CN1735564A - Aluminum hydroxide and method for production thereof - Google Patents
Aluminum hydroxide and method for production thereof Download PDFInfo
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- CN1735564A CN1735564A CN 200380108317 CN200380108317A CN1735564A CN 1735564 A CN1735564 A CN 1735564A CN 200380108317 CN200380108317 CN 200380108317 CN 200380108317 A CN200380108317 A CN 200380108317A CN 1735564 A CN1735564 A CN 1735564A
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- aluminium hydroxide
- slurry
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- sodium aluminate
- aluminate solution
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- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 title claims abstract description 171
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 239000002002 slurry Substances 0.000 claims abstract description 118
- 238000000034 method Methods 0.000 claims abstract description 74
- 239000002245 particle Substances 0.000 claims abstract description 52
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 33
- 230000002776 aggregation Effects 0.000 claims abstract description 25
- 239000000945 filler Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 154
- 238000010438 heat treatment Methods 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 26
- 238000005054 agglomeration Methods 0.000 claims description 24
- 239000005060 rubber Substances 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229920001971 elastomer Polymers 0.000 claims description 6
- 239000004033 plastic Substances 0.000 claims description 6
- 229920003023 plastic Polymers 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 238000004131 Bayer process Methods 0.000 abstract 1
- 238000004220 aggregation Methods 0.000 abstract 1
- 230000003028 elevating effect Effects 0.000 abstract 1
- 230000005484 gravity Effects 0.000 abstract 1
- 229940024545 aluminum hydroxide Drugs 0.000 description 145
- 239000011347 resin Substances 0.000 description 35
- 229920005989 resin Polymers 0.000 description 34
- 239000007787 solid Substances 0.000 description 27
- 230000035939 shock Effects 0.000 description 25
- 238000012360 testing method Methods 0.000 description 23
- 239000000843 powder Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 16
- 238000001914 filtration Methods 0.000 description 14
- 239000008187 granular material Substances 0.000 description 10
- 238000012546 transfer Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 8
- 238000010298 pulverizing process Methods 0.000 description 7
- 238000000746 purification Methods 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- 230000006835 compression Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 230000007812 deficiency Effects 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 239000003063 flame retardant Substances 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 5
- 238000012216 screening Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000012423 maintenance Methods 0.000 description 4
- 230000002265 prevention Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000012756 surface treatment agent Substances 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- 229920001187 thermosetting polymer Polymers 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 238000004438 BET method Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 238000002050 diffraction method Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000005357 flat glass Substances 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229920006337 unsaturated polyester resin Polymers 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- XFBXDGLHUSUNMG-UHFFFAOYSA-N alumane;hydrate Chemical compound O.[AlH3] XFBXDGLHUSUNMG-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000002356 laser light scattering Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000001507 sample dispersion Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 silicon ester Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Abstract
A method for the production of aluminum hydroxide includes the steps of suspending aluminum hydroxide obtained by the Bayer process in a sodium aluminate solution to obtain slurry and elevating a temperature of the slurry from 60 DEG C. or less to 90 DEG C. or more. The aluminum hydroxide has an average particle diameter D in a range of 1 to 10 mum, a BET specific surface area S of 1.5 m<SUP>2</SUP>/g or less, a degree of aggregation D/Dbet of less than 3, wherein Dbet stands for a particle diameter calculated by spherical approximation from the BET specific surface area S as Dbet=6(Sxrho), in which rho denotes a specific gravity of the aluminum hydroxide, and a content of particles having diameters exceeding 20 mum that is 0.5% or less by mass. A composition that contains the aluminum hydroxide as filler, can be formed.
Description
The cross reference of related application
The application submits to according to 35 U.S.C. § 111 (a), according to 35 U.S.C. § 119 (e) (1), requires all the right of the applying date of the provisional application 60/432,246 submitted on December 12nd, 2002 according to 35 U.S.C. § 111 (b) and 60/432,252.
Technical field
The present invention relates to aluminium hydroxide of using as plastics, rubber or the like fire-retardant filler and preparation method thereof.More particularly, the present invention relates to the production method of aluminium hydroxide, aluminium hydroxide and contain the composition of aluminium hydroxide, described aluminium hydroxide has minimum agglomerate content and disintegrates with primary granule, and when being filled in it in resin, can produce the resin combination of impact property excellence.
Background technology
Up to now, aluminium hydroxide has been widely used as the filler that is filled in rubber and the plastics.For example, found that it is used as fire retardant and at thermosetting resin, as being used as the toning filler in unsaturated polyester resin and the acrylic resin in thermoplastic resin, rubber and Resins, epoxy.
When aluminium hydroxide is used as fire retardant, during the concentration of the aluminium hydroxide that in improving resin, adds, just improved the degree of improving the flame retardant resistance of given resin by the adding fire retardant.But the rising of stacking factor causes the problem such as the kneading moment of torsion that reduces plasticity and raising resin.Also produce such as improving molding temperature and making part aluminium hydroxide produce dehydration and the problem of expand (foaming).
When aluminium hydroxide was used as filler, because aluminium hydroxide lacks enhancement, it had reduced the intensity of resin formed article, particularly shock strength.In order to suppress the reduction of shock strength, suggestion reduces the particle diameter of aluminium hydroxide as far as possible.Although by precipitation is not impossible obtain aluminium hydroxide with nominal particle size, but be difficult to aluminium hydroxide is filled in a large number as filler, because described aluminium hydroxide is the form of secondary agglomerated particle and therefore has the ability of very big absorption oil, described secondary agglomerated particle is produced by a large amount of agglomeration of primary granule.
Therefore, use diameter to be about 50-150 μ m usually, above-mentioned aluminum hydroxide particles is crushed to the aluminum hydroxide particles of department level particulate degree by using ball mill or other similar pulverizer.
By pulverizing aluminium hydroxide is crushed to the regulation particle diameter and needs big energy.When pulverizing, the primary granule of aluminium hydroxide breaks, and forms uneven surface and the chip that comes off and the powder that causes producing and has improved its specific surface area.Therefore, owing to reduced with the consistency of resin and improved viscosity, the aluminium hydroxide of pulverizing is difficult to fill at the resin camber.Particularly under the situation of thermosetting resin, prolonged set time.
