CN105924023B - Preparation method for magnesium oxide raw material and magnesium hydroxide with low particle size by using low-grade magnesite - Google Patents
Preparation method for magnesium oxide raw material and magnesium hydroxide with low particle size by using low-grade magnesite Download PDFInfo
- Publication number
- CN105924023B CN105924023B CN201610261182.7A CN201610261182A CN105924023B CN 105924023 B CN105924023 B CN 105924023B CN 201610261182 A CN201610261182 A CN 201610261182A CN 105924023 B CN105924023 B CN 105924023B
- Authority
- CN
- China
- Prior art keywords
- magnesium hydroxide
- magnesium oxide
- magnesium
- low
- slurry
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2/00—Lime, magnesia or dolomite
- C04B2/10—Preheating, burning calcining or cooling
-
- 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
- C01F5/16—Magnesium hydroxide by treating magnesia, e.g. calcined dolomite, with water or solutions of salts not containing magnesium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/40—Production or processing of lime, e.g. limestone regeneration of lime in pulp and sugar mills
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a preparation method for a magnesium oxide raw material and magnesium hydroxide with low particle size by using low-grade magnesite. Specifically, the invention provides a preparation method for a magnesium oxide raw material used for producing magnesium hydroxide by using low-grade magnesite. The method comprises the following steps: subjecting magnesite to calcining so as to obtain light calcined ore, and recycling carbon dioxide; crushing the light calcined ore, and preparing the crushed light calcined ore into a slurry with a concentration of 35%; subjecting the slurry and an ammonium chloride solution to reaction, then filtering the reacted slurry, and recycling ammonia gas; subjecting obtained filtrate, ammonia water and carbon dioxide to reaction, and carrying out filtering; subjecting the filtrate and excess ammonia water to reaction, then carrying out filtering, washing filter residue, and carrying out drying so as to obtain crude magnesium oxide; and detecting the content of calcium sulfate, and adding barium chloride so as to obtain the magnesium oxide raw material. The invention also provides a preparation method for magnesium hydroxide by using the magnesium oxide raw material. According to the invention, the low-grade magnesite can be utilized to prepare magnesium hydroxide with high hydration rate and D50 less than 1.0 micron.
Description
Technical field
The present invention relates to a kind of method that use low-grade magnesite prepares raw materials of magnesium oxide and low particle diameter magnesium hydroxide.
Background technology
Although the magnisite resource very abundant of China, through the exploitation of decades, the magnesite of commerical grade is
Fewer and feweri, particularly high-grade magnesite can not meet production needs in certain areas.And low-grade magnesite
The production of expensive goods is cannot be directly used to, especially the outer magnesite of substantial amounts of level is not used, and causes magnesite resource
Waste.Therefore, from long-term interest consider, in order to preferably utilize resource, how to make full use of low-grade magnesite to solve Pedicellus et Pericarpium Trapae
Low and the shortage of high-grade magnesite the problem of magnesium ore resources utilization rate is the highly important problem that this area faces.
Magnesium hydroxide also makes causticity magnesite, caustic-calcined magnesite etc., suspension of the magnesium hydroxide in water be referred to as hydroxide magnesia magma
Agent, abbreviation magnesia magma.Magnesium hydroxide is colourless hexagonal prism crystal or white powder, is insoluble in water and alcohol, is dissolved in diluted acid and ammonium salt is molten
Liquid, aqueous solution is in alkalescence.The density (g/mL, 20 DEG C) of magnesium hydroxide：2.36；Fusing point (DEG C)：350；Refractive index (n20/D)：
1.57 left and right.
