CN106044806B - Method for preparing magnesium hydrate by using magnesite - Google Patents

Method for preparing magnesium hydrate by using magnesite Download PDF

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CN106044806B
CN106044806B CN201610393799.4A CN201610393799A CN106044806B CN 106044806 B CN106044806 B CN 106044806B CN 201610393799 A CN201610393799 A CN 201610393799A CN 106044806 B CN106044806 B CN 106044806B
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magnesite
mineral aggregate
rotary kiln
magnesium
magnesium hydroxide
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CN106044806A (en
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姚胜铎
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Liu Xin
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Liaoning Haomei Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/14Magnesium hydroxide
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

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  • Organic Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention relates to a method for preparing magnesium hydrate by using magnesite. The method sequentially comprises the steps that the magnesite is calcined by using an external combustion type rotary kiln so that light burned magnesium oxide can be obtained; the content of calcium sulfate in the light burned magnesium oxide is measured; the magnesium oxide is prepared into slurry with distilled water, barium chloride is added into the slurry, stirring and reaction are conducted, liquid is filtered out, drying is conducted, and thus dry magnesium hydrate is prepared; and coarse particles of the dry magnesium hydrate are screened out, so that the low-particle-size magnesium hydrate is prepared, wherein the particle size of the magnesite used for calcination is not larger than 20 mm, the primary air speed of the external combustion type rotary kiln is 50-55 m/s, the particle size of coal dust is 5-10 mm, the secondary air speed is 16-18 m/s, the ratio of the distilled water to the light burned magnesium oxide is 10:1-15:1, and the molar ratio of the barium chloride to the calcium sulfate is 2:1-3:1. According to the method for preparing the magnesium hydrate by using the magnesite, the low-particle-size magnesium hydrate can be prepared by calcining the magnesite with the external combustion type rotary kiln.

Description

The method that magnesium hydroxide is prepared using magnesite
Technical field
The present invention relates to it is a kind of using external-burning calcined by rotary kiln magnesite come the method for preparing light calcined magnesia.
Background technology
Magnesium hydroxide purposes widely, is the excellent flame retardant of plastics, rubber etc., is the rubber and plastic row generally acknowledged at present There is in industry fire-retardant, suppression cigarette, the outstanding fire retardant of filling triple functions.As flue gas desulfurization agent in terms of environmental protection, can replace The nertralizer of Caustic soda and Calx as acid-bearing wastewater.Oil dope is also acted as, anti-corrosion and desulfidation is played.In addition, may be used also For electron trade, medicine, Saccharum Sinensis Roxb. it is refined, make insulation material and manufacture other magnesium salt products.For example, can be by hydroxide Magnesium is used as fire retardant or fire-retardant filler is added in polyethylene, polypropylene, polystyrene and ABS resin, thus gives good Fire-retardant and smoke elimination is acted on;Magnesium hydroxide can be also used for the manufacture of magnesium salt, the refined of Saccharum Sinensis Roxb., pharmaceuticals industry, daily-use chemical industry etc.;Hydrogen Magnesium oxide is also used as antiacid, permeability aperient etc..At present, magnesium hydroxide is widely used in rubber, chemical industry, builds In material, plastics and electronics, unsaturated polyester (UP) and paint, coating Polymer material.Particularly to mining air duct coating cloth, The whole core conveyer belts of PVC, flame-retardant aluminum plastic plate, fire-retardant tarpaulin, PVC cable material, mine cable sheath, cable accessory it is fire-retardant, Smoke elimination antistatic, can replace aluminium hydroxide, with excellent flame retardant effect.Magnesium hydroxide has compared with similar inorganic combustion inhibitor There is more preferable smoke suppressing effect.Magnesium hydroxide unharmful substance discharge in production, use and waste procedures, and can also neutralize The acid and corrosive gas produced in combustion process.As magnesium hydroxide and substrate resin have the good compatibility, it is thermoplastic The property excellent fire retardant of resin and rubber, is commonly used for additive flame retardant or fire-retardant filler in adhesive.It is commercially used for Manufacture refined magnesium salt, activated magnesia, medicine, fine ceramics, insulation material, Saccharum Sinensis Roxb., flue gas desulfurization agent, the addition of oil product anti-corrosion Agent, acid-bearing wastewater nertralizer, colour kinescope cone glass coating etc..Due to magnesium hydroxide have it is colourless, nontoxic, tasteless, without corruption The properties such as corrosion, are environmental type macromolecular material additives.Hydroxide with good lamellar or fibrous crystal form Magnesium, preferably can be matched with raw material, and not affect the physical propertys such as the intensity of raw material, thus improve scratching for macromolecular material Qu Qiangdu and elongation percentage.Either it is used for fire retardant, or for the additive of macromolecular material, either for food, medicine Product or industrial products, the size of magnesium hydroxide are the factor of the primary importance of the performance for affecting products obtained therefrom all the time, are made especially With magnesium hydroxide prepare nano material in the case of it is especially true, therefore be highly desirable to can be obtained low particle diameter magnesium hydroxide produce Product.
