JPH01249622A - Production of porous activated silica - Google Patents

Production of porous activated silica

Info

Publication number
JPH01249622A
JPH01249622A JP7738288A JP7738288A JPH01249622A JP H01249622 A JPH01249622 A JP H01249622A JP 7738288 A JP7738288 A JP 7738288A JP 7738288 A JP7738288 A JP 7738288A JP H01249622 A JPH01249622 A JP H01249622A
Authority
JP
Japan
Prior art keywords
activated silica
silica
porous activated
heating
silicon
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.)
Pending
Application number
JP7738288A
Other languages
Japanese (ja)
Inventor
Takeo Akiyama
秋山 健夫
Yuichi Hosoda
雄一 細田
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.)
NICHIEI KOGYO KK
Ikeda Corp
Original Assignee
NICHIEI KOGYO KK
Ikeda Bussan Co 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 NICHIEI KOGYO KK, Ikeda Bussan Co Ltd filed Critical NICHIEI KOGYO KK
Priority to JP7738288A priority Critical patent/JPH01249622A/en
Publication of JPH01249622A publication Critical patent/JPH01249622A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/181Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • 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
    • C01P2006/80Compositional purity

Landscapes

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

Abstract

PURPOSE:To obtain porous activated silica in the form of fine particles at a low cost by heating a silicon accumulated biomass in two steps by a specified method in an oxygen atmosphere. CONSTITUTION:A silicon accumulated biomass is slowly heated to 100-600 deg.C in an oxygen atmosphere and further heated at 400-1,000 deg.C. The pref. primary heating time is 2-3hr and the pref. secondary heating time is also 2-3hr. Since tar generated from the biomass is properly removed during the primary heating, pure porous, activated silica can be obtd. by the secondary heating.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は多孔質活性シリカの製造方法に関し、更に詳細
に説明すると、籾殻、稲わら等のケイ素集積バイオマス
から製造した多孔性質活性シリカの製造方法に関する。
[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing porous activated silica. More specifically, the present invention relates to a method for producing porous activated silica, and more specifically, a method for producing porous activated silica produced from silicon-integrated biomass such as rice husk and rice straw. Regarding the method.

(従来の技術及び課題〕 シリカは、地殻の構成元素として多量に存在し、全地殻
構成成分の約60%を占めている。これらはケイ酸塩と
して存在し、石英、リンケイ石、クリストバル石、その
他の結晶形を有するもの、ガラス状、コロイド状のもの
等が知られている。
(Prior art and problems) Silica exists in large quantities as a constituent element of the earth's crust, accounting for approximately 60% of all the constituent elements of the earth's crust.These exist as silicates, including quartz, phosphorite, cristobalite, Those having other crystalline forms, glassy, colloidal, etc. are known.

微粒子状シリカとしては、フェロシリコンを塩素化して
四塩化ケイ素としたものを精製し、加水分解して得られ
たものか挙げられる。しかし、斯るシリカは、製造工程
が複雑であるため、安価に提供することができないとい
・う欠点を有している。
Examples of the particulate silica include those obtained by chlorinating ferrosilicon to form silicon tetrachloride, purifying it, and hydrolyzing it. However, such silica has the disadvantage that it cannot be provided at low cost because the manufacturing process is complicated.

〔発明の目的〕[Purpose of the invention]

本発明の目的は、微粒子の多孔質活性シリカの安価な製
造方法を提供することにある。
An object of the present invention is to provide an inexpensive method for producing fine-particle porous activated silica.

〔課題を解決するための手段〕[Means to solve the problem]

本発明は上述せる課題に鑑みてなされたもので、ケイ素
集積バイオマスを酸素雰囲気中で100〜600℃に徐
々に加熱し、次いで、400〜1000℃で更に加熱す
ることを特徴とする。
The present invention has been made in view of the above-mentioned problems, and is characterized by gradually heating silicon-integrated biomass to 100 to 600°C in an oxygen atmosphere, and then further heating to 400 to 1000°C.

〔実施例〕〔Example〕

本発明において使用されるケイ素集積バイオマスとは、
シリカ成分を含有する植物(ケイ素集積植物)又はその
葉、茎等の部分を意味し、更に具体的には、稲等の籾殻
又は葉、笹の葉、トウモロコシやとくさの葉又は茎等が
挙げられる。
The silicon-integrated biomass used in the present invention is:
It refers to plants containing silica components (silicon-accumulating plants) or their leaves, stems, etc. More specifically, examples include rice husks or leaves, bamboo leaves, corn, and grass leaves or stems. It will be done.

