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WO2010147500A1 - Method for producing silicon dioxide - Google Patents

Method for producing silicon dioxide Download PDF

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Publication number
WO2010147500A1
WO2010147500A1 PCT/RU2010/000156 RU2010000156W WO2010147500A1 WO 2010147500 A1 WO2010147500 A1 WO 2010147500A1 RU 2010000156 W RU2010000156 W RU 2010000156W WO 2010147500 A1 WO2010147500 A1 WO 2010147500A1
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WO
WIPO (PCT)
Prior art keywords
solution
demineralized water
sodium silicate
reactor
battery acid
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.)
Ceased
Application number
PCT/RU2010/000156
Other languages
French (fr)
Russian (ru)
Inventor
Святослав Леонидович ЛОСЬ
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.)
OBSCHESTVO S OGRANICHENNOI OTVETSTVENNOSTYU "SINTETICHESKIE KREMNEZEMY"
Original Assignee
OBSCHESTVO S OGRANICHENNOI OTVETSTVENNOSTYU "SINTETICHESKIE KREMNEZEMY"
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Filing date
Publication date
Application filed by OBSCHESTVO S OGRANICHENNOI OTVETSTVENNOSTYU "SINTETICHESKIE KREMNEZEMY" filed Critical OBSCHESTVO S OGRANICHENNOI OTVETSTVENNOSTYU "SINTETICHESKIE KREMNEZEMY"
Publication of WO2010147500A1 publication Critical patent/WO2010147500A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
    • C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates

Definitions

  • the present invention relates to technological processes in the field of chemistry and can be used to obtain silicon dioxide in the form of a fine powder.
  • the solution from the collection with a solution of sodium silicate in demineralized water at room temperature is supplied at a speed of 20 l / min, and from the collection with a solution of battery acid at room temperature at a speed of 8 l / min.
  • This provides a pH of the growth medium from 10 to 1 1.
  • the supply of solutions to the reactor should not be less than 25 minutes.
  • the resulting silicon dioxide is a white fine powder having an amorphous structure.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The invention relates to the field of chemistry. A solution of sodium silicate in demineralized water and a solution of battery acid are prepared in separate vessels at room temperature. A hot solution of sodium silicate in demineralized water is prepared in a reactor during continuous agitation and heating, and the temperature of the solution is maintained at 94°C. The solutions of sodium silicate in demineralized water and battery acid are then fed simultaneously from the vessels into the reactor. Once a pH of from 10 to 11 has been reached in the reactor, battery acid is added to lower the pH to 4.5. The resulting suspension of precipitated silicon dioxide is isolated and dried. The silicon dioxide has an amorphous structure and is in the form of a white, fine-grained powder.

Description

Способ получения двуокиси кремния The method of producing silicon dioxide

Настоящее изобретение относится к технологическим процессам в области химии и может быть использовано для получения двуокиси кремния в форме мелкодисперсного порошка.The present invention relates to technological processes in the field of chemistry and can be used to obtain silicon dioxide in the form of a fine powder.

Сущность предложенного способа рассмотрим на примере его реализации.The essence of the proposed method, consider the example of its implementation.

1. В отдельном сборнике с объемом 0,5 м.куб. готовят раствор силиката натрия в деминерализованной воде при комнатной температуре путем предварительного залива в него 250 литров 30%-oгo раствора силиката натрия с модулем 3,0 и добавлении деминерализованной воды объемом 200 литров с непрерывным перемешиванием в течение 5 минут.1. In a separate collection with a volume of 0.5 cubic meters. prepare a solution of sodium silicate in demineralized water at room temperature by pre-pouring 250 liters of a 30% sodium silicate solution with a module of 3.0 into it and adding demineralized water with a volume of 200 liters with continuous stirring for 5 minutes.

2. Также в отдельном сборнике с объемом 0,5 м.куб. готовят раствор аккумуляторной кислоты при комнатной температуре путем предварительного залива в него 200 литров деминерализованной воды объемом 2с последующим добавлением 50 литров аккумуляторной кислоты с плотностью 1 ,835 г/см. куб.2. Also in a separate collection with a volume of 0.5 cubic meters. prepare a solution of battery acid at room temperature by pre-pouring 200 liters of demineralized water into it with a volume of 2s, followed by adding 50 liters of battery acid with a density of 1.835 g / cm. cube