Magnesium hydroxide purposes is the excellent flame retardant of plastics, rubber etc. widely, is rubber and plastic row generally acknowledged at present
There is fire-retardant, suppression cigarette, the outstanding fire retardant of filling triple functions in industry.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 effect；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.It is thermoplastic because magnesium hydroxide and substrate resin have the good compatibility
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 match 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 is the factor of the primary importance of the performance for affecting products obtained therefrom all the time, is 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 following several method.Salt lime method, the method will in advance first pass through purification
The salt of refinement treatment and Jing digestion except Slag treatment Calx made by lime cream precipitation is carried out in stillpot, obtaining
Slip in add flocculant, after being sufficiently mixed, separated into subsider, then Jing filter, washing, drying, crush, be obtained
Magnesium hydroxide finished product, but magnesium hydroxide obtained in this method haves the shortcomings that impurity is more, particle size is big.Salt ammonia
Method, with the purified salt for removing the impurity such as carbon dioxide, a small amount of boron that processes as raw material, using ammonia as precipitant in reactor
In carry out precipitation, a certain amount of crystal seed is put into before the reaction, be sufficiently stirred for.Reaction adds flocculant after ending, and sinks
After filtering, washing, drying, crushing are obtained magnesium hydroxide finished product to starch.But the method is present, and yield is low, washing cycle is long
The shortcomings of, and the little magnesium hydroxide of particle diameter cannot be obtained.Concentrated seawater extraction method, the method extracts pulpous state hydrogen-oxygen using concentrated seawater
Change magnesium, the presence of wherein calcium ion is to affect the key factor of product purity and quality, and equally exist that impurity is more, particle diameter is big
Problem.In addition method is to be prepared into magnesium hydroxide by hydrated magnesium, but the method presently, there are magnesium hydroxide aquation
Than low, big magnesium hydroxide particle diameter and the problems such as various processing step.
Therefore, this area is highly desirable to be prepared using low-grade magnesite and has aquation less than high and/or particle diameter
The method of magnesium hydroxide.
The content of the invention
In order to solve to prepare one or more the problems referred to above present in the existing method of magnesium hydroxide, the present invention is the
On the one hand 1, a kind of use low-grade magnesite prepares the method for producing the raw materials of magnesium oxide of magnesium hydroxide, and its feature exists
In methods described comprises the steps：
(1) magnesite is calcined 2 hours under 1000 DEG C of calcining heat, obtains light-burned Ore and reclaim in calcination process
The carbon dioxide of generation；
(2) the light-burned Ore is ground into into the powder of 300 mesh and is configured to the slurry that mass fraction is 35%；
(3) by the ammonium chloride solution of the slurry and 25 mass % with 1:1 volume ratio mixes and reacts 3 hours, generates
Reaction paste and ammonia, the condensed recovery of ammonia obtains ammonia, and reaction paste obtains the first filtrate by filtering；
(4) carbon dioxide reaction for being reclaimed the ammonia obtained by the filtrate of gained first and step (3) and step (1) and mistake
Filter, obtains the second filtrate；
(5) ammonia obtained by the second filtrate of gained step (3) excessive with 20 moles of % is reacted 1 hour at 85 DEG C,
Then reactant is filtered, obtains solid material；
(6) using solid material described in 85 DEG C of hot wash, then in 120 DEG C of dryings 5 hours, crude oxidation is obtained
Magnesium；
(7) calcium sulphate content of magnesium oxide is detected, and with 2:1 to 3:1 barium chloride is with the mol ratio of calcium sulfate to it
Middle addition barium chloride, obtains the magnesium hydroxide raw materials of magnesium oxide.
The present invention provides a kind of method of use Preparation of Magnesium Hydroxide Using Magnesium Oxide in second aspect, it is characterised in that institute
The method of stating comprises the steps：
(1) raw materials of magnesium oxide described in claim 1 is obtained；
(2) raw materials of magnesium oxide is prepared into slurry using distilled water, in 45 DEG C to 55 DEG C of temperature with 400 to 500 revs/min
Speed stir 6 to 7 hours so that magnesium oxide and distilled water reaction, then filter liquid, be obtained rough magnesium hydroxide；
(3) rough magnesium hydroxide is less than into 1 weight % in 45 DEG C to 55 DEG C dryings to water content, is obtained and is dried hydroxide
Magnesium；With
(4) sieved to being dried magnesium hydroxide using the mesh screen with the mesh that aperture is less than 200 microns, screened out thick
Granule, so as to magnesium hydroxide is obtained；
Wherein, 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.
