CN102923740A - Boehmite and preparation method thereof - Google Patents
Boehmite and preparation method thereof Download PDFInfo
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- CN102923740A CN102923740A CN 201110225576 CN201110225576A CN102923740A CN 102923740 A CN102923740 A CN 102923740A CN 201110225576 CN201110225576 CN 201110225576 CN 201110225576 A CN201110225576 A CN 201110225576A CN 102923740 A CN102923740 A CN 102923740A
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Abstract
The subject of the invention is to provide boehmite with a high length-width ratio, boehmite which has excellent filling performance for objects to be filled and can fully inhibit anisotropy of the objects to be filled, or boehmite with a high specific surface area. In addition, the subject of the invention is to provide a method for preparing boehmite with good yield and high efficiency. The invention relates to acicular boehmite, and the preparation method is characterized by the following steps: allowing aluminium hydroxide, acetate, formate, propionate, sulfate or nitrate of magnesium, nickel, manganese or cobalt in a pressurized state in water, and performing hydro-thermal synthesis at a temperature of 180-250 DEG C so as to obtain the acicular boehmite with an average particle length of 1-10 microns and a length-width ratio of more than 30 and less than 90.
Description
[technical field]
The present invention relates to have boehmite of the various forms such as tabular, cubic, needle-like and preparation method thereof.
[background technology]
The chemical constitution of boehmite is by AlO (OH) or Al
2O
3.H
2O represents, thereby generally is the alumina monohydrate that alumina trihydrate is carried out the stable chemical performance that heat treated or hydrothermal treatment consists prepare in air.Boehmite have as be filled into the stiffener, fire retardant, glittering material, refractory materials, tackifier, the lubricant that are filled in the thing, be coated with the worker with interior filling chock, printing ink accept material, thermal conduction is controlled the purposes such as various weighting materials of using with gas shield with braking material with polar expansion.And boehmite has the purposes such as aluminum oxide precursor material (raw material) that various raw materials, oil suction material, water-absorption material, fingerprint collecting powder, the color developing used with fluorescent material with electronic component with strainer with separatory membrane with humidity sensor with pottery with the easy-sintering aluminum oxide as support of the catalyst, conductivity weighting material mother metal, refractory body material, heat-stable material, high-purity alpha-alumina strengthen material, have the various forms of tabular cubic needle-like.
At present knownly have multi-purpose boehmite and have various forms.For example, at present known boehmite (with reference to patent documentation 1) with tabular (laminar) and needle-like (O-fiber shape) form, have the hexagonal platy morphology that prolongs to crystallographic axis (a axle) direction of regulation boehmite (with reference to patent documentation 2), have the polygonal platy morphology take the Square consisting of two isosceles right-angled triangles shape as representative boehmite (with reference to patent documentation 3), have that spindle shape, needle-like, flakey, hexagonal are tabular, the boehmite (with reference to patent documentation 4) of four jiaos of (square) platy morphology etc.
[prior art document]
[patent documentation]
Patent documentation 1: Japanese Patent Publication JP 55-116622 communique
Patent documentation 2: Japanese Patent Publication JP 60-46923 communique
Patent documentation 3: Japanese Patent Publication Unexamined Patent 5-279019 communique
Patent documentation 4: Japanese Patent Publication Unexamined Patent 4-50105 communique
[summary of the invention]
[problem that invention will solve]
But, known boehmite in the past is used in the situation of such use, there are the problems such as low to the fillibility that is filled thing, as can't fully to suppress to be filled thing anisotropy or specific surface area are little.And also there are the problems such as the low and preparation time of yield is long in the preparation method of boehmite in the past.
In view of this, the boehmite that problem of the present invention is to provide a kind of long-width ratio high, can fully suppress to be filled the anisotropic boehmite of thing to the fillibility excellence that is filled thing, perhaps the higher boehmite of specific surface area.In addition, problem of the present invention is to provide a kind of yield good, prepares efficiently the method for boehmite.
[solving the scheme of problem]
For solving above-mentioned problem, the invention provides the needle-like boehmite, it is characterized in that: in water, make acetate, formate, propionic salt, vitriol or the nitrate of aluminium hydroxide and magnesium, nickel, manganese or cobalt be in pressurized state, thereby carrying out Hydrothermal Synthesis under 180～250 ℃ temperature obtains, form needle-like, mean particle length is 1～10 μ m, and long-width ratio surpasses 30 and be below 90.