Only, can not easily obtain the particle of homogeneous diameter and still have thicker agglomerated particle (the not particle of Fen Suiing) by pulverizing.Confirm that when being filled in powder in the resin, the above-mentioned particle of not pulverizing has constituted the cause of fracture and caused reducing shock strength.In order to remove the above-mentioned particle of not pulverizing, generally use as making their isolating methods by air classifying after pulverizing or screening.But because they require huge original equipment investment, above-mentioned lock out operation is also uneconomical.
Therefore, proposed to be intended to obtain to have the whole bag of tricks of the aluminium hydroxide of uniform regulation particle diameter.
The flat 5-4336 of JP-B discloses a kind of by using continuous centrifugal separator that particle is applied the method that very big centrifugal force suppresses the particle chap, thereby the secondary agglomerated particle is disintegrated and does not destroy primary granule.
The primary particle diameter that aforesaid method will stand to apply the aluminium hydroxide of centrifugal force is limited in 1-4 μ m.It is reported, when diameter surpasses 4 μ m, by the dismembering deficiency of centrifugal force so that the secondary agglomerated particle disintegrate.Aforesaid method never is used for wide range of applications.
The clear 62-9256 of JP-B discloses a kind of by solid aluminum hydroxide being exposed to be heated in advance pyritous Bayer extraction agent, obtains to have the idea of the aluminium hydroxide of primary granule form or rhabdolith form.
But, owing in the process that exposes, carry out the dissolving of aluminium hydroxide, aforesaid method require long-time expose and reduce be on a sticky wicket aspect the production efficiency.
The flat 9-208740 of JP-A discloses a kind of by following steps generation surface dissolution and reduction method for specific area: at first use the dry type impact grinder that the secondary agglomerated particle in the aluminium hydroxide is pulverized, then resulting aluminium hydroxide is converted into the slurry in the sodium aluminate solution of specific alkali concn and slurry is heated up.
But same because it requires aluminium hydroxide filtered and be dry so that it can be pulverized by dry type in advance, aforesaid method has that production process prolongs and the problem of production cost raising.
The purpose of this invention is to provide aluminium hydroxide and the production method that aluminium hydroxide is provided, described aluminium hydroxide has minimum agglomerate content and disintegrates with primary granule, and when being filled in it in resin, produce the resin combination of shock strength excellence highly effectively.
Summary of the invention
The invention provides a kind of production method of aluminium hydroxide, this method may further comprise the steps: will be suspended in by the aluminium hydroxide that the Bayer method obtains in the sodium aluminate solution to obtain slurry; With with slurry temp from 60 ℃ or lowlyer be warming up to 90 ℃ or higher.
In the method, the ratio A/C that slurry has before the heating step is 0.4 or still less, and wherein A represents that alumina concentration (grams per liter) in the sodium aluminate solution and C represent the naoh concentration (grams per liter) in the sodium aluminate solution.
In the method, in heating step, with slurry temp from 60 ℃ or lower to be warming up to 90 ℃ or higher required time H be 15 minutes or shorter.
After the step that slurry heats up, this method further comprise with slurry temperature be 85 ℃ or more relative superiority or inferiority keep the step of (15-H) at least minute.
In the method, aluminium hydroxide has the solubleness ratio of passing through intensification that following general formula is represented:
Aluminium hydroxide concentration * 100 of slurry before heating up in C before solubleness ratio (%)=intensification * (A/C before the A/C-intensification after heating up) * 1.53/, wherein A represents that alumina concentration (grams per liter) in the sodium aluminate solution and C represent the naoh concentration (grams per liter) in the sodium aluminate solution, and described ratio is lower than 30%.
Preferably after the step that slurry heats up, this method further comprises the step of using continuous centrifugal separator slurry to be applied centrifugal force.Centrifugal force is preferably 300G or bigger.
In the method, heating step uses double-tube heat exchanger to carry out.
The invention still further relates to a kind of aluminium hydroxide, the median size D that described aluminium hydroxide has is 1-10 μ m, and BET specific surface area S is 1.5m
2/ g or still less, agglomeration degree D/Dbet is less than 3, wherein Dbet represent according to BET specific surface area S by spherical trial and error method according to Dbet=6 (S * ρ) calculate particle diameter, wherein ρ refers to the proportion of aluminium hydroxide, and the particulate content that diameter surpasses 20 μ m is 0.5 quality % or lower.The particulate content that diameter surpasses 20 μ m is preferably 0.1 quality % or lower.
The present invention also provides and has comprised the composition of aluminium hydroxide as filler.
Described composition comprises the body material of at least a rubber and plastics.
The aluminium hydroxide of producing by following steps of the present invention has minimum agglomerate content and disintegrates with primary granule: will be suspended in by the aluminium hydroxide that the Bayer method obtains in the sodium aluminate solution with the acquisition slurry and with slurry temp from 60 ℃ or lowlyer be warming up to 90 ℃ or higher.When employing applied the step of centrifugal force to slurry after heating up, the aluminium hydroxide of acquisition had littler agglomerate content.When being filled in aluminum hydroxide particles in the resin, can obtain the resin combination of shock strength excellence.
Implement preferred plan of the present invention
For the aluminium hydroxide that obtains to have minimum agglomerate content and disintegrate with primary granule, the inventor has carried out diligent in one's studies and has therefore found, by the following steps combination being obtained to be suitable for use as the desirable monocrystalline aluminium hydroxide with low specific surface area of filler: the temperature that contains the slurry that is suspended in the aluminium hydroxide in the specific sodium aluminate solution is raise, subsequently slurry is applied centrifugal force, thereby make the solid particulate in the slurry concentrate and make simultaneously the secondary flocculated particle to disintegrate.The result has finished the present invention.
The present invention relates to provide a kind of production method of aluminium hydroxide, this method may further comprise the steps: the temperature that will contain the slurry that is suspended in the sodium aluminate solution aluminium hydroxide that obtains by the Bayer method is from 60 ℃ or lowlyer be warming up to 90 ℃ or higher.
