CN106366700B - A kind of flame retardant of magnesium hydroxide wet preparation method - Google Patents
A kind of flame retardant of magnesium hydroxide wet preparation method Download PDFInfo
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- CN106366700B CN106366700B CN201610770292.6A CN201610770292A CN106366700B CN 106366700 B CN106366700 B CN 106366700B CN 201610770292 A CN201610770292 A CN 201610770292A CN 106366700 B CN106366700 B CN 106366700B
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- shepardite
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/028—Compounds containing only magnesium as metal
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of flame retardant of magnesium hydroxide wet preparation methods, it is related to wet dressing technical field.It is that raw material progress wet purification prepares flame retardant of magnesium hydroxide that it, which is using low-grade shepardite, and shepardite raw ore broken first is at rubble；Then rubble is put into overflow-type edge runner and carries out wet milling, shepardite slurries are made；Then hydrocyclone desanding purification is carried out to shepardite slurries；Then adding medicine flotation is classified, and is further purified；After finally carrying out natural sedimentation drainage, filters pressing, drying, ultra-fine grinding to the shepardite slurries after purification, the flame retardant of magnesium hydroxide of different-grain diameter is made.The present invention uses wet beneficiation craft, and process flow is coherent, so that low-grade shepardite is purified, and to prepare flame retardant of magnesium hydroxide, substantially increases the resource utilization of shepardite ore.
Description
Technical field
The present invention relates to wet dressing technical fields, and in particular to a kind of flame retardant of magnesium hydroxide wet preparation method.
Background technique
There are many existing method for preparing flame retardant of magnesium hydroxide, mainly there is physical method and chemical method two ways, physical method
It is as being carried out made from physics deep processing to natural minerals shepardite, chemical method mainly utilizes chemical synthesis, that is, passes through
Using the raw materials such as the brine containing magnesium chloride, halogen mine with bases reacting in an aqueous medium, chemical method mostly production process
Complexity, raw material are not easy to obtain, environment easy to pollute, are unacceptable from the point of view of industrial application cost.
It is largely relied on it is known that carrying out physical method using shepardite mineral and preparing flame retardant of magnesium hydroxide
The grade of mineral itself, high-grade brucite mineral are utilized by preferential exploitation, but with the exhaustion of high-grade mineral resources, are remained
Those lower low-grade brucite minerals just need a new technique by it by beneficiation enrichment, and removal is mixed in quartz therein
Rock class mineral, to reach available value.
Summary of the invention
The object of the present invention is to provide a kind of wet process systems using low-grade shepardite mineral production flame retardant of magnesium hydroxide
Preparation Method.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of flame retardant of magnesium hydroxide wet preparation method, it is that raw material carries out wet process which, which is using low-grade shepardite,
Prepare flame retardant of magnesium hydroxide, comprising the following steps:
A. shepardite raw ore is directly broken into the shepardite rubble that diameter is 5 ~ 10cm by crusher；
B. shepardite rubble obtained in step A is put into overflow-type edge runner, and is passed through clear water, edge runner is in water ring
It is a series of to the progress of shepardite rubble under border to roll, shear, be crushed, so that the shepardite slurries containing coarse sand be made；
C. the shepardite slurries obtained in step B containing coarse sand are passed through into precipitation tank for precipitation, utilizes the piece of shepardite ore particle
Shape suspendability leaves coarse sand behind, obtains shepardite slurries；
D. by shepardite slurries obtained in step C pass through the hydrocyclone group that is cascaded from big to small successively into
Row classification, desanding, purification, so that shepardite, which is made, purifies liquid；
E. shepardite obtained in step D purification liquid is pumped into the top floation tank in staged pond, is added certain
The shepardite purification liquid separation on pond upper layer is introduced into rank by the floating agent of amount, stirring, static rear progress gravity floatation classification
In the lower part settling tank in ladder type pond, shepardite refined liquid is obtained, floation tank bottom is then mixed with bulky grain brucite mineral
Grain and the shepardite of fine sand stone grain purification liquid are discharged by the pipeline of bottom of pond；
F., the natural sedimentation that shepardite refined liquid obtained in step E is carried out to several hours, then filters the clear of upper layer
Water；
G. it after the shepardite refined liquid after drainage enrichment in step F successively being carried out filters pressing, drying, ultra-fine grinding, is made
The flame retardant of magnesium hydroxide of different-grain diameter.