The synthetic method of magnesium hydroxide mainly has salt lime method, salt Ammonia Process, concentrated seawater extraction method and aqua oxidation Magnesium processes etc..But, magnesium hydroxide obtained in salt lime method haves the shortcomings that impurity is more, particle size is big;Salt Ammonia Process is deposited Yield it is low, washing cycle is long the shortcomings of, and the little magnesium hydroxide of particle diameter cannot be obtained;Concentrated seawater extraction method equally exists miscellaneous Matter is more, the problem that particle diameter is big;Aqua oxidation magnesium processes presently, there are that magnesium hydroxide aquation is bigger than low, magnesium hydroxide particle diameter and technique The problems such as step is various.
Magnesite is the mineral name of magnesium carbonate.It is the natural alkaline raw mineral materials with magnesium carbonate as main component.Work The magnesite applied in industry actually through the magnesite of processed, the magnesite mineral products crossed through processing, generally into For magnesite.China's magnesite resource enriches, distributed more widely, and quality is high, and reserves are big.Sparry magnesite is mainly in Liaoning Province Yingkou One band of Dashiqiao to Haicheng City, reserves account for the 80% of the whole nation.
The crystal structure of magnesite and property.Magnesite is common carbonate mineral, and the nothing such as calcite, dolomite Aqueous carbonate salt mineral are referred to as calcite race mineral together, mineralogically.Calcite race crystallizable mineral construction is similar, sun from Sub- radius is close, can form extensive isomorphism, in physical property again has similarity, often symbiosis and is mingled in one closely Rise.
The chemical composition of magnesite.The main chemical compositions of sparry magnesite stone be magnesium oxide, submember be calcium oxide, Silicon oxide, iron sesquioxide, aluminium sesquioxide.Content of magnesia is generally 35%-47%, calcium oxide 0.2%-4%, silicon oxide The content of 0.2%-8%, iron sesquioxide and aluminium sesquioxide is typically below 1%.Trace element has P, Mn, Ti, Cr, Ni etc. Kind more than 20, species are more, but without economic worth.
The physicochemical change of magnesite calcining.The chemical composition of giobertite still aoxidizes two containing three in addition to magnesium oxide The impurity such as ferrum, aluminium sesquioxide, silicon oxide, calcium oxide, the basic physicochemical change occurred in calcination process:One is magnesite The decomposition of ore deposit, the crystal growth of periclase crystal;Two is under high temperature action, between oxide impurity or oxide impurity and oxygen Change magnesium to interact to form new mineral.
Calcining is thermal dissociation or the crystal phase transition process of mineral or synthetic compounds.Now, compound is at a certain temperature Thermal dissociation is for the better simply compound of composition or crystal phase transition occurs, and is beneficial to subsequent treatment or making is selected product to be changed into be suitable to The form that user needs.The change of magnesite calcination process, can be summarized as it is following some:The crystal grain of magnesite when (1) 500 DEG C There is crackle;The magnesium oxide for occurring homogenizing when (2) 550 DEG C around magnesite granule gos deep into the inside of magnesite crystal grain;(3) When 650 DEG C, magnesite disappears, and magnesium oxide local is presented anisotropism;When (4) 1100 DEG C, small magnesioferrite is formed in periclase Therefore inclusion enclave, its color are also changed into brown.Temperature continues to be increased to what change is 1400 DEG C can't see, simply periclase brown Deepen.
