CN106366700A - Wet preparation method of magnesium hydrate flame retardant - Google Patents

Wet preparation method of magnesium hydrate flame retardant Download PDF

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Publication number
CN106366700A
CN106366700A CN201610770292.6A CN201610770292A CN106366700A CN 106366700 A CN106366700 A CN 106366700A CN 201610770292 A CN201610770292 A CN 201610770292A CN 106366700 A CN106366700 A CN 106366700A
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Prior art keywords
shepardite
flame retardant
magnesium hydroxide
liquid
brucite
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CN201610770292.6A
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CN106366700B (en
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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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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02Compounds of alkaline earth metals or magnesium
    • C09C1/028Compounds containing only magnesium as metal
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041Grinding
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/043Drying, calcination

Abstract

The invention discloses a wet preparation method of a magnesium hydrate flame retardant, and relates to the technical field of wet beneficiation. The magnesium hydrate flame retardant is prepared by taking low-grade brucite as a raw material through wet purification. The wet preparation method comprises the steps that firstly, brucite raw ore is crushed into broken stones; secondly, the broken stones are put into an overflow type wheel mill for wet ore milling, and brucite pulp is prepared; thirdly, degritting and purifying are conducted on the brucite pulp through a hydrocyclone; fourthly, flotation classification is conducted by adding agentia, and purifying is further conducted; lastly, after natural precipitating and draining, filter pressing, drying and ultrafine crushing are conducted on the purified brucite pulp, the magnesium hydrate flame retardant with the different particle sizes is obtained. According to the wet preparation method, the wet beneficiation technology is adopted, the technological process is coherent, the low-grade brucite can be purified and used for preparing the magnesium hydrate flame retardant, and therefore the resource utilization rate of brucite ore is greatly increased.