The present invention can prepare the magnesium hydroxide products that high-quality is prepared through magnesium oxide using low-grade magnesite.Separately
Outward, it is this miscellaneous often containing other impurity components such as calcium sulfate in for the raw materials of magnesium oxide for preparing magnesium hydroxide
Matter will not usually give what is thoroughly removed if not affecting the performance of obtained magnesium oxide.But, using routine
During the Preparation of Magnesium Hydroxide Using Magnesium Oxide of acquisition, if without post processings such as attrition grindings, can not usually obtain D50
Magnesium hydroxide products less than 1.0 microns.But, present inventors have surprisingly found that, if preparing hydrogen-oxygen using magnesium oxide
When adding appropriate barium chloride in slurry when changing magnesium, can be obtained with high yield value (high aquation ratio) and have low particle diameter (low
D50 magnesium hydroxide products).
Description of the drawings
Fig. 1 shows impact of the different mol ratio of barium chloride and magnesium hydroxide to D50, wherein abscissa be barium chloride and
The molar ratio of magnesium hydroxide, vertical coordinate is D50 (micron).
Fig. 2 shows that barium chloride and the appropriate mol ratio of magnesium hydroxide can obtain magnesium hydroxide products of the D50 less than 1.0
Product, wherein abscissa are the molar ratio of barium chloride and magnesium hydroxide, and vertical coordinate is D50 (micron).
Specific embodiment
As described above, the present invention provides one kind in first aspect being prepared for producing hydroxide using low-grade magnesite
The method of the raw materials of magnesium oxide of magnesium, it is characterised in that methods described comprises the steps：
(1) magnesite is calcined 2 hours under 1000 DEG C of calcining heat, obtains light-burned Ore and reclaim in calcination process
The carbon dioxide of generation；
(2) the light-burned Ore is ground into into the powder of 300 mesh and is configured to the slurry that mass fraction is 35%；
(3) by the ammonium chloride solution of the slurry and 25 mass % with 1:1 volume ratio mixes and reacts 3 hours, generates
Reaction paste and ammonia, the condensed recovery of ammonia obtains ammonia, and reaction paste obtains the first filtrate by filtering；
(4) carbon dioxide reaction for being reclaimed the ammonia obtained by the filtrate of gained first and step (3) and step (1) and mistake
Filter, obtains the second filtrate；
(5) ammonia obtained by the second filtrate of gained step (3) excessive with 20 moles of % is reacted 1 hour at 85 DEG C,
Then reactant is filtered, obtains solid material；
(6) using solid material described in 85 DEG C of hot wash, then in 120 DEG C of dryings 5 hours, crude oxidation is obtained
Magnesium；
(7) calcium sulphate content of magnesium oxide is detected, and with 2:1 to 3:1 barium chloride is with the mol ratio of calcium sulfate to it
Middle addition barium chloride, obtains the magnesium hydroxide raw materials of magnesium oxide.
In some embodiments, barium chloride and the mol ratio of calcium sulfate are 2.2:1 to 2.9:1, using this mol ratio,
Magnesium hydroxide products of the D50 less than 1.0 microns can be obtained in the case where any crushing program need not be carried out.It is excellent at some
In the embodiment of choosing, barium chloride is 2.3 with the mol ratio of calcium sulfate:1, so the D50 of magnesium hydroxide products can be controlled
It is the level close to 0.5 micron.
The present invention provides a kind of method of use Preparation of Magnesium Hydroxide Using Magnesium Oxide in second aspect, and its feature exists
In methods described comprises the steps：
(1) raw materials of magnesium oxide described in first aspect present invention is obtained；
(2) raw materials of magnesium oxide is prepared into slurry using distilled water, in 45 DEG C to 55 DEG C of temperature with 400 to 500 revs/min
Speed stir 6 to 7 hours so that magnesium oxide and distilled water reaction, then filter liquid, be obtained rough magnesium hydroxide；
(3) rough magnesium hydroxide is less than into 1 weight % in 45 DEG C to 55 DEG C dryings to water content, is obtained and is dried hydroxide
Magnesium；With
(4) sieved to being dried magnesium hydroxide using the mesh screen with the mesh that aperture is less than 200 microns, screened out thick
Granule, so as to magnesium hydroxide is obtained；
Wherein, 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.
In a second aspect of the present invention, if the temperature of step (2) is too high, it is impossible to obtain the chlorination of low particle diameter
Magnesium, if temperature is too low, mixing time can take long.In some embodiments, step (2) and/or step (3)
Temperature is 50 DEG C.Some preferred embodiment in, step (2) is identical with the temperature of step (3).It may further be preferable that
Temperature in step (2) and step (3) is 50 DEG C.
