CA2157389A1 - Crystalline aluminium hydroxide - Google Patents

Crystalline aluminium hydroxide

Info

Publication number
CA2157389A1
CA2157389A1 CA002157389A CA2157389A CA2157389A1 CA 2157389 A1 CA2157389 A1 CA 2157389A1 CA 002157389 A CA002157389 A CA 002157389A CA 2157389 A CA2157389 A CA 2157389A CA 2157389 A1 CA2157389 A1 CA 2157389A1
Authority
CA
Canada
Prior art keywords
aluminium hydroxide
crystalline aluminium
range
crystalline
na2o
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
CA002157389A
Other languages
French (fr)
Inventor
Neil Brown
Detlef Van Peij
Hans Bongartz
Dagmar Kohler
Norbert W. Putz
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Martinswerk GmbH
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Publication of CA2157389A1 publication Critical patent/CA2157389A1/en
Abandoned legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/46Purification of aluminium oxide, aluminium hydroxide or aluminates
    • C01F7/47Purification of aluminium oxide, aluminium hydroxide or aluminates of aluminates, e.g. removal of compounds of Si, Fe, Ga or of organic compounds from Bayer process liquors
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00Fireproofing materials
    • C09K21/02Inorganic materials
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Removal Of Specific Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Described is a new crystalline aluminium hydroxide which, because of its high-level purity and its outstanding electrical properties along with good viscosity characteristics, is especially well-suited for flarne-proofing of thermosetting plastics dlat are used in electrical applications.

Description

21573~9 Cry~talline aluminium hydroxide The invention relates to a crystalline aluminium hydroxide which is suitable for the flameproofing of thermosetting plastics.
In particular for thermosetting plastics which are used in the electronics field, there are official requirements to replace the toxic halogenated flameproof finishes by non-halogenated finishes.
Aluminium hydroxide would be an obvious choice, provided that, with respect to its properties, it can readily be processed with the thermosetting plastic and, in view of the electrical properties demanded, has a very high purity. An aluminium hydroxide which shows both the properties mentioned ha not been known hitherto.
It was therefore the object to develop an alumi-nium hydroxide which has the d~n~ed property profile, high purity, outst~n~; ng electrical properties and good viscosity behaviour.
It was possible to achieve the object by means of a cry~talline aluminium hydroxide according to Patent Claim 1.
The percentage data below relating to the par-ticle size distribution are given in % by weight (percent by weight).
According to the invention, this crystalline aluminium hydroxide has a particle size in the 50% range d50 of 15 - 50 ~m, preferably of 20 - 35 ~m.
The particle size in the 10% range dlo i8 ex-pediently between 2 and 6 ~m, preferably between 4 and 6 ~m. The particle size in the 90% range dgo is ex-pediently between 35 and 100 ~m, preferably between 40 and 95 ~m. The essential points for the electrical properties of the crystalline aluminium hydroxide are the Na20 content which, according to the invention, is ~ 0.1%
and the content of soluble Na20 which, according to the invention, is 5 0.005%. Preferably, the content of soluble Na20 is s O.004%.
The measure of the purity of the crystalline aluminium hydroxide is the electrical conductivity of a ~. ~ 215738~

