CN106115748B - A kind of method of preparing super fine magnesium hydroxide by wet method slurry - Google Patents
A kind of method of preparing super fine magnesium hydroxide by wet method slurry Download PDFInfo
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- CN106115748B CN106115748B CN201610425063.0A CN201610425063A CN106115748B CN 106115748 B CN106115748 B CN 106115748B CN 201610425063 A CN201610425063 A CN 201610425063A CN 106115748 B CN106115748 B CN 106115748B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
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- 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
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- 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
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Abstract
A kind of method of preparing super fine magnesium hydroxide by wet method slurry, is comprised the steps of：For step 1. first by the efficient surfactant of 1 10 parts by weight, the grinding aid of 10 30 parts by weight adds the water of 70 700 parts by weight, stand-by after being uniformly dispersed；The magnesium hydroxide powder that step 2. weighs 50 150 parts by weight again is added in the stand-by solution of step 1, scattered to be prepared into magnesium magma to be ground；The abrasive media ball that step 3. adds 400 600 parts by weight in the magnesium magma to be ground of step 2 is ground, and is ground to the super fine magnesium hydroxide slurry of target grain size；Step 4. adds the stable composition auxiliary agent of 0.1 5 parts by weight into the super fine magnesium hydroxide slurry in step 3；The inventive method is advantageous to environmental protection, and production cost is low, and on the premise of higher solids content is constant, can improve the stability of magnesium hydroxide slurry.
Description
Technical field
The invention belongs to chemical products preparing technical field, more particularly to a kind of preparing super fine magnesium hydroxide by wet method slurry
Method.
Background technology
Magnesium hydroxide is because it has a high activity, high absorption capacity, and stronger shock-absorbing capacity is safe to use and corrosion-free
Many special performances such as property, nontoxic, its raw material rich reserves, is widely studied in nearly recent decades in addition.Magnesium hydroxide according to
Form and purposes are divided into filter cake shape, powdery and pulp-like three major types, and three can phase co-conversion.Magnesium hydroxide therein
Slurry production process flow is simple, safe operation, non-environmental-pollution and enjoy high praise.The preparation method of magnesium hydroxide slurry a few days ago
Mainly include magnesia aquation method, the bittern precipitation method, shepardite wet pulverizing method.
The present situation of magnesium hydroxide slurry, the U.S. and Japan are the use consumption big countries of magnesium hydroxide, and its application field is main
In terms of environmental protection.Because magnesium hydroxide can be widely applied to acid waste water neutralization, heavy metal removing, water process and cigarette
The developed country such as desulfurization etc., the particularly U.S., Japan quickly grows in road gas.
1st, shepardite is the industrial mineral that a kind of main component is magnesium hydroxide, be can be used as after ultra-fine grinding is processed low
Cigarette, nontoxic fire-retardant filler；Existing scientific and technical literature is recorded：Wet-type super-fine disintegrating experiment is carried out to shepardite using medium stirring mill
Room and commerical test research, have studied shadow of the factor such as grinding aid species and dosage, pulp density, rotor speed to product granularity
Ring.Shortcoming is to realize the refinement of magnesium hydroxide granularity as abrasive media using the zirconium oxide microballoons of costliness, so in difference
The cost of magnesium hydroxide preparation is added in degree.
2nd, Application No. 200410005164.x patent of invention discloses that a kind of wet method prepares shepardite or sintered magnesia surpasses
The method of fine powder, it is to add 10~80 weight with the raw material brucite powder or sintering oxidation magnesium powder of the mesh of 1000 weight finenesses >=100
Molecular weight be one kind in 1500~4500 polyacrylic acid or its salt, alkyl benzene sulphonate or its salt, polyether phosphate, 5~70
One kind in the aliphatic acid of weight or its salt, phosphate or its salt, the water of 600~2000 weight is in grinding machine, at 50~90 DEG C
1h is crushed, slurry has good mobility such as milk, do not condense, do not bond between particle, does not need to separate and convection drying produces
Powder product, 5 μm of average grain diameter ＜, there is hydrophobic performance to float in water.Very high crush efficiency, easy technological process and energy
The superfine product for obtaining high quality is the characteristics of this technology protrudes.Shortcoming is that used magnesia is to use more than 800 DEG C
Light-burned magnesium hydroxide.
