CN103332858A - Preparation method of microcrystalline glass-grade beta-type spodumene - Google Patents

Preparation method of microcrystalline glass-grade beta-type spodumene Download PDF

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CN103332858A
CN103332858A CN2013102852603A CN201310285260A CN103332858A CN 103332858 A CN103332858 A CN 103332858A CN 2013102852603 A CN2013102852603 A CN 2013102852603A CN 201310285260 A CN201310285260 A CN 201310285260A CN 103332858 A CN103332858 A CN 103332858A
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triphane
beta
spodumene
preparation
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CN103332858B (en
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李南平
葛建敏
顾建超
陈东东
李小辉
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HAIMEN RONGHUI GENERAL LITHIUM CO Ltd
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HAIMEN RONGHUI GENERAL LITHIUM CO Ltd
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Abstract

The invention discloses a preparation method of a microcrystalline glass-grade beta-type spodumene. The preparation method comprises following steps: taking spodumene concentrate as a raw material, and subjecting the spodumene concentrate to high-temperature calcination in a rotary kiln at a temperature of 1050 to 1100 DEG C so as to transform the spodumene concentrate to beta-type spodumene; cooling the beta-type spodumene stepwise so as to reduce the temperature of the beta-type spodumene to 150 to 250 DEG C, wherein the granularity of the beta-type spodumene is 38 to 1200 microns; and adding water into the cooled beta-type spodumene by using automatic metering control water adding, and mixing so as to obtain the beta-type spodumene with Li2O mass percentage content of 5.9 to 6.1%, H2O mass percentage content of 1 to 3%, and Fe2O3 mass percentage content less than 1.0%, wherein the transforming rate is 90% or more. Advantages of the preparation method are that, processes are simple, operation steps are simplified, cost is low, and the lithium recovery rate is high; and in addition, water content of the beta-type spodumene is increased by automatic humidifying technologies, so that beta-type spodumene discharging temperature is further reduced, usability of the beta-type spodumene is improved, and environmental-friendly functions such as reduction of dust are realized. The products obtained by the preparation method can be used in the preparation of high-quality microcrystalline glass.

Description

The preparation method of a kind of devitrified glass level β-type triphane
Technical field
The present invention relates to the preparation method of a kind of devitrified glass level β-type triphane.
Background technology
Triphane (Spodumene) is mainly to contain one of lithium minerals, the general oxide containing lithium 5%~7% of its concentrate, and naturally occurring triphane ore deposit is α-type triphane, roasting to 1100 changes β type triphane rapidly into during ℃ left and right sides, and tool hot tearing character.
α-type triphane can be used as the additive that glass is made, and β-type triphane can be used as the additive that pottery is made.The adding of triphane not only makes the manufacturing energy consumption of glass or pottery reduce greatly, and makes the performance of the finished product be improved, and makes triphane have higher industrial value.The objective of the invention is to the effective means by a kind of economy, transforming α-type triphane is devitrified glass level β-type triphane, improves the value that triphane is used in non-metallurgical industry.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of devitrified glass level β-type triphane.
For achieving the above object, the technical solution used in the present invention is:
The preparation method of a kind of devitrified glass level β-type triphane may further comprise the steps:
A, to adopt the triphane concentrate be that raw material is β-type triphane 1~2 hour transition through 1050 ℃~1100 ℃ high-temperature calcinations in rotary kiln;
B, above-mentioned β-type triphane are down to 150 ℃~250 ℃, granularity 38 μ m~1200 μ m through cooling off the back temperature step by step;
C, through the β-type triphane of overcooling, adopt automatically that the control metering adds the water mixing, obtain Li 2O quality percentage composition 5.9%~6.1%, H 2O quality percentage composition 1%~3%, Fe 2O 3The β of quality percentage composition ﹤ 1.0%-type triphane, transition rate 〉=90%.
Described β-type triphane is the devitrified glass level.
Adopt control metering automatically to add water in the c step and finished by metering outfit, automatic humidification machine and twin-screw mixing procedure machine, metering outfit is made up of current stabilization screw feeder and spiral weighing balance.
The automatic humidification machine is controlled automatically by PLC, can be by preset proportion automatic ration humidification, and H in control β-type triphane 2O quality percentage composition is 1%~3%.
Advantage of the present invention: adopt rotary kiln at 1050 ℃~1100 ℃ high temperature α-type triphane concentrate to be made the transition and be β-type triphane, and through cooling several times, humidification obtains Li then 2O quality percentage composition 5.9%~6.1%, H 2O quality percentage composition 1%~3%, Fe 2O 3Devitrified glass level β-type triphane of quality percentage composition ﹤ 1.0%, not only technology is simple, cost is low, lithium rate of recovery height, and make devitrified glass level β-type triphane contain a certain amount of water by automatic humidification technology, namely play further reduction β-type triphane drop temperature, play the use properties of improving devitrified glass level β-type triphane again, reduce environmental-protection functions such as airborne dust in packing and the use.
Embodiment
Following examples are intended to illustrate the present invention rather than limitation of the invention further.
% is the quality percentage composition in following examples.
Embodiment 1
With the lithium concentrate of Lithium Oxide 98min 5.9% in rotary kiln 1050 ℃ temperature lower calcination 1 hour, make α-type triphane as far as possible fully be converted into β-type triphane, after calcining finishes, through rotary type cooling machine it is cooled to 150 ℃, granularity 100 μ m~1200 μ m;
Current stabilization screw feeder and the spiral weighing balance of cooled β-type triphane through the band refrigerating function cooled off step by step, metering, carry out humidification through the automatic humidification machine of being controlled automatically by PLC again, press 1% of β-type triphane weight and set amount of water, mix with the twin-screw mixing procedure machine, obtain water content and be 1%, Fe 2O 3The devitrified glass level β-type triphane of quality percentage composition 0.8%, transition, rate 94%.
Embodiment 2
With the lithium concentrate of oxide containing lithium 6.0% in rotary kiln 1070 ℃ temperature lower calcination 1.5 hours, make α-type triphane as far as possible fully be converted into β-type triphane, after calcining finishes, through rotary type cooling machine it is cooled to 200 ℃, granularity 50 μ m~100 μ m;
Current stabilization screw feeder and the spiral weighing balance of cooled β-type triphane through the band refrigerating function cooled off step by step, metering, carry out humidification through the automatic humidification machine of being controlled automatically by PLC again, press 2% of β-type triphane weight and set amount of water, mix with the twin-screw mixing procedure machine, obtain water content and be 2%, Fe 2O 3The devitrified glass level β-type triphane of quality percentage composition 0.9%, transition, rate 92%.
Embodiment 3
With the lithium concentrate of oxide containing lithium 6.1% in rotary kiln 1100 ℃ temperature lower calcination 2 hours, make α-type triphane as far as possible fully be converted into β-type triphane, after calcining finishes, through rotary type cooling machine it is cooled to 250 ℃, granularity 38 μ m~50 μ m;
Current stabilization screw feeder and the spiral weighing balance of cooled β-type triphane through the band refrigerating function cooled off step by step, metering, carry out humidification through the automatic humidification machine of being controlled automatically by PLC again, press 3% of β-type triphane weight and set amount of water, mix with the twin-screw mixing procedure machine, obtain water content and be 3%, Fe 2O 3The devitrified glass level β-type triphane of quality percentage composition 1.0%, transition, rate 90%.
The metering of above-mentioned employing and humidification can carry out chain automatic follow-up control, guarantee the stable and certainty ratio humidification of β-type triphane blanking.
β-type the triphane that obtains by the present invention can be used for making the devitrified glass novel material of property, according to the method described above, the product of the present invention of acquisition, i.e. devitrified glass level β-type triphane, mainly relevant physicochemical characteristic is:
Crystal habit β-type
Li 2The content of O (weight percentage) 5.9%~6.1%
H 2The content of O (weight percentage) 1%~3%
Fe 2O 3Content (weight percentage) ﹤ 1.0%
Granularity 38 μ m~1200 μ m
Adopt rotary kiln at 1050 ℃~1100 ℃ high temperature α-type triphane concentrate to be made the transition and be β-type triphane, and through cooling several times, humidification obtains Li then 2O content 5.9%~6.1%, H 2O content 1%~3%, Fe 2O 3Devitrified glass level β-type triphane of content ﹤ 1.0%, not only technology is simple, cost is low, lithium rate of recovery height, and make devitrified glass level β-type triphane contain a certain amount of water by automatic humidification technology, namely play further reduction β-type triphane drop temperature, play environmental-protection functions such as reducing airborne dust in use properties, packing and the use that improves devitrified glass level β-type triphane again.

