W, frequency by power
Rate for 2.45GHz micro-wave oven react 10~50 minutes, synthesized with(Texas Southern Clay company) ties
The similar product of structure.
The content of the invention
Present invention aim at providing a kind of method of utilization wet method super-fine equipment synthetic magnesium silicate lithium, its time is short, effect
Rate is high, is easy to implement continuous production and industrialization.
It is as follows using technical scheme to reach above-mentioned purpose：
A kind of method of Mechano-chemical Synthesizing lithium magnesium silicate, comprises the following steps：
1) synthetic magnesium silicate lithium presoma, and by the temperature control of presoma at 30 DEG C -99 DEG C；
2) presoma is input into wet method super-fine equipment, under conditions of being 90 DEG C -99 DEG C in temperature of charge, grinding 5min is extremely
90min, gained slurries drying obtains target product lithium magnesium silicate；The diameter of the abrasive media ball that the wet method super-fine equipment is used
For 0.1mm to 5mm；Abrasive media ball linear velocity is 8m/s-20m/s.
By such scheme, each ion proportioning of the lithium magnesium silicate presoma preparing raw material meets following proportion requirement：
{Si8(Mg6-x-yLixNay)O20[(OH)4-zFz](x+y)-·(x+y)M+
The value of x in above formula, y, z meets：0≤x≤2,0≤y≤2,0 ＜ x+y 2,0≤z of ＜ ＜ 4.M+It is alkali metal ion
Or quaternary ammonium salt cationic.
By such scheme, after the presoma input wet method super-fine equipment, in the condition that temperature of charge is 90 DEG C -99 DEG C
Under, grind 20min to 50min.
By such scheme, the ultra-fine equipment be vibromill, Ball-stirring mill, machine for cutting charge into pieces, nanon ball-mill, nanometer sand mill or
Nanometer impact grinding.
A diameter of 0.3mm to 1mm of the abrasive media ball used by such scheme, the wet method super-fine equipment.
By such scheme, the abrasive media ball in the wet method super-fine equipment, its manufacture material is zirconium oxide, cerium Stable Oxygen
Change zirconium, yttrium stable zirconium oxide or zirconium silicate.
The present invention has the beneficial effect that relative to prior art：
1st, the high-speed motion that the present invention passes through wet method super-fine device interior abrasive media, occurs violent between medium and medium
Collision and at a high speed rotation, produce powerful shearing force and extruding force, and in the substantial amounts of heat energy of abrupt release of collision, make grinding medium
HTHP is formed between matter.This HTHP continuous action that numerous abrasive media is produced makes synthesis anti-in reaction mass
It is deserved to carry out, powerful shearing force and extruding force makes presoma particle diameter diminish, and improves the extent of reaction and reaction efficiency.This
Outward, due to the continuous motion of abrasive media in ultra-fine equipment, it is ensured that the uniformity of reaction mass, it is to avoid traditional high temperature is high
During pressure Hydrothermal Synthesiss, because material viscosity rises in kettle, stirring homogenizing difficulty is caused, product quality is uneven caused by asks
Topic.Therefore the method for the invention synthetic magnesium silicate lithium, the reaction time greatly shortened, and production efficiency is greatly improved.
2nd, the method for the invention, because of the peculiar structure of ultra-fine equipment, can carry out continous way production, can solve traditional water
The problem of thermal response kettle batch production, is adapted to large-scale production.
3rd, the HTHP synthetic magnesium silicate lithium that the method for the invention is produced by abrasive media moment, to the resistance to height of equipment
Warm high pressure requirement is low, and cost is lower compared with conventional hydrothermal synthesizes, safer, it is easy to accomplish industrialization.
Brief description of the drawings
Fig. 1：The gained sample of embodiment 1 with it is commercially availableThe X ray diffracting spectrum of RD；
Fig. 2：The gained sample of embodiment 2 with it is commercially availableThe X ray diffracting spectrum of RD.
Specific embodiment
Following examples further explain technical scheme, but not as limiting the scope of the invention.
The building-up process of lithium magnesium silicate of the present invention is as follows：
1) synthetic magnesium silicate lithium presoma, and by the temperature control of presoma at 30 DEG C -99 DEG C；
2) presoma is input into wet method super-fine equipment, under conditions of being 90 DEG C -99 DEG C in temperature of charge, grinding 5min is extremely
90min, obtains target product lithium magnesium silicate；A diameter of 0.1mm of the abrasive media ball that the wet method super-fine equipment is used is extremely
5mm；Abrasive media ball linear velocity is 8m/s-20m/s.