The invention provides tabular boehmite, it is characterized in that: long-width ratio is 10～35, and specific surface area is 10～30m
2/ g.
The invention provides the preparation method of tabular boehmite, in water, make at least a alkaline earth metal compound and the aluminium hydroxide that are selected from calcium, strontium, the barium be in pressurized state, under 150～300 ℃ temperature, it is reacted, its resultant of reaction is carried out acid treatment, washing, remove the residual alkali earth metal compound.
The invention provides the tabular boehmite of hexagonal, it is characterized in that: form that roughly hexagonal is tabular, the long and short diameter ratio is 1～1.3, and long-width ratio is 40～100.
The invention provides the preparation method of the tabular boehmite of hexagonal, it is characterized in that: the sodium salt of aluminium hydroxide and boric acid or boric acid, calcium salt or ammonium salt are added at least a oxyhydroxide that is selected from sodium, potassium, barium, calcium and the strontium or aluminate as the pH adjusting agent, pH is adjusted under the state more than 8, under 130～250 ℃ temperature, carries out hydrothermal treatment consists.
The invention provides the preparation method of boehmite, it is characterized in that: the working pressure container heats in the aluminium hydrate powder under water vapor atmosphere, carries out the dry type maintenance.
The invention provides the cubic boehmite, it is characterized in that: major diameter is 1.3～3.5 μ m, slenderness ratio (major diameter/thickness) is 2.00～3.50, and long and short diameter is 1.68～1.37 than (major diameter/minor axis), and minor axis and Thickness Ratio (minor axis/thickness) are 1.42～2.55.
The invention provides the preparation method of needle-like boehmite, in water, make magnesium compound and aluminium hydroxide be in pressurized state, under 190～250 ℃ temperature, it is reacted.
The invention provides palpus shape metallic compound, thereby formate, acetate, propionic salt or the oxyhydroxide of magnesium, manganese, nickel or zinc is carried out the hydrothermal treatment consists preparation with at least a mixing the in aluminium hydroxide and the ironic hydroxide.
The invention provides the preparation method of palpus shape metallic compound, it is characterized in that: formate, acetate, propionic salt or oxyhydroxide and at least a mixing the in aluminium hydroxide and the ironic hydroxide of magnesium, manganese, nickel or zinc are carried out hydrothermal treatment consists.
The invention provides tabular boehmite, it is characterized in that: outside dimension is 2.5～15 μ m, and long-width ratio is 100～350.
The invention provides the preparation method of tabular boehmite, it is characterized in that: the polymkeric substance of aluminium hydroxide and (methyl) esters of acrylic acid is added at least a oxyhydroxide that is selected from sodium, potassium, barium, calcium and the strontium or aluminate as the pH adjusting agent, pH is adjusted under the state more than 8, under 130～250 ℃ of temperature, carries out hydrothermal treatment consists.
The invention provides discoid boehmite, it is characterized in that: outside dimension is 0.5～15 μ m, and long-width ratio is 10～100, contains at least a element that is selected from calcium, strontium, barium and the cerium.
The invention provides the preparation method of discoid boehmite, it is characterized in that: will be selected from organic acid salt, nitrate or vitriol (A), alkali metal hydroxide (B) and the alkaline earth metal hydroxides (C) of calcium, strontium, barium or cerium at least two kinds and under 130～300 ℃ temperature, carry out hydrothermal treatment consists with aluminium hydroxide.
The invention provides the tabular boehmite, it is characterized in that: insert organism, this organism is to have the C of hydroxy at least one end separately
3Any one insertion in above glycols, condensation glycols, the alkamine and the organism that forms.
[embodiment]
Below in conjunction with embodiment, further set forth the present invention.
(embodiment 1～embodiment 3)
Embodiment 1～embodiment 3 mixes following compounds ratio according to the rules, carries out Hydrothermal Synthesis in water is filled into autoclave.Hydrothermal Synthesis is to be heated to 205 ℃ by the heat-up rate according to 80 ℃/hour after leaving standstill, and keeps its temperature and pressure to carry out in 10 hours.After reaction finished, the naturally cooling reaction solution was collected resultant of reaction by filtering.Wash this resultant of reaction, under 105 ℃ temperature, make its drying, thereby had respectively the needle-like boehmite of claim 1,2 described characteristics.