Calcining manners and control light roasting temperature is selected to be to obtain the light calcined magnesia important means with good aquation activity. With the raising of calcining heat, the specific surface area of MgO is remarkably decreased.When temperature is more than 1300 DEG C, MgO recrystallization speed adds Hurry up, dispersion drastically declines, activity is deteriorated.Different calcining manners and calciner is adopted to be also to affect at that same temperature The key factor of MgO activity.
At present, the device for producing light calcined magnesia by high-temperature calcination magnesite mainly has reflecting kiln or shaft furnace, wherein adopts It is the method that generally adopts with shaft furnace calcined magnesite to produce light calcined magnesia, but the method typically adopts bulk magnesite Enter kiln calcining.As no constant temperature keeps process in the technical process, and enter stove magnesite nugget greatly, easily occur in the burning of surface The phenomenon of heart underburnt, therefore there is streaking and active low shortcoming in gained light calcined magnesia.Further, since receiving furnace binding And the restriction of process conditions, there is the requirement of any to entering furnace charge block size, such as shaft furnace enters furnace charge block size and requires not less than 40 Millimeter, so that large quantities of undersized material blocks and fine ore can not be used.On the other hand, during mining, output granularity is less than 25 millimeters of Ore accounts for 40 to 45%, and this part Ore is usually discarded or for paving the way, while the huge wasting of resources is caused Soil is also taken up, environment is polluted, is caused serious environmental issue.
The device that light calcined magnesia is produced by high-temperature calcination magnesite also has tunnel cave, and tunnel cave is the continuous of modernization Fixed wall and vault, bottom are arranged at the Thermal Equipment that formula is burnt till, usually one long linear tunnel, its both sides and top Kiln car is run on the track of laying.Combustion apparatus is located at the middle part both sides of tunnel cave, constitutes fixed thermal zone burn till Band (which is equipped with clinkering zone air-supply arrangement), effect of the high-temperature flue gas that burning is produced in tunnel cave front end chimney or air-introduced machine Under, flow along tunnel to kiln hood direction, while preheating the product in kiln step by step, this section constitutes the pre- of tunnel cave The torrid zone.Cold wind is blasted in the kiln tail of tunnel cave, latter section of product in cooling tunnel kiln, the cold wind for blasting flow through product and added After heat, then feeding exsiccator is extracted out as the thermal source for being dried green compact, this section just constitutes the cooling zone of tunnel cave.Adopt at present Tunnel cave calcines the mode of bulk magnesite, haves the shortcomings that calcination time is long, and often makes surface burning and internal raw Burn, all the activity for making light-magnesite powder is reduced.
Therefore, the art also exists to using external-burning calcined by rotary kiln magnesite the light of high aquation activity is obtained Burn oxidation magnesium oxide to prepare the needs of the method for the magnesium hydroxide of low granularity by hydration process.
The content of the invention
In order to solve the light-burned oxygen for preparing low granularity for utilizing external-burning calcined by rotary kiln magnesite to prepare high-quality Said one or multiple problems in the presence of change magnesium, the present invention provide one kind in first aspect and prepare hydrogen using magnesite Method of magnesium oxide, it is characterised in that methods described in turn includes the following steps:
A () obtains light calcined magnesia using external-burning calcined by rotary kiln magnesite;
B () measures the content of the calcium sulfate in the light calcined magnesia;
C magnesium oxide is prepared slurry using distilled water by (), and in slurry add barium chloride, in 45 DEG C to 55 DEG C of temperature Stirred 6 to 7 hours with 400 to 500 revs/min of speed, so that magnesium oxide and distilled water reaction, then filter liquid, be obtained Rough magnesium hydroxide;
D rough magnesium hydroxide is less than 1 weight % in 45 DEG C to 55 DEG C dryings to water content by (), be obtained and be dried hydroxide Magnesium;With
E () is sieved to being dried magnesium hydroxide using the mesh screen with the mesh that aperture is less than 200 microns, screen out thick Granule, so that be obtained magnesium hydroxide;
Wherein:
The external-burning rotary kiln is used for the magnesite of calcining with no more than 20 millimeters of particle diameter;
The wind speed of the First air for spray feed coal dust of the external-burning rotary kiln is 50 meter per seconds to 55 meter per seconds, coal dust Granularity is 5 millimeters to 10 millimeters;
The wind speed of the secondary wind of the external-burning rotary kiln is controlled as 16 meter per seconds to 18 meter per seconds;
The envelope-bulk to weight ratio of the volume of the distilled water counted with milliliter and magnesium oxide in gram is as 10:1 to 15:1;
Barium chloride is 2 with the mol ratio of calcium sulfate:1 to 3:1.
