JP2564150B2 - Synthetic calcium silicate hydrate - Google Patents
Synthetic calcium silicate hydrateInfo
- Publication number
- JP2564150B2 JP2564150B2 JP62258361A JP25836187A JP2564150B2 JP 2564150 B2 JP2564150 B2 JP 2564150B2 JP 62258361 A JP62258361 A JP 62258361A JP 25836187 A JP25836187 A JP 25836187A JP 2564150 B2 JP2564150 B2 JP 2564150B2
- Authority
- JP
- Japan
- Prior art keywords
- calcium silicate
- silicate hydrate
- water
- synthetic calcium
- silicon dioxide
- 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.)
- Expired - Fee Related
Links
- 239000000378 calcium silicate Substances 0.000 title description 9
- 229910052918 calcium silicate Inorganic materials 0.000 title description 9
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 title description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 10
- 239000000920 calcium hydroxide Substances 0.000 claims description 10
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 10
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 claims description 9
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 8
- 239000010419 fine particle Substances 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- 229910021487 silica fume Inorganic materials 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000011575 calcium Substances 0.000 description 4
- 239000004568 cement Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 3
- 235000012255 calcium oxide Nutrition 0.000 description 3
- -1 for example Substances 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 230000000887 hydrating effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011022 opal Substances 0.000 description 1
- 238000009931 pascalization Methods 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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
- C01B33/20—Silicates
- C01B33/24—Alkaline-earth metal silicates
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は合成ケイ酸カルシウム水和物、特に比表面積
が大きく、成形助剤、増粘剤、触媒担体、吸着剤、充填
材などとして使用される合成ケイ酸カルシウム水和物に
関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention is used as a synthetic calcium silicate hydrate, particularly with a large specific surface area, as a molding aid, thickener, catalyst carrier, adsorbent, filler, etc. To a synthetic calcium silicate hydrate.
従来、上記用途を目的とした合成ケイ酸カルシウム水
和物としては、ジャイロライト型ケイ酸カルシウム水和
物が市販されている。これはケイ酸ナトリウムなどの水
溶性ケイ酸塩と塩化カルシウムなどの水溶性カルシウム
塩を出発原料として水熱合成により製造されている（特
開昭54−93698号公報）。Conventionally, as a synthetic calcium silicate hydrate for the above purpose, a gyrolite type calcium silicate hydrate is commercially available. This is produced by hydrothermal synthesis using a water-soluble silicate such as sodium silicate and a water-soluble calcium salt such as calcium chloride as starting materials (JP-A-54-93698).
しかしながら、特開昭54−93698号公報の方法は150〜
250℃の温度でオートクレーブを用いて９〜23Kg/cm2の
水蒸気圧下で得られるものであって、このような方法は
現実の実施に際し、操作や装置が複雑となり大量生産が
困難であった。However, the method disclosed in JP-A-54-93698 is 150-
It was obtained at a temperature of 250 ° C. in an autoclave under a water vapor pressure of 9 to 23 kg / cm 2 , and such a method was difficult to mass-produce due to complicated operations and devices during actual implementation.
そこで、加圧を必要とせず、常温或いはわずかな加熱
で容易に製造できる微細な合成ケイ酸カルシウム水和物
が求められていた。Therefore, there has been a demand for a fine synthetic calcium silicate hydrate that does not require pressurization and can be easily produced at room temperature or with slight heating.
本発明は上記問題の解決を目的とし、その構成は、非
晶質二酸化ケイ素を主成分とする微細粒子、水酸化カウ
シウム及び水を主成分とする混練物を反応させて得られ
た合成ケイ酸カルシウム水和物であって、その比表面積
が100m2/g以上であることを特徴とする。The present invention is intended to solve the above problems, and the constitution thereof is a synthetic silicic acid obtained by reacting fine particles containing amorphous silicon dioxide as a main component, causium hydroxide and a kneaded product containing water as a main component. A calcium hydrate characterized by having a specific surface area of 100 m 2 / g or more.
