WO2010078821A1 - Procédé de préparation de sulfate de baryum sub-sphéroïde par un procédé à l'acide sulfurique et son utilisation dans un substrat de feuille de cuivre - Google Patents

Procédé de préparation de sulfate de baryum sub-sphéroïde par un procédé à l'acide sulfurique et son utilisation dans un substrat de feuille de cuivre Download PDF

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Publication number
WO2010078821A1
WO2010078821A1 PCT/CN2009/076262 CN2009076262W WO2010078821A1 WO 2010078821 A1 WO2010078821 A1 WO 2010078821A1 CN 2009076262 W CN2009076262 W CN 2009076262W WO 2010078821 A1 WO2010078821 A1 WO 2010078821A1
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WO
WIPO (PCT)
Prior art keywords
barium sulfate
sulfuric acid
barium
spherical
slurry
Prior art date
Application number
PCT/CN2009/076262
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English (en)
Chinese (zh)
Inventor
华东
刘正涛
Original Assignee
重庆科昌科技有限公司
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.)
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Publication date
Application filed by 重庆科昌科技有限公司 filed Critical 重庆科昌科技有限公司
Priority to JP2011542660A priority Critical patent/JP5575800B2/ja
Publication of WO2010078821A1 publication Critical patent/WO2010078821A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/46—Sulfates
    • C01F11/462—Sulfates of Sr or Ba
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • 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

Definitions

  • the present invention relates to barium sulfate, and in particular to a process for preparing barium sulfate by a sulfuric acid process. Background technique
  • Nano-barium sulphate has a wide range of applications in many industries such as rubber, plastics, inks, coatings, and paper.
  • Nano-barium sulphate has important structural properties such as quantum effect, size effect and surface effect. Its physical properties are different from ordinary materials. It is a new high-grade functional filling material, not only in rubber, plastics, inks, coatings, papermaking, etc. The field has broad application prospects. Moreover, it has broad application prospects in medicine, ceramics and composite materials.
  • the production process of barium sulfate is generally divided into natural ore processing and milling, mirabilite chemical synthesis and sulfuric acid synthesis.
  • the natural ore milling powder has a coarse particle size and a wide particle size distribution;
  • the Glauber's salt method contains sodium sulfide, and has a wide particle size distribution, and its particle morphology is amorphous, which is limited in some industries.
  • Chinese patent application CN 101134596 discloses a "barite sulfuric acid process for producing fine barium sulfate process", which patent prepares a fine barium sulfate product by a sulfuric acid process, but forms a precipitated barium sulfate slurry by adding sulfuric acid directly to the barium sulfide solution.
  • the barium sulfate particles have an amorphous morphology and also have a problem of a wide particle size distribution. Summary of the invention
  • One of the objects of the present invention is to provide a method for preparing barium sulfate which produces near-spherical barium sulfate to solve the problem of irregular shape and large particle size distribution of barium sulfate particles.
  • a method for preparing a near-spherical sulfuric acid barium sulfate comprising: (a) a step of calcining barite with coal to form barium sulfide, the key of which further comprises the following steps:
  • step (d) dehydrating, washing, drying, and pulverizing the barium sulfate slurry degassed in step (c) Spherical acid sour finished product.
  • the amount of air passing through the hot air is
  • the concentration of residual sulfuric acid in the barium sulfate slurry is controlled to be 0.5 to 25 g/L.
  • step (d) sodium silicate or sodium aluminate or a coupling agent is added to the washed barium sulfate slurry, and the reaction is carried out for 1.5 to 3 hours, followed by dehydration, washing and baking. Dry, smashed and finished.
  • the drying crucible is flash-dried, and the water content of the near-spherical barium sulfate finished product after drying is less than 0.2%.
  • Another object of the present invention is to provide the use of near spherical barium sulfate in a copper foil substrate.
  • the present invention obtains spherical or near-spherical barium sulfate by a cocurrent continuous synthesis process, so that the application range of barium sulfate is wider;
  • the present invention obtains a submicron-sized and continuously adjustable particle size distribution of barium sulfate by controlling the reaction rate to control the nucleation and growth rate of barium sulfate;
  • the present invention improves the whiteness of the barium sulfate product by degassing under hot conditions after the synthesis reaction;
  • the invention solves the problem of dispersion and precipitation in the downstream industry application by the surface modification of the barium sulfate powder by the coupling agent and the coating of different materials such as alumina;
  • the copper foil substrate of the present invention can improve the Tg value and flame retardancy of the substrate due to the continuous dispersion filling of the highly dispersible near-spherical submicron particles in the resin, and the higher thermal conductivity; Strictly controlled conductive ion content can support high CTI substrate production; in addition, lower hardness ensures substrate processing and mold performance.
  • FIG. 1 is a scanning electron micrograph of a barium sulfate obtained in Example 1 of the present invention. detailed description
  • step (d) Dehydrating the barium sulfate slurry degassed in step (c), washing (water ratio 1:7, temperature 90 ° C, time 2.0 h), then flash drying, hammering and pulverizing Spherical barium sulfate finished product.
  • the product was examined by electron microscopy as shown in Fig. 1.
  • the barium sulfate was spherical or nearly spherical.
  • the barium sulfate prepared in Example 1 was added to the epoxy glass fiber copper foil substrate formulation, and the amount of barium sulfate added was 2 to 35% of the total weight of the formulation.
  • step (d) filtering and dehydrating the barium sulfate slurry subjected to the degassing treatment in the step (c), washing with water, and then dissolving the filter cake in water to prepare a barium sulfate slurry, and adding a history of sodium or aluminum sulphate to the barium sulfate slurry Sodium, after reacting for 2h, filtered and dehydrated, and then washed three times with water (material ratio: 1:7, temperature: 90 ° C, time: 2.0 h), then flash-dried, pulverized to obtain near-spherical sulfuric acid coated with alumina ⁇ Finished product.
  • the barium sulfate prepared in Example 2 was added to the formulation of the phenolic resin copper foil substrate, barium sulfate The amount added is 2 - 35% of the total weight.
  • step (d) After dehydration and washing, the filter cake was dissolved in water to prepare a barium sulfate slurry, and a coupling agent KH-560 was added to the barium sulfate slurry.

