CN106348320A - Efficient magnesium hydroxide flame retardant wet-process preparation method - Google Patents

Efficient magnesium hydroxide flame retardant wet-process preparation method Download PDF

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Publication number
CN106348320A
CN106348320A CN201610770291.1A CN201610770291A CN106348320A CN 106348320 A CN106348320 A CN 106348320A CN 201610770291 A CN201610770291 A CN 201610770291A CN 106348320 A CN106348320 A CN 106348320A
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Prior art keywords
shepardite
wet
flame retardant
brucite
magnesium hydroxide
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CN201610770291.1A
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CN106348320B (en
Inventor
王立贵
朱军
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HEFEI ZHONGKE FLAME-RETARDANT NEW MATERIAL Co Ltd
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HEFEI ZHONGKE FLAME-RETARDANT NEW MATERIAL Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/14—Magnesium hydroxide
    • C01F5/145—Purification
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C21/00—Disintegrating plant with or without drying of the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/002—Inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00—Fireproofing materials
    • C09K21/02—Inorganic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/005—Dispersants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/007—Modifying reagents for adjusting pH or conductivity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; specified applications
    • B03D2203/02—Ores
    • B03D2203/04—Non-sulfide ores

Abstract

The invention discloses an efficient magnesium hydroxide flame retardant wet-process preparation method, and relates to the technical field of wet-process mineral separation. According to the preparation method, wet purification is performed on low-grade brucite to prepare a magnesium hydroxide flame retardant, and particularly comprises the following steps: crushing brucite raw ore into gravels; putting the gravels into an overflow type ball grinder for wet ore grinding to prepare brucite slurry; performing sand removal and purification on the brucite slurry through a spiral sand remover and a hydrocyclone; removing ferric micro powder impurities, mixed during ball grinding, through a high-gradient magnetic separator, then adding a medicine for flotation classification for further purification; performing natural settling, water filtering, pressure filtering, drying and ultrafine smashing on the purified brucite slurry to prepare the magnesium hydroxide flame retardant with different particle sizes. By the adoption of a wet-process mineral separation process, the low-grade brucite can be purified, and the resource utilization rate of the brucite ore is greatly increased; meanwhile, the whole mineral separation process is completed by reasonably adopting large-sized treatment machinery, so that the mineral separation efficiency is greatly improved.