10% su~pension in deionized water. The crystalline aluminium hydroxide according to the invention shows a value of advantageously 5 25 ~S/cm.
The specific surface area, meas-~red according to BET, of the crystalline aluminium hydroxide is expedient-ly within the range from 0.4 m2/g to 1.2 m2 /g The production of the crystalline aluminium hydroxide according to the invention ~tarts from an especially crystallized aluminium hydroxide having a 10particle size in the 50% range d50 of 25 - 90 m, prefer-ably of 35 - 75 ~m, an Na20 conte~t o~ ~ 0.15% and a content of soluble Na20 of < 0.02%. The particle size of the starting al~ nium hydroxide in the 10% range d1o i8 expediently 10 ~m to 30 ~m and in the 90% range dgo 15expediently 45 ~m to 150 ~m. The electrical conducti~ity of a 10% suspension of the starting aluminium hydroxide is expediently between 25 ~S/cm and 55 ~S/cm. The specific surface area according to BET of the starting aluminium hydroxide is in the range between c 0.1 m2/g and 1.0 m2/g.
The said starting aluminium hydroxide is first wa3hed with hot water (temperatures of expediently ~0C
to 95C), in order to lower the Na20 content. The pro-cedure at this point is expediently such that the alumi~ium hydroxide is treated, for example on a belt filter with a ~uantity of w~h;ng water from 1.5 m3/tonne to 2 m'/tonne of aluminium hydroxide.
The resulting aluminium hydroxide is then expediently dried. The Na20 content of thi~ alumini hydroxide is within the range of 5 0 .1%, and the content of soluble Na20 is in the range of 5 0.005%.
The subsequent deagglomeration is expediently carried out in a suitable mill, preferably in an impact mill.
35Ad~antageously, the deagglomeration is carried out continuously.
As regards the product properties according to the invention, it is important to set the mill parameters of speed of rotation of the separator (speed of rotatio~

~_ 3 21573~9 of the rotor body) of the impact mill and the % feed of the product (fraction of the continuously di~charged product, the difference from 100% is recycled into the mill) to appropriate ~alues.
S It has been found that the speed of rotation of the separator i8 expediently set in the range from 650 to 950 revolutions/minute. The % feed can ~ary in the range of 35% to 75%.
According to the in~ention, the resulting alumi-nium hydroxides can be used for the flameproofing of ~h~rmogetting plastics such as, for example, unsaturated polyester resins, acrylic resins or epoxy resins.
The degree of filling ranges here within the usual order of magnitude necessary for achie~ing a flame resi~tance in accordance with U~-94 (Underwriter Laboratories).
The flameproof thermosetting plastics are distin-guished by an excellent viscosity behaviour with at the same time out8t~n~; ng electrical properties.
ExamPles:
Ex~le 1:
Preparation of a crystalline deagglomerated aluminium hydroxide The aluminium hydroxide specially crystallized from the Bayer process and ha~ing the following properties:
- dlo (~m) : 20.4 - d50 (~m) : 40.9 - dgo (~m) : 66.7 - Solu~le Na2O (%) : 0.005 - Na2O (%) : 0.054 - Csn~cti~ity (~S/cm, : 26 10% suspension in deionized water) - Specific surface area according to BET : 0.3 m2/g was treated on a belt filter with a quantity of w~h; ng water (95C) of 1.8 m'/tonne and dried ~ia a ~low dryer to a moisture content of 0.15%.
The aluminium hydroxide treated in this way was ` _ 4 _ 21S738~

then deagglomerated in an impact mill (ACM mill) by means of the special impact technique thereof with a feed of about 70%, a separator speed of 850 rpm and without the use of impact bodies.
The aluminium hydroxide resulting from the above process showed the following properties: ~
- dlo (~m) : 3-~
- d50 (~m) :23.0 - dgo (~m~ :42.9 - Soluble Na2O (%) :0.003 - - Na2O (%) :0.049 - Conductivity (~S/cm, : 15 10% suspension in deionized water) - Specific surface area according to BET : 0.44 m2/g To measure the viscosity behaviour, 150 parts by weight of the aluminium hydroxide obtained were mixed into 100 parts of the unsaturated polyester resin (Synolite 0020 N-2; DSM Resins BV). The processing viscosity was measured at 23C, using a Brookfield ~BT
viscometer with a No. 3 spindle.
- starting hydroxide: 165 Pas - deagglomerated hydroxide: 52 Pas Example 2:
Correspon~;ng to Example 1, an aluminium hydrox-ide having the following properties:
dlo (~m) 5.9 d50 (~m) dgo (~m) 93 Soluble Na2O (%) 0.0034 Na2O (%) 0.093 Conductivity (~S/cm, 22 10% suspension in deionized water) Specific surface area 35 according to BET (m2/g) 0.44 was obtained from an aluminium hydroxide having the following properties:

