WO2005108291A1 - Processus ameliore de production de silice amorphe pure en particulier de xerogels destines a stabilisation de la biere et a d'autres fins d'isolation - Google Patents

Processus ameliore de production de silice amorphe pure en particulier de xerogels destines a stabilisation de la biere et a d'autres fins d'isolation Download PDF

Info

Publication number
WO2005108291A1
WO2005108291A1 PCT/NO2005/000155 NO2005000155W WO2005108291A1 WO 2005108291 A1 WO2005108291 A1 WO 2005108291A1 NO 2005000155 W NO2005000155 W NO 2005000155W WO 2005108291 A1 WO2005108291 A1 WO 2005108291A1
Authority
WO
WIPO (PCT)
Prior art keywords
silica
leaching
accordance
sio
temperature
Prior art date
Application number
PCT/NO2005/000155
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 WO2005108291A1 publication Critical patent/WO2005108291A1/fr

Links

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
    • 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
    • C01B33/16—Preparation of silica xerogels

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 silica on the market 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. Further, 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 includes the following steps:
  • MeCI 2l Heating the crushed ( ⁇ 100 ⁇ m) quartz or other SiO 2 based raw material together with MgCI 2 or CaCI 2 , or other chlorides like BeCI 2 , SrCI 2 and BaCI 2 , in the following referred to as MeCI 2l to a temperature in the range 800 - 1300 ° C preferably over a single or a two stage calcination steps for a period of 0.5 to 3 hours, depending on the temperature, wherein the ratio of MeCI 2 to the SiO 2 is equal to or 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 HCI wherein x is greater than y in order to obtain a conversion of SiO 2 to magnesium (or calcium) silicates in excess of 99.9%.
  • Step 3 Separating insoluble silica from the solution using filters (belt filter, press filter, filter press etc.) or another separation method.
  • the solution contains excess of HCI, MeCI 2 and impurities.
  • Step 4 Recycling of the chloride solution to step 1 and the HCI solution to step 2 using a recovery system in order to separate the solutions.
  • the impurities are removed prior to the reuse of the solutions in order to avoid build-up of impurities.
  • Several techniques can be used to remove impurities depending on the amount of impurities in the raw materials, but one way is to precipitate impurities as hydroxides at elevated pH.
  • the purity of acid-set silica gels A and B is very high, typically 99.96-99.98%SiO 2 , which makes them extremely useful in such applications as Zeolite production, insulation, in food industry etc.
  • Example 1 Silica A. Calcium silicate/water mixing. Calcium silicate produced in Step 1 with particle size ⁇ 200micron (200kg) was fed to a tank containing 360 litre of water under continuous agitation. Samples of the slurry were taken to test the homogeneity of the silicate distribution in water. Leaching. The slurry of calcium silicate and water was fed to the reactor filled with
  • Washing at the filter press was made in three steps: washing from diagonal 1 , washing from diagonal 2 and central washing. To get silica with purity >99.95% SiO 2 the repulping stage was repeated twice. The washing procedure was controlled by the chloride content in the wash water and in wet cake ( ⁇ 30ppm). The wet cake contained about 90%) water. Drying. The wet cake was dried in a Barr-Rosin ring drier, and the dried silica was jet milled.
  • Example 2 Silica B Calcium silicate/water mixing was made as in Example 1. Leaching. The slurry of calcium silicate and water was fed to the reactor filled with 15.85%) hydrochloric acid (1520 litre). Slurry feeding took about 30 min under agitation. After the slurry addition the final acid concentration in the reactor was 13%. The temperature in the reactor was 45°C and the agitator was operated with 100%) speed. The reactor was heated to 150°C. The leaching proceeded at this temperature for 60 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 passed to a filter press. Filtration and washing was made as in Example 1. The wet cake contained about 80%- 84%) water. Drying.
  • This type of silica had the following characteristics: Surface area, 480 m2/g; pore volume, 1.05 ml/g, pore radius, 4,2 nm; bulk density 0,25 g/ml; absorption, 180 ml oil/1 OOg; % of SiO 2 99,97; and pH 5,0.
  • Average particle size was 70 micron.
  • the particle size (D 5 n) was 20micron.
  • Spray dried silica A and B can be used for filtration purposes, as catalyst carriers, beer stabilizer or for other purposes that require very pure silica, e.g. zeolite production.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