Description

A kind of 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 flame retardant of magnesium hydroxide wet preparation 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.
Content of the invention
It is an object of the invention to provide a kind of wet method system producing flame retardant of magnesium hydroxide using low-grade shepardite mineral Preparation Method.
The purpose of the present invention is achieved through the following technical solutions:
A kind of flame retardant of magnesium hydroxide wet preparation method, this technique is to carry out wet method preparation using low-grade 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 5 ~ 10cm by disintegrating machine;
B. the shepardite rubble being obtained in step a is put in overflow-type edge runner mill, and be passed through clear water, edge runner mill is under water environment Shepardite rubble is carried out a series of roll, shear, broken, thus shepardite serosity containing coarse sand is obtained;
C. by the shepardite serosity containing coarse sand being obtained in step b through precipitation tank for precipitation, the lamellar using shepardite ore particle can Suspension leaves coarse sand behind, obtains shepardite serosity;
D. the shepardite serosity being obtained in step c is passed through the hydrocyclone group that is cascaded from big to small to carry out successively point Level, desanding, purification, thus be obtained shepardite purification liquid;
E. the shepardite being obtained in step d purification liquid is pumped in the top floation tank in staged pond, adds a certain amount of Floating agent, stirring, static after carry out gravity floatation classification, the shepardite on pond upper strata purification liquid is separated and is incorporated into staged In the bottom Sedimentation tank in pond, obtain shepardite refined liquid, then by floation tank bottom be mixed with bulky grain shepardite ore particle and The shepardite of grail grain is purified liquid and is discharged by the pipeline of at the bottom of pond;
F. the shepardite refined liquid being obtained in step e is carried out the natural sedimentation of some hours, then filter the clear water on upper strata;
G. the shepardite refined liquid after drainage enrichment in step f is carried out filter pressing, drying successively, after superfine grinding, difference is obtained The flame retardant of magnesium hydroxide of particle diameter.
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.
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.
Specific embodiment
The specific embodiment of the invention employs the following technical solutions:
Embodiment one:
A kind of flame retardant of magnesium hydroxide wet preparation method, this technique is to carry out wet method preparation using low-grade 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-type edge runner mill, and be passed through clear water, edge runner mill is under water environment Shepardite rubble is carried out a series of roll, shear, broken, thus shepardite serosity containing coarse sand is obtained;
C. by the shepardite serosity containing coarse sand being obtained in step b through precipitation tank for precipitation, the lamellar using shepardite ore particle can Suspension leaves coarse sand behind, obtains shepardite serosity;
D. the shepardite serosity being obtained in step c is passed through the hydrocyclone group that is cascaded from big to small to carry out successively point Level, desanding, purification, thus be obtained shepardite purification liquid;Wherein, described hydrocyclone group includes 300,150,75,50 With 25 5 kinds of specifications (according to cylinder internal diameter divide, unit is mm), according to order from big to small, the waterpower of a rear specification The quantity of cyclone group is 2 times of the water conservancy cyclone group of previous specification;The diameter of described hydrocyclone overfall is heavy 1.5 times of sand mouth diameter;
E. the shepardite being obtained in step d purification liquid is pumped in the top floation tank in staged pond, shepardite purifies liquid Concentration control in 10% (mass fraction), add a certain amount of floating agent, stirring, static after carry out gravity floatation classification, will The shepardite on pond upper strata purifies liquid and separates in the bottom Sedimentation tank being incorporated into staged pond, obtains shepardite refined liquid, so Afterwards floation tank bottom is mixed with bulky grain shepardite ore particle and the shepardite of grail grain purifies the pipeline row by the bottom of pond for the liquid Go out;Wherein, described floating agent includes sodium carbonate, sodium hexameta phosphate and waterglass, wherein sodium hexameta phosphate and waterglass and 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 ore pulp Acid-base value, to improve the peptizaiton of dispersant;The ph value that described shepardite purifies liquid controls 8;Described sodium hexameta phosphate Consumption controls 3 ‰ of shepardite ore particle weight in floation tank;The consumption of described waterglass controls brucite mineral in floation tank The 4 ‰ of grain weight;
F. the shepardite refined liquid being obtained in step e is carried out the natural sedimentation of some hours, then filter the clear water on upper strata;
G. the shepardite refined liquid after drainage enrichment in step f is carried out filter pressing, drying successively, after superfine grinding, difference is obtained The flame retardant of magnesium hydroxide of particle diameter.
Embodiment two:
A kind of flame retardant of magnesium hydroxide wet preparation method, this technique is to carry out wet method preparation using low-grade 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-type edge runner mill, and be passed through clear water, edge runner mill is under water environment Shepardite rubble is carried out a series of roll, shear, broken, thus shepardite serosity containing coarse sand is obtained;
C. by the shepardite serosity containing coarse sand being obtained in step b through precipitation tank for precipitation, the lamellar using shepardite ore particle can Suspension leaves coarse sand behind, obtains shepardite serosity;
D. the shepardite serosity being obtained in step c is passed through the hydrocyclone group that is cascaded from big to small to carry out successively point Level, desanding, purification, thus be obtained shepardite purification liquid;Wherein, described hydrocyclone group includes 300,150,75,50 With 25 5 kinds of specifications (according to cylinder internal diameter divide, unit is mm), according to order from big to small, the waterpower of a rear specification The quantity of cyclone group is 2 times of the water conservancy cyclone group of previous specification;The diameter of described hydrocyclone overfall is heavy 1.75 times of sand mouth diameter;
E. the shepardite being obtained in step d purification liquid is pumped in the top floation tank in staged pond, shepardite purifies 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 separate in the bottom Sedimentation tank being incorporated into staged pond, obtains shepardite refined liquid, Then floation tank bottom is mixed with the shepardite purification pipeline by the bottom of pond for the liquid of bulky grain shepardite ore particle and grail grain Discharge;Wherein, described floating agent includes sodium carbonate, sodium hexameta phosphate and waterglass, wherein sodium hexameta phosphate and waterglass and fills Work as dispersant, so that shepardite ore particle suspends in water according to itself radius-thickness ratio laminar dispersion;Sodium carbonate is used for adjusting ore pulp Acid-base value, to improve the peptizaiton of dispersant;The ph value that described shepardite purifies liquid controls 9;Described sodium hexameta phosphate Consumption control 3.5 ‰ of shepardite ore particle weight in floation tank;The consumption of described waterglass controls water magnesium in floation tank The 4.5 ‰ of stone ore grain weight;
F. the shepardite refined liquid being obtained in step e is carried out the natural sedimentation of some hours, then filter the clear water on upper strata;
G. the shepardite refined liquid after drainage enrichment in step f is carried out filter pressing, drying successively, after superfine grinding, difference is obtained The flame retardant of magnesium hydroxide of particle diameter.
Embodiment three:
A kind of flame retardant of magnesium hydroxide wet preparation method, this technique is to carry out wet method preparation using low-grade 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-type edge runner mill, and be passed through clear water, edge runner mill is under water environment Shepardite rubble is carried out a series of roll, shear, broken, thus shepardite serosity containing coarse sand is obtained;
C. by the shepardite serosity containing coarse sand being obtained in step b through precipitation tank for precipitation, the lamellar using shepardite ore particle can Suspension leaves coarse sand behind, obtains shepardite serosity;
D. the shepardite serosity being obtained in step c is passed through the hydrocyclone group that is cascaded from big to small to carry out successively point Level, desanding, purification, thus be obtained shepardite purification liquid;Wherein, described hydrocyclone group includes 300,150,75,50 With 25 5 kinds of specifications (according to cylinder internal diameter divide, unit is mm), according to order from big to small, the waterpower of a rear specification The quantity of cyclone group is 2 times of the water conservancy cyclone group of previous specification;The diameter of described hydrocyclone overfall is heavy 2 times of sand mouth diameter;
E. the shepardite being obtained in step d purification liquid is pumped in the top floation tank in staged pond, shepardite purifies liquid Concentration control in 20% (mass fraction), add a certain amount of floating agent, stirring, static after carry out gravity floatation classification, will The shepardite on pond upper strata purifies liquid and separates in the bottom Sedimentation tank being incorporated into staged pond, obtains shepardite refined liquid, so Afterwards floation tank bottom is mixed with bulky grain shepardite ore particle and the shepardite of grail grain purifies the pipeline row by the bottom of pond for the liquid Go out;Wherein, described floating agent includes sodium carbonate, sodium hexameta phosphate and waterglass, wherein sodium hexameta phosphate and waterglass and 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 ore pulp Acid-base value, to improve the peptizaiton of dispersant;The ph value that described shepardite purifies liquid controls 10;Described sodium hexameta phosphate Consumption controls 4 ‰ of shepardite ore particle weight in floation tank;The consumption of described waterglass controls brucite mineral in floation tank The 5 ‰ of grain weight;
F. the shepardite refined liquid being obtained in step e is carried out the natural sedimentation of some hours, then filter the clear water on upper strata;
G. the shepardite refined liquid after drainage enrichment in step f is carried out filter pressing, drying successively, after superfine grinding, difference is obtained The flame retardant of magnesium hydroxide of particle diameter.
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 (8)

