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WO2018167646A1 - Procédé de préparation de silicate de sodium à partir de cendre de balles de riz - Google Patents

Procédé de préparation de silicate de sodium à partir de cendre de balles de riz Download PDF

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Publication number
WO2018167646A1
WO2018167646A1 PCT/IB2018/051633 IB2018051633W WO2018167646A1 WO 2018167646 A1 WO2018167646 A1 WO 2018167646A1 IB 2018051633 W IB2018051633 W IB 2018051633W WO 2018167646 A1 WO2018167646 A1 WO 2018167646A1
Authority
WO
WIPO (PCT)
Prior art keywords
trona
husk ash
range
cate
sodi
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/IB2018/051633
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English (en)
Inventor
Debabrata Rautaray
Prabhat PARIDA
Mayura LOLAGE
Ashwini ANGAL
Sunil ROKADE
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.)
Tata Chemicals Ltd
Original Assignee
Tata Chemicals Ltd
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 Tata Chemicals Ltd filed Critical Tata Chemicals Ltd
Publication of WO2018167646A1 publication Critical patent/WO2018167646A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/32Alkali metal silicates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/126Preparation of silica of undetermined type
    • C01B33/128Preparation of silica of undetermined type by acidic treatment of aqueous silicate solutions
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/19Oil-absorption capacity, e.g. DBP values
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/90Other properties not specified above

