CN107159402B - A kind of technique of two-stage method mechanical activation boron concentrate - Google Patents
A kind of technique of two-stage method mechanical activation boron concentrate Download PDFInfo
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- CN107159402B CN107159402B CN201710338784.2A CN201710338784A CN107159402B CN 107159402 B CN107159402 B CN 107159402B CN 201710338784 A CN201710338784 A CN 201710338784A CN 107159402 B CN107159402 B CN 107159402B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/20—Disintegrating members
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/04—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with unperforated container
- B02C17/08—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with unperforated container with containers performing a planetary movement
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
- C01B35/126—Borates of alkaline-earth metals, beryllium, aluminium or magnesium
Abstract
The invention discloses a kind of techniques of two-stage method mechanical activation boron concentrate, and boron concentrate raw material is crushed to partial size less than 150 μm；Be divided to two sections of progress mechanical activations to broken boron concentrate raw material using high energy ball mill: first segment carries out in air medium, the mass ratio of abrading-ball and boron concentrate raw material is 8~16:1, ball radius is 3~10mm, ball milling revolves revolving speed as 100~300r/min, Ball-milling Time is 10~30min, obtains dry grinding product；Second segment carries out in liquid medium, water or ethyl alcohol is added in dry grinding product as liquid medium, the mass ratio of the liquid medium and dry grinding product is 0.5~2:1, and 5~20min of Ball-milling Time obtains wet-milling product；Wet-milling product is stood into 2~4h, recycling supernatant recycling, solid is deposited in 1~12h of drying process at 30~100 DEG C, obtains activation products.The present invention combines to improve boron concentrate activity by dry type and two step of wet type mechanical activation, is conducive to chemical reaction and carries out at a lower temperature, overcome agglomeration, boron concentrate activation products have higher specific surface area and higher activity.
Description
Technical field
The invention belongs to boron resources to utilize field, the in particular to a kind of active high energy ball mill method of raising boron concentrate.
Background technique
In recent years, with the fast development in the world and China's economy, demand of each field to boron product constantly increases, therefore
The development and utilization of boron resource have increasingly important role for the development of modern industry.China boron resource overwhelming majority collection
In in the Liao Dynasty, lucky, green, four provinces and regions of hiding.Liaoning Province's boron rock reserves account for the 64.13% of gross reserves, mainly with boron magnesium stone ore (6%) and boron
Iron ore (58%) form exists, depleted with high-grade boron magnesium stone ore, develops and uses low-grade boron resource and makees
Inexorable trend is had become for industrial raw material.
Boron concentrate is to be separated by paigeite through magnet-gravity, it can be used as the alternative materials of boron magnesium stone ore, and
Have been used for industrialized production now, but boron concentrate B2O3Grade is low, structure is complicated, physico-chemical property and boron magnesium stone ore differ greatly,
Poor activity causes its processing and utilization difficulty larger.
In recent years, it improves boron concentrate activity mainly to realize by roasting, including roasting direct and sodium roasting etc., warp
Activity increases after roasting, can substantially meet current boron industrial production needs, but utilization rate is still lower.In addition roasting process
Time is long, energy consumption is high and faces polluted gas such as SO2And NOxThe problem of Deng discharging.
The microwave roasting method method new as one replaces traditional roasting means, can also be used to improve boron concentrate living
Property, it can solve polluted gas emission problem, and obtain certain research achievement, but it is still in the initial research stage, and
And accurate comprehensive assessment is also not yet received in actual industrial production economy and feasibility.
The hot environment that method of roasting needs during activating boron concentrate, it is relatively high to place and safety devices requirement,
Mechanical activation method can just improve boron concentrate activity at a lower temperature, and can avoid the waste of firing stage resource and right
The destruction of environment.Boron concentrate mineral composition is complicated, each mine mutually it is close staggeredly, it is difficult to separate, with high energy ball mill to boron concentrate into
Row ball milling, can make the boromagnesite wrapped up exposure and it is significant refine boron concentrate particle, and destroy mineral crystal structure and
Surface chemistry key makes it have higher reactivity, so that chemical reaction is easier to carry out.Mechanical activation means are in wet process smelting
Many achievements are had been achieved in gold application, including traditional in the mechanical activation in dry environment and existing for the liquid medium
Mechanical activation in environment, however two methods have its defect, dry-type mechanical activation is more obvious to sample structure destruction, still
Particle is easy reunion and poor dispersion；And wet type mechanical activation its liquid medium makes particle can the peptizaiton of sample
With lasting refinement, but liquid makes sample structure execution not have the effect under dry conditions the buffer function of mechanical force
It is good.