本発明の多孔質活性シリカの製造方法は、上記ケイ素集
積バイオマスを加熱処理することにより得られる。
The method for producing porous activated silica of the present invention is obtained by heat-treating the silicon-integrated biomass.

本発明における多孔質活性シリカの製造方法は、先ずケ
イ素集積バイオマスとして、−に記したもののうち、例
えば、籾殻そのもの、あるいは籾殻を粉砕して得た籾殻
粉末を、空気中また!J酸素雰囲気中で、−次の加熱と
して100〜600℃1好ましくは150〜500’c
に徐々に加熱する。次いて二次加熱として400〜]O
OO’C1好ましく ia:soo〜700℃に加熱す
る。加熱時間は、−次加熱においては、1〜5時間、好
ましくは2〜3時間であり、二次加熱においては、1〜
5時間、好ましくは2〜3時間である。
In the method for producing porous activated silica in the present invention, first, as silicon-integrated biomass, among the materials listed in -, for example, rice husk itself or rice husk powder obtained by crushing rice husk is used in the air or! In an oxygen atmosphere, - 100 to 600°C as the next heating, preferably 150 to 500'c
Heat gradually. Then, as secondary heating, 400~]O
OO'C1 preferably heated to ia:soo~700°C. The heating time is 1 to 5 hours, preferably 2 to 3 hours in the secondary heating, and 1 to 3 hours in the secondary heating.
5 hours, preferably 2 to 3 hours.

本発明において、加熱処理を二段階で行う理由は、ケイ
素集積バイオマスを一次加熱した際にタール分が発生す
るが、−段階で急速に加熱すると、このタール分がシリ
カが焼結する際、結晶内に取り込まれて炭素として残留
し、純粋なシリカとはならないからである。本発明にお
いては、これらタール分が一次加熱の際に適切に除去さ
れるので、二次力11.815により純粋な多孔質活性
シリカを得ることができる。
In the present invention, the reason why the heat treatment is carried out in two stages is that tar is generated when the silicon-integrated biomass is primarily heated, but if it is rapidly heated in the - stage, this tar will crystallize when the silica sinters. This is because it is taken into the interior and remains as carbon, and does not become pure silica. In the present invention, since these tar components are appropriately removed during primary heating, pure porous activated silica can be obtained with a secondary force of 11.815.

本発明において、ケイ素集積バイオマスとして粉末状の
ものを使用する場合にGJ、粉末の粒径は適宜選択され
るか、一般に、152μIn以下(以下「タイプA」と
称する。)、152μm〜295μm(以下[タイプB
]と称する。)、295 p m〜]000m (以下
「タイプC」と称する。)又はこれらの混合物を使用す
ることが好ましい。
In the present invention, when powdered silicon-integrated biomass is used, the particle size of the GJ powder is appropriately selected, or generally, 152 μIn or less (hereinafter referred to as "Type A"), 152 μm to 295 μm (hereinafter referred to as "Type A"), or [Type B
]. ), 295 p m to ]000 m (hereinafter referred to as "Type C"), or a mixture thereof is preferably used.

本発明においては、上記タイプAのものを使用した場合
には、30〜150m/gの比表面積を有する多孔質活
性シリカが、同タイプBのものからは20〜]、OOm
/gのものが、更に同タイプCのものからは15〜50
i/gのものがそれぞれ得られた。
In the present invention, when the above type A is used, porous activated silica having a specific surface area of 30 to 150 m/g is used, whereas when the same type B is used, the porous activated silica has a specific surface area of 20 to
/g, and 15 to 50 from the same type C.
i/g of each were obtained.

〔発明の効果〕〔Effect of the invention〕

本発明に依れば、従来法である鉱物より得られたシリカ
に比較して、比表面積が大きく活性度が高いシリカが得
られた。又、ケイ素集積バイオマスを単に加熱焼成して
得られたシリカと比較して、炭素含有量が全くないシリ
カを得ることができる。
According to the present invention, silica with a large specific surface area and high activity was obtained compared to silica obtained from minerals using conventional methods. Furthermore, compared to silica obtained by simply heating and calcining silicon-integrated biomass, silica with no carbon content can be obtained.

