CN108383145A - A kind of preparation method of ultrafine aluminium hydroxide and its by-product sodium nitrate - Google Patents
A kind of preparation method of ultrafine aluminium hydroxide and its by-product sodium nitrate Download PDFInfo
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- CN108383145A CN108383145A CN201810469581.1A CN201810469581A CN108383145A CN 108383145 A CN108383145 A CN 108383145A CN 201810469581 A CN201810469581 A CN 201810469581A CN 108383145 A CN108383145 A CN 108383145A
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- aluminium hydroxide
- sodium nitrate
- preparation
- product sodium
- hydroxide
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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
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/04—Preparation with liquid nitric acid
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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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
- Geology (AREA)
- Agronomy & Crop Science (AREA)
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses the preparation methods of a kind of ultrafine aluminium hydroxide and its by-product sodium nitrate.Aluminium hydroxide is generated by the way that salpeter solution is added dropwise in aluminium hydroxide weight solution, the slurry of reaction prepares the aluminium hydroxide micro powder of different-grain diameter after suction filtration, washing, drying, and mother liquor obtains by-product sodium nitrate through evaporative crystallization.The present invention is using nitric acid, sodium hydroxide, low-quality aluminium as raw material, by way of acid-base neutralization, controls the conditions such as different speeds of agitator, and the by-product of the well dispersed uniform aluminum hydroxide product and high value of size distribution can be made, reduce production cost.
Description
Technical field
The present invention relates to the preparation methods of a kind of ultrafine aluminium hydroxide and its byproduct sodium nitrate, for electric wire, electricity
The flame-retardant additive of sub- wiring board etc., belongs to technical field of fine.
Background technology
Aluminium hydroxide is current dosage maximum and most widely used inorganic fire-retarded additive.Aluminium hydroxide as fire retardant not
It is only capable of fire-retardant, stability is good, toxic gas is not generated under high temperature, while product price is cheap, derived from a wealth of sources, therefore obtains extensive
Using.
Physics and chemical property are stablized under ultrafine aluminium hydroxide room temperature, and when burning not will produce secondary pollution, and whiteness is high, tool
There is excellent chromaticity index, the good dispersion in resin, even if additive amount is more to be not easy to the blushing that bends.In addition,
Abundance, price is cheaper than bromide fire retardant very much, therefore aluminium hydroxide has become the master of synthetic material halogen-free flameproof formula
Want one of selection.Currently, higher and higher to the performance requirement of fire retardant both at home and abroad, world fire retardant market high fire-retardance, low is complied with
Smog, innoxious development trend develop ultrafine aluminium hydroxide fire retardant and have a vast market application prospect.
The preparation of electric wire and electronic circuit board ultrafine aluminium hydroxide is a uniqueness but very effective technology, tool
There are very important theoretical research value and industrial utility value.But ultrafine aluminium hydroxide due to its it is cheap and be worth have
Limit, manufacturing cost is high, affects the economic benefit of enterprise.
Invention content
The preparation method of the present invention, a kind of by-product of high value is generated in preparation process, reduces aluminium hydroxide
Manufacturing cost, while its market value also can be improved.
The object of the present invention is to provide the preparation methods of a kind of ultrafine aluminium hydroxide and its by-product sodium nitrate.By in hydrogen
Salpeter solution is added dropwise in aluminium oxide weight solution and generates aluminium hydroxide, the slurry of reaction is prepared not after suction filtration, washing, drying
With the aluminium hydroxide micro powder of grain size, mother liquor obtains by-product sodium nitrate through evaporative crystallization.Steps are as follows for specific method：
1) by sodium hydroxide lye heating water bath；
2 are added to low-quality aluminium (D50=50~60 μm) in sodium hydroxide lye, and it is molten that weight is stirred under water bath condition；
3) it is Al to filter and obtain alumina content2O3=220~260g/L, Crater corrosion are the hydroxide of k=1.4~1.6 α
Aluminium weight solution；
4) the aluminium hydroxide weight solution for obtaining step 3) water-bath under the conditions of 65 DEG C~85 DEG C；
5) salpeter solution is added dropwise, is reacted under agitation；
6) reaction solution of step 5) filtered, washed, the aluminum hydroxide filter cake drying after separation is broken up to obtain ultra-fine
Aluminium hydroxide；
7) filtrate of step 6) is evaporated crystallization and obtains by-product sodium nitrate.
A concentration of the 30% of the step 1) sodium hydroxide lye；
Bath temperature described in step 2) is 90 DEG C；It is 3 hours to stir the weight molten time；
The quality g ratios of the sodium hydroxide lye volume ml and low-quality aluminium (D50=50~60 μm) are：2:0.95~
1.05。
A concentration of 65%-68% of the step 5) nitric acid；The molar ratio of solution and salpeter solution is aluminium hydroxide again：1:
1~2；Mixing speed is 400-800r/min, preferably 800r/min；Reaction time is 2-8 hours, preferably 6 hours, anti-after reaction
It is 9~11 to answer the pH value of liquid；
The meso-position radius of the step 6) ultrafine aluminium hydroxide is 1.4~2.0 μm.
