WO2005108290A1 - Procede perfectionne pour produire de la silice amorphe pure a partir de quartz, de preference a utiliser en tant que matiere de charge - Google Patents

Procede perfectionne pour produire de la silice amorphe pure a partir de quartz, de preference a utiliser en tant que matiere de charge Download PDF

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Publication number
WO2005108290A1
WO2005108290A1 PCT/NO2005/000154 NO2005000154W WO2005108290A1 WO 2005108290 A1 WO2005108290 A1 WO 2005108290A1 NO 2005000154 W NO2005000154 W NO 2005000154W WO 2005108290 A1 WO2005108290 A1 WO 2005108290A1
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WO
WIPO (PCT)
Prior art keywords
silica
quartz
leaching
solution
meci
Prior art date
Application number
PCT/NO2005/000154
Other languages
English (en)
Inventor
Birger Langseth
Christian Rosenkilde
Natalia Loboda
Original Assignee
Promeks As
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 Promeks As filed Critical Promeks As
Publication of WO2005108290A1 publication Critical patent/WO2005108290A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/126—Preparation of silica of undetermined type
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica

Definitions

  • the present invention relates to the production of pure amorphous silica from quartz or other SiO 2 based raw materials.
  • Several types of silica can be produced by using the techniques described in this application. Common for most of them is the purity of the silica, which is higher than commercial silicas on the marked today.
  • the silica content in the product silica might be as high as 99.98%.
  • the various types of silica can be used for beer stabilization, insulation, catalysts and silicon rubber, and other applications that require pure silica. There are small differences during the production process for the various types of silica.
  • Amorphous silica is mainly produced by acidulation of a soluble silicate, commonly by addition of sulphuric or hydrochloric acid to a sodium silicate (water glass) solution.
  • the products are either precipitated silica or silica gel depending upon details in the production process.
  • other known processes silicon tetrachloride/alkoxide reacts with hydrogen and oxygen to form fumed silica are used commonly in the present silica industry.
  • US patent No. 1 ,868,499 relates to a process for recovering alumina from silicious materials where silica is considered as an unwanted by-product and no further processing of this product is carried out.
  • US patent No. 4689315 describes a method for the production of amorphous silica particles where the lime and the hydrochloric acid are consumed in the process.
  • European patent, EP 1265812 B1 relates to a process for the preparation amorphous silica where the raw materials are similar to the present invention, but where the process is limited with respect to the type of silica that can be produced, the purity of the silica product and that CaCI 2 is the only reagent used in the mixture with the raw materials.
  • the silica product according to the present invention is very pure, having an amorphous silica content of more than 90%, and it can be used for several applications that never have been investigated before.
  • the chemical impurities are at a much lower level than the commercial silica types, and the produced amorphous silica can have a very high surface area.
  • the silica is produced from quartz or other SiO 2 based materials and all other reagents, chemicals like mineral acid and chlorides from all elements in the group II of the periodic table (Be-Mg-Ca-Sr-Ba-Ra), used in the process are recycled. Only minor amounts for make-up of these chemicals are required.
  • the process according to the invention for production of amorphous silica from quartz include the following steps:
  • MeCI 2 Heating the crushed ( ⁇ 100 ⁇ m) quartz together with MgCI 2 or CaCI 2 or other chlorides like BeCI 2 , SrCl 2 and BaCI 2 , in the following referred to as MeCI 2 , to a temperature in the range 800 - 1300 c preferably over a two stage calcinations step for a period of 0.5 to 3 hours, depending on the temperature, wherein the ratio of MeCI 2 to the quartz is greater than 2 and in the presence of water vapour in excess of the stoichiometric amount (preferable at least 7%) needed for the reaction: x MeCI 2 + y SiO 2 + x H 2 O - (MeO)x * (SiO 2 )y + 2x HCl wherein x is greater than y in order to obtain a conversion of quartz to magnesium (or calcium) silicates in excess of 99.9%.
  • the HCl produced during calcination is absorbed in a scrubber and via step 4 reused in step 2.
  • the solution contains excess of HCl, MeCI 2 and impurities.
  • Leaching 1000 litres of 20% HCl was fed to the reactor filled with 200kg of calcium silicate produced according to step 1. Acid feeding took about 45 minutes under agitation. The reactor was heated to 100°C, the agitator was operateed with 100% speed. The leaching proceeded at this temperature for 90 minutes. After cooling of the leaching slurry to 40°C-45°C the reactor was emptied to an intermediate tank from which the leaching slurry was passed to a filter press. Filtration and washing.
  • the wet cake was dried in a Barr-Rosin ring drier.
  • the silica properties were as follows.
  • Particle size (D 50 ) of silica C is 20-30micron
  • D 50 is 25-35 micron.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne un procédé de production de silice amorphe à partir de quartz. Ce procédé comprend les étapes consistant à: chauffer (étapes de calcination) le quartz ou un autre matériau à base de SiO2 comprenant du MgCl2 à une température comprise entre 800 et 1300 °C, le rapport pondéral de MgCl2 par rapport au quartz étant supérieur à 2, et la présence de vapeur d'eau étant en excès par rapport à la quantité stoechiométrique nécessaire pour obtenir MgSiO3 ou Mg2SiO4, lixivier, à des températures préférentielles comprises entre 50 et 150 °C, le silicate produit avec du HCl pour former une solution de MgCl2 avec de la silice insoluble, séparer la silice insoluble de cette solution, recycler le MgCl2 pour l'étape de chauffage et la solution de HCl pour l'étape de lixiviation. D'autres chlorures, notamment BeCl2, CaCl2, SrCl2 et BaCl2 peuvent être utilisés dans le procédé au lieu de MgCl2.
PCT/NO2005/000154 2004-05-12 2005-05-12 Procede perfectionne pour produire de la silice amorphe pure a partir de quartz, de preference a utiliser en tant que matiere de charge WO2005108290A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
NO20041961 2004-05-12
NO20041961 2004-05-12