Synthesis material includes：Silicon-containing material；Soluble acid；Soluble magnesium salt；Water soluble alkali；Soluble lithium salt；
Wherein, each ion proportioning of lithium magnesium silicate presoma preparing raw material meets following proportion requirement：
{Si8(Mg6-x-yLixNay)O20[(OH)4-zFz](x+y)-·(x+y)M+
The value of x in above formula, y, z meets：0≤x≤2,0≤y≤2,0 ＜ x+y 2,0≤z of ＜ ＜ 4.M+It is alkali metal ion
Or quaternary ammonium salt cationic.
The embodiment of optimization, after the presoma input wet method super-fine equipment, in the bar that temperature of charge is 90 DEG C -99 DEG C
Under part, 20min to 50min is ground.
By such scheme, the wet method super-fine equipment is vibromill, Ball-stirring mill, machine for cutting charge into pieces, nanon ball-mill, nanometer sand milling
Machine or nanometer impact grinding.
The embodiment of optimization, a diameter of 0.3mm to 1mm of the abrasive media ball that the wet method super-fine equipment is used.
The embodiment of optimization, the abrasive media ball in the wet method super-fine equipment, its manufacture material is steady zirconium oxide, cerium
Determine zirconium oxide, yttrium stable zirconium oxide or zirconium silicate.
Embodiment 1
It is prepared by presoma：
(1) by 860g waterglass (SiO228wt%, Na2O9wt%, modulus 3.22) dissolved in 4L water, then while stirring
Rapidly join 162g H2SO4；
(2)560g MgCl2·6H2O is dissolved in 1L water；
(3) in step (2) solution being added into step (1) gained slurry, and stir；
(4) keep persistently stirring and being slowly added to the NaOH solution 2.4L of 3N, be made somaplasm before co-precipitation；
(5) the preceding somaplasm of co-precipitation is centrifuged, and the filter cake obtained by centrifugation, slurry after being washed fully is washed with clear water；
(6)14.5g LiOH·H2O is dissolved in 200g water；
(7) after step (6) solution adds step (5) to wash in slurry, and stir；
(8) heat while stirring, system temperature is reached 70 DEG C, obtain presoma.
Obtained presoma is input into nanon ball-mill, its abrasive media is the zirconia ball of diameter 5mm, abrasive media
Linear velocity is 8m/s.Temperature of charge is increased to 90 DEG C -99 DEG C using equipment grinding heating, and keep the temperature to continue to grind 90
Minute, gained slurries obtain final product product lithium magnesium silicate in 90 DEG C of drying, crushing.Products therefrom (sample 1) its X ray diffracting spectrum is shown in
Accompanying drawing 1.From accompanying drawing 1 as can be seen that sample 1 special diffraction maximum andThe diffraction maximum of RD (sample 2) is similar to.Show
The present embodiment products obtained therefrom has typical lithium magnesium silicate structure.
Embodiment 2
It is prepared by presoma：
(1) by 800g waterglass (SiO212.5wt%, Na2O3.9wt%, modulus 3.54) dissolved in 4L water, then side is stirred
Mix side and rapidly join 143g HNO3；
(2)530g MgSO4It is dissolved in 1L water；
(3) in step (2) solution being added into step (1) gained slurry, and stir；
(4) keep persistently stirring and being slowly added to 1L ammoniacal liquor, be made somaplasm before co-precipitation.
(5) the preceding somaplasm of co-precipitation is centrifuged, and the filter cake obtained by centrifugation, slurry after being washed fully is washed with clear water；
(6)29.4g LiOH·H2O is dissolved in 400g water；
(7) after step (6) solution adds step (5) to wash in slurry, and stir；
(8) heat while stirring, system temperature is reached 30 DEG C, obtain presoma.
Obtained presoma is input into nanometer sand mill, its abrasive media is the yttrium stable zirconium oxide ball of diameter 0.3mm,
Abrasive media linear velocity is 12m/s.Temperature of charge is increased to 90 DEG C -99 DEG C using equipment grinding heating, and keep the temperature
Continue to grind 20min, gained slurries obtain final product product lithium magnesium silicate in 90 DEG C of drying, crushing.Products therefrom (sample 3) X-ray is spread out
Penetrate collection of illustrative plates and see accompanying drawing 2.From accompanying drawing 2 as can be seen that sample 3 special diffraction maximum andThe diffraction maximum class of RD (sample 2)
Seemingly.Show that the present embodiment products obtained therefrom has typical lithium magnesium silicate structure.
Embodiment 3
It is prepared by presoma：
(1) by 880g waterglass (SiO212.5wt%, Na2O3.9wt%, modulus 3.54) dissolved in 5L water, then side is stirred
Mix side and rapidly join 120g HCl；
(2)620g Mg(NO3)2It is dissolved in 2L water；
(3) in step (2) solution being added into step (1) gained slurry, and stir；
(4) keep persistently stirring and being slowly added to 2L ammoniacal liquor, be made somaplasm before co-precipitation.