本発明に用いる非晶質二酸化ケイ素を主成分とする微
細粒子は、フェロシリコンや金属シリコンの副生物の平
均粒径0.1μｍ程度の球状粒子であるシリカダスト（シ
リカフューム）やシリカ質ダストが好適であり、シリカ
ゲル、シリカガラス、オパール質珪石などを微粉砕（通
常は分級も組合わせる）して得られる微細粒子も使用で
きる。非晶質二酸化ケイ素を主成分とする微細粒子は、
セメント系の水和反応においてその反応が早く、また、
セメントの水和過程で生成するCa（OH）２を消費する。The fine particles containing amorphous silicon dioxide as the main component used in the present invention are preferably silica dust (silica fume) or siliceous dust, which are spherical particles having a mean particle size of about 0.1 μm of a by-product of ferrosilicon or metallic silicon. Therefore, fine particles obtained by finely pulverizing silica gel, silica glass, opal silica, etc. (usually in combination with classification) can also be used. Fine particles whose main component is amorphous silicon dioxide are
The reaction is fast in the hydration reaction of cement,
It consumes Ca (OH) 2 produced during the hydration process of cement.
上記したように非晶質二酸化ケイ素はセメントの水和
過程で生成するCa（OH）２とも速やかに反応するから、
水酸化カルシウムは、市販のCa（OH）２は勿論、水の存
在下でCa（OH）２を生成する物質、例えば生石灰、セメ
ント或いはカーバイト滓も水酸化カルシウム源として使
用される。その粒径は非晶質二酸化ケイ素に比べてそれ
ほど小さくなくともよい。As mentioned above, amorphous silicon dioxide reacts rapidly with Ca (OH) 2 produced during the hydration process of cement,
As calcium hydroxide, not only commercially available Ca (OH) 2 but also substances that produce Ca (OH) 2 in the presence of water, for example, quick lime, cement or carbide dregs are used as a source of calcium hydroxide. Its particle size need not be so small compared to amorphous silicon dioxide.
反応を進行させるにあたっては、非晶質二酸化ケイ素
を主成分とする微細粒子に水酸化カルシウム及び／又は
水の存在下で水酸化カルシウムを生成する物質を配合し
て出発組成とし、水と混練してペーストとするか或いは
粉体混合した後水を加えてスラリーとすればよい。反応
は20〜70℃に１〜40日放置することにより完結する。一
般に温度が高い程反応時間が短縮される。さらに、これ
に高温高圧処理、高温処理を行うことも可能である。特
にその場合は合成が目的ではなく、例えば殺菌という面
でオートクレーブ処理を行うことが多い。In order to proceed the reaction, fine particles containing amorphous silicon dioxide as a main component are mixed with a substance that forms calcium hydroxide in the presence of calcium hydroxide and / or water to obtain a starting composition, which is then kneaded with water. To form a paste, or after mixing powders, water may be added to form a slurry. The reaction is completed by leaving it at 20 to 70 ° C for 1 to 40 days. Generally, the higher the temperature, the shorter the reaction time. Furthermore, it is also possible to perform high temperature and high pressure processing and high temperature processing on this. In particular, in that case, synthesis is not the purpose, and for example, autoclave treatment is often performed in terms of sterilization.
この反応で生成する水和物はすべてケイ酸カルシウム
水和物であり、そのCaO/SiO2モル比は原料の配合比によ
り決まり、原料組成が重量比で1:2〜2:1であれば、その
範囲は0.6〜1.5である。The hydrates produced in this reaction are all calcium silicate hydrates, and the CaO / SiO 2 molar ratio is determined by the blending ratio of the raw materials, and if the raw material composition is 1: 2 to 2: 1 by weight ratio. , Its range is 0.6-1.5.