Publications (1)

Publication Number Publication Date
WO2005108290A1 true WO2005108290A1 (fr) 2005-11-17

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/NO2005/000154 WO2005108290A1 (fr) 2004-05-12 2005-05-12 Procede perfectionne pour produire de la silice amorphe pure a partir de quartz, de preference a utiliser en tant que matiere de charge

Country Status (1)

Country Link
WO (1) WO2005108290A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102225766A (zh) * 2011-03-29 2011-10-26 东海县圣达石英制品有限公司 太阳能光伏产业用超纯硅材料的制备方法
CN109292783A (zh) * 2018-10-31 2019-02-01 深圳市鑫美威自动化设备有限公司 一种含MgSiO3矿渣的综合利用方法
CN111908476A (zh) * 2020-08-19 2020-11-10 昆明理工大学 一种石英砂加压氯化浸出的提纯方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1868499A (en) * 1929-06-07 1932-07-26 Electric Smelting & Aluminum C Process of recovering alumina from silicious materials containing it
WO1997022554A1 (fr) * 1995-12-15 1997-06-26 Mashal Alumina Industries Ltd. Procede pour recuperer de l'alumine et de la silice
WO1999008959A1 (fr) * 1997-08-14 1999-02-25 Goodanew, Martin, Eric Procede de production d'acide de silice
EP1265812B1 (fr) * 2000-02-10 2003-11-19 Promeks AS Procede de preparation de silice amorphe

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1868499A (en) * 1929-06-07 1932-07-26 Electric Smelting & Aluminum C Process of recovering alumina from silicious materials containing it
WO1997022554A1 (fr) * 1995-12-15 1997-06-26 Mashal Alumina Industries Ltd. Procede pour recuperer de l'alumine et de la silice
WO1999008959A1 (fr) * 1997-08-14 1999-02-25 Goodanew, Martin, Eric Procede de production d'acide de silice
EP1265812B1 (fr) * 2000-02-10 2003-11-19 Promeks AS Procede de preparation de silice amorphe

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102225766A (zh) * 2011-03-29 2011-10-26 东海县圣达石英制品有限公司 太阳能光伏产业用超纯硅材料的制备方法
CN109292783A (zh) * 2018-10-31 2019-02-01 深圳市鑫美威自动化设备有限公司 一种含MgSiO3矿渣的综合利用方法
CN111908476A (zh) * 2020-08-19 2020-11-10 昆明理工大学 一种石英砂加压氯化浸出的提纯方法

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