~ _ 5 _ 2157389 dlo (~m) 26 d50 (~m) 70 dgo (~m) 100 Soluble Na20 (%) 0.015 Na2O (%) 0.121 Conductivity (~S/cm, - 50 10% suspension in deionized water) Speci~ic surface area according to BET (m2/g) c 0.1.
To measure the viscosity behaviour, 150 parts by weight of the aluminium hydroxide obtained were mixed into 100 parts of the unsaturated polyester resin (Synoiite 0020 N-2; DSM Resins BV). The processing viscosity was measured at 23C, using a Brookfield HBT
viscometer with a No. 3 spindle.
- Starting hydroxide: 368 Pas - deagglomerated hydroxide: 38 Pas Example 3:
Viscosity behaviour of further crystalline, deagglomerated aluminium hydroxides in ~P resins (Synolite 0020 N-2).
A8 compared with the specially crystallized starting product, the deagglomerated aluminium hydroxide ~hows a falling processing viscosity (here in Synolite 0020 N-2) dep~n~ing on the degree of deagglomeration.
Example:
Starting hydrate: dlo (~m) : 15.9 dso (~m) 36.3 dgo (~m) : 62.0 Viscosity at 150 phr~: 150 Pas Deagglomerated hydrate No. 1: dlo ( m) : 5.1 dso (~m) 24.6 dgo (~m) : 46.0 Viscosity at 150 phr~: 57 Pas 21~3~

Deagglomerated hydrate No. 2: dlo (~m) : 3.5 dso (~m) : 18.3 dgo (~m) : 39.6 Viscosity at 150 phr*: 41 Pas * Measurement conditions: Brookfield HBT; No. 3 spindle; 23C

Example 4:
The Al(OH)3 obtained in Example 2 was tested for comparison with commercially obt~;n~hle aluminium hydrox-ides with respect to the viscosity behaviour and elec-- trical properties.

Comparison aluminium hydroxides:
Apyral 2 (VAW) Higilite H 320 I
(Showa Denko) d50 (~m) 20 - 25 10 Soluble Na20 (%) 0.05 0.001 Na20 (%) 0.25 0.06 Specific surface area according to BET (m2/g) 0.2 3.5 ~ 50 ~m (%) 10 - 20 0 5 ~m (%) 5 - 15 25 - 35 120 parts by weight of the aluminium hydroxides concerned were wor~ed into 100 parts of the epoxy resin Rutapox 0167 (Bakelite AG, Duisburg). The viscosity measurements were carried out in accordance with the conditions in Examples 1 to 3.
For one measurement series, 1~ by weight, rela-tive to the aluminium hydroxide, of the visco~ity depres-sant BYR -W 995 (BY~ Chemie) was added to the resin 30 mixture.
Results in Pas without BYR-W 995 with BYR-W 995 Al(OH)3 according to Example 2 87 54 Apyral 2 73 53 Higilite H 320 I 138 65 21573g9 For measurement of the electrical properties (dielectric strength), a cast moulding according to I~C
St~n~rd 243 (3 mm, 20 seconds at 22C) was stored in a steam pressure vessel at 1.2 to 1.5 bar and 121C for 1, 2 and 3 days.
Results in kV/mm after 0 1 2 3 (days) Al(O~)3 according to Example 2 27 24 22 22 Apyral 2 29 7 6 5 Higilite H 320 I 28 17 16 16 For the measurement of the flame resistance according to UL-94 st~n~rd, the said epoxy resin had a degree of filling of 60% by weight. This resulted in a VO classification.

Claims (7)