The present invention mainly by improving the technological parameter of external-burning rotary kiln being obtained the light calcined magnesia of high-quality, and to Add barium chloride to prepare the magnesium hydroxide with low particle diameter in light calcined magnesia.
Specific embodiment
As described above, the present invention first aspect provide it is a kind of using magnesite come the method for preparing magnesium hydroxide, its It is characterised by, methods described in turn includes the following steps:
A () obtains light calcined magnesia using external-burning calcined by rotary kiln magnesite;
B () measures the content of the calcium sulfate in the light calcined magnesia;
C magnesium oxide is prepared slurry using distilled water by (), and in slurry add barium chloride, in 45 DEG C to 55 DEG C of temperature Stirred 6 to 7 hours with 400 to 500 revs/min of speed, so that magnesium oxide and distilled water reaction, then filter liquid, be obtained Rough magnesium hydroxide;
D rough magnesium hydroxide is less than 1 weight % in 45 DEG C to 55 DEG C dryings to water content by (), be obtained and be dried hydroxide Magnesium;With
E () is sieved to being dried magnesium hydroxide using the mesh screen with the mesh that aperture is less than 200 microns, screen out thick Granule, so that be obtained magnesium hydroxide;
Wherein:
The external-burning rotary kiln is used for the magnesite of calcining with no more than 20 millimeters of particle diameter;
The wind speed of the First air for spray feed coal dust of the external-burning rotary kiln is 50 meter per seconds to 55 meter per seconds, coal dust Granularity is 5 millimeters to 10 millimeters;
The wind speed of the secondary wind of the external-burning rotary kiln is controlled as 16 meter per seconds to 18 meter per seconds;
The envelope-bulk to weight ratio of the volume of the distilled water counted with milliliter and magnesium oxide in gram is as 10:1 to 15:1;
Barium chloride is 2 with the mol ratio of calcium sulfate:1 to 3:1.
The present invention is in second aspect there is provided magnesium hydroxide obtained in the method by described in first aspect present invention.
In some embodiments, the temperature of step (c) and/or step (d) is 50 DEG C.
In other embodiment, the mesh screen in step (e) has the mesh of 100 micron pore sizes.
In some preferred embodiments, the light calcined magnesia is obtained by including following method such as:
(1) magnesite powder is broken into the ore deposit of no more than 20 millimeters (being for example not more than 20 millimeters, 18,15 or 10 millimeters) Material;
(2) mineral aggregate is preheated in preheating zone so that mineral aggregate temperature reach 280 DEG C to 320 DEG C (such as 280,290, 300th, 310 or 320 DEG C);
(3) by pass through preheating mineral aggregate clinkering zone 950 DEG C to 1300 DEG C (such as 950 DEG C, 960 DEG C, 970 DEG C, 980 DEG C, 990 DEG C, 1000 DEG C, 1100 DEG C, 1200 DEG C or 1300 DEG C) calcining 30 minutes to 50 minutes (such as 30 minutes, 40 minutes, 50 minutes;
(4) by pass through calcining mineral aggregate cooling zone be cooled to 100 DEG C to 150 DEG C (such as 100 DEG C, 110 DEG C, 120 DEG C, 130 DEG C, 140 DEG C or 150 DEG C);
(5) mineral aggregate cooled down through step (4) is naturally cooled to into room temperature;With
(6) by the mineral aggregate of room temperature be crushed to granularity for no more than 100 microns (be for example not more than 100 microns, be not more than it is 90 micro- Rice, be not more than 80 microns, be not more than 70 microns, be not more than 60 microns, be not more than 50 microns), obtain light calcined magnesia product;
Wherein:For spray feed coal dust First air wind speed be 50 meter per seconds to 55 meter per seconds (such as 50 meter per seconds, 51 meters/ Second, 52 meter per seconds, 53 meter per seconds, 54 meter per seconds or 55 meter per seconds), the granularity of coal dust be 5 millimeters to 10 millimeters (such as 5 millimeters, 6 Millimeter, 7 millimeters, 8 millimeters, 9 millimeters or 10 millimeters);The blast velocity control of secondary wind be 16 meter per seconds to 18 meter per seconds (16 meter per seconds, 17 meter per seconds or 18 meter per seconds).