Description

A kind of high efficiency flame retardant of magnesium hydroxide wet preparation method
Technical field
The present invention relates to wet dressing technical field is and in particular to a kind of high efficiency flame retardant of magnesium hydroxide wet method preparation side Method.
Background technology
The existing method preparing flame retardant of magnesium hydroxide a lot, mainly has Physical and chemical method two ways, Physical It is to be obtained by natural minerals shepardite is carried out with physics deep processing, chemical method mainly uses chemical synthesiss, that is, pass through Using the raw material and bases reaction in aqueous medium such as the salt containing magnesium chloride, halogen ore deposit, chemical method mostly production process Complexity, raw material is difficult to obtain, and easily pollutes environment, is unacceptable from the point of view of commercial Application cost.
Rely on to a great extent it is known that carrying out Physical using shepardite mineral and preparing flame retardant of magnesium hydroxide The grade of mineral itself, high-grade brucite mineral is utilized by preferential exploitation, but is as the exhaustion in high-grade ore goods and materials source, remains Those low-grade brucite minerals lower are accomplished by a new technique and are passed through beneficiation enrichment, remove and are mixed in quartz therein Rock class mineral, to reach available value.Meanwhile, the production efficiency of also ore dressing to be taken into account, to reach industrially scalable.
Content of the invention
It is an object of the invention to provide a kind of high efficiency producing flame retardant of magnesium hydroxide using low-grade shepardite mineral Wet preparation method.
The purpose of the present invention is achieved through the following technical solutions:
A kind of high efficiency flame retardant of magnesium hydroxide wet preparation method, this technique be carried out for raw material using low-grade shepardite wet Method prepares flame retardant of magnesium hydroxide, comprises the following steps:
A. shepardite raw ore is directly broken into the shepardite rubble of a diameter of 5 ~ 10cm by disintegrating machine；
B. the shepardite rubble being obtained in step a is put in overflow ball mill, and be passed through clear water, ball mill is under water environment By the cooperation of its internal cast steel ball and waveform liner plate, shepardite rubble is carried out with a series of shock, shearing, crushes, thus Shepardite serosity containing coarse sand is obtained；
C. by the shepardite serosity containing coarse sand being obtained in step b through spiral sand removing machine, the lamellar using shepardite ore particle can Suspension removes contained coarse sand；
D. the hydrocyclone group passing through to be cascaded from big to small by the shepardite serosity removing coarse sand in step c is entered successively Row classification, desanding, purification, thus be obtained shepardite purification liquid；
E. the shepardite being obtained in step d purification liquid is pumped into high gradient magnetic separator, micro- to remove the ferrum being mixed in ball milling Powder impurity；In order to avoid having influence on the whiteness of mineral.
F. the shepardite purification liquid after except ferrum in step e is pumped in the top floation tank in staged pond, plus Enter a certain amount of floating agent, stirring, static after carry out gravity floatation classification, the shepardite purification liquid on pond upper strata is separated and draws Enter in the bottom Sedimentation tank in staged pond, obtain shepardite refined liquid, then floation tank bottom is mixed with bulky grain water The shepardite of magnesite ore particle and grail grain is purified liquid and is discharged by the pipeline of at the bottom of pond；
G. the shepardite refined liquid after except ferrum in step f is carried out centrifuge dewatering, obtain shepardite wet feed；
H. the shepardite obtaining in step g wet feed is carried out successively expansion drying, after superfine grinding, the hydrogen-oxygen of prepared different-grain diameter Change magnesium fire retardant.
Further, described floating agent includes sodium carbonate, sodium hexameta phosphate and waterglass, wherein sodium hexameta phosphate and water Glass serves as dispersant, so that shepardite ore particle suspends in water according to itself radius-thickness ratio laminar dispersion；Sodium carbonate is used for adjusting The acid-base value of section ore pulp, to improve the peptizaiton of dispersant.
Further, the ph value of described shepardite purification liquid controls 8 ~ 10.
Further, the consumption of described sodium hexameta phosphate controls 3 ‰ ~ 4 ‰ of shepardite ore particle weight in floation tank.
Further, the consumption of described waterglass controls 4 ‰ ~ 5 ‰ of shepardite ore particle weight in floation tank.
Further, the concentration of described shepardite purification liquid controls in 10% ~ 20% (mass fraction), if concentration is too low, no Beneficial to the lifting of yield, if excessive concentration, it is unfavorable for the effect of gravity floatation.
Further, described hydrocyclone group include 300,150,75,50 and 25 5 kind of specification (according to cylinder Internal diameter divides, and unit is mm), according to order from big to small, the quantity of the hydrocyclone group of a rear specification is previous 2 times of the water conservancy cyclone group of specification, using the hydrocyclone group series connection of this five kinds of specifications, classification carries layer by layer from big to small Pure, be conducive to improving desanding effect, the quantity of these cyclone groups, successively with 2 times of increased number, is to reach place simultaneously The balance of reason amount.