La présente invention concerne la production de silice amorphe à partir de quartz ou d'une autre matière première à base de SiO2, qui comprend l'étape suivante: chauffage (étape de calcination) de quartz ou d'une autre matière première à base de SiO2 avec MgCl2, CaCl2 ou d'autres chlorures tels que BeCl2, SrCl2 et BeCl2 (communément regroupés en MeCl 2) à une température comprise entre 800 et 1300 °C, le rapport de masse de MeCl2 sur SiO2 étant supérieur ou égal à 2 et la présence de vapeur d'eau en excès de la quantité stoéchiométrique nécessaire, lessivage de préférence à des températures comprises entre 50 et 95 °C ou entre 110 et 170 °C de la silice produite avec HCI de façon à former une solution de MeCl2 avec une silice insoluble, séparation de la silice insoluble de la solution, recyclage de MeCl2 à l'étape de chauffage et de la solution HCI restante à l'étape du lessivage.
PCT/NO2005/000155 2004-05-12 2005-05-12 Processus ameliore de production de silice amorphe pure en particulier de xerogels destines a stabilisation de la biere et a d'autres fins d'isolation WO2005108291A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
NO20041960 2004-05-12
NO20041960 2004-05-12
NO20042646A NO20042646D0 (no) 2004-05-12 2004-06-23 Forbedret prosess for fremstilling av ren amorf siliciumoksyd spesielt zerogel for stabilisering av ol, samt for isolasjonsformal
NO20042646 2004-06-23

Publications (1)

Publication Number Publication Date
WO2005108291A1 true WO2005108291A1 (fr) 2005-11-17

Family

ID=35005955

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/NO2005/000155 WO2005108291A1 (fr) 2004-05-12 2005-05-12 Processus ameliore de production de silice amorphe pure en particulier de xerogels destines a stabilisation de la biere et a d'autres fins d'isolation

Country Status (2)

Country Link
NO (1) NO20042646D0 (fr)
WO (1) WO2005108291A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9205375B2 (en) 2007-09-20 2015-12-08 Skyonic Corporation Removing carbon dioxide from waste streams through co-generation of carbonate and/or bicarbonate minerals
US9359221B2 (en) 2010-07-08 2016-06-07 Skyonic Corporation Carbon dioxide sequestration involving two-salt-based thermolytic processes
US9968883B2 (en) 2014-01-17 2018-05-15 Carbonfree Chemicals Holdings, Llc Systems and methods for acid gas removal from a gaseous stream
US10583394B2 (en) 2015-02-23 2020-03-10 Carbonfree Chemicals Holdings, Llc Carbon dioxide sequestration with magnesium hydroxide and regeneration of magnesium hydroxide

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 (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9205375B2 (en) 2007-09-20 2015-12-08 Skyonic Corporation Removing carbon dioxide from waste streams through co-generation of carbonate and/or bicarbonate minerals
US9359221B2 (en) 2010-07-08 2016-06-07 Skyonic Corporation Carbon dioxide sequestration involving two-salt-based thermolytic processes
US9968883B2 (en) 2014-01-17 2018-05-15 Carbonfree Chemicals Holdings, Llc Systems and methods for acid gas removal from a gaseous stream
US10583394B2 (en) 2015-02-23 2020-03-10 Carbonfree Chemicals Holdings, Llc Carbon dioxide sequestration with magnesium hydroxide and regeneration of magnesium hydroxide
US11498029B2 (en) 2015-02-23 2022-11-15 Carbonfree Chemicals Holdings, Llc Carbon dioxide sequestration with magnesium hydroxide and regeneration of magnesium hydroxide
US11772046B2 (en) 2015-02-23 2023-10-03 Carbonfree Chemicals Holdings, Llc Carbon dioxide sequestration with magnesium hydroxide and regeneration of magnesium hydroxide