In a second aspect of the present invention, the inventors discovered that the particle diameter of most granules of barium sulfate precipitate is both greater than
200 microns, therefore, it is suggested that selecting to be screened out using the barium sulfate by the overwhelming majority that mesh aperture is no more than 200 microns.One
It is a little preferred embodiment in, the mesh screen in step (4) has the mesh of 100 micron pore sizes, if can be by gained hydroxide
The residue on sieve mass fraction (75 microns of testing sieves) of magnesium products is controlled below 0.02 mass %, so as to reach Grade A hydroxide
The requirement of magnesium.
In a second aspect of the present invention, if mixing speed is less than 400 revs/min, aquation is tailed over than too low
Thing is excessive.In some embodiments, the mixing speed in step (2) is 400 revs/min.
In a second aspect of the present invention, the present invention is not particularly limited to mixing time, as long as material can be made abundant
Mix and magnesium oxide and distilled water is fully reacted.In some embodiments, the mixing time in step (2) is 6
To 7 hours, such as 6.5 hours.
In some preferred embodiments of a second aspect of the present invention, the temperature in step (2) and (3) is 50
℃；Mixing speed is 400 revs/min；Mixing time is 6.5 hours；It is 100 microns that mesh screen in step (4) has aperture
Mesh；The envelope-bulk to weight ratio of the distilled water and the magnesium oxide is 15：1；Wherein, barium chloride is with the mol ratio of calcium sulfate
2.3:1。
The present invention additionally provides the method by described in first aspect present invention and the raw materials of magnesium oxide is obtained in the third aspect
Preparing the application in low particle diameter magnesium hydroxide.
Hereafter the present invention will be further detailed by way of embodiment.
Embodiment 1
Using by obtained in bischofite, after testing calcium sulphate content is the magnesium oxide of 0.61 mass %.According to shown in table 1
Ratio by magnesium oxide and distilled water and barium chloride (using without barium chloride as control) addition is positioned in 50 DEG C of water-baths
Reactor in, stirred 6 hours with 400 revs/min of speed, liquid is filtered by sucking filtration, rough magnesium hydroxide is obtained.Then
50 DEG C of dryings to constant weight (water content is less than 1 weight %), it is obtained and is dried magnesium hydroxide, is screened out using 100 micron mesh screens
Residue on sieve, obtains final magnesium hydroxide products, and (is issued within 04 13rd, 2007,2007 according to HG/T 3607-2007
On October 01, implements) described in method measurement D50.As a result in being displayed in table 1 below and Fig. 1.
Table 1
| Barium chloride：The molar ratio of calcium sulfate | D50 (micron) |
| 1 | 12.0 |
| 2 | 1.4 |
| 3 | 1.3 |
| 4 | 1.6 |
| 5 | 2.5 |
| 6 | 2.7 |
| 7 | 3.0 |
| 8 | 3.8 |
Can be seen that when appropriate barium chloride is added from table 1 and Fig. 1, can be in the situation without any post processing
It is lower to obtain the much lower magnesium hydroxide products of particle diameter (D50 of control is 18.75 microns).When barium chloride and the mol ratio of barium sulfate
For 2:1 to 4:When 1, without any post processing, D50 can be basically reached or connect the magnesium hydroxide products of the gained of embodiment 1
The standard of the I class products that nearly HG/T 3607-2007 specify.But, if add excessive barium chloride, D50 increases on the contrary,
Wherein reason is temporarily failed to understand, it may be possible to because chloride ion or barium ionss cause unforeseeable agglutination.
Embodiment 2
In addition to content shown in table 2 below, to carry out embodiment 2 with embodiment identical method.