Further, the diameter of described hydrocyclone overfall is 1.5 ~ 2 times of spigot diameter, so can improve The effect of desanding, reduces the chance that thicker shepardite ore particle is excluded from spigot.
Further, described cast steel ball include 30,40,50 and 60 4 kind of specification (divide according to sphere diameter, unit It is mm), the ratio of input is 1:1.5:1.5:1, and so different size of cast steel ball mix and match is conducive to shepardite Ore to exist Fully pulverized in ball mill.
The beneficial effects of the present invention is:
The present invention adopts wet beneficiation craft, and technological process links up so that low-grade shepardite is purified, and in order to prepare Go out flame retardant of magnesium hydroxide, substantially increase the resource utilization of shepardite Ore, rationally adopt in whole ore dressing process meanwhile Large-scale process machinery, substantially increases beneficiating efficiency.
Specific embodiment
The specific embodiment of the invention employs the following technical solutions:
Embodiment one:
A kind of high efficiency flame retardant of magnesium hydroxide wet preparation method, this technique is to carry out wet method preparation using shepardite for raw material Flame retardant of magnesium hydroxide, comprises the following steps:
A. shepardite raw ore is directly broken into the shepardite rubble of a diameter of 5cm by disintegrating machine；
B. the shepardite rubble being obtained in step a is put in overflow ball mill, and be passed through clear water, ball mill is under water environment By the cooperation of its internal cast steel ball and waveform liner plate, shepardite rubble is carried out with a series of shock, shearing, crushes, thus Shepardite serosity containing coarse sand is obtained；
C. by the shepardite serosity containing coarse sand being obtained in step b through spiral sand removing machine, the lamellar using shepardite ore particle can Suspension removes contained coarse sand；
D. the hydrocyclone group passing through to be cascaded from big to small by the shepardite serosity removing coarse sand in step c is entered successively Row classification, desanding, purification, thus be obtained shepardite purification liquid；Wherein, described hydrocyclone group include 300,150,75, 50 and 25 5 kind of specification (dividing according to cylinder internal diameter, unit is mm), according to order from big to small, the water of a rear specification The quantity of power cyclone group is 2 times of the water conservancy cyclone group of previous specification；The diameter of described hydrocyclone overfall is 1.5 times of spigot diameter；
E. the shepardite being obtained in step d purification liquid is pumped into high gradient magnetic separator, micro- to remove the ferrum being mixed in ball milling Powder impurity；
F. the shepardite purification liquid after except ferrum in step e is pumped in the top floation tank in staged pond, shepardite Purification liquid concentration control in 10% (mass fraction), add a certain amount of floating agent, stirring, static after carry out gravity floatation Classification, the shepardite on pond upper strata is purified liquid and separates in the bottom Sedimentation tank being incorporated into staged pond, obtain shepardite essence Then floation tank bottom is mixed with bulky grain shepardite ore particle and the shepardite of grail grain purifies liquid by the bottom of pond by liquid processed Pipeline is discharged；Wherein, described floating agent includes sodium carbonate, sodium hexameta phosphate and waterglass, wherein sodium hexameta phosphate and water glass Glass serves as dispersant, so that shepardite ore particle suspends in water according to itself radius-thickness ratio laminar dispersion；Sodium carbonate is used for adjusting The acid-base value of ore pulp, to improve the peptizaiton of dispersant；The ph value that described shepardite purifies liquid controls 8；Described six inclined phosphorus The consumption of sour sodium controls 3 ‰ of shepardite ore particle weight in floation tank；The consumption of described waterglass controls water in floation tank The 4 ‰ of magnesite ore particle weight；
G. the shepardite refined liquid after except ferrum in step f is carried out centrifuge dewatering, obtain shepardite wet feed；
H. the shepardite obtaining in step g wet feed is carried out successively expansion drying, after superfine grinding, the hydrogen-oxygen of prepared different-grain diameter Change magnesium fire retardant.
Embodiment two:
A kind of high efficiency flame retardant of magnesium hydroxide wet preparation method, this technique is to carry out wet method preparation using shepardite for raw material Flame retardant of magnesium hydroxide, comprises the following steps:
A. shepardite raw ore is directly broken into the shepardite rubble of a diameter of 7.5cm by disintegrating machine；
B. the shepardite rubble being obtained in step a is put in overflow ball mill, and be passed through clear water, ball mill is under water environment By the cooperation of its internal cast steel ball and waveform liner plate, shepardite rubble is carried out with a series of shock, shearing, crushes, thus Shepardite serosity containing coarse sand is obtained；
C. by the shepardite serosity containing coarse sand being obtained in step b through spiral sand removing machine, the lamellar using shepardite ore particle can Suspension removes contained coarse sand；
D. the hydrocyclone group passing through to be cascaded from big to small by the shepardite serosity removing coarse sand in step c is entered successively Row classification, desanding, purification, thus be obtained shepardite purification liquid；Wherein, described hydrocyclone group include 300,150,75, 50 and 25 5 kind of specification (dividing according to cylinder internal diameter, unit is mm), according to order from big to small, the water of a rear specification The quantity of power cyclone group is 2 times of the water conservancy cyclone group of previous specification；The diameter of described hydrocyclone overfall is 1.75 times of spigot diameter；