Further, the floating agent includes sodium carbonate, calgon and waterglass, wherein calgon and water
Glass serves as dispersing agent, so that shepardite ore particle suspends in water according to itself radius-thickness ratio laminar dispersion；Sodium carbonate is for adjusting
The pH value of ore pulp is saved, to improve the peptizaiton of dispersing agent.
Further, the pH value of the shepardite purification liquid is controlled 8 ~ 10.
Further, the dosage of the calgon controls 3 ‰ ~ 4 ‰ of the shepardite ore particle weight in floation tank.
Further, the dosage of the waterglass controls 4 ‰ ~ 5 ‰ of the shepardite ore particle weight in floation tank.
Further, the concentration of the shepardite purification liquid is controlled in 10% ~ 20% (mass fraction), if concentration is too low, no
Conducive to the promotion of yield, if excessive concentration, it is unfavorable for the effect of gravity floatation.
Further, the hydrocyclone group is including 300,150,75,50 and 25 5 kind of specification (according to cylinder
Internal diameter divides, and unit is mm), according to sequence from big to small, the quantity of the hydrocyclone group of the latter specification is previous
2 times of the water conservancy cyclone group of specification are connected using the hydrocyclone group of this five kinds of specifications, and classification mentions layer by layer from big to small
It is pure, be conducive to improve desanding effect, while the quantity of these cyclone groups is successively with 2 times of increased number, is to reach place
The balance of reason amount.
Further, the diameter of the hydrocyclone overflow port is 1.5 ~ 2 times of sand sinking port diameter, be can be improved in this way
The effect of desanding reduces the chance that thicker shepardite ore particle is excluded from sand sinking port.
The beneficial effects of the present invention are:
The present invention uses wet beneficiation craft, and process flow is coherent, so that low-grade shepardite is purified, and to
Flame retardant of magnesium hydroxide is prepared, the resource utilization of shepardite ore is substantially increased.
Specific embodiment
The specific embodiment of the invention uses following technical scheme:
Embodiment one:
A kind of flame retardant of magnesium hydroxide wet preparation method, it is that raw material carries out wet process which, which is using low-grade shepardite,
Prepare flame retardant of magnesium hydroxide, comprising the following steps:
A. shepardite raw ore is directly broken into the shepardite rubble that diameter is 5cm by crusher；
B. shepardite rubble obtained in step A is put into overflow-type edge runner, and is passed through clear water, edge runner is in water ring
It is a series of to the progress of shepardite rubble under border to roll, shear, be crushed, so that the shepardite slurries containing coarse sand be made；
C. the shepardite slurries obtained in step B containing coarse sand are passed through into precipitation tank for precipitation, utilizes the piece of shepardite ore particle
Shape suspendability leaves coarse sand behind, obtains shepardite slurries；
D. by shepardite slurries obtained in step C pass through the hydrocyclone group that is cascaded from big to small successively into
Row classification, desanding, purification, so that shepardite, which is made, purifies liquid；Wherein, the hydrocyclone group include 300,150,75,
50 and 25 5 kind of specification (being divided according to cylinder internal diameter, unit is mm), according to sequence from big to small, the water of the latter specification
The quantity of power cyclone group is 2 times of the water conservancy cyclone group of previous specification；The diameter of the hydrocyclone overflow port is
1.5 times of sand sinking port diameter；
E. shepardite obtained in step D purification liquid is pumped into the top floation tank in staged pond, shepardite mentions
A certain amount of floating agent is added in 10% (mass fraction) in the concentration control of pure liquid, and stirring, the static rear gravity floatation that carries out divide
The shepardite purification liquid separation on pond upper layer is introduced into the lower part settling tank in staged pond, obtains shepardite purification by grade
Then the shepardite that floation tank bottom is mixed with bulky grain shepardite ore particle and fine sand stone grain is purified pipe of the liquid by bottom of pond by liquid
Road discharge；Wherein, the floating agent includes sodium carbonate, calgon and waterglass, wherein calgon and waterglass
Dispersing agent is served as, so that shepardite ore particle suspends in water according to itself radius-thickness ratio laminar dispersion；Sodium carbonate is for adjusting mine
The pH value of slurry, to improve the peptizaiton of dispersing agent；The pH value of the shepardite purification liquid is controlled 8；The hexa metaphosphoric acid
The dosage of sodium controls 3 ‰ of the shepardite ore particle weight in floation tank；The dosage of the waterglass controls the water magnesium in floation tank
The 4 ‰ of stone ore grain weight；
F., the natural sedimentation that shepardite refined liquid obtained in step E is carried out to several hours, then filters the clear of upper layer
Water；
G. it after the shepardite refined liquid after drainage enrichment in step F successively being carried out filters pressing, drying, ultra-fine grinding, is made
The flame retardant of magnesium hydroxide of different-grain diameter.