Advantageous effect：Using nitric acid, sodium hydroxide, low-quality aluminium as raw material, by way of acid-base neutralization, control is different
The conditions such as speed of agitator, the by-product of the well dispersed uniform aluminum hydroxide product and high value of size distribution can be made, drop
Low production cost.
Specific embodiment
Following embodiment is that the present invention is explained further, and is the preferable embodiment of the present invention, but the reality of the present invention
It applies mode and is not limited by the following examples.
Embodiment 1
The sodium hydroxide lye of 100ml30% is added to heating water bath in reactor, weighs the low-quality aluminium (D50=50 of 50g
~60 μm) it is added in reactor, weight is stirred under 90 DEG C of water bath conditions molten about 3 hours, suction filtration obtains oxygen aluminium content and is
Al2O3=239.56g/L, the aluminium hydroxide weight solution that Crater corrosion is α k=1.45.
4.70mol aluminium hydroxides weight solution is taken to be placed in reactor, bath temperature is set in 65 DEG C, weighs
In the nitric acid dropping to reactor of 4.70mol65%, stirs 6 hours under 800r/min rotating speeds, later take out reaction solution
Filter washing, the aluminum hydroxide filter cake after separation, which is dried, breaks up to obtain ultrafine aluminium hydroxide 32.61g, yield 89%, after testing
D50=1.5 μm, 5% decomposition temperature is 256.9 DEG C, and filtrate is evaporated crystallization and obtains by-product sodium nitrate 36.35g, and master contains
Amount reaches 95.64%.
Embodiment 2
The sodium hydroxide lye of 100ml30% is added to heating water bath in reactor, weighs the low-quality aluminium (D50=50 of 49g
~60 μm) it is added in reactor, weight is stirred under 90 DEG C of water bath conditions molten about 3 hours, suction filtration obtains oxygen aluminium content and is
Al2O3=231.54g/L, the aluminium hydroxide weight solution that Crater corrosion is α k=1.50.
4.54mol aluminium hydroxides weight solution is taken to be placed in reactor, bath temperature is set in 65 DEG C, weighs 6.81mol nitre
Acid is added drop-wise in reactor, is stirred 2 hours under 600r/min rotating speeds, reaction solution is carried out filtering and washing later, after separation
Aluminum hydroxide filter cake, which is dried, breaks up to obtain ultrafine aluminium hydroxide 30.45g, yield 86%, D50=1.78 μm after testing, 5%
Decomposition temperature is 255.5 DEG C, and filtrate is evaporated crystallization and obtains by-product sodium nitrate 56.12g, and main content reaches 95.12%.
Embodiment 3
The sodium hydroxide lye of 100ml30% is added to heating water bath in reactor, weighs the low-quality aluminium (D50=of 47.5g
50~60 μm) it is added in reactor, weight is stirred under 90 DEG C of water bath conditions molten about 3 hours, suction filtration obtains oxygen aluminium content and is
Al2O3=223.97g/L, the aluminium hydroxide weight solution that Crater corrosion is α k=1.58.
4.39mol aluminium hydroxides weight solution is taken to be placed in reactor, bath temperature is set in 65 DEG C, weighs 5.27mol nitre
Acid is added drop-wise in reactor, is stirred 4 hours under 400r/min rotating speeds, reaction solution is carried out filtering and washing later, after separation
Aluminum hydroxide filter cake, which is dried, breaks up to obtain ultrafine aluminium hydroxide 29.11g, yield 85%, D50=1.9 μm after testing, 5%
Decomposition temperature is 251.2 DEG C, and filtrate is evaporated crystallization and obtains by-product sodium nitrate 44.72g, and main content reaches 94.65%.
Embodiment 4
The sodium hydroxide lye of 100ml30% is added to heating water bath in reactor, weighs the low-quality aluminium (D50=50 of 48g
~60 μm) it is added in reactor, weight is stirred under 90 DEG C of water bath conditions molten about 3 hours, suction filtration obtains oxygen aluminium content and is
Al2O3=230.88g/L, the aluminium hydroxide weight solution that Crater corrosion is α k=1.56.
4.53mol aluminium hydroxides weight solution is taken to be placed in reactor, bath temperature is set in 85 DEG C, weighs 7.70mol nitre
Acid is added drop-wise in reactor, is stirred 8 hours under 600r/min rotating speeds, reaction solution is carried out filtering and washing later, after separation
Aluminum hydroxide filter cake, which is dried, breaks up to obtain ultrafine aluminium hydroxide 29.31g, yield 83%, D50=1.82 μm after testing, 5%
Decomposition temperature is 254.9 DEG C, and filtrate is evaporated crystallization and obtains by-product sodium nitrate 36.56g, and main content reaches 94.32%.
Embodiment 5
The sodium hydroxide lye of 100ml30% is added to heating water bath in reactor, weighs the low-quality aluminium (D50=of 49.5g
50~60 μm) it is added in reactor, weight is stirred under 90 DEG C of water bath conditions molten about 3 hours, suction filtration obtains oxygen aluminium content and is
Al2O3=235.48g/L, the aluminium hydroxide weight solution that Crater corrosion is α k=1.52.