Some preferred embodiment in, in step (1), magnesite powder is broken into into no more than 15 millimeters of mineral aggregate.
Some preferred embodiment in, in step (3), clinkering zone 950 DEG C by pass through preheating mineral aggregates forge Burn 50 minutes.Other preferred embodiment in, in step (3), clinkering zone 1300 DEG C calcine 30 minutes.
Some preferred embodiment in, in step (2), mineral aggregate is preheated to into 300 DEG C with 5 DEG C/min of speed. Other preferred embodiment in, in step (4), will pass through calcining mineral aggregate it is mineral aggregate is cold with 5 DEG C/min of speed But to 120 DEG C.
Some preferred embodiment in, the gradient of the external-burning rotary kiln is 3.5% to 3.8%, for example, 3.5%th, 3.6%, 3.7% or 3.8%.
The present invention is in second aspect there is provided magnesium hydroxide obtained in the method by described in first aspect present invention.
External-burning rotary kiln refers to rotary calcining kiln, belongs to building equipment class.In many such as building materials, metallurgy, chemical industry, environmental protection In production industry, being widely used external-burning rotary kiln carries out machinery, physical or chemical treatment to solid material.
The structure of external-burning rotary kiln is known, generally comprises cylinder, wheel belt, support roller, gear wheel, sealing device, transmission (axial flow blower of such as clinkering zone, beneficial to the formation of kliner coating, so that protect cylinder for device and auxiliary device;Sensing barrel temperature Barrel temperature sensor and for measuring ammeter or power meter of torque etc.).Cylinder is usually by different-thickness steel plate thing First be rolled into, in cylinder, be inlaid with refractory material such as refractory brick, outside cylinder, be cased with a few road wheel belt, cylinder into constant slope, It is seated on the support roller corresponding with wheel belt.Actuating device include gear wheel, little gear, shaft coupling, main gear reducer and mair motor, Attached reductor and accessory motor.
External-burning rotary kiln needs air-supply.Including offer First air and secondary wind.
First air is typically room temperature wind, is the natural air being forcibly fed into by main burner in kiln, by kiln hood once Blower fan is supplied.Effect is mainly the required oxygen of fugitive constituent burning in pulverized coal conveying, and coal supply.It is thought that if air quantity mistake Greatly, absorb heat after entering kiln, increase the heat consumption of quantity calcining, the thermal efficiency is reduced, and is unfavorable for the discharge of NOx.But, if First air Very few, fugitive constituent burning is slow, affects burning of coal speed, therefore, the wind speed of First air is generally 50 meter per seconds to 70 metre per second (m/s)s.
Secondary wind is, in order to not allow material to be limited by various conditions in kiln, to set up the offer of post-blast device Wind, because calcining materials are in moving process, the thing section in surface is subject to the convection current of thermal current and heat radiation heating, is also subject to The radiant heating of scorching hot refractory lining;The material for pressing close to liner is then directly heated by scorching hot refractory material;In heap Material in the middle of product section is then heated by the conduction of heat of calcining materials itself.Thing is trembled because kiln body is rotated and does not stop to stir, and Shi Wu sections hand over For being heated, temperature of charge is than more uniform.After setting up post-blast, from material escape volatile matters burning required air mainly by Post-blast is supplied.The general Jing coolers of secondary wind are preheated to 650 DEG C to 1000 DEG C, after enter kiln, air-flow is produced and strong is disturbed It is dynamic, be conducive to the burning of carbon.The wind speed size of secondary wind determines the size of convulsion ability in kiln, it is considered that, the wind of secondary wind Speed is too small, and flame is too short, and the wind speed of secondary wind is big, and flame is long, thus it is general by the wind speed of secondary wind adjusting the length of flame Degree.In order to control the length of flame and the burning velocity of coal dust, typically by the blast velocity control of secondary wind 9 meter per seconds to 12 meters/ Second.