Embodiment 1: sal epsom 23mol%, aluminium hydroxide 100mol%
Embodiment 2: nickel acetate 58mol%, aluminium hydroxide 100mol%
Embodiment 3: zinc acetate 58mol%, aluminium hydroxide 100mol%
(embodiment 4～embodiment 8)
Embodiment 4～embodiment 8 mixes following compounds ratio according to the rules, is filled in the autoclave with 5000g water, makes in the autoclave as pressurized state and leaves standstill mixed solution, is heated to 200 ℃ with 200 ℃/hour heat-up rates.This temperature is kept the mixed solution in the autoclave being reacted in 12 hours.Next, by with reacted mixed solution naturally cooling, filter this mixed solution and obtain resultant of reaction.This resultant of reaction is carried out after the acid treatment through washing moisture resultant of reaction being carried out drying under 105 ℃, obtain having the tabular boehmite of characteristic claimed in claim 3.
Except embodiment 4, all Heating temperature is made as 170 ℃.
Embodiment 4: hydrated barta eight hydrate 337g, aluminium hydroxide 1000g
Embodiment 5: hydrated barta eight hydrate 337g, aluminium hydroxide 1000g, sodium hydroxide 30g
Embodiment 6: calcium hydroxide 79g, aluminium hydroxide 1000g
Embodiment 7: calcium hydroxide 55g, calcium sulfate 44g, aluminium hydroxide 1000g
Embodiment 8: strontium hydroxide eight hydrate 283g, aluminium hydroxide 1000g
(embodiment 9～embodiment 10, comparative example 1)
Embodiment 9,10, comparative example 1 are that following compounds ratio is according to the rules mixed, and are filled in the autoclave and are 170 ℃ with the Temperature Setting in the autoclave with 39.0kg water.This temperature was kept 10 hours, leaving standstill the reaction raw materials that makes in the autoclave under spontaneous pressure reacts, resultant behind washing, filtration, the dry reaction, the tabular boehmite of hexagonal (except the comparative example 1) that obtains having characteristic claimed in claim 6.Comparative example 1 is that long-width ratio is 30 the tabular boehmite of hexagonal.
Embodiment 9: boric acid 2.5mol, sodium hydroxide (pH adjusting agent) 25mol, aluminium hydroxide (median size 0.5 μ m) 100mol
Embodiment 10: boric acid 2.0mol, sodium metaaluminate (NaAlO
2, the pH adjusting agent) 25mol, aluminium hydroxide (median size 2.5 μ m) 100mol
Comparative example 1: sodium hydroxide (pH adjusting agent) 25mol, aluminium hydroxide (median size 0.5 μ m) 100mol
(embodiment 11～13)
Embodiment 11～13rd, and the 1kg aluminium hydrate powders that following particle diameter is different are filled in the container, use autoclave under the water vapor atmosphere of state of saturation, heat under following temperature in 1～10 hour and carry out the dry type maintenance.Naturally place the cooling autoclave after the maintenance, under 130 ℃, make its drying, obtain tabular boehmite by the described method of claim 9～11.With prepare boehmite by the wet type maintenance and compare, the preparation time for preparing boehmite by the dry type maintenance is shorter.
In addition, the dry type maintenance means and does not add water but keep powdery to carry out maintenance in the aluminium hydroxide of starting raw material.In addition, the wet type maintenance is as the antonym of dry type maintenance, refers to add water in aluminium hydroxide and becomes pasty state (aqueous) and carry out maintenance.
Embodiment 11: the aluminium hydroxide of median size 0.8 μ m, 170 ℃
Embodiment 12: the aluminium hydroxide of median size 2 μ m, 170 ℃
Embodiment 13: the aluminium hydroxide of median size 0.8 μ m, 150 ℃
(embodiment 14)
Embodiment 14 is with after 300g water (the water ratio is 3) fully mixes with 100g aluminium hydroxide, put into autoclave, under spontaneous pressure (approximately 900kPa), after carrying out 12 hours hydrothermal treatment consists under 180 ℃, with resultant dewater, drying, the cubic boehmite that obtains having the described characteristic of claim 12.
