EP1989263A1 - Sulfate de baryum - Google Patents

Sulfate de baryum

Info

Publication number
EP1989263A1
EP1989263A1 EP07704685A EP07704685A EP1989263A1 EP 1989263 A1 EP1989263 A1 EP 1989263A1 EP 07704685 A EP07704685 A EP 07704685A EP 07704685 A EP07704685 A EP 07704685A EP 1989263 A1 EP1989263 A1 EP 1989263A1
Authority
EP
European Patent Office
Prior art keywords
barium sulfate
barium
sulfate
sodium
compounds
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.)
Withdrawn
Application number
EP07704685A
Other languages
German (de)
English (en)
Inventor
Sonja Grothe
Jochen Winkler
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.)
Venator Germany GmbH
Original Assignee
Sachtleben Chemie GmbH
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 Sachtleben Chemie GmbH filed Critical Sachtleben Chemie GmbH
Publication of EP1989263A1 publication Critical patent/EP1989263A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/027—Barium sulfates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
    • Y10T428/2995—Silane, siloxane or silicone coating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2998—Coated including synthetic resin or polymer

Definitions

  • the present invention is a process for the preparation of barium sulfate with an organically modified surface, the barium sulfate prepared by this process and its use.
  • Barium sulfate is used as an inert filler in many applications.
  • the use of barium sulphate in polymeric materials has a positive effect on the properties of these materials.
  • barium sulfate shows no interaction with the polymeric materials.
  • the targeted adjustment of the interactions between filler and polymer is one way to adjust the properties of these composites. Therefore, it is desirable to be able to specifically modify the surface of barium sulfate particles in order to be able to adjust these interactions in a targeted manner.
  • EP-A-0293622 discloses a process for producing barium sulfate having a chemoreactive surface by coprecipitation of barium ions with organic compounds.
  • organic compounds for example, alkyl or aryl sulfates are used, which are optionally substituted with functional groups. This process has the disadvantage that the coprecipitation of barium sulfate and organic compounds, the particle size and the
  • the object of the present invention is to overcome the disadvantages of the prior art.
  • the object of the present invention is to provide a process for producing barium sulfate with an organically modified surface, by which the particle size and the particle morphology of the precipitated barium sulfate are not influenced.
  • Another object of the present invention is to provide a process for producing barium sulfate having an organically modified surface, in which the barium sulfate is subsequently organically modified, that is to say after the precipitation.
  • Another object of the present invention is to provide a process for producing organically modified surface barium sulfate which prevents foaming by the organic compounds used for modification during precipitation.
  • Another object of the present invention is to provide a process for the production of barium sulfate with an organically modified surface which reduces the high organic load of the effluent from the concentration of precipitation suspensions.
  • the objects are achieved by a method that allows to carry out the organic modification of the surface of the barium sulfate only after the precipitation of the barium sulfate.
  • This procedure has the advantage that the particle formation in the precipitation of barium sulfate can be carried out in the usual way. That is, on the one hand, the Particle formation is not adversely affected by coprecipitates, but on the other hand it is easier to control the particle size and morphology of the barium sulfate particles.
  • the precipitation of the barium sulfate to be used according to the invention can be carried out by all methods known from the prior art.
  • Barium sulfate is preferably used in a precipitation reactor for precipitating nanoscale particles, in particular a reaction cell for the ultrafast mixing of several reactants, for example of aqueous solutions of barium hydroxide and sodium and / or zinc sulfide and / or
  • the barium sulfate is present after precipitation in the form of a precipitation suspension.
  • the barium sulfate used according to the invention is washed and concentrated, so that the wastewater produced is not organically contaminated.
  • the barium sulfate is now in the form of a concentrated barium sulfate suspension.
  • the preparation of the barium sulfate according to the invention can be carried out by processes known per se.
  • the barium sulfate suspension is mixed with a barium component, so that a barium excess is formed.
  • the barium component used may be any water-soluble barium compound, for example barium sulphide, barium chloride and / or barium hydroxide.
  • the barium ions adsorb on the surfaces of the barium sulfate particles.
  • organic compounds are added to this suspension with vigorous stirring and / or during dispersion.
  • the organic compounds should be selected so that they form a sparingly soluble compound with barium ions.
  • the organic compounds precipitate with the excess barium ions on the surface of the barium sulfate.
  • Suitable organic compounds are compounds selected from the group of the alkyl and / or arylsulfonates, alkyl and / or aryl sulfates, alkyl and / or aryl phosphoric acid esters or mixtures of at least two of these compounds, wherein the alkyl or aryl radicals may be substituted by functional groups.
  • the organic compounds may be fatty acids, which may have functional groups. It is also possible to use mixtures of at least two such compounds.
  • the barium sulfate modified according to the invention can either be used directly in the form of the present aqueous paste or dried before use.
  • the drying can be carried out by methods known per se become.