However, based on the reason for as described above, in prior art, the wind speed of First air is generally 50 meter per seconds to 70 meter per seconds In the range of, the wind speed general control of secondary wind is in the range of 9 meter per seconds to 12 meter per seconds.In such First air wind speed and two Under conditions of secondary wind wind speed, it is impossible to be adapted to generate the light-burned oxidation of high-quality by the temperature control of the clinkering zone of external-burning rotary kiln In the range of the temperature (it is generally acknowledged that 900 DEG C to 1300 DEG C) of magnesium.The present inventor is had found through further investigation, if by First air Wind speed be limited in not higher than 55 meter per seconds, such as in the range of 50 meters/meter to 55 meter per seconds, and the wind speed of secondary wind is provided To more than 16 meter per seconds, for example, improve to 16 meter per seconds to 18 meter per seconds, then the temperature stabilization of clinkering zone is maintained at into calcining and is prepared 900 DEG C to 1300 DEG C needed for light calcined magnesia are just possibly realized, and can be prepared using such process conditions and have The light calcined magnesia of high aquation activity and burn tinctuer.
In the light calcined magnesia product by obtained in magnesite, often containing other impurity components such as calcium sulfate, This impurity will not usually give what is thoroughly removed if not affecting the performance of obtained magnesium oxide.The present inventor If it was unexpectedly observed that adding suitable in slurry when using using Preparation of Magnesium Hydroxide Using Magnesium Oxide obtained in the method for the present invention During the barium chloride of amount, can be with magnesium hydroxide products of the acquisition with low particle diameter (low D50).Specifically, by light-burned oxidation Magnesium powder is broken to desired particle size and is for example not more than 100 microns, such as no more than 80 microns or no more than 50 microns afterwards, measures institute State contained calcium sulphate content in light calcined magnesia, and with 2:1 to 3:1 barium chloride and the mol ratio of calcium sulfate are to described light Add barium chloride in burned magnesium oxide, so as to the chloride containing barium raw material for preparing hydro-oxidation magnesium is obtained.Then pass through hydration method Magnesium hydroxide is prepared using the chloride containing barium raw material, it is possible thereby to be worth the magnesium hydroxide product of low particle diameter.
Embodiment
Hereafter the present invention will be further detailed using embodiment by way of illustration, but these Embodiment is not construed as limiting the invention.
, purchased from Shanghai with power heavy-duty machinery company limited, its specification is as follows for external-burning rotary kiln used in embodiment:
Diameter:4m;Length:60m;Gradient:3.8%;Production capacity:2500 ton days;
Kiln body rotating speed:0.41 to 4.07 rev/min;
Main transmission:Motor:ZSN4-355-092;Reductor:YNS1110-22.4V.Accessory drive:Motor: Y180L-4;Decelerator:YNS440-45-II.
From Henan table mountain, content of magnesia is 45.89 weight % to the magnesite used by embodiment, theoretical burn tinctuer For 51.5%, theoretical aquation activity is 43.2%.Using jaw crusher, (PE250 × 400, purchased from Shanghai with power heavy-duty machinery Company limited) magnesite is broken into into the mineral aggregate with no more than 20 millimeters of granularity, then by the mineral aggregate rotating speed be 0.8 Rev/min the preheating zone of the external-burning rotary kiln be preheated to 300 DEG C with 5 DEG C/min of speed;The mineral aggregate of preheating will be passed through Calcine 40 minutes at 1030 DEG C in clinkering zone.After calcining, will through mineral aggregate calcining in cooling zone with 5 DEG C/min of cooling Speed is cooled to 120 DEG C, then naturally cools to room temperature again.Then, room temperature mineral aggregate is crushed to into the powder that granularity is 80 microns, So as to obtain light calcined magnesia product.
The aquation activity of measurement gained light calcined magnesia and burn tinctuer.Wherein, aquation activity characterizes the suction of light calcined magnesia Outlet capacity, aquation activity are high then high with the ability of water reaction, i.e. the aquation activity of light calcined magnesia is big.Aquation activity determination method It is as follows.Light calcined magnesia of the weight for Wi is weighed, then with the abundant moistening of water (do not drip and be defined), then in an oven 150 DEG C dry to 2 hours, then weigh the weight (Wwd) of the light calcined magnesia after drying, aquation is calculated by equation below then Activity (A):
A=(Wwd Wi)/Wwd X100% (1)
Burn tinctuer characterizes magnesite through the lost percentage by weight of calcining, can be calculated with equation below (2):
Burn out rate=(W1-W2)/W1X100% (2)
Wherein, the weight of magnesite before W1 is calcining, W2 are the light-burned oxygen of gained after the magnesite of corresponding weight is calcined Change the weight of magnesium.As a result referring to table 2.