In the present invention in the step of Sheng Wening, the grain boundary of the insufficient secondary agglomerated particle of force of cohesion on the selective dissolution crystallography, and by the aluminium hydroxide in the slurry being applied thermal shocking the secondary agglomerated particle is disintegrated, described slurry contains to be suspended in the sodium aluminate solution and obtains aluminium hydroxide by the Bayer method.
That is, in heating step, slurry temp is 60 ℃ or lower before heating up, preferred 55 ℃ or lower.If described temperature is higher than 60 ℃, this excessive applying in prevention is on a sticky wicket aspect the big thermal shocking that is enough to realize the selective dissolution of grain boundary only in temperature-rise period.
Temperature after heating up is 90 ℃ or higher, preferred 95 ℃ or higher, and more preferably 97 ℃ or higher.If described temperature is lower than 90 ℃, this deficiency applies in prevention and is on a sticky wicket aspect the big thermal shocking that is enough to realize the selective dissolution of grain boundary only, agglomerated particle is existed and makes the particle surface roughen.
In addition, the boiling point of sodium aluminate solution does not limit, because it changes with concentration sodium hydroxide.But under the situation of the sodium aluminate solution that is used for the Bayer method, described boiling point is about 104 ℃.
As mentioned above, be 0.4 or still less, wherein A refers to the aluminum oxide (Al in the sodium aluminate solution before heating up than A/C
2O
3) concentration (grams per liter) and C represent sodium hydroxide (NaOH) concentration (grams per liter) in the sodium aluminate solution.Preferred this ratio is 0.35 or still less, and more preferably 0.3 or still less.If be higher than 0.4 than A/C, this is excessive to make the dissolving of the loose required aluminum oxide part in grain boundary and agglomerated particle is on a sticky wicket aspect existing in prevention.
With slurry temp from 60 ℃ or lowlyer be warming up to 90 ℃ or higher process required time within 15 minutes, preferably within 10 minutes, and more preferably within 5 minutes.If the described time surpasses 15 minutes, this is excessive to apply in prevention and is on a sticky wicket aspect the big thermal shocking that is enough to realize the selective dissolution of grain boundary only, agglomerated particle is existed and makes whole particles dissolvings.
Is that 60 ℃ or the lower temperature that is heated to are that 90 ℃ or higher method are not particularly limited with slurry from temperature.Temperature can linearly raise; Or in starting stage appropriateness rising and rising fast during the late stages of developmet; Or in starting stage rising and appropriateness rising during the late stages of developmet fast.The lower limit of the time length of described intensification is not particularly limited.Heating step can carry out fast.
After slurry temp has been increased to above-mentioned terminal level, slurry is remained on depend under the specified conditions of time length of intensification.In the scope of the time length (in 15 minutes) of heating up, the reduction of hold-time with the time length of heating up increases.In the method for the invention, when the used time of heating up was H minute (in 15 minutes), the hold-time was (15-H) at least minute.Therefore, when the time length of heating up was 15 minutes, this method can not keep step.Maintenance temperature after heating up is 85 ℃ or higher, and preferred 90 ℃ or higher.If described maintenance temperature is lower than 85 ℃, this deficiency is impelling isolating particle to be on a sticky wicket aspect the agglomeration once more.The upper limit of maintenance temperature is generally the boiling point of sodium aluminate solution.
The heat riser that uses in the heating step is preferably double-tube heat exchanger.
Solubleness ratio owing to the aluminium hydroxide of heating step suitably is lower than 30% in the method for the invention, preferably is lower than 25%.If the solubleness ratio is higher than 30%, this is excessive to be on a sticky wicket aspect output that reduces aluminium hydroxide and the reduction production efficiency.
Solubleness ratio owing to the aluminium hydroxide of heating step is defined by following general formula:
Aluminium hydroxide concentration * 100 of slurry before heating up in C before solubleness ratio (%)=intensification * (A/C before the A/C-intensification after heating up) * 1.53/
Wherein A represents that alumina concentration (grams per liter) in the sodium aluminate solution and C represent the naoh concentration (grams per liter) in the sodium aluminate solution.
Can add and apply the step of implementing centrifugal force.Centrifugal force can be applied to the solids-enriched that makes on the slurry in the slurry and because the phase mutual friction of adjacent particle is disintegrated the secondary agglomerated particle.This can make the secondary agglomerated particle more effectively disintegrate.
Implement in the method for the invention in the step of centrifugal force, be applied to centrifugal force on the slurry, preferred 500G or bigger, and more preferably 1000G or bigger suitably for 300G or bigger.If centrifugal force is less than 300G, this deficiency is on a sticky wicket aspect the centrifugal force that is enough to the secondary agglomerated particle is disintegrated suppressing to apply.
Implement in the method for the invention in the step of centrifugal force, the device that applies centrifugal force is preferably continuous centrifugal separator.Use continuous centrifugal separator to make to show with the secondary agglomerated particle by being applied to the effect that adds of shearing force disintegration on the solid, will from centrifuge separator, take out continuously by the spissated solid of centrifuge separator simultaneously.
In addition, known two types continuous centrifugal separator, i.e. separating plate formula and decant formula.The separating plate formula is with two types of acquisitions, i.e. valve discharging formula and nozzle discharging formula.The decant formula comprises spiral decant formula.As the continuous centrifugal separator that uses among the present invention, preferably use spiral decant formula device, because it can be by disintegrating the secondary agglomerated particle applying shearing force on the spissated solid by centrifuge separator.
Method of the present invention is by using the slurry that will be suspended in by the aluminium hydroxide that the Bayer method obtains in the sodium aluminate solution as raw material and carry out heating step, with ought be in case of necessity, carry out centrifugal force is applied to step on the slurry, can obtain primary granule aluminium hydroxide, avoid making the coarse or lasting existence of inhibition agglomerated particle of particle surface simultaneously.