得られる合成ケイ酸カルシウム水和物は非常に小さ
く、原料のCaO/SiO2モル比が0.6の場合には、得られる
水和物の比表面積は100m2/g以上に達した。非晶質二酸
化ケイ素を主成分とする微細粒子がシリカフュームの場
合、水酸化カルシウム：シリカフュームが重量比で1:2
の試料では反応温度20℃ないし40℃の場合には150m2/g
以上に達した。一般に、反応の進行と共に比表面積は更
に増大する。The obtained synthetic calcium silicate hydrate was very small, and when the CaO / SiO 2 molar ratio of the raw material was 0.6, the specific surface area of the obtained hydrate reached 100 m 2 / g or more. If the fine particles based on amorphous silicon dioxide are silica fume, calcium hydroxide: silica fume is 1: 2 by weight.
Sample of 150m 2 / g at reaction temperature of 20 ℃ to 40 ℃
The above is reached. In general, the specific surface area further increases as the reaction progresses.
測定方法を非晶質二酸化ケイ素としてシリカフューム
を使用した場合を例にして説明する。The measurement method will be described by taking a case where silica fume is used as the amorphous silicon dioxide as an example.
試料は所定の期間水和した後、アセトンで水和を停止
し、−50℃の水蒸気圧下で１週間以上乾燥したものを使
用した。The sample was used after being hydrated for a predetermined period, stopped hydrating with acetone, and dried under a water vapor pressure of −50 ° C. for 1 week or more.
水和物の同定はＸ線回折で行った。強熱減量は1000
℃、１時間で測定し、未反応の水酸化カルシウムの測定
はDSC法によった。測定条件は以下の通りである。試料
量:10〜20mg、昇温速度:10℃/min、雰囲気:N2gas100ml/
min.。The hydrate was identified by X-ray diffraction. Ignition loss is 1000
Measurement was carried out at 1 ° C for 1 hour, and unreacted calcium hydroxide was measured by the DSC method. The measurement conditions are as follows. Sample amount: 10 to 20 mg, heating rate: 10 ° C / min, atmosphere: N 2 gas 100 ml /
min ..
未反応シリカフューム量は、未反応石英の定量法であ
る塩酸及び炭酸ナトリウムによる選択溶解法に準じて、
以下の方法で行った。The amount of unreacted silica fume is based on the selective dissolution method using hydrochloric acid and sodium carbonate, which is a quantitative method of unreacted quartz,
The procedure was as follows.
内容積50mlのテフロン製遠心分離管に試料を約0.5g入
れ、正しく秤量した後、2N塩酸40mlを加える。これを60
℃湯浴中で時々ガラス棒で攪拌しながら、約15分間保持
した後、6000RPM以上の回転数で10分程度遠心分離を行
う。上澄液を捨て温水で１回洗浄して、さきと同様の条
件で遠心分離し上澄液を捨てる。つぎに５％炭酸ナトリ
ウム溶液40mlを加え、70℃湯浴中でときどきガラス棒で
攪拌しながら約20分間保持した後、遠心分離、温水洗浄
をさきと同様に行う。これを165℃で乾燥した後、重量
を測定する。シリカフュームにこの方法を適用すると、
塩酸処理で約５％、炭酸ナトリウム処理で約10％が溶解
した。各水和試料の測定結果は15％のシリカフュームが
溶解するとして補正した。Approximately 0.5 g of the sample is put into a Teflon centrifuge tube with an internal volume of 50 ml, weighed correctly, and then 40 ml of 2N hydrochloric acid is added. This is 60
After stirring for 15 minutes in a hot water bath with glass rods for about 15 minutes, centrifuge at a rotation speed of 6000 RPM or higher for about 10 minutes. Discard the supernatant, wash once with warm water, centrifuge under the same conditions as above, and discard the supernatant. Next, 40 ml of a 5% sodium carbonate solution was added, and the mixture was kept in a hot water bath at 70 ° C for about 20 minutes while occasionally stirring with a glass rod, followed by centrifugation and washing with warm water in the same manner as above. After drying this at 165 ° C, the weight is measured. Applying this method to silica fume
Hydrochloric acid treatment dissolved about 5%, and sodium carbonate treatment dissolved about 10%. The measurement results of each hydrated sample were corrected assuming that 15% of silica fume was dissolved.