Definitions

  • a process for preparing sodium silicate from rice husk ash is disclosed. Particularly, a process for preparing silica from rice husk ash is disclosed.
  • sil ica finds application as a catalyst carrier, absorbent for an active material, viscosity, texturizing or anti-caking agent element for battery separators, toothpaste or paper additive, reinforcing filler in silicone matrices or in compositions based on natural or synthetic polymer(s), in particular on elastomers), particularly diene elastomers.
  • V arious methods are known for preparing silica. It is further known that the method used for prepari ng si I i ca also i nf I uences the physi cal and chemi cal properti es thereof.
  • silica is prepared by a precipitation reaction between a silicate, in particular an alkali metal silicate, and an acidifying agent, followed by a filtration and a washing step and, then optionally a step for disintegrating the obtained filter cake.
  • sil icate required for production of silica was obtained by fusing sil ica sand with sodium carbonate.
  • a major quantity of silicate is obtained from rice husk ash.
  • Rice husk is an agricultural residue, available abundantly in rice producing countries. India alone produces approximately 12 million tons of rice husk annually.
  • Silica is the major constituent of rice husk ash, making it economically feasible to extract silica, which has wide market.
  • Using rice husk ash for production of silica also addresses the issue of appropri ate di sposal of ri ce husk ash.
  • si I i ca To prepare si I i ca, si I i cate i s obtai ned from ri ce husk ash by fusing rice husk ash with sodium hydroxide.
  • sodium hydroxide being expensive, increases the overall cost of the production of silica
  • T is therefore a need to devise an improved process which could reduce the overall cost of production of silica. It is also required that the such a process is able to produce silica having desired characteristics.
  • a process for preparing sodium silicate from rice husk ash comprises fusing the rice husk ash with trona at an elevated temperature ranging between 1200- 1500 eC for a ti me peri od rangi ng between 2-4 hours to obtai n sodi um si I i cate.
  • a process for preparing silica from rice husk ash comprises f usi ng the ri ce husk ash with trona at an el evated temperature rangi ng between 1200- 1500 eC for a time period ranging between 2-4 hours to obtain sodium silicate; dissolving the obtained sodium silicate in an aqueous medium to obtain sodium silicate solution at a temperature of 100-160eC; acidifying said sodium silicate solution to cause precipitation of silica.
  • Figure 1 illustrates the process of preparing silica in accordance with an embodiment of the present disclosure
  • Figure 2 shows the X -ray Diffraction measurements of silica extracted from rice husk ash usi ng the process of the present di scl osure
  • Figures 3 shows the Transmission E lectron Microscopy (TE M) analysis of silica extracted from rice husk ash using the process of the present disclosure
  • Figure 4 shows Field emission scanning electron microscopy analysis of silica extracted from rice husk ash using the process of the present disclosure.
  • TE M Transmission E lectron Microscopy
  • the present di scl osure rel ates to a process for prepari ng si I i cate from rice husk ash.
  • said process comprises fusing the rice husk ash with trona at an el evated temperature rangi ng between 1200- 1500 eC for a ti me peri od rangi ng between 2-4 hours to obtai n sodi um si I i cate.
  • S ai d process comprises fusing the rice husk ash with trona at an elevated temperature ranging between 1200- 1500 eC for a time period ranging between 2-4 hours to obtain sodium silicate; dissolving the obtained sodium silicate in an aqueous medium to obtain sodium silicate solution at a temperature of 100-160eC; acidifying said sodium silicate solution to cause precipitation of silica.
  • the above disclosed process results in obtaining precipitated silica having the foil owing physico-chemical characteristic data: a CT A B surface area i n a range of 80-350 n /g;
  • V 2 i n a sears number (V 2) i n a range of 12-30 ml/ (5g) .
  • said precipitated silica alongside the parameters mentioned above has one or more of the following physico-chemical parameters, independently of one another:
  • trona comprises sodium carbonate and sodium bicarbonate. In accordance with an embodiment, trona comprises sodium carbonate in an amount ranging between 40-50% and preferably 44%. In accordance with an embodiment, trona comprises sodium bicarbonate in an amount ranging between 25-35%. Trona may also comprise 2-3 % Sodium fluoride, about 2% Sodium chloride and about 6%, insoluble impurities. The composition of trona is illustrated in table 1, below. In accordance with an embodiment, trona is processed to reduce the impurities. Any known process may be used to process trona so as to reduce the amount of impurities. The composition of said processed trona is illustrated below, in table 2. Table 1 : Composition of Trona
  • the rice husk ash and trona are fused i n wA/v ratio ranging between 1 :0.8 to 1 :1.5.
  • the rice husk ash and trona are fused in w/w ratio in a range of 1 : 1.
  • the rice husk ash and trona are fused under a pressure in a range of 1 to 6 atm.
  • the rice husk ash and trona are fused under a pressure in a range of 1 atm.
  • the sodi um si I i cate and the aqueous medi um are mixed in w/w ratio in a range of 1 :10- 1 :20.
  • sodium silicate and the aqueous medium are mixed in w/w ratio in a range of 1 :10.
  • the aqueous medium is maintained at a temperature in a range of 90-150eC .
  • the aqueous medi um is water.
  • the acidification is carried out until silica is precipitated completely.
  • acidification is caused using a mineral acid selected from a group consisting of sulphuric acid, hydrochloric acid, nitric acid, organic acids like citric acid, acetic acid, oxalic acid.
  • the mineral acid has a molarity in a range of 0.1 M to 2 M, and preferably around 0.625 M.
  • the acidification is caused by passing carbon dioxide or sulphur dioxide.
  • Such acidification is caused using carbon di oxi de and/or sul phur di oxi de i n an amount rangi ng between 3.5-5 gm of C 0 2 per 100 gm of sodium silicate having 5-7% Na 2 0 and 5-8 gm of S0 2 per 100 gm of sodium silicate having 5-7% Na 2 0.
  • Preferably, 4.96 gm C0 2 and 7.5 gm S0 2 per 100gm of sodium silicate having 5-7% Na 2 0 is used.
  • the precipitated silica obtained upon completion of reaction is filtered followed by washing. Washing is done to eliminate the by-products, obtained as a result of reaction.
  • precipitated silica is then subjected to a drying step.
  • the drying step may be carried out by spray drying, spin flash drying, or vacuum tray dryi ng.
  • the wet cake is subj ected to short-term dryi ng, f ol I owed by addition of a dispersing agent in a suitable solvent.
  • the dispersion may then be dried to obtain precipitated silica.
  • the dispersion of silica is prepared using a dispersing agent selected from a group consisting of metal salt of saturated and unsaturated fatty esters with long hydrocarbon chain/ fatty acids in an appropriate solvent selected from a group consisting of butanol, butanone, toluene and acetone.
  • a dispersing agent selected from a group consisting of metal salt of saturated and unsaturated fatty esters with long hydrocarbon chain/ fatty acids in an appropriate solvent selected from a group consisting of butanol, butanone, toluene and acetone.
  • T he si I i ca accordi ng to the present di scl osure can be used i n tyre rubber, ri ce rol I er rubber, shoe sole rubber or any other elastomers, cosmetic especially dental application, in environmental remediation, and in paints.
  • the silica disclosed herein is suitable for use as filler in vulcanizable or vulcanized elastomer compositions.
  • the vulcanized elastomer composition can be used for the manufacture of tyre and other rubber products.
  • sai d si I i ca may be used as a rei nf orci ng f i 11 er in a quantity in a range of 7 to 90 phr. Any conventional process may be used to form vulcanizable or vulcanized elastomer compositions using the above disclosed silica as reinforcing filler.
  • Any conventional process may be used to form vulcanizable or vulcanized elastomer compositions using the above disclosed silica as reinforcing filler.
  • the process disclosed here in an inexpensive and easy process of preparing silica.
  • the process enables using rice husk ash for production of commercially viable silica, which has otherwise not been obtained in any prior known processes.
  • the silica according to the present disclosure can be used in tyre rubber, rice roller rubber, shoe sole rubber or any other elastomers, cosmetic especially dental application, environmental remediation and paints.
  • Trona is a cheaper source of sodium carbonate and hence reduces the cost of production of silica, as compared to prior known processes.