The present invention can obtain a kind of aluminium hydroxide, and the median size D that described aluminium hydroxide has is 1-10 μ m, and the BET specific surface area S that measures by nitrogen adsorption method (BET method) is 1.5m
2/ g or littler, agglomeration degree D/Dbet be less than 3, and wherein Dbet refers to the particle diameter that is calculated by spherical trial and error method by S, and the particulate content that diameter surpasses 20 μ m is 0.5 quality % or lower, preferred 0.1 quality % or lower.Herein, Dbet is expressed as Dbet=6/ (S * ρ), wherein ρ refers to the proportion of aluminium hydroxide.
As mentioned above, method of the present invention uses the slurry that will be suspended in by the aluminium hydroxide that the Bayer method obtains in the sodium aluminate solution as raw material.By considering particle diameter that expection obtains after the dissolving and the primary particle diameter of selecting secondary agglomerated particle in the feed slurry, can obtain to have the primary granule aluminium hydroxide of target grain size and low BET specific surface area.
Thus obtained aluminium hydroxide can suitably be used as all kinds filler.As the specific examples of the body material that is advantageously used in the aluminium hydroxide composition, can enumerate plastic substance such as rubber and thermoplastic resin, Resins, epoxy and thermosetting resin (as unsaturated polyester resin and acrylic resin).
In the time will being filled in the resin by the aluminium hydroxide that described method obtains, consider the reduction compound viscosity, its independent use or the aluminium hydroxide kind different with multiple other particle diameter can be used in combination.
The aluminium hydroxide that obtains by described method can use known surface treatment agent to carry out surface treatment before using.Surface treatment agent does not need special qualification.As the specific examples of the surface treatment agent of preferred use, can enumerate various coupling agents, for example silane coupling agent and titanate coupling agent; Lipid acid, for example oleic acid and stearic acid; The ester of described lipid acid; And silicon ester, for example methyl silicate and tetraethyl silicate.
Now, below with reference to embodiment the present invention is described more specifically.The present invention does not need to be limited to following examples, and can be embodied in described content in the scope that does not change additional claim by any way.Solid state properties described in the specification sheets of the present invention can be measured by the following method.
＜median size D 〉
The median size D of aluminium hydroxide measures by the laser light scattering diffraction approach.
＜BET specific surface area S 〉
The specific surface area S of aluminium hydroxide measures by nitrogen adsorption method (BET method).
＜agglomeration degree D/Dbet 〉
The agglomeration degree D/Dbet of aluminium hydroxide is by calculating median size D and as Dbet=6/ (S * ρ) estimate that by the ratio of the particle diameter Dbet of spherical trial and error method calculating wherein ρ refers to the proportion of aluminium hydroxide by S.
＜diameter surpasses the particulate content of 20 μ m 〉
The particulate content that diameter surpasses 20 μ m calculates by the following method: with the 5g sample dispersion in 1.5 liters of tap water (it is flow through can remove the solid strainer that diameter surpasses 1 μ m); Resulting dispersion soln was carried out ultrasonic dispersing 10 minutes, and while employing sieve mesh in fine-powder classifier (made by Yokohama Rika K.K. and sell with product code " PS-80 ") is that the stainless steel sift of 20 μ m screens it; Resistates weighing to screening; And calculate the residue weight of screening with respect to the percentage that screens preceding example weight.
＜shock strength 〉
By with 100 mass parts vinyl ester resins (make and sell), 200 mass parts aluminium hydroxides, 2 mass parts solidifying agent with trade names " Ripoxy RF-300 series " by Showa Kobunshi K.K. (by Nippon Oils ﹠amp; Fats Co., Ltd. make and sell with trade names " PercureWO ") and 0.75 mass parts auxiliary agent (by Nippon Oils ﹠amp; Fats Co., Ltd. make and sell with trade names " Peroil TCP ") be mixed together, with its stirring, under vacuum, make simultaneously its froth breaking, resulting mixture is poured in the gap between the relative sheet glass, and with mixture between sheet glass 60 ℃ down heating 1 hour and 90 ℃ down heating obtained moulded piece until making its curing in 30 minutes.The test part that does not contain breach is by the moulded piece preparation and measure its Izod shock strength.
The solubleness ratio of＜aluminium hydroxide 〉
Solubleness ratio owing to the aluminium hydroxide of heating step can be calculated by following formula:
Aluminium hydroxide concentration * 100 of slurry before heating up in C before solubleness ratio (%)=intensification * (A/C before the A/C-intensification after heating up) * 1.53/
Wherein A represents that alumina concentration (grams per liter) in the sodium aluminate solution and C represent the naoh concentration (grams per liter) in the sodium aluminate solution.
Embodiment 1
To be suspended in the slurry (median size of aluminium hydroxide: 57.6 μ m that sodium aluminate solution obtains by the aluminium hydroxide that the Bayer method obtains, naoh concentration: 158 grams per liters, A/C=0.31, the aluminium hydroxide concentration of slurry: 200 grams per liters, and slurry temp: 41 ℃) with speed 3m
3(interior tube body is long-pending: 0.019m to the interior pipe of double-tube heat exchanger in/hr feeding
3, and heating-surface area: 3.2m
2) in (hold-time in the interchanger: 23 seconds).Steam is added outer tube until its temperature is increased to 96 ℃.Then, slurry was kept 15 minutes down at 85 ℃.The A/C of slurry be 0.49 and its solubleness ratio be 21.8%.