(embodiment 15～embodiment 17)
Embodiment 15～embodiment 17 puts into autoclave with following compounds with water ratio according to the rules to mix.When this mixed solution is stirred with the revolution of 150rpm, be heated to 205 ℃ with 80 ℃/hour heat-up rates, keep this temperature and pressure that the mixed solution in the autoclave is reacted.Stop to stir, behind the naturally cooling reaction solution, collect resultant of reaction by filtering.Wash this resultant of reaction, under 105 ℃ temperature, make its drying, thereby obtain the needle-like boehmite of white by claim 14,15 described methods.According to this preparation method, can improve yield and prepare efficiently the needle-like boehmite.
In addition, embodiment 16 does not mix liquid and allows it leave standstill, and is heated to 215 ℃, keeps 10 hours.In addition, embodiment 17 is heated to 190 ℃.
Embodiment 15: magnesium acetate tetrahydrate 0.92kg, aluminium hydroxide 2.0kg, water 4.0kg
Embodiment 16: magnesium acetate tetrahydrate 0.69kg, calcium acetate 0.37kg, aluminium hydroxide 2.0kg, water 5.0kg
Embodiment 17: magnesium acetate tetrahydrate 0.92kg, aluminium hydroxide (median size 10 μ m) 2.0kg, water 4.0kg
(embodiment 18～embodiment 22)
Embodiment 18～embodiment 22 mixes following compounds ratio according to the rules under the temperature that is incorporated in 200 ℃ to carry out 48 hours hydrothermal treatment consists, obtains the described palpus of claim 16 shape boehmite (palpus shape metallic compound).In addition, this boehmite of sintering is 1 hour under 1000 ℃ temperature, obtains the described MgAl of claim 18
2O
3The mixture of (palpus shape composite oxide of metal) and aluminum oxide.
In addition, must the shape metallic compound be the resultant of reaction that generates when at least a and organic acid metal compound in aluminium hydroxide and the ironic hydroxide is carried out hydrothermal treatment consists, be called AlOOH (boehmite) or FeOOH with palpus shape form.
Embodiment 18: magnesium acetate 23.1mol, aluminium hydroxide (size of particles 1 μ m) 100mol
Embodiment 19: magnesium formiate 57.8mol, aluminium hydroxide (size of particles 1 μ m) 100mol
Embodiment 20: manganese acetate 23.1mol, aluminium hydroxide (size of particles 1 μ m) 100mol
Embodiment 21: propionic acid nickel 57.8mol, aluminium hydroxide (size of particles 1 μ m) 100mol
Embodiment 22: zinc acetate 23.1mol, aluminium hydroxide (size of particles 1 μ m) 100mol
(embodiment 23, comparative example 2)
Embodiment 23 and comparative example 2 are filled into autoclave in 39.0kg water following compounds ratio according to the rules and are 170 ℃ with the Temperature Setting in the autoclave.Kept this temperature 10 hours, leaving standstill the reaction raw materials that makes in the autoclave under spontaneous pressure reacts, resultant behind washing, filtration, the dry reaction, the tabular boehmite (except the comparative example 2) that obtains having the described characteristic of claim 20.Comparative example 2 is that long-width ratio is 50 tabular boehmite.
Embodiment 23: aluminium hydroxide (median size 0.5 μ m)) 100mol, acrylate copolymer (clear and polymer system; AE-710W) 50 % by weight, sodium hydroxide (pH adjusting agent) 25mol
Comparative example 2: aluminium hydroxide (median size 0.5 μ m) 100mol, ammonium phosphate 0.5 % by weight, aluminium hydroxide (pH adjusting agent) 25mol
(embodiment 24～embodiment 29)
Embodiment 24～embodiment 29 is filled into following compounds ratio according to the rules in the autoclave with 39.0kg water, is 170 ℃ with the Temperature Setting in the autoclave.Kept this temperature 10 hours, and under spontaneous pressure, left standstill the reaction raw materials that makes in the autoclave and react, the resultant behind washing, filtration, the dry reaction, the discoid boehmite that obtains having the described characteristic of claim 22.