Summary of the invention
In order to overcome the defect of boron concentrate tradition machinery activation method, the present invention provides a kind of two-stage method mechanical activation raising
The active technique of boron concentrate, it is therefore an objective in such a way that wet process and dry method mechanical activation combine, hence it is evident that improve the object of boron concentrate
Physicochemical property, so that being obtained under conditions of reaction condition is more mild, process flow is simple, activation time is shorter higher
B2O3Activity.
Realize that the object of the invention two-stage method mechanical activation improves the active technique of boron concentrate and follows the steps below:
A kind of technique of two-stage method mechanical activation boron concentrate,
(1) prepared by raw material
Boron concentrate raw material is crushed to partial size less than 150 μm；The boron concentrate raw material is preferably dried at 105 DEG C pre-
Handle 12~48h；
(2) mechanical activation
It is divided to two sections of progress mechanical activations to broken boron concentrate raw material using high energy ball mill:
First segment carries out in air medium, and the mass ratio of abrading-ball and boron concentrate raw material is (8~16): 1, ball radius is
3~10mm, ball milling revolve revolving speed as 100~300r/min, and Ball-milling Time is 10~30min, obtains dry grinding product；
Second segment carries out in liquid medium, and water or ethyl alcohol are added in dry grinding product as liquid medium, liquid medium
Mass ratio with dry grinding product is (0.5~2): 1,5~20min of Ball-milling Time obtain wet-milling product；
(3) dry
Wet-milling product is stood into 2~4h, (recycling supernatant recycling) solid is deposited at 30~100 DEG C dry 1~
12h, (1~4h, 3~12h when using water as liquid medium when using ethyl alcohol as liquid medium), obtains activation products.
Preferably, B in the boron concentrate raw material2O3Content is 9%~13%.
Preferably, the high energy ball mill is planetary high-energy ball mill.
Preferably, every operation 15min, parked 10min in the high energy ball mill operational process, to reduce in mechanical milling process
Temperature increases the influence to sample and equipment；It reruns until reaching the Ball-milling Time of setting.
Preferably, the material of the abrading-ball is zirconium oxide.
Preferably, the leaching rate of the boron concentrate after the activation is 74.8%~93.4%.
Compared with prior art, the features of the present invention and beneficial effect are:
The present invention combines to improve boron concentrate activity by dry type and two step of wet type mechanical activation.First by boron concentrate
The activation of dry ball tool is carried out under air dielectric, particle surface chemical bond stability reduces, the reaction of boron concentrate particle surface
Active site increases, while the thermal stability of boron concentrate sample also declines, and is conducive to chemical reaction and carries out at a lower temperature, and
The agglomeration of particle is not obvious in the dry-type mechanical activation process of short time；Then liquid medium is added in ball grinder,
The activation of wet ball grinding machinery is carried out under liquid medium.In the presence of liquid medium by the fragmentation of mechanical force and
The peptizaiton of liquid medium, boron concentrate particle overcome agglomeration caused by dry grinding, and sample is further crushed, specific surface
Product greatly increases, and increases the boron concentrate miberal powder of activity raising and the contact area of other reactants, so that chemical reaction is more held
Easily carry out.
The result shows that the boron concentrate particle of small particle can obtain in a relatively short period of time, it is in ball mill revolution revolving speed
When 250rpm, within the identical mechanical activation time, it is higher that two-stage method mechanical activation can be such that boron concentrate activation products have
Specific surface area and higher activity.Relative to the sample after simple dry-type mechanical activation and wet type mechanical activation 50min, two sections
Method mechanical activation can within the time of 30min higher boron concentrate activity.Utilize two-stage method mechanical activation boron concentrate, Neng Gou
In mechanical activation 50min, the activity of boron concentrate is made to be increased to 93.4% by not activated 65% or so.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
It is removed in the boron concentrate used in the embodiment of the present invention and contains boromagnesite (MgBO2(OH)) outside, also contain serpentine
(Mg3Si2O5(OH)), biotite (K [Mg, Fe]3[Al,Fe]Si3O10(OH,F)2) etc. mineralogical compositions.