Embodiment two:
A kind of flame retardant of magnesium hydroxide wet preparation method, it is that raw material carries out wet process which, which is using low-grade shepardite,
Prepare flame retardant of magnesium hydroxide, comprising the following steps:
A. shepardite raw ore is directly broken into the shepardite rubble that diameter is 7.5cm by crusher；
B. shepardite rubble obtained in step A is put into overflow-type edge runner, and is passed through clear water, edge runner is in water ring
It is a series of to the progress of shepardite rubble under border to roll, shear, be crushed, so that the shepardite slurries containing coarse sand be made；
C. the shepardite slurries obtained in step B containing coarse sand are passed through into precipitation tank for precipitation, utilizes the piece of shepardite ore particle
Shape suspendability leaves coarse sand behind, obtains shepardite slurries；
D. by shepardite slurries obtained in step C pass through the hydrocyclone group that is cascaded from big to small successively into
Row classification, desanding, purification, so that shepardite, which is made, purifies liquid；Wherein, the hydrocyclone group include 300,150,75,
50 and 25 5 kind of specification (being divided according to cylinder internal diameter, unit is mm), according to sequence from big to small, the water of the latter specification
The quantity of power cyclone group is 2 times of the water conservancy cyclone group of previous specification；The diameter of the hydrocyclone overflow port is
1.75 times of sand sinking port diameter；
E. shepardite obtained in step D purification liquid is pumped into the top floation tank in staged pond, shepardite mentions
A certain amount of floating agent is added in 15% (mass fraction) in the concentration control of pure liquid, and stirring, the static rear gravity floatation that carries out divide
The shepardite purification liquid separation on pond upper layer is introduced into the lower part settling tank in staged pond, obtains shepardite purification by grade
Then the shepardite that floation tank bottom is mixed with bulky grain shepardite ore particle and fine sand stone grain is purified pipe of the liquid by bottom of pond by liquid
Road discharge；Wherein, the floating agent includes sodium carbonate, calgon and waterglass, wherein calgon and waterglass
Dispersing agent is served as, so that shepardite ore particle suspends in water according to itself radius-thickness ratio laminar dispersion；Sodium carbonate is for adjusting mine
The pH value of slurry, to improve the peptizaiton of dispersing agent；The pH value of the shepardite purification liquid is controlled 9；The hexa metaphosphoric acid
The dosage of sodium controls 3.5 ‰ of the shepardite ore particle weight in floation tank；The dosage of the waterglass controls the water in floation tank
The 4.5 ‰ of magnesite ore particle weight；
F., the natural sedimentation that shepardite refined liquid obtained in step E is carried out to several hours, then filters the clear of upper layer
Water；
G. it after the shepardite refined liquid after drainage enrichment in step F successively being carried out filters pressing, drying, ultra-fine grinding, is made
The flame retardant of magnesium hydroxide of different-grain diameter.
Embodiment three:
A kind of flame retardant of magnesium hydroxide wet preparation method, it is that raw material carries out wet process which, which is using low-grade shepardite,
Prepare flame retardant of magnesium hydroxide, comprising the following steps:
A. shepardite raw ore is directly broken into the shepardite rubble that diameter is 10cm by crusher；
B. shepardite rubble obtained in step A is put into overflow-type edge runner, and is passed through clear water, edge runner is in water ring
It is a series of to the progress of shepardite rubble under border to roll, shear, be crushed, so that the shepardite slurries containing coarse sand be made；
C. the shepardite slurries obtained in step B containing coarse sand are passed through into precipitation tank for precipitation, utilizes the piece of shepardite ore particle
Shape suspendability leaves coarse sand behind, obtains shepardite slurries；
D. by shepardite slurries obtained in step C pass through the hydrocyclone group that is cascaded from big to small successively into
Row classification, desanding, purification, so that shepardite, which is made, purifies liquid；Wherein, the hydrocyclone group include 300,150,75,
50 and 25 5 kind of specification (being divided according to cylinder internal diameter, unit is mm), according to sequence from big to small, the water of the latter specification
The quantity of power cyclone group is 2 times of the water conservancy cyclone group of previous specification；The diameter of the hydrocyclone overflow port is
2 times of sand sinking port diameter；
E. shepardite obtained in step D purification liquid is pumped into the top floation tank in staged pond, shepardite mentions