By filtering solid aluminum hydroxide is separated from slurry under the purification state, be dried then.Find that the median size D that the aluminium hydroxide that obtains like this has is 8.2 μ m, BET specific surface area S is 0.5m
2/ g, agglomeration degree are 1.7, and the particulate content that diameter surpasses 20 μ m is 0.23 quality %.By described powder being filled into the Izod shock strength that the test part made in the resin shows is 2.2kJ/m
2
Embodiment 2
To be 1m with the used identical slurry feeding that is suspended with aluminium hydroxide to internal volume among the embodiment 1
3The SUS jar in and continue to stir therein.Simultaneously, the temperature with jar is increased to 90 ℃ in 15 minutes time.Find A/C that slurry has be 0.47 and the solubleness ratio be 19.3%.By filtering solid aluminum hydroxide is separated from slurry under the purification state, be dried then.Find that the median size D that the aluminium hydroxide that obtains like this has is 8.8 μ m, BET specific surface area S is 0.5m
2/ g, agglomeration degree are 1.8, and the particulate content that diameter surpasses 20 μ m is 0.35 quality %.By described powder being filled into the Izod shock strength that the test part made in the resin shows is 2.1kJ/m
2
Embodiment 3
To be suspended in the slurry (median size of aluminium hydroxide: 55.3 μ m that sodium aluminate solution obtains by the aluminium hydroxide that the Bayer method obtains, naoh concentration: 156 grams per liters, A/C=0.38, the aluminium hydroxide concentration of slurry: 180 grams per liters, and slurry temp: 43 ℃) feeding to embodiment 2 in the employed identical SUS jar and continue therein to stir.Simultaneously, the temperature with jar is increased to 90 ℃ in 15 minutes time.Find A/C that slurry has be 0.48 and its solubleness ratio be 13.3%.By filtering solid aluminum hydroxide is separated from slurry under the purification state, be dried then.Find that the median size D that the aluminium hydroxide that obtains like this has is 9.1 μ m, BET specific surface area S is 0.4m
2/ g, agglomeration degree are 1.5, and the particulate content that diameter surpasses 20 μ m is 0.41 quality %.By described powder being filled into the Izod shock strength that the test part made in the resin shows is 2kJ/m
2
Embodiment 4
According to the method for embodiment 2 handle with embodiment 1 in the used identical slurry that is suspended with aluminium hydroxide, the while is heated to slurry 47 ℃ in advance.After heating up, find A/C that slurry has be 0.49 and the solubleness ratio be 21.8%.By filtering solid aluminum hydroxide is separated from slurry under the purification state, be dried then.Find that the median size D that the aluminium hydroxide that obtains like this has is 9.7 μ m, BET specific surface area S is 0.4m
2/ g, agglomeration degree are 1.6, and the particulate content that diameter surpasses 20 μ m is 0.4 quality %.By described powder being filled into the Izod shock strength that the test part made in the resin shows is 2kJ/m
2
Comparative example 1
Will with the used identical slurry feeding that is suspended with aluminium hydroxide among the embodiment 1 to the used identical SUS jar of embodiment 2 in and continue therein to stir.Simultaneously, the temperature with jar is increased to 83 ℃ in 15 minutes time.Find A/C that slurry has be 0.44 and the solubleness ratio be 15.7%.By filtering solid aluminum hydroxide is separated from slurry under the purification state, be dried then.Find that the median size D that the aluminium hydroxide that obtains like this has is 27.2 μ m, BET specific surface area S is 0.2m
2/ g, agglomeration degree are 2.2, and the particulate content that diameter surpasses 20 μ m is 1.09 quality %.By described powder being filled into the Izod shock strength that the test part made in the resin shows is 1.9kJ/m
2
Comparative example 2
Will with the used identical slurry feeding that is suspended with aluminium hydroxide among the embodiment 1 to the used identical SUS jar of embodiment 2 in and continue therein to stir.Simultaneously, the temperature with jar is increased to 90 ℃ in 30 minutes time.Find A/C that slurry has be 0.5 and the solubleness ratio be 23%.By filtering solid aluminum hydroxide is separated from slurry under the purification state, be dried then.Find that the median size D that the aluminium hydroxide that obtains like this has is 12.3 μ m, BET specific surface area S is 0.4m
2/ g, agglomeration degree are 2, and the particulate content that diameter surpasses 20 μ m is 0.74 quality %.By described powder being filled into the Izod shock strength that the test part made in the resin shows is 1.8kJ/m
2
Comparative example 3
According to the method for embodiment 2 handle with embodiment 1 in the used identical slurry that is suspended with aluminium hydroxide, the while is heated to slurry 68 ℃ in advance.After heating up, find A/C that slurry has be 0.49 and the solubleness ratio be 21.8%.By filtering solid aluminum hydroxide is separated from slurry under the purification state, be dried then.Find that the median size D that the aluminium hydroxide that obtains like this has is 14.5 μ m, BET specific surface area S is 0.4m
2/ g, agglomeration degree are 2.3, and the particulate content that diameter surpasses 20 μ m is 0.63 quality %.By described powder being filled into the Izod shock strength that the test part made in the resin shows is 1.8kJ/m
2
The result of above embodiment 1-4 and comparative example 1-3 concentrates on and describes in the table 1 and demonstration.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Performance as the aluminium hydroxide of raw material: median size (μ m) | 57.6 | 57.6 | 55.3 | 57.6 | 57.6 | 57.6 | 57.6 |
| The performance of sodium aluminate solution: NaOH concentration (grams per liter) A/C | 158 0.31 | 158 0.31 | 156 0.38 | 158 0.31 | 158 0.31 | 158 0.31 | 158 0.31 |
| The slurry performance: slurry concentration (grams per liter) slurry temp (℃) | 200 41 | 200 41 | 180 43 | 200 47 | 200 41 | 200 41 | 200 68 |
| Intensification condition: its terminal point, (℃) its time length maintenance temperature, (℃) hold-time A/C solubleness ratio thereafter, (%) | 96 23s 85 15m 0.49 21.8 | 90 15m 0.47 19.3 | 90 15m 0.48 13.3 | 90 15m 0.49 21.8 | 83 15m 0.44 15.7 | 90 30m 0.5 23 | 90 15m 0.49 21.8 |
| Aluminium hydroxide performance: median size D (μ m) Bet specific surface area S (m 2/ g) agglomeration degree grain amount ,+20 μ (weight %) | 8.2 0.5 1.7 0.23 | 8.8 0.5 1.8 0.35 | 9.1 0.4 1.5 0.41 | 9.7 0.4 1.6 0.4 | 27.2 0.2 2.2 1.09 | 12.3 0.4 2 0.74 | 14.5 0.4 2.3 0.63 |
| The performance of moulded piece: Izod shock strength (kJ/m 2) | 2.2 | 2.1 | 2 | 2 | 1.9 | 1.8 | 1.8 |
Embodiment 5
To be suspended in the slurry (median size of aluminium hydroxide: 57.6 μ m that sodium aluminate solution obtains by the aluminium hydroxide that the Bayer method obtains, naoh concentration: 158 grams per liters, A/C=0.31, the aluminium hydroxide concentration of slurry: 200 grams per liters, and slurry temp: 41 ℃) with speed 3m
3(interior tube body is long-pending: 0.019m to the interior pipe of double-tube heat exchanger in/hr feeding
3, and heating-surface area: 3.2m
2) in (hold-time in the interchanger: 23 seconds).Steam is added outer tube until its temperature is increased to 96 ℃.Then, with the part slurry with speed 1m
3/ hr transfer in the continuous centrifugal separator (have Tomoe Kogyo K.K. to make and sell) with trade names " Sharpless Super Decanter P-660 " and by centrifugal force be 1000G with its compression so that solids-enriched therein.To from device, take out continuously by the spissated solid of screw rod on the interior pipe that is fixed on continuous centrifugal separator.