B in the boron concentrate raw material used in the embodiment of the present invention2O3Content is 11.9%.
The 4 type planet of Pulverisette that the high energy ball mill used in the embodiment of the present invention produces for Fritsch company
Formula high energy ball mill.
The abrading-ball used in the embodiment of the present invention is zirconium oxide material；Ball radius is 8mm；The solid of wet-milling product
The drying condition of precipitating is the dry 2h at 50 DEG C；When Ball-milling Time is more than 10min, setting ball milling method is operation
15min stops 10min, circuits sequentially operation.
The activity determination method of boron concentrate of the embodiment of the present invention are as follows: take activation products, use mass concentration for 20%
NaOH solution carries out alkaline hydrolysis leaching, solid-to-liquid ratio 1g/10ml to activation products, and extraction temperature is 105 ± 1 DEG C, and extraction time is
2h, measuring activation products according to volumetric method (2956 3-2001 of HG/T), (mechanical activation does not change B in boron concentrate2O3Content, institute
With the B of activation products2O3B in content and boron concentrate raw material2O311.9%) and the B of leached mud content is identical, for2O3Content, then
According to the B of leached mud and activation products2O3Content, which calculates, determines B2O3Leaching rate, with B2O3Leaching rate come characterize activation produce
Object, i.e., the boron concentrate activity after two-stage method mechanical activation.
The embodiment of the present invention measures the specific surface of analyzing activated product using NOVA 1200e type BET specific surface area analyzer
Product.
Embodiment 1
(1) raw material preparation
By boron concentrate raw material, for 24 hours, Mechanical Crushing to partial size is standby as raw material less than 75 μm for dry pretreatment at 105 DEG C
With；
(2) mechanical activation
It is divided to two sections of progress mechanical activations to broken boron concentrate raw material using high energy ball mill:
First segment carries out in air medium, and the mass ratio of abrading-ball and boron concentrate raw material is 12:1, ball mill revolution revolving speed
Dry grinding product is obtained for 250rpm, Ball-milling Time 15min；
Second segment carries out in liquid medium, dry grinding product in be added dehydrated alcohol be used as liquid medium, ethyl alcohol with do
The mass ratio for grinding product is 1:1, and at the revolving speed 250rpm that revolves, ball milling 15min obtains wet-milling product；
(3) dry
After wet-milling product is stood 3h, supernatant is recycled, and obtains activation products after solid precipitating is dry, analysis measures
B in leached mud2O3Content is 1.36%, calculate boron concentrate leaching rate be 90.0%.
(4) specific surface area
Through measuring, the specific surface area of gained activation products is 30.02m2/g。
Comparative example 1-1
(1) raw material preparation
With embodiment 1；
(2) mechanical activation --- wet grinding
Mechanical activation, ethyl alcohol and boron concentrate are carried out to broken boron concentrate raw material in ethanol medium using high energy ball mill
Mass ratio be 1:1, the mass ratio of abrading-ball and boron concentrate raw material is 12:1, and the ball mill revolving speed that revolves is 250rpm, Ball-milling Time
For 30min, wet-milling product is obtained；
(3) determination of activity
After wet-milling product is stood 1.5h, supernatant is recycled, and activation products are obtained after solid precipitating is dry, and analysis is surveyed
Obtain B in leached mud2O3Content is 2.47%, calculate boron concentrate leaching rate be 82.9%.
(4) specific surface area
Through measuring, the specific surface area of gained activation products is 26.94m2/g。
Comparative example 1-2
(1) raw material preparation
With embodiment 1；
(2) mechanical activation --- dry milling processes
Mechanical activation, abrading-ball and boron concentrate raw material are carried out to broken boron concentrate raw material using high energy ball mill in air
Mass ratio be 12:1, the ball mill revolving speed that revolves is 250rpm, and Ball-milling Time 30min obtains dry grinding product；
(3) determination of activity
Analysis measures B in dry grinding product leached mud2O3Content is 2.30%, calculate boron concentrate leaching rate be 84.2%.