Claims
1. Crystalline aluminium hydroxide, characterized by a particle size in the 50% range d50 of 15 - 50 µm, an Na2O content of 0.1%, a content of soluble Na2O of 0.005% and a specific surface area according to BET of 0.4 m2/g to 1.2 m2/g.
2. Crystalline aluminium hydroxide according to Patent Claim 1, characterized by a particle size in the 10% range d10 of 2 - 6 µm and in the 90% range d90 of 35 - 100 µm.
3. Crystalline aluminium hydroxide according to one of Patent Claims 1 to 2, characterized by the electrical conductivity of a 10% suspension of the crystalline aluminium hydroxide in deionized water of 5 25 µS/cm.
4. Process for preparing a crystalline aluminium hydroxide having tke properties according to one of Patent Claims 1 to 3, characterized by washing an aluminium hydroxide having a particle size in the 50%
range d50 of 25 - 95 µm, an Na2O content of 0.15% and a content of soluhle Na2O of 0.02% with hot water and subsequent deagglomeration of the aluminium hydroxide obtained.
5. Crystalline aluminium hydroxide, obtainable by the process according to Patent Claim 4.
6. Use of a crystalline aluminium hydroxide according to one of Claims 1 to 3 or 5 as filler for the flameproof finishing of thermosetting plastics.
7. Flameproofed thermosetting plastics, containing a crystalline aluminium hydroxide according to one of Claims 1 to 3 or 5.
CA002157389A 1993-03-15 1994-03-15 Crystalline aluminium hydroxide Abandoned CA2157389A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DEP4308176.2 1993-03-15
DE4308176A DE4308176A1 (en) 1993-03-15 1993-03-15 Crystalline aluminum hydroxide
PCT/EP1994/000798 WO1994021559A1 (en) 1993-03-15 1994-03-15 Crystalline aluminum hydroxide

Publications (1)

Publication Number Publication Date
CA2157389A1 true CA2157389A1 (en) 1994-09-29

Family

ID=6482832

Family Applications (1)

Application Number Title Priority Date Filing Date
CA002157389A Abandoned CA2157389A1 (en) 1993-03-15 1994-03-15 Crystalline aluminium hydroxide

Country Status (11)

Country Link
EP (1) EP0689519B1 (en)
JP (1) JP3536129B2 (en)
KR (1) KR100296164B1 (en)
AT (1) ATE159504T1 (en)
AU (1) AU6426094A (en)
CA (1) CA2157389A1 (en)
DE (3) DE4308176A1 (en)
DK (1) DK0689519T3 (en)
ES (1) ES2110227T3 (en)
GR (1) GR3025786T3 (en)
WO (1) WO1994021559A1 (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10020820C2 (en) * 2000-04-28 2002-03-28 Astrium Gmbh Laser beam welding device and method for laser beam welding
CZ297741B6 (en) * 2004-04-15 2007-03-21 Výzkumný ústav anorganické chemie, a. s. Process for preparing aluminium hydroxide with bayerite crystalline structure
JP2006124419A (en) * 2004-10-26 2006-05-18 Sumitomo Bakelite Co Ltd Epoxy resin composition and semiconductor device
US20080293867A1 (en) * 2005-10-18 2008-11-27 Albermarle Corporation Thermally Stable Aluminum Hydroxide Particles and Their Use as Fillers in Epoxy Laminate Resins

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3860688A (en) 1973-07-17 1975-01-14 Kaiser Aluminium Chem Corp Production of high purity alumina hydrate
DE2852273C3 (en) * 1978-12-02 1986-07-31 Vereinigte Aluminium-Werke AG, 1000 Berlin und 5300 Bonn Flame-retardant, aluminum trihydroxide-containing resin composition based on polymeric substances
GB8617387D0 (en) * 1986-07-16 1986-08-20 Alcan Int Ltd Alumina hydrates
DE4024044C2 (en) * 1990-07-28 1998-09-10 Nabaltec Gmbh Process for the production of a filler, use of the filler for flame fixing and flame-retardant plastic

Also Published As

Publication number Publication date
KR100296164B1 (en) 2001-10-22
DK0689519T3 (en) 1998-02-02
AU6426094A (en) 1994-10-11
WO1994021559A1 (en) 1994-09-29
EP0689519B1 (en) 1997-10-22
ATE159504T1 (en) 1997-11-15
DE4308176A1 (en) 1994-09-22
DE4491562D2 (en) 1996-04-25
DE59404435D1 (en) 1997-11-27
ES2110227T3 (en) 1998-02-01
JPH08508459A (en) 1996-09-10
JP3536129B2 (en) 2004-06-07
GR3025786T3 (en) 1998-03-31
EP0689519A1 (en) 1996-01-03

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Legal Events

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EEER Examination request
FZDE Discontinued