Be 0.46 through the A/C of the slurry of double-tube heat exchanger and be 18.1% owing to the solubleness ratio of the aluminium hydroxide of the heating step of slurry.,, be dried then through the aluminium hydroxide washing of decanting vessel by filtering separation.
Find that the median size D that the aluminium hydroxide that obtains like this has is 8.9 μ m, BET specific surface area S is 0.5m
2/ g, agglomeration degree D/Dbet is 1.8, and the particulate content that diameter surpasses 20 μ m is 0.03 quality %.
By described powder being filled into the Izod shock strength that the test part made in the resin shows is 2.6kJ/m
2
Embodiment 6
To be suspended in the slurry (median size of aluminium hydroxide: 55.3 μ m that sodium aluminate solution obtains by the aluminium hydroxide that the Bayer method obtains, naoh concentration: 156 grams per liters, A/C=0.38, the aluminium hydroxide concentration of slurry: 180 grams per liters, and slurry temp: 43 ℃) with speed 3m
3/ hr transfers in the interior pipe with the used identical double-tube heat exchanger of embodiment 5 (hold-time in the interchanger: 23 seconds), and steam is added outer tube until its temperature is increased to 96 ℃.With the part slurry with speed 1m
3/ hr transfer to the used identical continuous centrifugal separator of embodiment 5 in and by centrifugal force be 1000G with its compression so that the solids-enriched in slurry.Method by embodiment 5 is taken out solid from device.
Find that A/C that the slurry through double-tube heat exchanger has is 0.45 and is 9.3% owing to the solubleness ratio of the aluminium hydroxide of the heating step of slurry.,, be dried then through the aluminium hydroxide washing of decanting vessel by screening and separating.
Find that the median size D that the aluminium hydroxide that obtains like this has is 7.8 μ m, BET specific surface area S is 0.9m
2/ g, agglomeration degree D/Dbet is 2.8, and the particulate content that diameter surpasses 20 μ m is 0.05 quality %.
The method that adopts embodiment 5 finds that by aluminium-hydroxide powder being filled into manufacturing test part in the resin Izod shock strength that test part has is 3.1kJ/m
2
Embodiment 7
With part embodiment 5 through the slurry of double-tube heat exchanger with speed 1m
3/ hr transfer to the used identical continuous centrifugal separator of embodiment 6 in and by centrifugal force be 500G with its compression so that the solids-enriched in slurry.Adopt with embodiment 6 in identical method with solid taking-up from device.,, be dried then through the aluminium hydroxide washing of decanting vessel by screening and separating.
Find that the median size D that the aluminium hydroxide that obtains like this has is 9.3 μ m, BET specific surface area S is 0.5m
2/ g, agglomeration degree D/Dbet is 1.9, and the particulate content that diameter surpasses 20 μ m is 0.04 quality %.
The method that adopts embodiment 5 finds that by aluminium-hydroxide powder being filled into manufacturing test part in the resin Izod shock strength that test part has is 2.7kJ/m
2
Embodiment 8
Slurry according to the method Processing Example 5 of embodiment 5 is heated to 47 ℃ in advance with slurry simultaneously.Through the A/C of the slurry of double-tube heat exchanger be 0.45 and the solubleness ratio be 16.9%.,, be dried then through the aluminium hydroxide washing of decanting vessel by filtering separation.
Find that the median size D that the aluminium hydroxide that obtains like this has is 9.5 μ m, BET specific surface area S is 0.4m
2/ g, agglomeration degree D/Dbet is 1.5, and the particulate content that diameter surpasses 20 μ m is 0.08 quality %.
The method that adopts embodiment 1 finds that by aluminium-hydroxide powder being filled into manufacturing test part in the resin Izod shock strength that test part has is 2.9kJ/m
2
Comparative example 4
With part embodiment 5 through the slurry of double-tube heat exchanger with speed 1m
3/ hr transfer to the used identical continuous centrifugal separator of embodiment 5 in and by centrifugal force be 200G with its compression so that the solids-enriched in slurry.Adopt with embodiment 5 in identical method with solid taking-up from device.,, be dried then through the aluminium hydroxide washing of decanting vessel by filtering separation.
Find that the median size D that the aluminium hydroxide that obtains like this has is 9.6 μ m, BET specific surface area S is 0.3m
2/ g, agglomeration degree D/Dbet is 1.2, and the particulate content that diameter surpasses 20 μ m is 0.15 quality %.
The method that adopts embodiment 5 finds that by aluminium-hydroxide powder being filled into manufacturing test part in the resin Izod shock strength that test part has is 2kJ/m
2
Comparative example 5
Will with used identical aluminium hydroxide slurry among the embodiment 5 with speed 3m
3/ hr transfer to embodiment 5 in the interior pipe of used identical double-tube heat exchanger (hold-time in the interchanger: 23 seconds), simultaneously steam is added outer tube so that slurry temp is increased to 87 ℃.With the part slurry with speed 1m
3/ hr transfer to embodiment 5 in the used identical continuous centrifugal separator and by centrifugal force be 1000G with its compression so that the solids-enriched in slurry.Adopt with embodiment 5 in identical method with solid taking-up from device.