(4) specific surface area
Through measuring, the specific surface area of gained dry grinding product is 24.19m2/g。
Embodiment 2
(1) raw material preparation
By boron concentrate raw material, for 24 hours, Mechanical Crushing to partial size is standby as raw material less than 75 μm for dry pretreatment at 105 DEG C
With；
(2) mechanical activation
It is divided to two sections of progress mechanical activations to broken boron concentrate raw material using high energy ball mill:
First segment carries out in air medium, and the mass ratio of abrading-ball and boron concentrate raw material is 12:1, ball mill revolution revolving speed
Dry grinding product is obtained for 250rpm, Ball-milling Time 30min；
Second segment carries out in liquid medium, dry grinding product in be added dehydrated alcohol be used as liquid medium, ethyl alcohol with do
The mass ratio for grinding product is 1:1, and at the revolving speed 250rpm that revolves, ball milling 20min obtains wet-milling product；
(3) dry
After wet-milling product is stood 1.5h, supernatant is recycled, and activation products are obtained after solid precipitating is dry, and analysis is surveyed
Obtain B in leached mud2O3Content is 0.93%, calculate boron concentrate leaching rate be 93.4%.
(4) specific surface area
Through measuring, the specific surface area of gained activation products is 36.40m2/g。
Comparative example 2-1
(1) raw material preparation
With embodiment 2；
(2) mechanical activation --- wet grinding
Mechanical activation, ethyl alcohol and boron concentrate are carried out to broken boron concentrate raw material in ethanol medium using high energy ball mill
Mass ratio be 1:1, the mass ratio of abrading-ball and boron concentrate raw material is 12:1, and the ball mill revolving speed that revolves is 250rpm, Ball-milling Time
For 50min, wet-milling product is obtained；
(3) determination of activity
After wet-milling product is stood 1.5h, supernatant is recycled, and activation products are obtained after solid precipitating is dry, and analysis is surveyed
Obtain B in leached mud2O3Content is 2.32%, calculate boron concentrate leaching rate be 84.1%.
(4) specific surface area
Through measuring, the specific surface area of gained activation products is 32.87m2/g。
Comparative example 2-2
(1) raw material preparation
With embodiment 2；
(2) mechanical activation --- dry milling processes
Mechanical activation, abrading-ball and boron concentrate raw material are carried out to broken boron concentrate raw material using high energy ball mill in air
Mass ratio be 12:1, the ball mill revolving speed that revolves is 250rpm, and Ball-milling Time 50min obtains dry grinding product；
(3) determination of activity
Analysis measures B in dry grinding product leached mud2O3Content is 1.77%, calculate boron concentrate leaching rate be 87.8%.
(4) specific surface area
Through measuring, the specific surface area of gained dry grinding product is 27.71m2/g。
Embodiment 3
The active high energy ball mill method of raising boron concentrate of the present embodiment follows the steps below:
(1) raw material preparation
By boron concentrate raw material, for 24 hours, Mechanical Crushing to partial size is standby as raw material less than 75 μm for dry pretreatment at 105 DEG C
With；
(2) mechanical activation
It is divided to two sections of progress mechanical activations to broken boron concentrate raw material using high energy ball mill:
First segment carries out in air medium, and the mass ratio of abrading-ball and boron concentrate raw material is 12:1, ball mill revolution revolving speed
Dry grinding product is obtained for 100rpm, Ball-milling Time 10min；
Second segment carries out in liquid medium, dry grinding product in be added dehydrated alcohol be used as liquid medium, ethyl alcohol with do
The mass ratio for grinding product is 1:1, and at the revolving speed 100rpm that revolves, ball milling 5min obtains wet-milling product；
(3) dry
After wet-milling product is stood 2h, supernatant is recycled, and obtains activation products after solid precipitating is dry, analysis measures
B in leached mud2O3Content is 3.20%, calculate boron concentrate leaching rate be 74.8%.