Claims (4)

1. the preparation method of devitrified glass level β-type triphane is characterized in that, may further comprise the steps:
A, to adopt the triphane concentrate be that raw material is β-type triphane through 1050 ℃~1100 ℃ high-temperature calcination 1-2 hour transition in rotary kiln;
B, above-mentioned β-type triphane are down to 150 ℃~250 ℃, granularity 38 μ m~1200 μ m through cooling off the back temperature step by step;
C, through the β-type triphane of overcooling, adopt automatically that the control metering adds the water mixing, obtain Li 2O quality percentage composition 5.9%~6.1%, H 2O quality percentage composition 1%~3%, Fe 2O 3The β of quality percentage composition ﹤ 1.0%-type triphane, transition rate 〉=90%.
2. the preparation method of a kind of devitrified glass level β according to claim 1-type triphane, it is characterized in that: described β-type triphane is the devitrified glass level.
3. the preparation method of a kind of devitrified glass level β according to claim 1-type triphane, it is characterized in that: adopt control metering automatically to add water in the c step and finished by metering outfit, automatic humidification machine and twin-screw mixing procedure machine, metering outfit is made up of current stabilization screw feeder and spiral weighing balance.
4. the preparation method of a kind of devitrified glass level β according to claim 3-type triphane, it is characterized in that: the automatic humidification machine is controlled automatically by PLC, can be by preset proportion automatic ration humidification, H in control β-type triphane 2O quality percentage composition is 1%~3%.
CN201310285260.3A 2013-07-09 2013-07-09 A kind of preparation method of devitrified glass level β-type spodumene Active CN103332858B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112552032A (en) * 2020-10-26 2021-03-26 胡勇波 Synthetic beta-spodumene solid solution, microcrystalline glass prepared from synthetic beta-spodumene solid solution and preparation method of microcrystalline glass

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1640816A (en) * 2004-01-16 2005-07-20 北京奥凯元科技发展有限公司 Method for preparing quality beta-type spodumene
CN101224900A (en) * 2007-10-11 2008-07-23 钟辉 Novel method for spodumene calcining transformation

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1640816A (en) * 2004-01-16 2005-07-20 北京奥凯元科技发展有限公司 Method for preparing quality beta-type spodumene
CN101224900A (en) * 2007-10-11 2008-07-23 钟辉 Novel method for spodumene calcining transformation

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112552032A (en) * 2020-10-26 2021-03-26 胡勇波 Synthetic beta-spodumene solid solution, microcrystalline glass prepared from synthetic beta-spodumene solid solution and preparation method of microcrystalline glass

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