Embodiment 24: calcium acetate 8.3mol, aluminium hydroxide (averaged particles footpath 3 μ m) 100mol, sodium hydroxide 4.2mol
Embodiment 25: calcium acetate 11.1mol, aluminium hydroxide (averaged particles footpath 3 μ m) 100mol, calcium hydroxide 7.8mol
Embodiment 26: sodium hydroxide 5.6mol, aluminium hydroxide (averaged particles footpath 3 μ m) 100mol, calcium hydroxide 11.1mol
Embodiment 27: strontium acetate 11.1mol, aluminium hydroxide (averaged particles footpath 3 μ m) 100mol, strontium hydroxide 3.3mol
Embodiment 28: nitrocalcite 11.1mol, aluminium hydroxide (averaged particles footpath 3 μ m) 100mol, sodium hydroxide 11.1mol, calcium hydroxide 1.6mol
Embodiment 29: calcium formiate 11.1mol, aluminium hydroxide (averaged particles footpath 3 μ m) 100mol, potassium hydroxide 5.6mol
(embodiment 30)
Embodiment 30 uses autoclave to carry out 20 hours heat treated under 200 ℃ of temperature in 64 milli mol aluminium hydroxides and 98.6 milli mol 1,2-PDs in the presence of 167 milli mol methane amides.Clean successively the test portion that obtains with distilled water and ethanol afterwards, drying is 2 hours in 120 ℃ airbath, thereby obtains inserting organic tabular boehmite with the described characteristic of claim 24.
Claims (25)
1. needle-like boehmite, it is characterized in that: in water, make acetate, formate, propionic salt, vitriol or the nitrate of aluminium hydroxide and magnesium, nickel, manganese or cobalt be in pressurized state, thereby carrying out Hydrothermal Synthesis under 180～250 ℃ temperature obtains, be needle-like, mean particle length is 1～10 μ m, and long-width ratio surpasses 30 and be below 90.
2. needle-like boehmite according to claim 1 is characterized in that: the blending ratio of the acetate of described magnesium, nickel, manganese or cobalt, formate, propionic salt, vitriol or nitrate and aluminium hydroxide is to carry out Hydrothermal Synthesis in 1: 0.5～1: 40 according to mol ratio.
3. tabular boehmite, it is characterized in that: long-width ratio is 10～35, specific surface area is 10～30m
2/ g.
4. preparation method who prepares tabular boehmite claimed in claim 3, it is characterized in that: in water, make at least a alkaline earth metal compound and the aluminium hydroxide that are selected from calcium, strontium, the barium be in pressurized state, under 150～300 ℃ temperature, it is reacted, its resultant of reaction is carried out acid treatment, washing, remove the residual alkali earth metal compound.
5. the preparation method of tabular boehmite according to claim 4, it is characterized in that: described alkaline earth metal compound is at least a compound that is selected from oxyhydroxide, oxide compound, muriate, vitriol and the organic acid salt.
6. tabular boehmite of hexagonal is characterized in that: form that roughly hexagonal is tabular, the long and short diameter ratio is 1～1.3, and long-width ratio is 40～100.
7. preparation method who prepares the tabular boehmite of hexagonal claimed in claim 6, it is characterized in that: to sodium salt, calcium salt or the ammonium salt of aluminium hydroxide and boric acid or boric acid, add at least a oxyhydroxide be selected from sodium, potassium, barium, calcium and the strontium or aluminate as the pH adjusting agent, pH is adjusted under the state more than 8, under 130～250 ℃ temperature, carries out hydrothermal treatment consists.
8. preparation method who prepares the tabular boehmite of hexagonal claimed in claim 6, it is characterized in that: to aluminium hydroxide and nitric acid, acetic acid, formic acid, propionic acid, sulfuric acid, vinylformic acid, methacrylic acid, polyacrylic acid or these sour sodium salts, calcium salt or ammonium salt, add at least a oxyhydroxide be selected from sodium, potassium, barium, calcium and the strontium or aluminate as the pH adjusting agent, pH is adjusted under the state more than 8, under 130～250 ℃ temperature, carries out hydrothermal treatment consists.
9. the preparation method of a boehmite, it is characterized in that: the working pressure container carries out the dry type maintenance when heating aluminium hydrate powder under water vapor atmosphere.