E. the shepardite being obtained in step d purification liquid is pumped into high gradient magnetic separator, micro- to remove the ferrum being mixed in ball milling Powder impurity；
F. the shepardite purification liquid after except ferrum in step e is pumped in the top floation tank in staged pond, shepardite Purification liquid concentration control in 15% (mass fraction), add a certain amount of floating agent, stirring, static after carry out gravity floatation Classification, the shepardite on pond upper strata is purified liquid and separates in the bottom Sedimentation tank being incorporated into staged pond, obtain shepardite essence Then floation tank bottom is mixed with bulky grain shepardite ore particle and the shepardite of grail grain purifies liquid by the bottom of pond by liquid processed Pipeline is discharged；Wherein, described floating agent includes sodium carbonate, sodium hexameta phosphate and waterglass, wherein sodium hexameta phosphate and water glass Glass serves as dispersant, so that shepardite ore particle suspends in water according to itself radius-thickness ratio laminar dispersion；Sodium carbonate is used for adjusting The acid-base value of ore pulp, to improve the peptizaiton of dispersant；The ph value that described shepardite purifies liquid controls 9；Described six inclined phosphorus The consumption of sour sodium controls 3.5 ‰ of shepardite ore particle weight in floation tank；The consumption of described waterglass controls in floation tank The 4.5 ‰ of shepardite ore particle weight；
G. the shepardite refined liquid after except ferrum in step f is carried out centrifuge dewatering, obtain shepardite wet feed；
H. the shepardite obtaining in step g wet feed is carried out successively expansion drying, after superfine grinding, the hydrogen-oxygen of prepared different-grain diameter Change magnesium fire retardant.
Embodiment three:
A kind of high efficiency flame retardant of magnesium hydroxide wet preparation method, this technique is to carry out wet method preparation using shepardite for raw material Flame retardant of magnesium hydroxide, comprises the following steps:
A. shepardite raw ore is directly broken into the shepardite rubble of a diameter of 10cm by disintegrating machine；
B. the shepardite rubble being obtained in step a is put in overflow ball mill, and be passed through clear water, ball mill is under water environment By the cooperation of its internal cast steel ball and waveform liner plate, shepardite rubble is carried out with a series of shock, shearing, crushes, thus Shepardite serosity containing coarse sand is obtained；
C. by the shepardite serosity containing coarse sand being obtained in step b through spiral sand removing machine, the lamellar using shepardite ore particle can Suspension removes contained coarse sand；
D. the hydrocyclone group passing through to be cascaded from big to small by the shepardite serosity removing coarse sand in step c is entered successively Row classification, desanding, purification, thus be obtained shepardite purification liquid；Wherein, described hydrocyclone group include 300,150,75, 50 and 25 5 kind of specification (dividing according to cylinder internal diameter, unit is mm), according to order from big to small, the water of a rear specification The quantity of power cyclone group is 2 times of the water conservancy cyclone group of previous specification；The diameter of described hydrocyclone overfall is 2 times of spigot diameter；
E. the shepardite being obtained in step d purification liquid is pumped into high gradient magnetic separator, micro- to remove the ferrum being mixed in ball milling Powder impurity；
F. the shepardite purification liquid after except ferrum in step e is pumped in the top floation tank in staged pond, shepardite Purification liquid concentration control in 20% (mass fraction), add a certain amount of floating agent, stirring, static after carry out gravity floatation Classification, the shepardite on pond upper strata is purified liquid and separates in the bottom Sedimentation tank being incorporated into staged pond, obtain shepardite essence Then floation tank bottom is mixed with bulky grain shepardite ore particle and the shepardite of grail grain purifies liquid by the bottom of pond by liquid processed Pipeline is discharged；Wherein, described floating agent includes sodium carbonate, sodium hexameta phosphate and waterglass, wherein sodium hexameta phosphate and water glass Glass serves as dispersant, so that shepardite ore particle suspends in water according to itself radius-thickness ratio laminar dispersion；Sodium carbonate is used for adjusting The acid-base value of ore pulp, to improve the peptizaiton of dispersant；The ph value that described shepardite purifies liquid controls 10；Described six inclined phosphorus The consumption of sour sodium controls 4 ‰ of shepardite ore particle weight in floation tank；The consumption of described waterglass controls water in floation tank The 5 ‰ of magnesite ore particle weight；
G. the shepardite refined liquid after except ferrum in step f is carried out centrifuge dewatering, obtain shepardite wet feed；
H. the shepardite obtaining in step g wet feed is carried out successively expansion drying, after superfine grinding, the hydrogen-oxygen of prepared different-grain diameter Change magnesium fire retardant.
The above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned enforcement Example, all technical schemes belonging under thinking of the present invention belong to protection scope of the present invention.It should be pointed out that for the art Those of ordinary skill for, some improvements and modifications without departing from the principles of the present invention, these improvements and modifications Should be regarded as protection scope of the present invention.