  • the use of convection dryers, spray dryers, grind dryers, freeze dryers and / or pulsation dryers is particularly suitable for drying.
  • other dryers are likewise usable according to the invention.
  • subsequent grinding of the dried powders may be necessary.
  • the grinding can be carried out by methods known per se.
  • inventively modified barium sulfate can be further treated after the orgnanischen modification with functional silane derivatives or functional siloxanes.
  • inventively modified barium sulfate can be further treated after the orgnanischen modification with functional silane derivatives or functional siloxanes.
  • Methyltriethoxysilane ⁇ -methacryloxypropyltrimethoxysilane, ⁇ -glycidyloxypropyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane, ⁇ -isocyanatopropyltriethoxysilane.
  • the barium sulfate modified according to the invention can be used in the field of composite materials, for example for improving the mechanical properties of plastics, preferably thermoplastics, thermosets and / or elastomers.
  • the inventively modified barium sulfate can be used in polymeric materials as nucleating agents.
  • the crystallinity of polymeric materials is through the use of the inventively modified barium sulfate increases.
  • it is used in paints and coatings, while also having a positive effect on mechanical properties and other properties such as glass transition temperature and chemical resistance.
  • Further examples of fields of use of the barium sulfate modified according to the invention are: adhesives, composites in conjunction with metals or ceramic materials, cosmetics, synthetic fibers.
  • the particle size and morphology of the barium sulfate particles that is, for example, whether cubic, platelet or spherical particles are formed, in the precipitation is easier to control, since the precipitation is not affected by coprecipitates;
  • the organic compound preferably precipitates on the barium sulfate surface, since the excess barium ions are deposited on the particle surface;
  • a process for producing organically modified surface barium sulfate comprising the steps of: a) adding a concentrated barium sulfate suspension with a barium component and then b) adding organic compounds to the suspension.
  • a process for the production of barium sulfate with an organically modified surface which comprises the following steps: a) addition of a concentrated barium sulfate suspension with a barium component, then b) addition of organic compounds to the suspension and c) aftertreatment of the organically modified barium sulfate particles with functional silane derivatives and / or functional siloxanes.
  • the barium component in step a) is a water-soluble barium compound, preferably selected from barium sulphide, barium chloride and / or barium hydroxide;
  • the organic compounds in step b) are those which form compounds sparingly soluble with barium ions,
  • the organic compounds are selected from the group of alkyl and / or arylsulfonates, alkyl and / or aryl sulfates, alkyl and / or Arylphosphorklareester, wherein the alkyl or aryl radicals may be substituted by functional groups, and / or fatty acids which optionally have functional groups, or mixtures of at least two of these compounds;
  • the organic compounds are selected from: alkylsulfonic acid salts,
  • step c) The organically modified Bariumsulfatpumble in step c) are aftertreated with functional silane derivatives and / or functional siloxanes;
  • the functional silane derivatives and / or functional siloxanes are selected from:
  • Octyltriethoxysilane methyltriethoxysilane, ⁇ -methacryloxypropyltrimethoxysilane, ⁇ -glycidyloxypropyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane, ⁇ -isocyanatopropyltriethoxysilane, or mixtures of at least two of these compounds;
  • a barium sulfate obtainable by the process according to the invention for the production of barium sulfate with an organically modified surface
  • barium sulfate according to the invention for use in polymeric materials, preferably in thermoplastics, thermosets and / or elastomers;
  • barium sulfate according to the invention in adhesives, composites in connection with metals or ceramic materials, in cosmetics, and / or
  • barium sulfate according to the invention as nucleating agent in polymeric materials.
  • barium sulfate is precipitated from one liter of 0.5 molar barium chloride solution and one liter of 0.5 molar sodium sulfate solution.
  • the flow rates of the educts are 100 mL / min.
  • the precipitate is filtered and washed to pH 6.
  • the washed filter cake is dispersed in a dissolver at speeds of 1000 min -1 for 15 min and adjusted to a solids content of 30% with demineralized water .. During dispersion in the dissolver, a barium excess is adjusted by the addition of 0.1 molar barium hydroxide solution.
  • 0.3 molar barium hydroxide solution is added to the dispersed barium sulfate suspension with vigorous stirring, so that a pH of 1 1, 5 established.
  • the suspension is mixed with 100 g Oleylcetylalkoholsulfat, Na-SaIz, and stirred for a further 20 min. With 0.4 molar sulfuric acid, the pH of the suspension is then adjusted to 6.5. The product is then spray-dried. The carbon content of the product is 4.4%. After extraction in ethanol, a carbon content of 4.3% is determined.
  • the barium sulfate powder prepared according to Example 3 is used in an acrylate clearcoat to improve the mechanical properties of the paint.
  • a millbase is prepared with the following composition: Macrynal SM 510 n: 42.3 parts by weight
  • Barium sulfate 55.0 parts by weight.
  • This millbase is dispersed on Skandex using 2 mm glass beads for 75 min.
  • the dispersing fineness of the thus-dispersed millbase is ⁇ 5 ⁇ m.
  • the millbase was then diluted with hardener and adjuvant solution as follows:
  • Lacquered elevators with wet film thicknesses of 50 ⁇ m, 100 ⁇ m and 150 ⁇ m were produced on black glass plates and dried overnight.
  • the remission of the dried lacquer layers are:
  • the pendulum hardness of the thus modified clearcoat was increased by 10% compared to the unfilled clearcoat.