Table 2
| Barium chloride：The molar ratio of calcium sulfate | D50 (micron) |
| 2.0 | 1.41 |
| 2.1 | 1 |
| 2.2 | 0.82 |
| 2.3 | 0.51 |
| 2.4 | 0.53 |
| 2.5 | 0.57 |
| 2.6 | 0.61 |
| 2.7 | 0.69 |
| 2.8 | 0.78 |
| 2.9 | 0.88 |
| 3.0 | 1.32 |
| 3.1 | 1.34 |
| 3.2 | 1.33 |
| 3.3 | 1.35 |
| 3.4 | 1.46 |
| 3.5 | 1.47 |
| 3.6 | 1.42 |
| 3.7 | 1.38 |
| 3.8 | 1.52 |
| 3.9 | 1.58 |
| 4.0 | 1.6 |
From the result of Fig. 2 and Biao 2 and combine the result of Fig. 1 and can be seen that the mol ratio of barium chloride in FIG and calcium sulfate
For 2:1 to 4:1 planar section, is 2.3 in the mol ratio：1 to 2.9:There is one " dell " unexpectedly between 1, in this area
Between D50 can be stably 0.5 to 1.0 micron, the less magnesium hydroxide of particle diameter can be obtained using the interval mol ratio and produced
Product.
Embodiment 3
In addition to the content described in table 3 below, embodiment 3 is carried out by the way of same as Example 1.As a result referring under
Table 3.
Table 3
Note：
(1) not over 75 micron mesh when * residue on sieves mass fraction refers to be sieved using 75 microns of testing sieves
Material account for the mass percent of whole material.
(2) residue on sieve mass fraction and D50 (are issued, 2007 10 on 04 13rd, 2007 using HG/T 3607-2007
Month 01 day implement) method of industry standard defined carries out, the wherein mark of residue on sieve mass fraction II classes Grade A and certified products
Standard is respectively less than or equal to 0.02% and less than or equal to 0.05%；The standard difference of Group III Grade A and certified products
It is less than or equal to 0.5 and less than or equal to 1.0.D50I class standards are 0.5 to 1.5 micron.
(3) measuring method of aquation ratio is as follows：The magnesium hydroxide products of the 5g through sieving are weighed with one thousandth balance
Calcine at 600 DEG C 30 minutes, then aquation ratio is calculated according to equation below：Matter after (quality after quality-calcining before calcining)/calcining
Amount * magnesium oxide molal weights/water molal weight * 100%.
From the results shown in Table 3,10 are adopted:More than 1 liquid-solid ratio and more than 400 revs/min of mixing speed are
Higher aquation ratio can be obtained.
Embodiment 4
2000g magnesite is taken, 2h (burn tinctuer is 48.5%) is calcined at 1000 DEG C in calcining furnace, calcining and decomposing is reclaimed and is gone out
Carbon dioxide；Light-burned Ore after by calcining is ground into the powder of 300 mesh；Water is added in powder and is stirred, prepared
Into the slurry that mass fraction is 35%.Prepare 25% ammonium chloride solution；The slurry is pressed into 1 with the ammonium chloride solution:1
Volume ratio is reacted 3 hours in enamel still at 110 DEG C, ammonia, magnesium chloride and the calcium chloride generated in course of reaction, reclaims ammonia
And it is condensed into ammonia；The carbon dioxide of recovery, ammonia and calcium chloride generation Calcium Carbonate is reacted in stainless steel cauldron with by its
Removing carbon, gained ammonia and magnesium chloride solution so as to obtain magnesium chloride solution, stirred in reactor and react 1 at 85 DEG C
Hour, ammonia volume more than 20 moles of %, then using 85 DEG C of hot water original position countercurrent washing 5 times, by gained solid material at 120 DEG C
Lower drying 5 hours, then calcines 2h at 600 DEG C, obtains crude oxidation magnesium, and the calcium sulphate content of detection gained magnesium oxide is
0.85 mass %, and with 2.3:1 barium chloride and the mol ratio of calcium sulfate add barium chloride to crude oxidation magnesium, are obtained for making
The raw materials of magnesium oxide of standby magnesium hydroxide.
Magnesium hydroxide is prepared according to the parameter shown in the identical method table 4 below of embodiment 3 using the raw materials of magnesium oxide,
And according to the corresponding performance indications of method measurement measurement shown in embodiment 3, as a result referring to table 4 below.
Table 4
From the results shown in Table 4, it is similar with the result of embodiment 3, passed through by magnesite using the method for the present invention
Magnesium oxide equally can with high aquation than be obtained low particle diameter high-quality magnesium hydroxide products.