Also Published As

Publication number Publication date
NO20042646D0 (no) 2004-06-23

Similar Documents

Publication Publication Date Title
EP2519470B1 (fr) Procédés pour produire du trifluorure de aluminium
CA1095877A (fr) Traduction non-disponible
US20100129279A1 (en) Extraction and Purification of Minerals From Aluminium Ores
US5000933A (en) Process for hydrothermal production of sodium silicate solutions
CA1082881A (fr) Traitement de fines en suspension dans l'air, contenant du dioxyde de silicium afin de precipiter les silicates et la silice
IE904224A1 (en) Process for preparing alkali metal silicates
WO2005108291A1 (fr) Processus ameliore de production de silice amorphe pure en particulier de xerogels destines a stabilisation de la biere et a d'autres fins d'isolation
CA1093535A (fr) Traduction non-disponible
US7534411B2 (en) Process for the preparation of pure silica
KR101788891B1 (ko) 사플루오르화 규소의 제조 방법
WO2005108290A1 (fr) Procede perfectionne pour produire de la silice amorphe pure a partir de quartz, de preference a utiliser en tant que matiere de charge
EP3277631B1 (fr) Fluorite synthétique de haute pureté, procédé pour sa préparation et appareil utilisé à cet effet
Krysztafkiewicz et al. Silica recovery from waste obtained in hydrofluoric acid and aluminum fluoride production from fluosilicic acid
WO2005108292A1 (fr) Procede ameliore de production de silice amorphe et hydrophobe pure a partir du quartz
AU3912200A (en) Production of fumed silica
WO2005108293A1 (fr) Procede ameliore de production de silice mesoporeuse amorphe pure a partir de quartz
WO1999008959A1 (fr) Procede de production d'acide de silice
CA2592499C (fr) Procede de preparation de zeolite a, un adjuvant pour detergent, a partir de residus de kimberlite
CN1044632A (zh) 热液生产硅酸钠溶液的方法
CN1197765A (zh) 一种用铝土矿提纯氧化铝的方法
JPS6152082B2 (fr)
US20040025637A1 (en) Method for rendering inert dust residue containing silicon metal
OA18423A (en) High purity synthetic fluorite, process for preparing the same and apparatus therefor.

Legal Events

Date Code Title Description
AK Designated states

Kind code of ref document: A1

Designated state(s): AE AG AL AM AT AU AZ BA BB BG BR BW BY BZ CA CH CN CO CR CU CZ DE DK DM DZ EC EE EG ES FI GB GD GE GH GM HR HU ID IL IN IS JP KE KG KM KP KR KZ LC LK LR LS LT LU LV MA MD MG MK MN MW MX MZ NA NG NI NO NZ OM PG PH PL PT RO RU SC SD SE SG SK SL SM SY TJ TM TN TR TT TZ UA UG US UZ VC VN YU ZA ZM ZW

AL Designated countries for regional patents

Kind code of ref document: A1

Designated state(s): BW GH GM KE LS MW MZ NA SD SL SZ TZ UG ZM ZW AM AZ BY KG KZ MD RU TJ TM AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LT LU MC NL PL PT RO SE SI SK TR BF BJ CF CG CI CM GA GN GQ GW ML MR NE SN TD TG

121 Ep: the epo has been informed by wipo that ep was designated in this application
NENP Non-entry into the national phase

Ref country code: DE

WWW Wipo information: withdrawn in national office

Country of ref document: DE

122 Ep: pct application non-entry in european phase