Claims (2)

1. a kind of high efficiency flame retardant of magnesium hydroxide wet preparation method is it is characterised in that this technique is using low-grade water magnesium Stone carries out wet method for raw material and prepares flame retardant of magnesium hydroxide, comprises the following steps:
A. shepardite raw ore is directly broken into the shepardite rubble of a diameter of 5 ~ 10cm by disintegrating machine；
B. the shepardite rubble being obtained in step a is put in overflow ball mill, and be passed through clear water, ball mill is under water environment By the cooperation of its internal cast steel ball and waveform liner plate, shepardite rubble is carried out with a series of shock, shearing, crushes, thus Shepardite serosity containing coarse sand is obtained；
C. by the shepardite serosity containing coarse sand being obtained in step b through spiral sand removing machine, the lamellar using shepardite ore particle can Suspension removes contained coarse sand；
D. the hydrocyclone group passing through to be cascaded from big to small by the shepardite serosity removing coarse sand in step c is entered successively Row classification, desanding, purification, thus be obtained shepardite purification liquid；
E. the shepardite being obtained in step d purification liquid is pumped into high gradient magnetic separator, micro- to remove the ferrum being mixed in ball milling Powder impurity；
F. the shepardite purification liquid after except ferrum in step e is pumped in the top floation tank in staged pond, adds one Quantitative floating agent, stirring, static after carry out gravity floatation classification, the shepardite purification liquid on pond upper strata is separated and is incorporated into In the bottom Sedimentation tank in staged pond, obtain shepardite refined liquid, then floation tank bottom is mixed with bulky grain shepardite The shepardite of ore particle and grail grain is purified liquid and is discharged by the pipeline of at the bottom of pond；
G. the shepardite refined liquid after except ferrum in step f is carried out centrifuge dewatering, obtain shepardite wet feed；
H. the shepardite obtaining in step g wet feed is carried out successively expansion drying, after superfine grinding, the hydrogen-oxygen of prepared different-grain diameter Change magnesium fire retardant.
2. method according to claim 1 it is characterised in that described floating agent include sodium carbonate, sodium hexameta phosphate and Waterglass, wherein sodium hexameta phosphate and waterglass serve as dispersant, so that shepardite ore particle is according to the layering point of itself radius-thickness ratio Dissipate and suspend in water；Sodium carbonate is used for adjusting the acid-base value of ore pulp, to improve the peptizaiton of dispersant.
CN201610770291.1A 2016-08-31 2016-08-31 A kind of high efficiency flame retardant of magnesium hydroxide wet preparation method Active CN106348320B (en)

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Publication number Priority date Publication date Assignee Title
CN109626402A (en) * 2019-01-28 2019-04-16 包头钢铁（集团）有限责任公司 The purification process of magnesium oxide product and the preparation method of magnesia
WO2019218295A1 (en) * 2018-05-16 2019-11-21 东北大学 Efficient purification method for high-silicon, high-calcium, high-iron and low-grade brucite
CN113318866A (en) * 2021-06-01 2021-08-31 合肥皖燃新材料科技有限公司 High-whiteness superfine magnesium hydroxide flame retardant by physical method and preparation method thereof
CN113980490A (en) * 2021-11-16 2022-01-28 江西广源化工有限责任公司 Magnesium hydroxide with high specific surface area, and preparation method and application thereof

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CN103694496A (en) * 2013-09-16 2014-04-02 合肥中科阻燃新材料有限公司 Preparation method of active magnesium hydroxide fire retardants

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019218295A1 (en) * 2018-05-16 2019-11-21 东北大学 Efficient purification method for high-silicon, high-calcium, high-iron and low-grade brucite
CN109626402A (en) * 2019-01-28 2019-04-16 包头钢铁（集团）有限责任公司 The purification process of magnesium oxide product and the preparation method of magnesia
CN113318866A (en) * 2021-06-01 2021-08-31 合肥皖燃新材料科技有限公司 High-whiteness superfine magnesium hydroxide flame retardant by physical method and preparation method thereof
CN113318866B (en) * 2021-06-01 2023-02-10 合肥皖燃新材料科技有限公司 Aeration type flotation machine for processing high-white superfine magnesium hydroxide fire retardant by physical method
CN113980490A (en) * 2021-11-16 2022-01-28 江西广源化工有限责任公司 Magnesium hydroxide with high specific surface area, and preparation method and application thereof

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