In addition, in addition to the content that table 1 below and its table are betted, to carry out with 1 described program identical mode of embodiment Embodiment 1 to 14.
Flame temperature and its standard deviation (n=20) of the table 1 using the clinkering zone obtained by different wind speed
Note:
*:Breeze is crushed to no more than 25 millimeters.
#:Mineral aggregate is preheated to 400 DEG C.
Flame temperature is using the YT-16 external-burnings revolution dispensed with power heavy-duty machinery company limited from Shanghai in clinkering zone position The data that kiln temperature measurer is measured, data every 5 minutes in the middle part of clinkering zone flame central position gather once, for collection 20 times, Ask calculation meansigma methodss and standard deviation (i.e. temperature is inclined).
As it can be seen from table 1 stably will obtain to be suitable for calcining the calcining needed for obtaining light calcined magnesia by magnesite Temperature needs low secondary wind speed and is in the higher secondary wind wind speed of proper range.
The burn tinctuer and water activity (n=5) of the light calcined magnesia obtained by 2 embodiment 1 to 14 of table.
Embodiment is numbered Light calcined magnesia Burn tinctuer (%) Water activity (%)
15 Embodiment 1 49.2 38.1
16 Embodiment 2 51.3 40.9
17 Embodiment 3 51.4 41.1
18 Embodiment 4 43.6 28.0
19 Embodiment 5 41.8 27.6
20 Embodiment 6 38.2 22.8
21 Embodiment 7 42.1 29.6
22 Embodiment 8 44.6 30.1
23 Embodiment 9 51.2 41.5
24 Embodiment 10 50.9 40.5
25 Embodiment 11 45.9 26.4
26 Embodiment 12 43.2 21.7
27 Embodiment 13 37.1 33.4
28 Embodiment 14 50.6 39.8
If from Table 2, it can be seen that the wind speed of First air is excessive and secondary wind wind speed is too low or too high, can affect The degree of calcination (reducing burn tinctuer) of magnesite is reduced, and is reduced through light-burned oxygen obtained in external-burning calcined by rotary kiln Change the aquation activity of magnesium, thus it is speculated that there may be relation with temperature and its stability.
Magnesium hydroxide is prepared by hydration process using light calcined magnesia obtained in section Example of the present invention 2 and 7.Specifically Say that the calcium sulphate content for measuring light calcined magnesia obtained in embodiment 2 and 7 is respectively 0.63 mass % and 0.69 weight % in ground. According to 1:10 w/v (g/ml) by magnesium oxide and distilled water and barium chloride (using without barium chloride as control) Mix and be positioned in the reactor in 50 DEG C of water-baths, stirred 6 hours with 400 revs/min of speed, liquid is filtered by sucking filtration Body, is obtained rough magnesium hydroxide.Then 50 DEG C of dryings to constant weight (water content is less than 1 weight %), it is obtained and is dried hydrogen-oxygen Change magnesium, residue on sieve is screened out using 100 micron mesh screens, obtain final magnesium hydroxide products, and according to HG/T 3607-2007 Method measurement D50 described in (issuing on 04 13rd, 2007, on October 01st, 2007 implements).As a result it is displayed in table 3 below.
D50 (micron) of the table 3 using magnesium hydroxide obtained in the light calcined magnesia obtained by embodiment 2 and 7.
Embodiment is numbered Light calcined magnesia Barium chloride:The molar ratio of calcium sulfate D50 (micron)
29 Embodiment 2 0 9.0
30 Embodiment 2 1 4.4
31 Embodiment 2 2 1.2
32 Embodiment 2 3 1.5
33 * embodiment 7 0 15.0
34 Embodiment 7 1 12.0
35 Embodiment 7 2 8.1
36 Embodiment 7 3 6.8
From table 3 it can be seen that when appropriate barium chloride is added, can obtain in the case of without any post processing The much lower magnesium hydroxide products of particle diameter.When barium chloride is 2 with the mol ratio of barium sulfate:1 to 3:Hydrogen when 1, obtained by embodiment 2 Magnesium oxide product can basically reach or be close to the I class products that HG/T 3607-2007 specify without any post processing, D50 Standard.But, if the barium chloride for adding is too low, D50 is still larger, thus it is speculated that possibly barium chloride plays dispersion wherein The effect of agent.Especially for the light calcined magnesia obtained by embodiment 2, the effect of barium chloride is more significantly.