3. В реакторе с объемом 2,0 м.куб. готовят горячий раствор силиката натрия в деминерализованной воде путем предварительного залива в реактор деминерализованной воды объемом 300 литров с непрерывным перемешиванием и подогревом, добавлением в горячую деминерализованную воду 5 литров 30%-oгo раствора силиката натрия с модулем 3,0 и дополнительного залива деминерализованной воды объемом 300 литров. Температуру горячего раствора силиката натрия в деминерализованной воде поддерживают равной 940C. 4. Далее производят одновременную подачу в реактор с горячим раствором силиката натрия в деминерализованной воде подачи растворов из сборника с раствором силиката натрия в деминерализованной воде при комнатной температуре и сборника с раствором аккумуляторной кислоты при комнатной температуре. При этом, подачу раствора из сборника с раствором силиката натрия в деминерализованной воде при комнатной температуре осуществляют со скоростью 20 л/мин, а из сборника с раствором аккумуляторной кислоты при комнатной температуре - со скоростью 8л/мин. Это обеспечивает рН ракционной среды от 10 до 1 1. Подача растворов в реактор не должна быть меньше 25 минут.3. In a reactor with a volume of 2.0 cubic meters. prepare a hot solution of sodium silicate in demineralized water by pre-pouring 300 liters of demineralized water into the reactor with continuous stirring and heating, adding 5 liters of a 30% sodium silicate solution with module 3.0 and additional 300 demineralized water to the hot demineralized water liters. The temperature of the hot solution of sodium silicate in demineralized water is maintained equal to 94 0 C. 4. Next, a simultaneous feed into the reactor with a hot solution of sodium silicate in demineralized water is the supply of solutions from the collector with a solution of sodium silicate in demineralized water at room temperature and the collector with a solution of battery acid at room temperature. In this case, the solution from the collection with a solution of sodium silicate in demineralized water at room temperature is supplied at a speed of 20 l / min, and from the collection with a solution of battery acid at room temperature at a speed of 8 l / min. This provides a pH of the growth medium from 10 to 1 1. The supply of solutions to the reactor should not be less than 25 minutes.

5. Затем производят добавляют аккумуляторной кислоты для доведения рН до 4,5.5. Then, battery acid is added to adjust the pH to 4.5.

6. Заключительные операции касаются стандартных процедур фильтрации, сушки и измельчения.6. Final operations relate to standard filtration, drying and grinding procedures.

Полученный диоксид кремния представляет собой белый мелкозернистый порошок, имеющий аморфную структуру. The resulting silicon dioxide is a white fine powder having an amorphous structure.