比表面積はN2吸着法で測定した。The specific surface area was measured by the N 2 adsorption method.
シリカフュームと試薬水酸化カルシウム（粒径１μ以
下）を第１表の組成比で充分混練後、水と固体の比率が
1.5となるようにペーストを作成し、ポリプロピレン製
試験管に入れて密封し、20℃で養生した場合の結果を第
１表に示した。また、40℃で養生した場合の結果を第２
表に示した。After sufficiently mixing silica fume and reagent calcium hydroxide (particle size 1 μm or less) at the composition ratio shown in Table 1, the ratio of water to solid is
Table 1 shows the results when a paste was prepared so as to have a weight of 1.5, placed in a polypropylene test tube, sealed, and cured at 20 ° C. In addition, the result of curing at 40 ° C
Shown in the table.
なお、使用したシリカフュームはシリカ含有量約90％
で、そのうち非晶質部分以外に約３％の石英を含んでい
た。またシリカ以外の構成成分は約３％のFe2O3と約2.8
％のカーボンであった。The silica fume used is approximately 90% silica content.
In addition, it contained about 3% of quartz in addition to the amorphous portion. The constituents other than silica are about 3% Fe 2 O 3 and about 2.8%.
% Carbon.
〔発明の効果〕 本発明により常温、常圧で単にペースト状に混練放置
するのみで比表面積の大きい合成ケイ酸カルシウム水和
物が得られる。 [Effects of the Invention] According to the present invention, a synthetic calcium silicate hydrate having a large specific surface area can be obtained by simply kneading in a paste form at room temperature and atmospheric pressure.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭54−109096（ＪＰ，Ａ) 特開 昭61−111910（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of the front page (56) Reference JP-A-54-109096 (JP, A) JP-A-61-111910 (JP, A)
Claims (1)
子、水酸化カルシウム及び水を主成分とする混練物を反
応させて得られた、比表面積が100m2/g以上の合成ケイ
酸カルシウム水和物。1. A synthetic silicic acid having a specific surface area of 100 m 2 / g or more obtained by reacting fine particles containing amorphous silicon dioxide as a main component, a kneaded product containing calcium hydroxide and water as a main component. Calcium hydrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62258361A JP2564150B2 (en) | 1987-10-15 | 1987-10-15 | Synthetic calcium silicate hydrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62258361A JP2564150B2 (en) | 1987-10-15 | 1987-10-15 | Synthetic calcium silicate hydrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01103914A JPH01103914A (en) | 1989-04-21 |
| JP2564150B2 true JP2564150B2 (en) | 1996-12-18 |
Family
ID=17319166
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62258361A Expired - Fee Related JP2564150B2 (en) | 1987-10-15 | 1987-10-15 | Synthetic calcium silicate hydrate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2564150B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003040048A2 (en) * | 2001-11-07 | 2003-05-15 | Metallkraft As | Method for utilising silica soot from quartz glass production |
| KR20050073608A (en) * | 2002-11-05 | 2005-07-14 | 제임스 하디 인터내셔널 파이낸스 비.브이. | Method and apparatus for producing calcium silicate hydrate |
| JP5930535B2 (en) * | 2011-06-24 | 2016-06-08 | 太平洋セメント株式会社 | Phosphorus recovery and fertilizer method |
| JP5972050B2 (en) * | 2012-05-25 | 2016-08-17 | 太平洋セメント株式会社 | Method for producing phosphorus recovery material |
| JP6723341B2 (en) | 2016-02-25 | 2020-07-15 | 旭化成株式会社 | Inorganic particles for non-aqueous electrolyte battery and non-aqueous electrolyte battery |
-
1987
- 1987-10-15 JP JP62258361A patent/JP2564150B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01103914A (en) | 1989-04-21 |
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