3rd, the patent of invention of Application No. 200810300453.0 discloses a kind of sodium-hydroxide method and prepares high pure and ultra-fine hydrogen
The technique of magnesia, using decomposition of crystal seed method, purified brine is mixed with magnesium hydroxide crystal seed addition reaction tank, 60~80 DEG C
Insulation, then sodium hydroxide solution is added in reaction tank and carries out precipitation reaction, crystallization ageing, reaction extracts magnesium hydroxide after terminating
Slurry filtration, washing, filter cake produce magnesium hydroxide crystal product through drying, crushing.Shortcoming is to need the ageing of long period,
Operate complex, and caused filtrate does not reuse.
4th, the method that the patent of invention of Application No. 01127343.7 discloses One-step production magnesium hydroxide：It will contain
The bittern and ammoniacal liquor of magnesium chloride mix according to the ratio that the mol ratio of magnesium chloride and free ammonia is 1: 1.3-2.0, and make mixture
5-30 minutes are reacted in the environment of 45 degree -90 Celsius degree, reaction solution is consolidated after filtering, wash, dry, crush
Body magnesium hydroxide.Shortcoming is that this method uses ammoniacal liquor to participate in producing as alkali lye, pollution environment, output ammonium chloride discarded object, and
And the dispersive property of the product is poor, final products are needed by drying, pulverization process.
5th, the patent of invention of Application No. 200610146040.2 discloses a kind of shepardite wet method and prepares ultra-fine hydroxide
The method of magnesium powder：It is first existing that by brucite powder, for raw material, the ball milling 36 after 450 DEG C of -700 DEG C of calcinings, addition absolute ethyl alcohol+water is small
When, 120 DEG C of dryings, crushing prepare ultrafine magnesium hydroxide powder.Shortcoming is that this method uses absolute ethyl alcohol to participate in producing as solvent,
Potential safety hazard be present, and the process time of the product is longer, and final products are needed by drying, pulverization process.
In summary, there is an urgent need to a kind of operating procedure is easy, product is easily isolated, solid content is high and right for this area
Environment-friendly magnesium hydroxide slurries preparation method for material.
The content of the invention
It is an object of the invention to provide a kind of method of preparing super fine magnesium hydroxide by wet method slurry, and it is advantageous to environment guarantor
Shield, production cost is low, and on the premise of higher solids content is constant, can improve the stability of magnesium hydroxide slurry.
The technical scheme adopted by the invention to solve the technical problem is that：A kind of preparing super fine magnesium hydroxide by wet method slurry
Method, comprise the following steps：
The efficient surfactant of 1-10 parts by weight, the grinding aid of 10-30 parts by weight are first added 70-700 by step 1.
The water of parts by weight, it is stand-by after being uniformly dispersed；
The magnesium hydroxide powder that step 2. weighs 50-150 parts by weight again is added in the stand-by solution of step 1, scattered to be prepared into
Magnesium magma to be ground；
The abrasive media ball that step 3. adds 400-600 parts by weight in the magnesium magma to be ground of step 2 enters
Row grinding, it is ground to the super fine magnesium hydroxide slurry of target grain size；
Step 4. adds the stable composition auxiliary agent of 0.1-5 parts by weight into the super fine magnesium hydroxide slurry in step 3, and adjusts
Save the solid content of super fine magnesium hydroxide slurry.
Wherein, the particle size of magnesium hydroxide powder is 2.8-20 microns in step 2.