Embodiment 4
The active high energy ball mill method of raising boron concentrate of the present embodiment follows the steps below:
(1) raw material preparation
By boron concentrate raw material, for 24 hours, Mechanical Crushing to partial size is standby as raw material less than 75 μm for dry pretreatment at 105 DEG C
With；
(2) mechanical activation
It is divided to two sections of progress mechanical activations to broken boron concentrate raw material using high energy ball mill:
First segment carries out in air medium, and the mass ratio of abrading-ball and boron concentrate raw material is 12:1, ball mill revolution revolving speed
Dry grinding product is obtained for 250rpm, Ball-milling Time 10min；
Second segment carries out in liquid medium, dry grinding product in be added dehydrated alcohol be used as liquid medium, ethyl alcohol with do
The mass ratio for grinding product is 1:1, and at the revolving speed 250rpm that revolves, ball milling 5min obtains wet-milling product；
(3) dry
After wet-milling product is stood 2h, supernatant is recycled, and obtains activation products after solid precipitating is dry, analysis measures
B in leached mud2O3Content is 1.66%, calculate boron concentrate leaching rate be 87.8%.
Embodiment 5
The technique that the mechanical activation of the present embodiment improves boron concentrate leaching boron rate follows the steps below:
(1) raw material preparation
By boron concentrate raw material, for 24 hours, Mechanical Crushing to partial size is standby as raw material less than 75 μm for dry pretreatment at 105 DEG C
With；
(2) mechanical activation
It is divided to two sections of progress mechanical activations to broken boron concentrate raw material using high energy ball mill:
First segment carries out in air medium, and the mass ratio of abrading-ball and boron concentrate raw material is 12:1, ball mill revolution revolving speed
Dry grinding product is obtained for 250rpm, Ball-milling Time 10min；
Second segment carries out in liquid medium, dry grinding product in be added dehydrated alcohol be used as liquid medium, ethyl alcohol with do
The mass ratio for grinding product is 1:1, and at the revolving speed 250rpm that revolves, ball milling 20min obtains wet-milling product；
(3) dry
After wet-milling product is stood 2h, supernatant is recycled, and obtains activation products after solid precipitating is dry, analysis measures
B in leached mud2O3Content is 1.60%, calculate boron concentrate leaching rate be 88.4%.
Claims (6)
1. a kind of technique of two-stage method mechanical activation boron concentrate,
(1) prepared by raw material
Boron concentrate raw material is crushed to partial size less than 150 μm；
(2) mechanical activation
It is divided to two sections of progress mechanical activations to broken boron concentrate raw material using high energy ball mill:
First segment carries out in air medium, and the mass ratio of abrading-ball and boron concentrate raw material is 8~16:1, and ball radius is 3~
10mm, ball milling revolve revolving speed as 100~300r/min, and Ball-milling Time is 10~30min, obtains dry grinding product；
Second segment carries out in liquid medium, and water or ethyl alcohol are added in dry grinding product as liquid medium, the liquid medium
Mass ratio with dry grinding product is 0.5~2:1, and 5~20min of Ball-milling Time obtains wet-milling product；
(3) dry
Wet-milling product is stood into 2~4h, solid is deposited at 30~100 DEG C dry 1~12h, obtains activation products.
2. the technique of two-stage method mechanical activation boron concentrate according to claim 1, which is characterized in that the boron concentrate raw material
Middle B2O3Content is 9%~13%.
3. the technique of two-stage method mechanical activation boron concentrate according to claim 1, which is characterized in that the high energy ball mill
For planetary high-energy ball mill.
4. the technique of two-stage method mechanical activation boron concentrate according to claim 1, which is characterized in that the high energy ball mill
Every operation 15min, parked 10min in operational process rerun until reaching the Ball-milling Time of setting.
5. the technique of two-stage method mechanical activation boron concentrate according to claim 1, which is characterized in that the material of the abrading-ball
For zirconium oxide.
6. the technique of two-stage method mechanical activation boron concentrate according to claim 1, which is characterized in that the activation products
B2O3Leaching rate is 74.8%~93.4%.
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