Claims (9)

1. a kind of method that use magnesite prepares magnesium hydroxide, it is characterised in that methods described in turn includes the following steps:
A () obtains light calcined magnesia using external-burning calcined by rotary kiln magnesite;
B () measures the content of the calcium sulfate in the light calcined magnesia;
C magnesium oxide is prepared slurry using distilled water by (), and in slurry add barium chloride, 45 DEG C to 55 DEG C of temperature with 400 to 500 revs/min of speed is stirred 6 to 7 hours, so that magnesium oxide and distilled water reaction, then filter liquid, is obtained thick Hydrogen manufacturing magnesium oxide;
D rough magnesium hydroxide is less than 1 weight % in 45 DEG C to 55 DEG C dryings to water content by (), be obtained and be dried magnesium hydroxide;With
E () is sieved to being dried magnesium hydroxide using the mesh screen with the mesh that aperture is less than 200 microns, screen out thick Grain, so that be obtained magnesium hydroxide;
Wherein:
The external-burning rotary kiln is used for the magnesite of calcining with no more than 20 millimeters of particle diameter;
The wind speed of the First air for spray feed coal dust of the external-burning rotary kiln be 50 meter per seconds to 55 meter per seconds, the granularity of coal dust For 5 millimeters to 10 millimeters;
The wind speed of the secondary wind of the external-burning rotary kiln is controlled as 16 meter per seconds to 18 meter per seconds;
The envelope-bulk to weight ratio of the volume of the distilled water counted with milliliter and magnesium oxide in gram is as 10:1 to 15:1;
Barium chloride is 2 with the mol ratio of calcium sulfate:1 to 3:1.
2. method according to claim 1, it is characterised in that the temperature of step (c) and/or step (d) is 50 DEG C.
3. method according to claim 1, it is characterised in that the mesh screen in step (e) has the net of 100 micron pore sizes Hole.
4. method according to claim 1, it is characterised in that the light calcined magnesia is obtained by the following method:
(1) magnesite powder is broken into no more than 20 millimeters of mineral aggregate;
(2) mineral aggregate is preheated in preheating zone, so that mineral aggregate temperature reaches 280 DEG C to 320 DEG C;
(3) mineral aggregate for passing through preheating is calcined 30 minutes to 50 minutes at 950 DEG C to 1300 DEG C in clinkering zone;
(4) mineral aggregate for passing through calcining is cooled to into 100 DEG C to 150 DEG C in cooling zone;
(5) mineral aggregate cooled down through step (4) is naturally cooled to into room temperature;With
(6) mineral aggregate of room temperature is crushed to into granularity for no more than 100 microns, obtains light calcined magnesia product.
5. magnesite powder is broken into no more than 15 millis by method according to claim 4, it is characterised in that in step (1) The mineral aggregate of rice.
6. method according to claim 4, it is characterised in that in step (2), breeze is preheating to into 300 DEG C.
7. method according to claim 4, it is characterised in that in step (3), will be through pre- at 950 DEG C in clinkering zone The mineral aggregate of heat is calcined 50 minutes.
8. method according to claim 4, it is characterised in that the rotating speed of the external-burning rotary kiln be 0.6 rev/min extremely 0.9 rev/min.
9. method according to claim 4, it is characterised in that in step (4), will pass through the mineral aggregate of calcining with 5 DEG C/minute Mineral aggregate is cooled to 120 DEG C by the speed of clock.
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CN108314335A (en) * 2018-04-18 2018-07-24 镇江苏博特新材料有限公司 A kind of light-burned MgO suspension kilns coproduction Mg (OH)2Production technology and device
CN111348844B (en) * 2020-03-12 2021-11-26 辽宁科大中驰镁建材科技有限公司 System and process for preparing light-burned magnesia powder by using low-grade high-calcium magnesite
CN112066720B (en) * 2020-08-04 2022-09-23 广东摩德娜科技股份有限公司 Cooling method for quenching section of tunnel kiln and tunnel kiln control device

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WO2015051482A1 (en) * 2013-10-11 2015-04-16 河北联合大学 Method for manufacturing sheet monodisperse nano-magnesium hydroxide by using magnesite

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