The fineness of magnesium hydroxide slurry is in step 3：Particle less than 2 microns accounts for whole particle volumes
80-100%, the particle less than 1 micron account for the 50-60% of whole particle volumes.
Described stable composition auxiliary agent includes anion surfactant and nonionic surfactant, wherein anion table
Face activating agent accounts for the 92-98% of stable composition auxiliary agent total amount, and nonionic surfactant accounts for the 2-8% of stable composition auxiliary agent total amount.
The anion surfactant be neopelex and polyacrylate in one kind, non-ionic surface
Activating agent be APES, anhydrous sodium metasilicate, sodium carboxymethylcellulose, poly-epoxy succinic acid and polyvinyl alcohol its
In one kind, two or more mixture.
Described efficient surfactant is sodium tripolyphosphate, calgon, polyacrylic acid sodium salt and polycarboxylate, its
In one kind, two or more mixture.
Described grinding aid is alcamine compound.
Described abrasive media is one kind in bead, ceramic bead, zirconium silicate pearl, and the specification of abrasive media is 0.1-
The combination of media of a kind of specification, two kinds of specifications or three kinds of specifications between 3.0mm mixture by a certain percentage.
The beneficial effects of the invention are as follows：
（1）By the 70-90 level magnesium hydroxide slurries for handling to obtain to magnesium hydroxide raw material wet pulverizing, it is starched the present invention
The solid content of material brings up to more than 50%, and on the premise of keeping its solid content constant, improves the stabilization of magnesium hydroxide slurry
Property；And preferable mobility can be kept in the case where placing 2-3 weeks, no lamination, meet the requirement of stability slurry.
（2）The magnesium hydroxide slurry prepared by the present invention has stronger shock-absorbing capacity, higher activity and energy of adsorption
Power, and there is non-settleability, non-coherency and preferable mobility, and be easy to pump and store, do not have corrosivity, without special
Anticorrosion equipment disposal, it is safe and nontoxic, harmless.
（3）Preparation method of the present invention is carried out in inorganic mineral wet grinding workshop, and equipment need not change, and simple to operate；
Abrasive media is cheap, and use cost is low, and grinding efficiency is high, and service wear is low.
（4）The super fine magnesium hydroxide slurry prepared using the present invention, wet processing mode reduce the dust of processing site
Pollution, be advantageous to environmental protection, save production cost, cost of transportation, increase the competitiveness of product in market.
Embodiment
Experimental raw：Magnesium hydroxide powder：Butt is by 100 parts of calculating；Efficient surfactant：Sodium tripolyphosphate, six inclined phosphorus
Sour sodium, polyacrylic acid sodium salt and polycarboxylate, solution is configured to, concentration 30-50%, molecular weight is between 1000-10000, folding
Dry relative dry hydrogen magnesia addition 10-20 ‰；Grinding aid：Alcamine compound, relative dry hydrogen magnesia of giving money as a gift add 10-
25‰；Abrasive media is bead, ceramic bead, zirconium silicate pearl.
The technical scheme of invention is further illustrated below by specific embodiment.
Embodiment 1
It is 2.8 microns of parts by weight of magnesium hydroxide powder 50 to select particle diameter, add be equipped with 1 parts by weight efficient surfactant,
15 parts by weight grinding aids, 70 parts by weight water lab scale grinder in carry out wet grinding；The parts by weight of abrasive media 400, use
1.0-3.0mm zirconium silicate pearl, real density 4g/cm2, charge ratio of media 2%；Wherein efficient surfactant is trimerization phosphorus
Acid sodium solution, grinding aid are monoethanolamine solution, and milling time is after 30 minutes, and the particle diameter of grinding product is measured by sampling, grinds
The 80-100% that the particle in obtained super fine magnesium hydroxide slurry less than 2 microns accounts for whole particle volumes is ground, less than 1 micron
Particle accounts for the 50-60% of whole particle volumes；Then the stable composition auxiliary agent of 5 parts by weight is added, dodecane in stable composition auxiliary agent
Base benzene sulfonic acid sodium salt accounts for 93%, and anhydrous sodium metasilicate accounts for 7%；The solid content for adjusting super fine magnesium hydroxide slurry is 55%, places two weeks
Existing lamination.