Abstract

L'invention concerne un procédé de préparation de sulfate de baryum sub-sphéroïde par un procédé à l'acide sulfurique visant à résoudre les problèmes de morphologie non façonnée et de large distribution de tailles de particules des particules de sulfate de baryum, le procédé comprenant concrètement les étapes suivantes : (a) calcination de barytine avec du charbon pour produire du sulfure de baryum; (b) dissolution du sulfure de baryum dans l'eau pour préparer une solution de sulfure de baryum ayant une concentration de 70-130 g/l, et ajustement de sa température à 45-85 °C, addition de la solution de sulfure de baryum et d'acide sulfurique en excès de manière synchrone dans un réacteur continu pour produire une pâte de sulfate de baryum et de sulfure d'hydrogène, la solution de sulfure de baryum étant ajoutée au débit de 500 l/h-7000 l/h; (c) introduction d'air chaud dans la pâte de sulfate de baryum pour évacuer le sulfure d'hydrogène; et (d) déshydratation, lavage, séchage et pulvérisation de la pâte de sulfate de baryum pour obtenir le produit fini de sulfate de baryum sub-sphéroïde. On peut obtenir du sulfate de baryum sphérique ou sub-sphéroïde avec une distribution de tailles de particules ajustable en continu par ce procédé de préparation. L'invention concerne aussi l'utilisation de sulfate de baryum sub-sphéroïde comme matériau de remplissage dans des substrats de feuille de cuivre.
PCT/CN2009/076262 2009-01-06 2009-12-30 Procédé de préparation de sulfate de baryum sub-sphéroïde par un procédé à l'acide sulfurique et son utilisation dans un substrat de feuille de cuivre WO2010078821A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2011542660A JP5575800B2 (ja) 2009-01-06 2009-12-30 硫酸法による球形の硫酸バリウムの製造方法及び銅箔基板における使用

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN2009101030130A CN101475200B (zh) 2009-01-06 2009-01-06 近球形硫酸法硫酸钡的制备方法及在铜箔基板中的应用
CN200910103013.0 2009-01-06

Publications (1)

Publication Number Publication Date
WO2010078821A1 true WO2010078821A1 (fr) 2010-07-15

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PCT/CN2009/076262 WO2010078821A1 (fr) 2009-01-06 2009-12-30 Procédé de préparation de sulfate de baryum sub-sphéroïde par un procédé à l'acide sulfurique et son utilisation dans un substrat de feuille de cuivre

Country Status (3)

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JP (1) JP5575800B2 (fr)
CN (1) CN101475200B (fr)
WO (1) WO2010078821A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102010063325A1 (de) * 2010-12-17 2012-06-21 Sachtleben Chemie Gmbh Verfahren zur Herstellung von Bariumsulfat
CN102675922A (zh) * 2012-05-23 2012-09-19 贵州红星发展股份有限公司 亚微米级球状硫酸锶、其制备及应用
US10227239B2 (en) * 2014-11-10 2019-03-12 Sakai Chemical Industry Co., Ltd. Method for producing barium sulfate powder and barium sulfate powder
CN113371750A (zh) * 2021-06-08 2021-09-10 龙蟒佰利联集团股份有限公司 联合氯化法钛白废酸、硫酸法钛白废酸制备硫酸钡的方法