Be 0.4 through the A/C of the slurry of double-tube heat exchanger and be 10.9% owing to the solubleness ratio of the aluminium hydroxide of the heating step of slurry.,, be dried then through the aluminium hydroxide washing of decanting vessel by filtering separation.
Find that the median size D that the aluminium hydroxide that obtains like this has is 14 μ m, BET specific surface area S is 0.3m
2/ g, agglomeration degree D/Dbet is 1.7, and the particulate content that diameter surpasses 20 μ m is 0.73 quality %.
The method that adopts embodiment 1 finds that by aluminium-hydroxide powder being filled into manufacturing test part in the resin Izod shock strength that test part has is 1.9kJ/m
2
Comparative example 6
The aluminium hydroxide slurry (median size of aluminium hydroxide: 56.5 μ m, naoh concentration: 159 grams per liters, A/C=0.45, the aluminium hydroxide concentration of slurry: 200 grams per liters, and slurry temp: 45 ℃) that will obtain by the Bayer method is with speed 3m
3/ hr transfer to embodiment 5 in the interior pipe of used identical double-tube heat exchanger (hold-time in the interchanger: 23 seconds), simultaneously steam is added outer tube so that slurry temp is increased to 96 ℃.With the part slurry with speed 1m
3/ hr transfer to embodiment 5 in the used identical continuous centrifugal separator and by centrifugal force be 1000G with its compression so that the solids-enriched in slurry.Adopt with embodiment 5 in identical method with solid taking-up from device.
Be 0.47 through the A/C of the slurry of double-tube heat exchanger and be 2.4% owing to the solubleness ratio of the aluminium hydroxide of the heating step of slurry.,, be dried then through the aluminium hydroxide washing of decanting vessel by filtering separation.
Find that the median size D that the aluminium hydroxide that obtains like this has is 30.4 μ m, BET specific surface area S is 0.2m
2/ g, agglomeration degree D/Dbet is 2.5, and the particulate content that diameter surpasses 20 μ m is 1.26 quality %.
The method that adopts embodiment 5 finds that by aluminium-hydroxide powder being filled into manufacturing test part in the resin Izod shock strength that test part has is 1.8kJ/m
2
Comparative example 7
Slurry according to the method Processing Example 5 of embodiment 5 is heated to 65 ℃ in advance with slurry simultaneously.Through the A/C of the slurry of double-tube heat exchanger be 0.46 and the solubleness ratio be 18.1%.,, be dried then through the aluminium hydroxide washing of decanting vessel by filtering separation.
Find that the median size D that the aluminium hydroxide that obtains like this has is 10.6 μ m, BET specific surface area S is 0.5m
2/ g, agglomeration degree D/Dbet is 2.1, and the particulate content that diameter surpasses 20 μ m is 0.22 quality %.
The method that adopts embodiment 1 finds that by aluminium-hydroxide powder being filled into manufacturing test part in the resin Izod shock strength that test part has is 2.2kJ/m
2
The result of above embodiment 5-8 and comparative example 4-7 concentrates on and describes in the table 2 and demonstration.
Table 2
| Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Comparative example 4 | Comparative example 5 | Comparative example 6 | Comparative example 7 | |
| Performance as the aluminium hydroxide of raw material: median size (μ m) | 57.6 | 55.3 | 57.6 | 57.6 | 57.6 | 57.6 | 56.5 | 57.6 |
| The performance of sodium aluminate solution: NaOH concentration (grams per liter) A/C | 158 0.31 | 156 0.38 | 158 0.31 | 158 0.31 | 158 0.31 | 158 0.31 | 159 0.45 | 158 0.31 |
| The slurry performance: slurry concentration (grams per liter) slurry temp (℃) | 200 41 | 180 43 | 200 41 | 200 47 | 200 41 | 200 41 | 200 45 | 200 65 |
| The intensification condition: its terminal point (℃) its time length (second) A/C solubleness ratio (%) thereafter | 96 23 0.46 18.1 | 96 23 0.45 9.3 | 96 23 0.46 18.1 | 96 23 0.45 16.9 | 96 23 0.46 18.1 | 87 23 0.4 10.9 | 96 23 0.47 2.4 | 96 23 0.46 18.1 |
| The condition of centrifugation: centrifugal force (G) | 1000 | 1000 | 500 | 1000 | 200 | 1000 | 1000 | 1000 |
| Aluminium hydroxide performance by filtering separation: median size D (μ m) Bet specific surface area S (m 2/ g) agglomeration degree grain amount ,+20 μ m (weight %) | 8.9 0.5 1.8 0.03 | 7.8 0.9 2.8 0.05 | 9.3 0.5 1.9 0.04 | 9.5 0.4 1.5 0.08 | 9.6 0.3 1.2 0.15 | 14 0.3 1.7 0.73 | 30.4 0.2 2.5 1.26 | 10.6 0.5 2.1 0.22 |
| The performance of moulded piece: Izod shock strength (kJ/m 2) | 2.6 | 3.1 | 2.7 | 2.9 | 2 | 1.9 | 1.8 | 2.2 |
The industry practicality
As previously mentioned, produce in the method for aluminium hydroxide in the present invention, aluminium hydroxide in slurry applies thermal shock, thereby the grain boundary of selectively only dissolving two grades of agglomerated particles of cohesive force deficiency on the crystallography, and in case of necessity, apply thus centrifugal force, thereby make two grades of agglomerated particles that strong being in contact with one another occur, in order to show the effect that the two grades of agglomerated particles of sening as an envoy to disintegrate.
Different from conventional production method, the method that the present invention produces aluminium hydroxide demonstrates the epoch-making ability of the aluminium hydroxide of producing the first grade particles that contains extremely few remaining agglomerated particle and enjoys very large industry and is worth, described conventional method with dry type sieve and air classification device with utilize because the method that the physical impact power of the collision between the medium is pulverized or utilize as the friction of Reymond mill and pulverize or make up as the method for colliding between the particle that sprays mill.