Embodiment 2
It is 5.0 microns of parts by weight of magnesium hydroxide powder 100 to select particle diameter, add be equipped with 5 parts by weight efficient surfactants,
15 parts by weight grinding aids, 100 parts by weight water lab scale grinder in carry out wet grinding；400 parts of abrasive media, using 1.0-
3.0mm ceramic bead, real density 4g/cm2, charge ratio of media 3%；Wherein efficient surfactant be sodium tripolyphosphate and
The mixed solution of polyacrylic acid sodium salt, grinding aid are the mixed solution of monoethanolamine and diethanol amine, and milling time is 90 minutes
Afterwards, the particle diameter of grinding product is measured by sampling, the particle in the super fine magnesium hydroxide slurry for grinding to obtain less than 2 microns accounts for whole
The 80-100% of plastochondria product, the particle less than 1 micron account for the 50-60% of whole particle volumes；Then the compound of 5 parts by weight is added
Stabilization aid, Sodium Polyacrylate accounts for 95% in compound stabilizer, and APES accounts for 2%, and polyvinyl alcohol accounts for 3%；Regulation is super
The solid content of thin magnesium hydroxide slurry is 52%, lamination occurs after placing two weeks.
Embodiment 3
Particle diameter is selected to add the efficient surfactant equipped with 10 parts by weight, 30 weight for 20 microns of magnesium hydroxide powder
Part grinding aid, 700 parts by weight water lab scale grinder in carry out wet grinding, 600 parts of abrasive media, using 1.0-3.0mm's
Zirconium silicate pearl, real density 4g/cm2, charge ratio of media 4%；Wherein efficient surfactant is calgon, polypropylene
The mixed solution of acid sodium-salt and polycarboxylate, grinding aid are triethanolamine solution, and milling time is that sampling and measuring is ground after 50 minutes
The particle diameter of product is ground, the particle in the super fine magnesium hydroxide slurry for grinding to obtain less than 2.0 microns accounts for the 80- of whole particle volumes
100%, the particle less than 1 micron accounts for the 50-60% of whole particle volumes；Then the stable composition auxiliary agent of 3 parts by weight is added, it is compound
Neopelex accounts for 98% in stabilization aid, and sodium carboxymethylcellulose accounts for 2%, adjusts super fine magnesium hydroxide slurry solid content
For 60%, two weeks are placed without lamination.
Embodiment 4
It is 120 parts of the magnesium hydroxide powder that median is 15 microns to select granularity, and addition is equipped with 10 parts by weight efficient surfaces
Activating agent, 15 parts by weight grinding aids, 300 parts by weight water lab scale grinder in carry out wet grinding, 400 parts of abrasive media, adopt
With 1.0-3.0mm bead, real density 4g/cm2, charge ratio of media 4%；Wherein efficient surfactant is six inclined phosphorus
The mixed solution of sour sodium, polyacrylic acid sodium salt and polycarboxylate, grinding aid are triethanolamine solution, and milling time is 70 minutes
Afterwards, the particle diameter of grinding product is measured by sampling, the particle in the super fine magnesium hydroxide slurry for grinding to obtain less than 2 microns accounts for whole
The 80-100% of particle volume, the particle less than 1 micron account for the 50-60% of whole particle volumes；Add the stable composition of 2 parts by weight
Auxiliary agent, neopelex accounts for 95% in stable composition auxiliary agent, and APES accounts for 5%；Adjust ultra-fine hydroxide
Magnesium slurry solid content is 62%, places three weeks and starts lamination occur.