10. the preparation method of boehmite according to claim 9, it is characterized in that: the boehmite of preparation is tabular.
11. according to claim 9 or the preparation method of boehmite claimed in claim 10, it is characterized in that: Heating temperature is 140～300 ℃.
12. a cubic boehmite is characterized in that: major diameter is that 1.3～3.5 μ m, slenderness ratio (major diameter/thickness) are 2.00～3.50, long and short diameter is 1.68～1.37 than (major diameter/minor axis), minor axis and Thickness Ratio (minor axis/thickness) are 1.42～2.55.
13. preparation method who prepares the described cubic boehmite of claim 12, it is characterized in that: preseting water than the Na ion concentration that contains in the reaction filtrate after making the generation boehmite is 0.001～0.100 quality %, and aluminium hydroxide is carried out Hydrothermal Synthesis as raw material.
14. the preparation method of a needle-like boehmite is characterized in that: in water, make magnesium compound and aluminium hydroxide be in pressurized state, under 190～250 ℃ temperature, it is reacted.
15. the preparation method of needle-like boehmite according to claim 14 is characterized in that: described magnesium compound is at least a compound that is selected from magnesium acetate, magnesium hydroxide and the magnesium borate.
16. a palpus shape metallic compound is characterized in that: carry out hydrothermal treatment consists and prepare by at least a in formate, acetate, propionic salt or the oxyhydroxide of magnesium, manganese, nickel or zinc and aluminium hydroxide and the ironic hydroxide mixed.
17. a preparation method who prepares the described palpus of claim 16 shape metallic compound is characterized in that: formate, acetate, propionic salt or oxyhydroxide and at least a mixing the in aluminium hydroxide and the ironic hydroxide of magnesium, manganese, nickel or zinc are carried out hydrothermal treatment consists.
18. a palpus shape composite oxide of metal is characterized in that: represented with following structural (1), contain the spinel type structure,
AB
2-XC
XO
4…(1)
(in the formula, A represents magnesium, manganese, nickel or zinc atom, and B represents iron atom, and C represents the aluminium atom, and the scope of x is 0＜x≤2).
19. the preparation method of a palpus shape composite oxide of metal is characterized in that: sintering claim 16 must the shape metallic compound under 500～1600 ℃ temperature.
20. a tabular boehmite is characterized in that: outside dimension is 2.5～15 μ m, and long-width ratio is 100～350.
21. preparation method who prepares the described tabular boehmite of claim 20, it is characterized in that: to the polymkeric substance of aluminium hydroxide with (methyl) esters of acrylic acid, add at least a oxyhydroxide be selected from sodium, potassium, barium, calcium and the strontium or aluminate as the pH adjusting agent, pH is adjusted under the state more than 8, under 130～250 ℃ temperature, carries out hydrothermal treatment consists.
22. a discoid boehmite is characterized in that: outside dimension is 0.5～15 μ m, and long-width ratio is 10～100, contains at least a element that is selected from calcium, strontium, barium and the cerium.
23. a preparation method who prepares the described discoid boehmite of claim 22 is characterized in that: will be selected from organic acid salt, nitrate or vitriol (A), alkali metal hydroxide (B) and the alkaline earth metal hydroxides (C) of calcium, strontium, barium or cerium at least two kinds and under 130～300 ℃ temperature, carry out hydrothermal treatment consists with aluminium hydroxide.
24. a tabular boehmite is characterized in that: insert organism, this organism is to have the C of hydroxy at least one end separately
3Any one insertion of above glycols, condensation glycols, alkamine and the organism that forms.
25. a preparation method who prepares the described tabular boehmite of claim 24 is characterized in that: insert organism, this organism is to having C in aluminium hydroxide and at least one end separately in having the solvent of high-k
3Any one organism of heat-treating in the glycols of above hydroxy, condensation glycols, the alkamine.
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| CN113479919A (en) * | 2021-08-24 | 2021-10-08 | 安徽壹石通材料科技股份有限公司 | Low-conductivity boehmite and preparation method thereof |
| CN113955783A (en) * | 2021-11-25 | 2022-01-21 | 大连理工大学 | Method for controlling particle size of hydrothermal product of aluminum hydroxide |
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