Abstract

La présente invention concerne un procédé de production de sulfate de baryum à surface modifiée organiquement, le sulfate de baryum produit selon ledit procédé et son utilisation.
EP07704685A 2006-02-21 2007-02-21 Sulfate de baryum Withdrawn EP1989263A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006008413 2006-02-21
PCT/EP2007/051672 WO2007096385A1 (fr) 2006-02-21 2007-02-21 Sulfate de baryum

Publications (1)

Publication Number Publication Date
EP1989263A1 true EP1989263A1 (fr) 2008-11-12

Family

ID=38057371

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07704685A Withdrawn EP1989263A1 (fr) 2006-02-21 2007-02-21 Sulfate de baryum

Country Status (5)

Country Link
US (1) US7645334B2 (fr)
EP (1) EP1989263A1 (fr)
JP (1) JP5448461B2 (fr)
CN (1) CN101400744A (fr)
WO (1) WO2007096385A1 (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2057218A1 (fr) * 2006-08-25 2009-05-13 Sachtleben Chemie GmbH Composite contenant du sulfate de baryum
GB2469991B (en) * 2009-04-21 2013-08-07 Invibio Ltd Polymeric materials
CN103881418B (zh) * 2014-03-05 2016-04-06 苏州克莱明新材料有限公司 改性纳米硫酸钡的制备及其应用
CN104709934B (zh) * 2015-02-05 2016-03-23 成都新柯力化工科技有限公司 一种纤维状硫酸钡的制备方法
CN104845410B (zh) * 2015-04-02 2018-10-26 上海奥塞尔材料科技有限公司 一种塑料改性剂的制备及其应用
KR102470961B1 (ko) * 2016-10-28 2022-11-24 사카이 가가쿠 고교 가부시키가이샤 황산바륨 분체 및 그것을 함유하는 수지 조성물
EP3581269B1 (fr) * 2017-04-11 2022-09-28 Cataler Corporation Catalyseur pour la purification de gaz d'échappement et procédé de preparation
CN107987560A (zh) * 2017-10-20 2018-05-04 英德市日昇矿业有限公司 一种百叶窗叶用改性重质碳酸钙及其制备方法
CN112299467B (zh) * 2019-07-31 2022-10-28 北京化工大学 一种单分散油相纳米硫酸钡分散体的制备方法
CN111234565A (zh) * 2020-03-16 2020-06-05 库车塔北泥浆材料有限公司 活化重晶石粉的改性方法
CN113234333B (zh) * 2021-04-09 2021-11-05 苏州吉人高新材料股份有限公司 一种光致变色硫酸钡粉体的制备方法

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DE3718277A1 (de) * 1987-05-30 1988-12-15 Metallgesellschaft Ag Verfahren zur herstellung von bariumsulfat mit chemoreaktiver oberflaeche
JP3799558B2 (ja) * 1995-12-12 2006-07-19 日本化学工業株式会社 硫酸バリウムとその製造方法ならびに樹脂組成物
US6274662B1 (en) * 1999-04-09 2001-08-14 J.M. Huber Corporation Vulcanizable elastomeric compositions containing surface treated barium sulfate and vulcanizates thereof
US6194070B1 (en) * 1999-04-09 2001-02-27 J. M. Huber Corporation Surface treated barium sulfate and method of preparing the same
DE10005685A1 (de) * 2000-02-09 2001-08-23 Sachtleben Chemie Gmbh Bariumsulfat, Verfahren zu dessen Herstellung und dessen Verwendung
DE10026791A1 (de) * 2000-05-31 2001-12-06 Solvay Barium Strontium Gmbh Mikronisiertes Bariumsulfat
JP3755745B2 (ja) * 2001-08-09 2006-03-15 株式会社ノエビア 粉体固型ファンデーション
US6849673B2 (en) * 2003-07-02 2005-02-01 J. M. Huber Corporation Film forming coating composition containing surface treated barium sulfate, and methods of use
DE10357116A1 (de) * 2003-12-06 2005-07-07 Solvay Barium Strontium Gmbh Desagglomeriertes Bariumsulfat
EP1753827B1 (fr) * 2004-05-04 2011-10-12 Centrum für Angewandte Nanotechnologie (CAN) GmbH Procede de preparation d'un sulfate dispersible, de preference des nanoparticules de sulfate de baryum
JP4583147B2 (ja) * 2004-11-19 2010-11-17 三井金属鉱業株式会社 導電性複合粉末及びその製造方法
DE102005047807A1 (de) * 2005-06-04 2006-12-07 Solvay Infra Bad Hönningen GmbH Modifizierte Nanopartikel
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Also Published As

Publication number Publication date
JP2009527452A (ja) 2009-07-30
JP5448461B2 (ja) 2014-03-19
WO2007096385A1 (fr) 2007-08-30
US20080314291A1 (en) 2008-12-25
US7645334B2 (en) 2010-01-12
CN101400744A (zh) 2009-04-01

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