Comparative example 1
Particle diameter is selected to be added for 15 microns of 120 parts of magnesium hydroxide powder equipped with 2 parts by weight stable composition auxiliary agents, 10 weight
Part efficient surfactant, 15 parts by weight grinding aids, 300 parts by weight water lab scale grinder in carry out wet grinding, grinding medium
400 parts of matter, using 1.0-3.0mm bead, real density 4g/cm2, charge ratio of media 4%；Wherein high effective surface active
Agent is the mixed solution of calgon, polyacrylic acid sodium salt and polycarboxylate, and grinding aid is triethanolamine solution, milling time
After 70 minutes, the particle diameter of grinding product is measured by sampling, less than 2.0 microns in the super fine magnesium hydroxide slurry for grinding to obtain
Particle accounts for the 80-100% of whole particle volumes, and the particle less than 1 micron accounts for the 50-60% of whole particle volumes, and stable composition helps
Neopelex accounts for 95% in agent, and APES accounts for 5%；Regulation super fine magnesium hydroxide slurry solid content be
30%, place 4 days and lamination occur.
Comparative example 2
It is 15 microns of parts by weight of magnesium hydroxide powder 120 to select particle diameter, is added equipped with 10 parts by weight efficient surfactants, 15
Parts by weight grinding aid, 300 parts by weight water lab scale grinder in carry out wet grinding, the parts by weight of abrasive media 400, using 1.0-
3.0mm bead, real density 4g/cm2, charge ratio of media 4%；Wherein efficient surfactant is calgon, gathered
The mixed solution of acrylic acid sodium salt and polycarboxylate, grinding aid are triethanolamine solution, and milling time is after 70 minutes, and sampling is surveyed
Determine the particle diameter of grinding product, the particle in the super fine magnesium hydroxide slurry for grinding to obtain less than 2.0 microns accounts for whole granules
Long-pending 80-100%, the particle less than 1 micron account for the 50-60% of whole particle volumes.Consolidating for super fine magnesium hydroxide slurry of regulation contains
Measure as 20%, lamination occurs after placing 2 days.
The present invention passes through a series of research, experiment, it was demonstrated that the super fine magnesium hydroxide slurry made from this method, its slurry
Solid content bring up to more than 50%, as solid content improves, the refinement of granularity, magnesium hydroxide slurry has magnesium hydroxide slurry
Stronger shock-absorbing capacity, activity significantly increase；Magnesium hydroxide slurry has non-settleability, non-coherency and preferably flowing
Property, and be easy to pump and store.By adding stable composition auxiliary agent in this preparation method, the stability indicator of its slurry meets surely
The requirement of qualitative slurry, without lamination after placing one week~tri- weeks, preparation method of the present invention is carried out in wet grinding workshop, wet
Method sand mill is simple to operate, and super fine magnesium hydroxide slurry reduces the dust pollution of processing site using wet processing mode, has
Beneficial to environmental protection, production cost, cost of transportation are saved, increases the competitiveness of product in market.
Claims (8)
- A kind of 1. method of preparing super fine magnesium hydroxide by wet method slurry, it is characterised in that comprise the following steps：The efficient surfactant of 1-10 parts by weight, the grinding aid of 10-30 parts by weight are first added 70-700 weight by step 1. The water of part, it is stand-by after being uniformly dispersed；The magnesium hydroxide powder that step 2. weighs 50-150 parts by weight again is added in the stand-by solution of step 1, and scattered be prepared into waits to grind Grind magnesium magma；The abrasive media ball that step 3. adds 400-600 parts by weight in the magnesium magma to be ground of step 2 is ground Mill, it is ground to the super fine magnesium hydroxide slurry of target grain size；Step 4. adds the stable composition auxiliary agent of 0.1-5 parts by weight into the super fine magnesium hydroxide slurry in step 3, and adjusts super The solid content of thin magnesium hydroxide slurry.