In addition, the present invention's who obtains by said method aluminium hydroxide can be widely used as the various types of fillers that are filled in rubber and the plastics. Can form the moulded parts of high impact strength, and not meet with the reduction of the impact strength that above-mentioned conventional filling aluminium hydrate stands.
Claims (14)
1. the production method of aluminium hydroxide, this method comprise will be suspended in by the aluminium hydroxide that the Bayer method obtains in the sodium aluminate solution with obtain slurry and with slurry temp from 60 ℃ or lowlyer be warming up to 90 ℃ or higher step.
2. the production method of the aluminium hydroxide of claim 1, the ratio A/C that wherein slurry has before heating step is 0.4 or still less, and wherein A represents that the concentration (grams per liter) of the aluminum oxide in the sodium aluminate solution and C represent the naoh concentration (grams per liter) in the sodium aluminate solution.
3. the production method of claim 1 or 2 aluminium hydroxide, wherein in heating step, with slurry temp from 60 ℃ or lower to be warming up to 90 ℃ or higher required time H be 15 minutes or shorter.
4. the production method of the aluminium hydroxide of claim 3, this method further is included in after the slurry heating step, with slurry temperature be 85 ℃ or more relative superiority or inferiority keep the step of (15-H) at least minute.
5. the production method of each aluminium hydroxide among the claim 1-4, this method further are included in the step that applies centrifugal force after the slurry heating step to slurry.
6. the production method of each aluminium hydroxide among the claim 1-5, wherein has the solubleness ratio that following general formula is represented: aluminium hydroxide concentration * 100 of slurry before heating up in the C before solubleness ratio (%)=intensification * (A/C before the A/C-intensification after heating up) * 1.53/ by intensification aluminium hydroxide, wherein A represents that alumina concentration (grams per liter) in the sodium aluminate solution and C represent the naoh concentration (grams per liter) in the sodium aluminate solution, and described ratio is lower than 30%.
7. the production method of claim 5 or 6 aluminium hydroxide, wherein centrifugal force is 300G or bigger.
8. the production method of each aluminium hydroxide among the claim 5-7 wherein adopts continuous centrifugal separator to apply centrifugal force.
9. the production method of each aluminium hydroxide among the claim 1-8, wherein the heating step of slurry uses double-tube heat exchanger to carry out.
10. aluminium hydroxide, the median size D that described aluminium hydroxide has is 1-10 μ m, BET specific surface area S is 1.5m
2/ g or still less, agglomeration degree D/Dbet is less than 3, wherein Dbet represents that (particle diameter of S * ρ) calculate, wherein ρ refers to the proportion of aluminium hydroxide, and the particulate content that diameter surpasses 20 μ m is 0.5 quality % or lower according to Dbet=6 by spherical trial and error method according to BET specific surface area S.
11. the aluminium hydroxide of claim 10, wherein diameter is 0.1 quality % or lower above the particulate content of 20 μ m.
12. aluminium hydroxide, described aluminium hydroxide obtains by each method among the claim 1-9.
13. composition, described composition comprise among the claim 10-12 each aluminium hydroxide as filler.
14. the composition of claim 13, wherein said composition comprises the body material of at least a rubber and plastics.
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| JP353504/2002 | 2002-12-05 | ||
| JP353506/2002 | 2002-12-05 | ||
| JP2002353504A JP4172765B2 (en) | 2002-12-05 | 2002-12-05 | Aluminum hydroxide and method for producing the same |
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|---|---|
| CN1735564A true CN1735564A (en) | 2006-02-15 |
| CN100336726C CN100336726C (en) | 2007-09-12 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249276A (en) * | 2010-04-15 | 2011-11-23 | 新日铁高新材料股份有限公司 | Method for producing spherical aluminum powder |
| CN102352137A (en) * | 2011-08-18 | 2012-02-15 | 中国铝业股份有限公司 | Method for preparing aluminum bydroxide powder used for flame retardance or filling |
| CN101970356B (en) * | 2008-02-05 | 2013-07-17 | 日本轻金属株式会社 | Mixed aluminum hydroxide powder |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006199565A (en) * | 2004-05-13 | 2006-08-03 | Showa Denko Kk | Aluminum hydroxide and use thereof |
| JP4986444B2 (en) * | 2005-12-12 | 2012-07-25 | 株式会社トクヤマ | Hydrophobic inorganic powder and method for producing the same |
| WO2021053922A1 (en) * | 2019-09-17 | 2021-03-25 | 昭和電工株式会社 | Thermosetting resin composition and electrical/electronic component which contains cured product of same |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE68923171D1 (en) * | 1989-01-26 | 1995-07-27 | Showa Denko Kk | ALUMINUM HYDROXYD, METHOD FOR THE PRODUCTION AND COMPOSITION. |
| JP3132077B2 (en) * | 1991-08-27 | 2001-02-05 | 日本軽金属株式会社 | Aluminum hydroxide having low content of aggregated particles and narrow particle distribution and method for producing the same |
-
2002
- 2002-12-05 JP JP2002353504A patent/JP4172765B2/en not_active Expired - Lifetime
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2003
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101970356B (en) * | 2008-02-05 | 2013-07-17 | 日本轻金属株式会社 | Mixed aluminum hydroxide powder |
| TWI468347B (en) * | 2008-02-05 | 2015-01-11 | Nippon Light Metal Co | Aluminum hydroxide mixed powder |
| CN102249276A (en) * | 2010-04-15 | 2011-11-23 | 新日铁高新材料股份有限公司 | Method for producing spherical aluminum powder |
| US8815205B2 (en) | 2010-04-15 | 2014-08-26 | Nippon Steel & Sumikin Materials Co., Ltd. | Method for producing spherical alumina powder |
| CN102249276B (en) * | 2010-04-15 | 2015-07-08 | 新日铁住金高新材料株式会社 | Method for producing spherical aluminum powder |
| CN102352137A (en) * | 2011-08-18 | 2012-02-15 | 中国铝业股份有限公司 | Method for preparing aluminum bydroxide powder used for flame retardance or filling |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2004182555A (en) | 2004-07-02 |
| CN100336726C (en) | 2007-09-12 |
| JP4172765B2 (en) | 2008-10-29 |
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