1. a kind of flame retardant of magnesium hydroxide wet preparation method it is characterised in that this technique be using low-grade shepardite be former Material carries out wet method 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-type edge runner mill, and be passed through clear water, edge runner mill is under water environment Shepardite rubble is carried out a series of roll, shear, broken, thus shepardite serosity containing coarse sand is obtained;
C. by the shepardite serosity containing coarse sand being obtained in step b through precipitation tank for precipitation, the lamellar using shepardite ore particle can Suspension leaves coarse sand behind, obtains shepardite serosity;
D. the shepardite serosity being obtained in step c is passed through the hydrocyclone group that is cascaded from big to small to carry out successively point Level, desanding, purification, thus be obtained shepardite purification liquid;
E. the shepardite being obtained in step d purification liquid is pumped in the top floation tank in staged pond, adds a certain amount of Floating agent, stirring, static after carry out gravity floatation classification, the shepardite on pond upper strata purification liquid is separated and is incorporated into staged In the bottom Sedimentation tank in pond, obtain shepardite refined liquid, then by floation tank bottom be mixed with bulky grain shepardite ore particle and The shepardite of grail grain is purified liquid and is discharged by the pipeline of at the bottom of pond;
F. the shepardite refined liquid being obtained in step e is carried out the natural sedimentation of some hours, then filter the clear water on upper strata;
G. the shepardite refined liquid after drainage enrichment in step f is carried out filter pressing, drying successively, after superfine grinding, difference is obtained The flame retardant of magnesium hydroxide of particle diameter.
2. flame retardant of magnesium hydroxide wet preparation method according to claim 1 is it is characterised in that described floating agent bag Include sodium carbonate, sodium hexameta phosphate and waterglass, wherein sodium hexameta phosphate and waterglass and serve as dispersant, so that shepardite ore particle Suspend 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 dividing of dispersant Dissipate effect.
3. flame retardant of magnesium hydroxide wet preparation method according to claim 2 is it is characterised in that described shepardite purifies The ph value of liquid controls 8 ~ 10.
4. flame retardant of magnesium hydroxide wet preparation method according to claim 2 is it is characterised in that described sodium hexameta phosphate Consumption control 3 ‰ ~ 4 ‰ of shepardite ore particle weight in floation tank.
5. flame retardant of magnesium hydroxide wet preparation method according to claim 2 is it is characterised in that the use of described waterglass Amount controls 4 ‰ ~ 5 ‰ of shepardite ore particle weight in floation tank.
6. flame retardant of magnesium hydroxide wet preparation method according to claim 1 is it is characterised in that described shepardite purifies The concentration of liquid controls in 10% ~ 20% (mass fraction).
7. flame retardant of magnesium hydroxide wet preparation method according to claim 1 is it is characterised in that described hydrocyclone Group includes 300,150,75,50 and 25 5 kind of specification (dividing, unit is mm) according to cylinder internal diameter, according to from big to small Order, the quantity of the hydrocyclone group of a rear specification is 2 times of the water conservancy cyclone group of previous specification.
8. flame retardant of magnesium hydroxide wet preparation method according to claim 7 is it is characterised in that described hydrocyclone The diameter of overfall is 1.5 ~ 2 times of spigot diameter.
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