Claims (10)
1. a kind of use low-grade magnesite prepares the method for producing the raw materials of magnesium oxide of magnesium hydroxide, it is characterised in that
Methods described comprises the steps：
(1) magnesite is calcined 2 hours under 1000 DEG C of calcining heat, obtains light-burned Ore and reclaim in calcination process to produce
Carbon dioxide；
(2) the light-burned Ore is ground into into the powder of 300 mesh and is configured to the slurry that mass fraction is 35%；
(3) by the ammonium chloride solution of the slurry and 25 mass % with 1:1 volume ratio mixes and reacts 3 hours, reaction of formation
Slurry and ammonia, the condensed recovery of ammonia obtains ammonia, and reaction paste obtains the first filtrate by filtering；
(4) carbon dioxide reaction that reclaimed the ammonia obtained by the filtrate of gained first and step (3) with step (1) is simultaneously filtered,
Obtain the second filtrate；
(5) ammonia obtained by the second filtrate of gained step (3) excessive with 20 moles of % is reacted into 1 hour at 85 DEG C, then
Reactant is filtered, solid material is obtained；
(6) using solid material described in 85 DEG C of hot wash, then in 120 DEG C of dryings 5 hours, crude oxidation magnesium is obtained；
(7) calcium sulphate content of magnesium oxide is detected, and with 2:1 to 3:1 barium chloride adds thereto with the mol ratio of calcium sulfate
Plus barium chloride, obtain the raw materials of magnesium oxide for producing magnesium hydroxide.
2. method according to claim 1, it is characterised in that barium chloride is 2.2 with the mol ratio of calcium sulfate:1 to 2.9:
1。
3. method according to claim 2, it is characterised in that barium chloride is 2.3 with the mol ratio of calcium sulfate:1.
4. a kind of method of use Preparation of Magnesium Hydroxide Using Magnesium Oxide, it is characterised in that methods described comprises the steps：
(1) raw materials of magnesium oxide described in claim 1 is obtained；
(2) raw materials of magnesium oxide is prepared into slurry using distilled water, in 45 DEG C to 55 DEG C of temperature with 400 to 500 revs/min of speed
Degree stirring 6 to 7 hours, so that magnesium oxide and distilled water reaction, then filter liquid, is obtained rough magnesium hydroxide；
(3) rough magnesium hydroxide is less than into 1 weight % in 45 DEG C to 55 DEG C dryings to water content, is obtained and is dried magnesium hydroxide；With
(4) 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 as to magnesium hydroxide is obtained；
Wherein, 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.
5. method according to claim 4, it is characterised in that the temperature of step (2) and/or step (3) is 50 DEG C.
6. method according to claim 4, it is characterised in that the mesh screen in step (4) has the net of 100 micron pore sizes
Hole.
7. method according to claim 4, it is characterised in that the mixing speed in step (2) is 400 revs/min.
8. method according to claim 4, it is characterised in that the mixing time in step (2) is 6.5 hours.
9. method according to claim 4, it is characterised in that the temperature in step (2) and (3) is 50 DEG C；Mixing speed
For 400 revs/min；Mixing time is 6.5 hours；Mesh screen in step (4) has the mesh that aperture is 100 microns；The steaming
The envelope-bulk to weight ratio of distilled water and the magnesium oxide is 15：1；Wherein, barium chloride and the mol ratio of calcium sulfate are 2.3:1.