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101475200B (zh) * 2009-01-06 2012-02-29 重庆科昌科技有限公司 近球形硫酸法硫酸钡的制备方法及在铜箔基板中的应用
CN102674428B (zh) * 2012-05-17 2014-04-23 贵州红星发展股份有限公司 一种高白度球形纳米硫酸钡的制备方法及设备
MY183323A (en) * 2012-07-06 2021-02-18 Sakai Chemical Industry Co Barium sulfate composite particle, resin composition comprising the same, and production method thereof
CN103693671B (zh) * 2013-12-19 2015-10-21 贵州红星发展股份有限公司 一种亚微米片状硫酸钡及其制备方法
CN105381855A (zh) * 2015-10-20 2016-03-09 湖北天工物新材料科技股份有限公司 一种超细硫酸钡粉体及其生产方法
CN108473332B (zh) * 2015-12-25 2020-10-09 堺化学工业株式会社 低α射线量硫酸钡颗粒以及其利用和其制造方法
JP6176422B1 (ja) * 2015-12-25 2017-08-09 堺化学工業株式会社 低α線量硫酸バリウム粒子とその利用とその製造方法
CN105712604B (zh) * 2016-01-28 2019-03-19 乐清市拓展机械科技有限公司 一种改进的物料处理系统
CN106186027A (zh) * 2016-07-01 2016-12-07 深州嘉信化工有限责任公司 一种微粒径沉淀硫酸钡生产方法
CN108773850A (zh) * 2018-07-13 2018-11-09 贵州紫云月华新材料有限公司 一种重晶石矿化剂生产方法及其工艺

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JPS5751119A (en) * 1980-09-11 1982-03-25 Onahama Sakai Kagaku Kk Ultrafine barium sulfate
CN101121819A (zh) * 2007-09-27 2008-02-13 湖北省化学研究院 改性马来酰亚胺封端型聚酰亚胺树脂组合物及其应用
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CN101475200A (zh) * 2009-01-06 2009-07-08 重庆科昌科技有限公司 近球形硫酸法硫酸钡的制备方法及在铜箔基板中的应用
CN101475215A (zh) * 2009-01-06 2009-07-08 重庆科昌科技有限公司 一种复合二氧化钛及其制备方法

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JPS59122554A (ja) * 1982-12-28 1984-07-16 Onahama Sakai Kagaku Kk 表面処理球状硫酸バリウムの製造方法
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JP2002009443A (ja) * 2000-06-22 2002-01-11 Nec Corp 多層プリント配線板の製造方法とその製造装置
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Publication number Priority date Publication date Assignee Title
JPS5253794A (en) * 1975-10-30 1977-04-30 Nippon Chem Ind Co Ltd:The Prepartion of barium sulfate
JPS5751119A (en) * 1980-09-11 1982-03-25 Onahama Sakai Kagaku Kk Ultrafine barium sulfate
CN101134596A (zh) * 2006-08-31 2008-03-05 红星（新晃）精细化学有限责任公司 重晶石硫酸法生产精细硫酸钡工艺
CN101121819A (zh) * 2007-09-27 2008-02-13 湖北省化学研究院 改性马来酰亚胺封端型聚酰亚胺树脂组合物及其应用
CN101475200A (zh) * 2009-01-06 2009-07-08 重庆科昌科技有限公司 近球形硫酸法硫酸钡的制备方法及在铜箔基板中的应用
CN101475215A (zh) * 2009-01-06 2009-07-08 重庆科昌科技有限公司 一种复合二氧化钛及其制备方法

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102010063325A1 (de) * 2010-12-17 2012-06-21 Sachtleben Chemie Gmbh Verfahren zur Herstellung von Bariumsulfat
CN102675922A (zh) * 2012-05-23 2012-09-19 贵州红星发展股份有限公司 亚微米级球状硫酸锶、其制备及应用
US10227239B2 (en) * 2014-11-10 2019-03-12 Sakai Chemical Industry Co., Ltd. Method for producing barium sulfate powder and barium sulfate powder
CN113371750A (zh) * 2021-06-08 2021-09-10 龙蟒佰利联集团股份有限公司 联合氯化法钛白废酸、硫酸法钛白废酸制备硫酸钡的方法

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JP2012513365A (ja) 2012-06-14
CN101475200A (zh) 2009-07-08
CN101475200B (zh) 2012-02-29
JP5575800B2 (ja) 2014-08-20

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