更に、従来法は複雑な精製二「程を要するのに対し、本
発明方法に依れば、沖縄な工程で、且つ、籾殻等の安価
な原料が使用可能であるため、供給か安定で安価な多孔
質活性シリカを得ることかできる。
Furthermore, while the conventional method requires two complicated refining steps, the method of the present invention uses an Okinawan process and can use inexpensive raw materials such as rice husks, resulting in a stable and inexpensive supply. Porous activated silica can be obtained.

〔発明の実施例〕[Embodiments of the invention]

水分率7〜9%の籾殻を準備し、これを温度200〜3
00℃、圧力50〜]−5(lton/c+d及び摩擦
熱により、全体を固形状とした。次いてこの固形物を粉
砕機を用いて、粒径152μm以下の粒子(タイプΔ)
、粒径152〜295μmの粒子(タイプB)及びオイ
ノ径295〜1000μmの粒子(タイプC)の3種類
に分割した。
Prepare rice husks with a moisture content of 7-9% and heat them at a temperature of 200-3.
00°C, pressure 50~]-5 (lton/c+d and frictional heat, the whole was made into a solid state. Next, this solid was crushed into particles with a particle size of 152 μm or less (type Δ) using a pulverizer.
The particles were divided into three types: particles with a diameter of 152 to 295 μm (type B) and particles with a diameter of 295 to 1000 μm (type C).

次に、上記3種類の籾殻粉末を、酸素雰囲気中において
、それぞれ温度150℃1200’C3300°(゛及
び400’Cで各1時間の一次加熱をし、次いて、5 
(l 0℃1600℃及び700°(じで各30分、及
O・ε100’cで5時間のニー次加熱をして桃白色の
粉末を1″、また。1)j、られたシリカ微粒子の比表
面積及び平均粒度を測定し、その結果を第1表に示す。
Next, the above three types of rice husk powders were first heated in an oxygen atmosphere at a temperature of 150°C, 1200°C, and 3300°C for 1 hour each.
(L 0℃ 1600℃ and 700℃ (30 minutes each, and 5 hours at O ε 100'c) to produce a pink white powder of 1". The specific surface area and average particle size of the sample were measured, and the results are shown in Table 1.

また上記シリカ微粒子の化学分+Jr (lI′cを第
2表に示す。
Further, the chemical content + Jr (lI'c) of the silica fine particles is shown in Table 2.

第  1  表 第  2  表 以上の結果から明らかなように、本発明方法に依れば、
簡便な操作で、比表面積が大きく活性度が高い多孔質活
性シリカを安価に得ることができた。
As is clear from the results shown in Table 1 and Table 2, according to the method of the present invention,
With simple operations, porous activated silica with a large specific surface area and high activity could be obtained at low cost.

特許出願人  池田物産株式会社Patent applicant: Ikeda Bussan Co., Ltd.

Claims (1)

【特許請求の範囲】[Claims] ケイ素集積バイオマスを酸素雰囲気中で100〜600
℃に徐々に加熱し、次いで、400〜1000℃で更に
加熱することを特徴とする多孔質活性シリカの製造方法
100-600 silicon-integrated biomass in oxygen atmosphere
A method for producing porous activated silica, which comprises gradually heating to 400 to 1000°C.
JP7738288A 1988-03-30 1988-03-30 Production of porous activated silica Pending JPH01249622A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP7738288A JPH01249622A (en) 1988-03-30 1988-03-30 Production of porous activated silica

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP7738288A JPH01249622A (en) 1988-03-30 1988-03-30 Production of porous activated silica

Publications (1)

Publication Number Publication Date
JPH01249622A true JPH01249622A (en) 1989-10-04

Family

ID=13632340

Family Applications (1)

Application Number Title Priority Date Filing Date
JP7738288A Pending JPH01249622A (en) 1988-03-30 1988-03-30 Production of porous activated silica

Country Status (1)

Country Link
JP (1) JPH01249622A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008207169A (en) * 2007-01-31 2008-09-11 Suminoe Textile Co Ltd Manufacturing method of white chaff ash

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4952472A (en) * 1972-07-28 1974-05-21
JPS526397A (en) * 1975-07-01 1977-01-18 Deii Sutanbuuku Deii Horuhe Manufacturing process for silica or silicate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4952472A (en) * 1972-07-28 1974-05-21
JPS526397A (en) * 1975-07-01 1977-01-18 Deii Sutanbuuku Deii Horuhe Manufacturing process for silica or silicate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008207169A (en) * 2007-01-31 2008-09-11 Suminoe Textile Co Ltd Manufacturing method of white chaff ash

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