Claims

Формула изобретения Claim 1. Способ получения двуокиси кремния, включающий подготовку в реакторе раствора аккумуляторной кислоты и силиката для их взаимодействия для получения суспензии осажденной двуокиси кремния, а также последующее выделение и высушивание полученной суспензии, отличающийся тем, что, перед подготовкой в реакторе раствора аккумуляторной кислоты и силиката, в качестве которого используют силикат натрия, предварительно в реакторе готовят горячий раствор силиката натрия в деминерализованной воде, готовят в отдельных сборниках раствор силиката натрия в деминерализованной воде при комнатной температуре и раствор аккумуляторной кислоты при комнатной температуре, а подготовку в реакторе раствора аккумуляторной кислоты и силиката натрия производят путем одновременной подачи растворов в реактор с горячим раствором силиката натрия в деминерализованной воде из сборника с раствором силиката натрия в деминерализованной воде при комнатной температуре и сборника с раствором аккумуляторной кислоты при комнатной температуре с последующим добавлением аккумуляторной кислоты для получения в реакторе значения рН раствора, равном 4,5.1. A method of producing silicon dioxide, comprising preparing in the reactor a solution of battery acid and silicate for their interaction to obtain a suspension of precipitated silicon dioxide, as well as the subsequent isolation and drying of the resulting suspension, characterized in that, before preparing a solution of battery acid and silicate in the reactor, which is used as sodium silicate, previously in the reactor a hot solution of sodium silicate in demineralized water is prepared, a silicate solution is prepared in separate collections sodium in demineralized water at room temperature and a solution of battery acid at room temperature, and preparation of a solution of battery acid and sodium silicate in the reactor is carried out by simultaneously supplying solutions to the reactor with a hot solution of sodium silicate in demineralized water from a collector with a solution of sodium silicate in demineralized water at room temperature and a collector with a solution of battery acid at room temperature, followed by the addition of battery acid to the floor cheniya reactor solution pH equal to 4.5. 2. Способ по п. l , отличающийся тем, что температуру горячего раствора силиката натрия в деминерализованной воде устанавливают равной 940C.2. The method according to p. L, characterized in that the temperature of the hot solution of sodium silicate in demineralized water is set equal to 94 0 C. 3. Способ по п. l , отличающийся тем, что горячий раствор силиката натрия в деминерализованной воде готовят в реакторе путем предварительного залива в реактор деминерализованной воды объемом 300 литров с непрерывным перемешиванием и подогревом, добавлением в горячую деминерализованную воду 5 литров 30%-oгo раствора силиката натрия с модулем 3,0 и дополнительного залива деминерализованной воды объемом 300 литров.3. The method according to p. L, characterized in that a hot solution of sodium silicate in demineralized water is prepared in the reactor by pre-pouring 300 liters of demineralized water into the reactor with continuous stirring and heating, adding 5 liters of a 30% solution to the hot demineralized water silicate sodium with a module of 3.0 and an additional bay of demineralized water with a volume of 300 liters. 4. Способ по п. l , отличающийся тем, что раствор силиката натрия в деминерализованной воде при комнатной температуре готовят в сборнике путем предварительного залива в него 250 литров 30%-oгo раствора силиката натрия с модулем 3,0 и добавлении деминерализованной воды объемом 200 литров с непрерывным перемешиванием в течение 5 минут.4. The method according to p. L, characterized in that a solution of sodium silicate in demineralized water at room temperature is prepared in the collection by pre-filling it with 250 liters of a 30% sodium silicate solution with a module of 3.0 and adding demineralized water with a volume of 200 liters with continuous stirring for 5 minutes. 5. Способ по п. l , отличающийся тем, что раствор аккумуляторной кислоты при комнатной температуре готовят в сборнике путем предварительного залива в него 200 литров деминерализованной воды объемом 2с последующим добавлением 50 литров аккумуляторной кислоты с плотностью 1 ,835 г/см. куб.5. The method according to p. L, characterized in that the solution of the battery acid at room temperature is prepared in the collector by pre-pouring 200 liters of demineralized water into it in a volume of 2 seconds, followed by the addition of 50 liters of battery acid with a density of 1.835 g / cm. cube 6. Способ по п. l , отличающийся тем, что одновременную подачу в реактор с горячим раствором силиката натрия в деминерализованной воде из сборника с раствором силиката натрия в деминерализованной воде при комнатной температуре осуществляют со скоростью 20 л/мин, а из сборника с раствором аккумуляторной кислоты при комнатной температуре - со скоростью 8л/мин. 6. The method according to p. L, characterized in that the simultaneous feed into the reactor with a hot solution of sodium silicate in demineralized water from the collection with a solution of sodium silicate in demineralized water at room temperature is carried out at a speed of 20 l / min, and from the collection with a solution of battery acid at room temperature - at a rate of 8l / min.
PCT/RU2010/000156 2009-06-19 2010-04-05 Method for producing silicon dioxide Ceased WO2010147500A1 (en)

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RU2009123259 2009-06-19
RU2009123259/05A RU2407703C1 (en) 2009-06-19 2009-06-19 Method of producing silicon dioxide

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104066683A (en) * 2012-01-25 2014-09-24 罗地亚运作公司 Precipitated-silica production method
CN105540926A (en) * 2016-01-07 2016-05-04 华新珍 Method for cooperatively producing white carbon black and inorganic salt with acid wastewater

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008000761A1 (en) * 2006-06-27 2008-01-03 Rhodia Operations Precipitated silica for paper application
WO2008136019A2 (en) * 2007-05-03 2008-11-13 Council Of Scientific & Industrial Research A process for the preparation of finely divided precipitated silica

Family Cites Families (2)

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Publication number Priority date Publication date Assignee Title
US4973462A (en) * 1987-05-25 1990-11-27 Kawatetsu Mining Company, Ltd. Process for producing high purity silica
FR2732330B1 (en) * 1995-03-29 1997-06-20 Rhone Poulenc Chimie NOVEL PROCESS FOR PREPARING PRECIPITATED SILICA, NOVEL PRECIPITATED SILICA CONTAINING ZINC AND THEIR USE FOR REINFORCING ELASTOMERS

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008000761A1 (en) * 2006-06-27 2008-01-03 Rhodia Operations Precipitated silica for paper application
WO2008136019A2 (en) * 2007-05-03 2008-11-13 Council Of Scientific & Industrial Research A process for the preparation of finely divided precipitated silica

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
A. G. AMELIN ET AL.: "Vysshaya shkola", PROIZBODSTVO SERNOY KISLOTY., 1974, MOSCOW, pages 12, 178, 179 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104066683A (en) * 2012-01-25 2014-09-24 罗地亚运作公司 Precipitated-silica production method
CN105540926A (en) * 2016-01-07 2016-05-04 华新珍 Method for cooperatively producing white carbon black and inorganic salt with acid wastewater
CN105540926B (en) * 2016-01-07 2018-02-16 江苏盛吉化工有限公司 A kind of method using acid waste water co-producing white carbon black and inorganic salts

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