10. application of the raw materials of magnesium oxide in low particle diameter magnesium hydroxide is prepared is obtained by the method described in claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610261182.7A CN105924023B (en) | 2016-04-25 | 2016-04-25 | Preparation method for magnesium oxide raw material and magnesium hydroxide with low particle size by using low-grade magnesite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610261182.7A CN105924023B (en) | 2016-04-25 | 2016-04-25 | Preparation method for magnesium oxide raw material and magnesium hydroxide with low particle size by using low-grade magnesite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105924023A CN105924023A (en) | 2016-09-07 |
| CN105924023B true CN105924023B (en) | 2017-05-03 |
Family
ID=56837110
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610261182.7A Active CN105924023B (en) | 2016-04-25 | 2016-04-25 | Preparation method for magnesium oxide raw material and magnesium hydroxide with low particle size by using low-grade magnesite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105924023B (en) |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1059711A (en) * | 1996-08-12 | 1998-03-03 | Daicel Amiboshi Sangyo Kk | Magnesium hydroxide and production of aqueous liquid suspension thereof |
| GB0812714D0 (en) * | 2008-07-10 | 2008-08-20 | Imerys Minerals Ltd | Magnesium hydroxide |
| CN103011630B (en) * | 2012-12-26 | 2015-09-09 | 新疆蓝天镁业股份有限公司 | Low-grade magnesite produces high purity magnesium hydroxide and method of magnesium oxide |
-
2016
- 2016-04-25 CN CN201610261182.7A patent/CN105924023B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105924023A (en) | 2016-09-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102502720B (en) | Process for producing battery-grade lithium carbonate through processing carbonate type lithium concentrate by deep carbonation method | |
| CN104532339B (en) | A kind of method that calcium sulfate crystal whiskers are prepared using low grade natural gypsum or gypsum mine | |
| TW201228937A (en) | Production of high purity precipitated calcium carbonate | |
| US3306700A (en) | Method of lithium recovery | |
| CN110078390A (en) | A kind of preparation method of high-purity high-quality calcium oxide and calcium hydroxide powder | |
| CA2939418C (en) | Process for producing high grade hydromagnesite and magnesium oxide | |
| EA010106B1 (en) | Process for complete utilization of olivine constituents | |
| CN101844815A (en) | Method for producing iron oxide red pigments by using calcium mineral salt as neutralizer for two-step oxidation | |
| CN112714751B (en) | Active high-purity magnesium oxide and production method thereof | |
| CN1228247C (en) | Process for producing super fine barium sulfate and calcium carbonate using chloralkali salt mud | |
| CN102703982A (en) | Method for preparing magnesium carbonate trihydrate crystal whisker by utilizing serpentine | |
| CN110606982B (en) | Basic magnesium borate/magnesium hydroxide composite flame retardant and preparation method thereof | |
| CN105776258B (en) | A kind of method using Preparation of Magnesium Hydroxide Using Magnesium Oxide | |
| CN106629806A (en) | Method for producing dihydrate gypsum from waste liquid in laterite nickel ore wet process | |
| CN105924023B (en) | Preparation method for magnesium oxide raw material and magnesium hydroxide with low particle size by using low-grade magnesite | |
| CN104556158B (en) | A kind of method for preparing calcium sulfate crystal whiskers and magnesium sulfate | |
| US3029133A (en) | Method of producing strontium carbonate and strontium sulfate from brines containing calcium and strontium halides | |
| CN113716588B (en) | Low-cost preparation method of magnesium-aluminum hydrotalcite | |
| US3080215A (en) | Production of mg(oh)2 | |
| CN102115813B (en) | Comprehensive utilization method for low-grade magnesite | |
| US4078043A (en) | Process for preparing calcium fluoride from hexafluoro silicic acid and production of silicic acid gel or active silicic acid from said calcium fluoride | |
| US3294485A (en) | Process for producing magnesium hydroxide and a noncontaminated effluent solution | |
| US3007776A (en) | Production of mg(oh) | |
| KR101908297B1 (en) | Preparation process of incombustible magnesium hydroxide from bitterns | |
| CN105084376A (en) | Method for recycling alkali generated when calcium silicate is prepared from low-modulus water glass |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20191204 Address after: No.17, yingnaili, Dashiqiao, Yingkou, Liaoning Province 41-03-6 Patentee after: Yao Shengduo Address before: Water Economic Development Zone South Village 115100 Liaoning city of Yingkou Province Patentee before: LIAONING HAOMEI TECHNOLOGY CO., LTD. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200820 Address after: 41-11-2, No. 17, yingnaili, Dashiqiao City, Yingkou City, Liaoning Province, 115100 Patentee after: Liu Xin Address before: No.17, yingnaili, Dashiqiao, Yingkou, Liaoning Province 41-03-6 Patentee before: Yao Shengduo |
|
| TR01 | Transfer of patent right | ||
| PP01 | Preservation of patent right |
Effective date of registration: 20201113 Granted publication date: 20170503 |
|
| PP01 | Preservation of patent right |