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

Abstract

L'invention concerne un procédé de préparation de silicate de sodium à partir de cendre de balles de riz. Ledit procédé comprend la fusion de cendre de balles de riz avec du trona à une température élevée comprise entre 1200 et 1500 °C pendant une durée comprise entre 2 et 4 heures pour obtenir du silicate de sodium.
PCT/IB2018/051633 2017-03-14 2018-03-13 Procédé de préparation de silicate de sodium à partir de cendre de balles de riz Ceased WO2018167646A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IN201721008780 2017-03-14
IN201721008780 2017-03-14

Publications (1)

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WO2018167646A1 true WO2018167646A1 (fr) 2018-09-20

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109384237A (zh) * 2018-10-31 2019-02-26 昆明理工大学 一种稻壳中提取高纯SiO2的方法
CN110002425A (zh) * 2019-04-22 2019-07-12 天津大学 一种离子液体超级电容器用三维多孔碳材料的制备方法
WO2023195300A1 (fr) * 2022-04-05 2023-10-12 東ソー・シリカ株式会社 Solution aqueuse de silicate alcalin et sa méthode de production
WO2024089003A1 (fr) * 2022-10-28 2024-05-02 Rhodia Operations Procédé de préparation de silicate à partir de cendres végétales comprenant de la silice cristalline à l'aide d'un sel contenant un anion multivalent
CN118791006A (zh) * 2024-09-13 2024-10-18 山东联科科技股份有限公司 利用稻壳制备硅酸钠的方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004073600A2 (fr) * 2003-02-18 2004-09-02 The Registrar, Indian Institute Of Science Procede et appareil de fabrication de silice precipitee a partir de cendre de balle de riz

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004073600A2 (fr) * 2003-02-18 2004-09-02 The Registrar, Indian Institute Of Science Procede et appareil de fabrication de silice precipitee a partir de cendre de balle de riz

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
I. OZKAN: "Production of Sodium Silicate Cullets by Using Trona", ACTA PHYSICA POLONICA A, vol. 129, no. 4, 16 April 2015 (2015-04-16), pages 451 - 454, XP055538610 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109384237A (zh) * 2018-10-31 2019-02-26 昆明理工大学 一种稻壳中提取高纯SiO2的方法
CN110002425A (zh) * 2019-04-22 2019-07-12 天津大学 一种离子液体超级电容器用三维多孔碳材料的制备方法
WO2023195300A1 (fr) * 2022-04-05 2023-10-12 東ソー・シリカ株式会社 Solution aqueuse de silicate alcalin et sa méthode de production
JP2023153621A (ja) * 2022-04-05 2023-10-18 東ソー・シリカ株式会社 ケイ酸アルカリ水溶液およびその製造方法
JP7607002B2 (ja) 2022-04-05 2024-12-26 東ソー・シリカ株式会社 ケイ酸アルカリ水溶液およびその製造方法
WO2024089003A1 (fr) * 2022-10-28 2024-05-02 Rhodia Operations Procédé de préparation de silicate à partir de cendres végétales comprenant de la silice cristalline à l'aide d'un sel contenant un anion multivalent
CN118791006A (zh) * 2024-09-13 2024-10-18 山东联科科技股份有限公司 利用稻壳制备硅酸钠的方法

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