(5) the preceding somaplasm of co-precipitation is centrifuged, and the filter cake obtained by centrifugation, slurry after being washed fully is washed with clear water；
(6)25g LiOH·H2O is dissolved in 400g water；
(7) after step (6) solution adds step (5) to wash in slurry, and stir；
(8) heat while stirring, system temperature is reached 50 DEG C, obtain presoma.
Obtained presoma is input into machine for cutting charge into pieces, its abrasive media is the zirconium silicate ball of diameter 1mm, abrasive media linear speed
It is 16m/s to spend.Temperature of charge is increased to 90 DEG C -99 DEG C using equipment grinding heating, and keep the temperature to continue to grind
50min, gained slurries obtain final product product lithium magnesium silicate in 90 DEG C of drying, crushing.
Embodiment 4
It is prepared by presoma：
(1) by 700g waterglass (SiO228wt%, Na2O9wt%, modulus 3.22) dissolved in 4L water, then while stirring
Rapidly join 140g H2SO4；
(2)490g MgCl2·6H2O is dissolved in 1L water；
(3) in step (2) solution being added into step (1) gained slurry, and stir；
(4) keep persistently stirring and being slowly added to the NaOH solution 2.1L of 3N, be made somaplasm before co-precipitation；
(5) the preceding somaplasm of co-precipitation is centrifuged, and the filter cake obtained by centrifugation, slurry after being washed fully is washed with clear water；
(6)12.7g LiOH·H2O is dissolved in 200g water；
(7) after step (6) solution adds step (5) to wash in slurry, and stir；
(8) heat while stirring, system temperature is reached 99 DEG C, obtain presoma.
Obtained presoma is input into nanometer impact grinding, its abrasive media is the cerium stabilizing zirconium oxide ball of diameter 0.1mm,
Abrasive media linear velocity is 20m/s.Material maintains the temperature at 99 DEG C of grinding 5min in nanometer impact grinding, and gained slurries are at 90 DEG C
Drying, crushing obtains final product product lithium magnesium silicate.
Claims (5)
1. a kind of method of Mechano-chemical Synthesizing lithium magnesium silicate, it is characterised in that comprise the following steps：
1) synthetic magnesium silicate lithium presoma, and by the temperature control of presoma at 30 DEG C -99 DEG C；The lithium magnesium silicate forerunner system
Each ion proportioning of standby raw material meets following proportion requirement：
{Si8(Mg6-x-yLixNay)O20[(OH)4-zFz](x+y)-·(x+y)M+
The value of x in above formula, y, z meets：0≤x≤2,0≤y≤2,0 ＜ x+y 2,0≤z of ＜ ＜ 4；M+It is alkali metal ion or quaternary ammonium
Salt cation；
2) presoma is input into wet method super-fine equipment, under conditions of being 90 DEG C -99 DEG C in temperature of charge, grinds 5min to 90min,
The drying of gained slurries obtains target product lithium magnesium silicate；The abrasive media ball that the wet method super-fine equipment is used it is a diameter of
0.1mm to 5mm；Abrasive media ball linear velocity is 8m/s-20m/s.
2. a kind of method of Mechano-chemical Synthesizing lithium magnesium silicate as claimed in claim 1, it is characterised in that presoma input
After wet method super-fine equipment, under conditions of being 90 DEG C -99 DEG C in temperature of charge, 20min to 50min is ground.
3. a kind of method of Mechano-chemical Synthesizing lithium magnesium silicate as claimed in claim 1, it is characterised in that the ultra-fine equipment is
Vibromill, Ball-stirring mill, machine for cutting charge into pieces, nanon ball-mill, nanometer sand mill or nanometer impact grinding.
4. as claimed in claim 1 a kind of method of Mechano-chemical Synthesizing lithium magnesium silicate, it is characterised in that the wet method super-fine sets
A diameter of 0.3mm to 1mm of the standby abrasive media ball for using.
5. as claimed in claim 1 a kind of method of Mechano-chemical Synthesizing lithium magnesium silicate, it is characterised in that the wet method super-fine sets
Abrasive media ball in standby, its manufacture material is zirconium oxide, cerium stabilizing zirconium oxide, yttrium stable zirconium oxide or zirconium silicate.
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| CN106745013A (en) * | 2016-12-27 | 2017-05-31 | 江南大学 | A kind of lithium magnesium silicate compound and preparation method thereof |
| CN106946263B (en) * | 2017-04-19 | 2018-10-02 | 江苏海明斯新材料科技有限公司 | A kind of high temperature process heat method of the easy disperse silicic acid magnesium lithium of high transparency |
| CN113120914A (en) * | 2020-01-15 | 2021-07-16 | 北京化工大学 | Method for preparing porous magnesium silicate by ball milling method and prepared magnesium silicate |
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