A certain amount of floating agent is added in 20% (mass fraction) in the concentration control of pure liquid, and stirring, the static rear gravity floatation that carries out divide
The shepardite purification liquid separation on pond upper layer is introduced into the lower part settling tank in staged pond, obtains shepardite purification by grade
Then the shepardite that floation tank bottom is mixed with bulky grain shepardite ore particle and fine sand stone grain is purified pipe of the liquid by bottom of pond by liquid
Road discharge；Wherein, the floating agent includes sodium carbonate, calgon and waterglass, wherein calgon and waterglass
Dispersing agent is served as, so that shepardite ore particle suspends in water according to itself radius-thickness ratio laminar dispersion；Sodium carbonate is for adjusting mine
The pH value of slurry, to improve the peptizaiton of dispersing agent；The pH value of the shepardite purification liquid is controlled 10；The hexa metaphosphoric acid
The dosage of sodium controls 4 ‰ of the shepardite ore particle weight in floation tank；The dosage of the waterglass controls the water magnesium in floation tank
The 5 ‰ of stone ore grain weight；
F., the natural sedimentation that shepardite refined liquid obtained in step E is carried out to several hours, then filters the clear of upper layer
Water；
G. it after the shepardite refined liquid after drainage enrichment in step F successively being carried out filters pressing, drying, ultra-fine grinding, is made
The flame retardant of magnesium hydroxide of different-grain diameter.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (4)
1. a kind of flame retardant of magnesium hydroxide wet preparation method, which is characterized in that it is original that the technique, which is using low-grade shepardite,
Material carries out wet process and prepares flame retardant of magnesium hydroxide, comprising the following steps:
A. shepardite raw ore is directly broken into the shepardite rubble that diameter is 5 ~ 10cm by crusher；
B. shepardite rubble obtained in step A is put into overflow-type edge runner, and is passed through clear water, edge runner is under water environment
It is a series of to the progress of shepardite rubble to roll, shear, be crushed, so that the shepardite slurries containing coarse sand be made；
C. the shepardite slurries obtained in step B containing coarse sand are passed through into precipitation tank for precipitation, it can using the sheet of shepardite ore particle
Suspension leaves coarse sand behind, obtains shepardite slurries；
D. shepardite slurries obtained in step C are passed through the hydrocyclone group being cascaded from big to small successively to be divided
Grade, desanding, purification, so that shepardite, which is made, purifies liquid；
E. shepardite obtained in step D purification liquid is pumped into the top floation tank in staged pond, is added a certain amount of
The shepardite purification liquid separation on pond upper layer is introduced into staged by floating agent, stirring, static rear progress gravity floatation classification
In the lower part settling tank in pond, obtain shepardite refined liquid, then by floation tank bottom be mixed with bulky grain shepardite ore particle and
The shepardite purification liquid of fine sand stone grain is discharged by the pipeline of bottom of pond；
F., the natural sedimentation that shepardite refined liquid obtained in step E is carried out to several hours, then filters the clear water on upper layer；
G. after the shepardite refined liquid after drainage enrichment in step F successively being carried out filters pressing, drying, ultra-fine grinding, difference is made
The flame retardant of magnesium hydroxide of partial size；
The floating agent includes sodium carbonate, calgon and waterglass, and wherein calgon and waterglass serve as dispersion
Agent, so that shepardite ore particle suspends in water according to itself radius-thickness ratio laminar dispersion；Sodium carbonate is used to adjust the soda acid of ore pulp
Degree, to improve the peptizaiton of dispersing agent；
The pH value of the shepardite purification liquid is controlled 8 ~ 10；
The dosage of the calgon controls 3 ‰ ~ 4 ‰ of the shepardite ore particle weight in floation tank；
The dosage of the waterglass controls 4 ‰ ~ 5 ‰ of the shepardite ore particle weight in floation tank.
2. the method according to claim 1, wherein the concentration of shepardite purification liquid is controlled in mass fraction
Between 10% ~ 20%.
3. interior the method according to claim 1, wherein the hydrocyclone group is divided according to cylinder internal diameter
Diameter unit is mm, including 300,150,75,50 and 25 5 kind of specification, according to sequence from big to small, the latter specification
The quantity of hydrocyclone group is 2 times of the water conservancy cyclone group of previous specification.
4. the method according to claim 1, wherein the diameter of the hydrocyclone overflow port is that sand sinking port is straight
1.5 ~ 2 times of diameter.
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