- 2. the method for preparing super fine magnesium hydroxide by wet method slurry according to claim 1, it is characterised in that：Hydrogen in step 2 The particle size of magnesia powder is 2.8-20 microns.
- 3. the method for preparing super fine magnesium hydroxide by wet method slurry according to claim 1, it is characterised in that：Hydrogen in step 3 The fineness of magnesia slurry is：Particle less than 2 microns accounts for the 80-100% of whole particle volumes, and the particle less than 1 micron accounts for entirely The 50-60% of portion's particle volume.
- 4. the method for preparing super fine magnesium hydroxide by wet method slurry according to claim 1, it is characterised in that：Described is compound Stabilization aid includes anion surfactant and nonionic surfactant, and wherein anion surfactant accounts for stable composition The 92-98% of auxiliary agent total amount, nonionic surfactant account for the 2-8% of stable composition auxiliary agent total amount.
- 5. the method for preparing super fine magnesium hydroxide by wet method slurry according to claim 4, it is characterised in that：The anion Surfactant is one kind in neopelex and polyacrylate, and nonionic surfactant is alkyl phenol polyoxy Vinethene, anhydrous sodium metasilicate, sodium carboxymethylcellulose, poly-epoxy succinic acid and polyvinyl alcohol one or more therein Mixture.
- 6. the method for preparing super fine magnesium hydroxide by wet method slurry according to claim 1, it is characterised in that：Described is efficient Surfactant is sodium tripolyphosphate, calgon, polyacrylic acid sodium salt and polycarboxylate, one or more therein Mixture.
- 7. the method for preparing super fine magnesium hydroxide by wet method slurry according to claim 1, it is characterised in that：Described grinding aid Agent is alcamine compound.
- 8. the method for preparing super fine magnesium hydroxide by wet method slurry according to claim 1, it is characterised in that：Described grinding Medium is bead, ceramic bead, one kind in zirconium silicate pearl, the specification of abrasive media be a kind of specification between 0.1-3.0mm, Two kinds of specifications or three kinds of specifications press the combination of media of predetermined ratio mixture.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108440995A (en) * | 2018-01-15 | 2018-08-24 | 大连亚泰科技新材料股份有限公司 | A kind of method that wet method prepares modified micro-nano flame retardant of magnesium hydroxide |
| CN111437973B (en) * | 2020-04-15 | 2022-03-29 | 山东格润德环保科技有限公司 | Grinding method and application of magnesium hydroxide suspension with uniform particle size distribution |
| CN111439766B (en) * | 2020-04-15 | 2022-08-09 | 山东格润德环保科技有限公司 | Method for preparing magnesium hydroxide suspension by hydrating magnesium oxide |
| CN111517800B (en) * | 2020-04-20 | 2022-04-01 | 中国科学院合肥物质科学研究院 | Method for preparing high-purity superfine zirconium boride powder by grinding aid auxiliary sanding |
| CN112588138A (en) * | 2020-11-18 | 2021-04-02 | 潍坊凯博镁盐有限公司 | Method for preparing high-stability magnesium hydroxide suspension |
| CN112403213B (en) * | 2020-11-25 | 2022-07-15 | 大连海事大学 | Magnesium hydroxide slurry and preparation method thereof |
| CN114213875B (en) * | 2021-12-24 | 2022-05-20 | 大连理工大学 | High-stability magnesium hydroxide suspension and preparation method thereof |
| CN114395274A (en) * | 2022-01-12 | 2022-04-26 | 江西广源化工有限责任公司 | Superfine modified magnesium hydroxide, preparation method and application thereof, and flame-retardant polyolefin cable material |
| CN115537040B (en) * | 2022-08-30 | 2023-09-15 | 江西广源化工有限责任公司 | Superfine magnesium hydroxide and preparation method and application thereof |
| CN116356605B (en) * | 2023-03-14 | 2024-04-02 | 江西广源化工有限责任公司 | Brucite flame-retardant slurry and preparation method and application thereof |
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