4.62mol aluminium hydroxides weight solution is taken to be placed in reactor, bath temperature is set in 85 DEG C, weighs 9.23mol nitre
Acid is added drop-wise in reactor, is stirred 6 hours under 600r/min rotating speeds, reaction solution is carried out filtering and washing later, after separation
Aluminum hydroxide filter cake, which is dried, breaks up to obtain ultrafine aluminium hydroxide 29.53g, yield 82%, D50=2.0 μm after testing, 5%
Decomposition temperature is 255.8 DEG C, and filtrate is evaporated crystallization and obtains by-product sodium nitrate 68.68, and main content reaches 94.20%.
Embodiment 6
The sodium hydroxide lye of 100ml30% is added to heating water bath in reactor, weighs the low-quality aluminium (D50=50 of 52g
~60 μm) it is added in reactor, weight is stirred under 90 DEG C of water bath conditions molten about 3 hours, suction filtration obtains oxygen aluminium content and is
Al2O3=240.75g/L, the aluminium hydroxide weight solution that Crater corrosion is α k=1.42.
4.72mol aluminium hydroxides weight solution is taken to be placed in reactor, bath temperature is set in 75 DEG C, weighs 4.72mol nitre
Acid is added drop-wise in reactor, is stirred 8 hours under 800r/min rotating speeds, reaction solution is carried out filtering and washing later, after separation
Aluminum hydroxide filter cake, which is dried, breaks up to obtain ultrafine aluminium hydroxide 32.03g, yield 87%, D50=1.40 μm after testing, 5%
Decomposition temperature is 253.5 DEG C, and filtrate is evaporated crystallization and obtains by-product sodium nitrate 38.12g, and main content reaches 92.58%.
Claims (9)
1. the preparation method of a kind of ultrafine aluminium hydroxide and its by-product sodium nitrate, which is characterized in that include the following steps：
1) by sodium hydroxide lye heating water bath；
2) the low-quality aluminium of D50=50~60 μm is added in sodium hydroxide lye, it is molten that weight is stirred under water bath condition；
3) it is Al to filter and obtain alumina content2O3=220~260g/L, Crater corrosion are the aluminium hydroxide weight of k=1.4~1.6 α
Solution；
4) the aluminium hydroxide weight solution for obtaining step 3) heating water bath under the conditions of 65 DEG C~85 DEG C；
5) salpeter solution is added drop-wise in aluminium hydroxide weight solution, is reacted under agitation；
6) reaction solution of step 5) filtered, washed, the aluminum hydroxide filter cake drying after separation breaks up to obtain ultra-fine hydrogen-oxygen
Change aluminium；
7) filtrate of step 6) is evaporated crystallization and obtains by-product sodium nitrate.
2. the preparation method of ultrafine aluminium hydroxide according to claim 1 and its by-product sodium nitrate, which is characterized in that step
A concentration of the 30% of rapid 1) the described aluminium hydroxide lye.
3. the preparation method of ultrafine aluminium hydroxide according to claim 1 and its by-product sodium nitrate, which is characterized in that step
The temperature of rapid 2) the described water-bath is 90 DEG C；It is 3 hours to stir the weight molten time.
4. the preparation method of ultrafine aluminium hydroxide according to claim 1 and its by-product sodium nitrate, which is characterized in that institute
The volume ml/ mass g ratios for stating sodium hydroxide lye and low-quality aluminium are：2:0.95~1.05.
5. the preparation method of ultrafine aluminium hydroxide according to claim 1 and its by-product sodium nitrate, which is characterized in that step
A concentration of 65%-68% of rapid 5) the described nitric acid.
6. the preparation method of ultrafine aluminium hydroxide according to claim 1 and its by-product sodium nitrate, which is characterized in that institute
Stating aluminium hydroxide, the molar ratio of solution and salpeter solution is again：1:1~2.
7. the preparation method of ultrafine aluminium hydroxide according to claim 1 and its by-product sodium nitrate, which is characterized in that step
The speed of rapid 5) the described stirring is 400~800r/min；Reaction time is 2-8 hour, after reaction the pH value of reaction solution for 9~
11。
8. the preparation method of ultrafine aluminium hydroxide according to claim 1 and its by-product sodium nitrate, which is characterized in that step
The speed of rapid 5) the described stirring is 800r/min；Reaction time is 6 hours.
9. special according to the preparation method of claim 1-8 any one of them ultrafine aluminium hydroxide and its by-product sodium nitrate
Sign is that the average grain diameter of the step 6) ultrafine aluminium hydroxide is 1.4~2.0 μm.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214013A (en) * | 2013-04-27 | 2013-07-24 | 昆明冶金研究院 | Preparation method of high-purity alumina powder |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214013A (en) * | 2013-04-27 | 2013-07-24 | 昆明冶金研究院 | Preparation method of high-purity alumina powder |
Non-Patent Citations (1)
| Title |
|---|
| 康文通等: ""钴钼废催化剂回收钼联产氢氧化铝和硝酸钠新工艺研究"", 《四川化工与腐蚀控制》 * |
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Application publication date: 20180810 |