JP4014882B2 - Method for producing silica sol - Google Patents
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- JP4014882B2 JP4014882B2 JP2002021879A JP2002021879A JP4014882B2 JP 4014882 B2 JP4014882 B2 JP 4014882B2 JP 2002021879 A JP2002021879 A JP 2002021879A JP 2002021879 A JP2002021879 A JP 2002021879A JP 4014882 B2 JP4014882 B2 JP 4014882B2
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- silica sol
- sodium silicate
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Description
【０００１】
【発明の属する技術分野】
本発明は、Ｙ字型の反応装置を使用したシリカゾルの新規な製造方法に関する。詳しくは、Ｙ字型の反応装置に鉱酸と珪酸ソーダ溶液とを供給し、接触させてシリカゾルを得る方法において、反応生成物時に微細なゲル化物の発生を防止し、均質なシリカゾルを効率よく製造することができるシリカゾルの製造方法を提供するものである。
【０００２】
【従来の技術】
従来、工業的に製造されるシリカゾルは、攪拌中の鉱酸に珪酸ソーダ溶液を添加する方法、イオン交換樹脂を用いて珪酸ソーダ水溶液から製造する方法、アルキルシリケートを酸あるいはアルカリにより加水分解する方法等により製造されてきた。
【０００３】
その中で、我々は、シリカゾルを簡易的に製造するため、２つの原料供給管が合流し、該合流部にて排出管と連結してなるＹ字型の反応装置を使用して、高濃度の鉱酸と珪酸ソーダ溶液とを１０ｍ／秒以上の流速で接触させることにより、高濃度のシリカゾルを効率よく製造する方法を見出し提案した（特開昭６１−２２７９１５号）。上記方法の目的は、このようにして得られた高濃度のシリカゾルより均質なシリカゲルを得ることである。
【０００４】
近年、シリカゾルの用途として、シリカゲルの原料に使用される濃度よりも希薄な溶液を原料とする、水処理剤、製紙用等がある。これらの用途においては、ゲル化物を実質的に含まない均質なシリカゾルであって、数分間でゲル化することも無く、そのゾルの粘度が６〜３０ｍＰａ．ｓ程度にコントロールされたシリカゾルが望まれる。そのため、これらの用途に適用したシリカゾルを得るためには、特開昭６１−２２７９１５号の実施形態よりも、鉱酸の濃度が低く、珪酸ソーダ溶液のＳｉＯ２含量を低い原料が使用される。
【０００５】
そこで、我々は、上記用途に適用したシリカゾルを得る目的で、前記Ｙ字型の反応装置を使用して、鉱酸の濃度、珪酸ソーダ溶液のＳｉＯ２含量の低い原料を用いてシリカゾルの製造を試みた。しかしながら、得られたシリカゾルは一部微細なゲル化物を含むため、上記用途の原料としてはそのまま使用することが出来ず、ゲル化物を実質的に含まない均質なシリカゾルの製造方法の開発が望まれていた。
【０００６】
【発明が解決しようとする課題】
従って、本発明の目的は、Ｙ字型の反応装置を使用して、微細なゲル化物を実質的に含まない均質なシリカゾルを、効率よく製造できる方法を提供するものである。
【０００７】
【課題を解決するための手段】
本発明者らは、上記課題を解決するために鋭意研究を続けてきた。その結果、Ｙ字型の反応装置において、鉱酸と珪酸ソーダ溶液とが衝突混合後、反応液は排出管内を満たし液流として流出するが、その際の流速が遅い場合は、混合が十分に行われず、微細なゲル化物が生成し易い状態になるとの知見を得た。そして、かかる知見に基づき、更に研究を重ねた結果、鉱酸と珪酸ソーダ溶液を接触させて得られる反応生成物を特定の流速以上で流出させることにより、鉱酸と珪酸ソーダ溶液が十分に混合されゲル化物の発生もなく、均質なシリカゾルを製造できることを見出し、本発明を提案するに至った。即ち本発明は、２つの原料供給管が合流し、該合流部にて１つの排出管と連結してなり、それぞれの原料供給管には絞り部径が各々ｄ１及びｄ１’の絞り部が設けられ、これら絞り部の流出口から合流部までの距離Ｒは等しく、かつ該距離Ｒは、絞り部径ｄ１及びｄ１’の１〜９倍であるＹ字型の反応装置を使用し、該反応装置の原料供給管から鉱酸と珪酸ソーダ溶液を各々供給し、上記合流部にて両成分を接触させて得られた反応生成物を、流速１．０ｍ／秒以上で排出管から流出させることを特徴とするシリカゾルの製造方法である。
【０００８】
【発明の実施の形態】
以下本発明を詳細に説明する。
【０００９】
本発明に用いるＹ字型の反応装置としては、基本的には２つの原料供給管が合流し、該合流部にて１つの排出管と連結した構造を有する。図１に本発明に使用するＹ字型の反応装置の例を示す。図１に示すように、このＹ字型の反応装置は、鉱酸または珪酸ソーダ溶液が供給される原料供給管１、１’が合流し、合流部３にて排出管２が連結してなる。また、このＹ字型の反応装置は、原料供給管１、１’において、原料の流速を調整するための絞り部４、４’を設けたものを使用することができる。
【００１０】
本発明に用いる鉱酸としては、例えば硫酸、塩酸、硝酸等が挙げられ、特に硫酸が好適に用いられる。また、均質であって短時間でゲル化しないシリカゾルを得るためには、鉱酸の濃度は２〜７Ｎ、特に３〜６Ｎが好ましい。
【００１１】
本発明に用いる珪酸ソーダ溶液は、一般式ＳｉＯ２／Ｎａ２Ｏで示される水溶性の珪酸ソーダで該溶液のＳｉＯ２とＮａ２Ｏのモル比（ＳｉＯ２／Ｎａ２Ｏ）が２．５〜４．０のものが使用される。また、均質であって短時間でゲル化しないシリカゾルを得るためには、ＳｉＯ２成分の含有量は１００〜３００ｇ／Ｌ、特に２００〜２９０ｇ／Ｌが好ましい。
【００１２】
上記濃度の鉱酸及び珪酸ソーダ溶液を原料として、特開昭６１−２２７９１５号の実施例に記載されている条件でシリカゾルを製造したところ、得られたシリカゾル中に微細なゲル化物が生成し、水処理剤、製紙用等の原料として使用する場合、有効なシリカ量の減少を招くばかりでなく、該ゲル化物を除去するための工程を別途必要とした。そのため、Ｙ字型の反応装置を用いて、ゲル化物の出来ない均質なシリカゾルを得るために様々な検討を行ったところ、本発明にあっては、鉱酸と珪酸ソーダ溶液を接触させて得られた反応生成物を流速１．０m／秒以上で排出管から流出させ、合流部にて十分混合させることにより、微細なゲル化物が生じる問題を解決した。
【００１３】
即ち、本発明の最大の特徴は、図１に示すようなＹ字型の反応装置を使用して、鉱酸と珪酸ソーダ溶液を接触させて得られた反応生成物を流速１．０ｍ／秒以上、好ましくは１．３ｍ／秒以上で排出管から流出させることにある。該反応生成物の流速が１．０ｍ／秒未満の場合は、供給する原料の流速を上げて衝突による混合を強く行っても微細なゲル化物の発生を抑えることができない。一方、該反応生成物を流出させる流速の上限については制限されないが、一般には２０ｍ／秒で、それ以上速くすることはポンプの多大エネルギーを必要とし、また効果も同様となり、それ以上の効果を得ることはできない。
【００１４】
本発明において、均質なシリカゾルが得られる効果は、Ｙ字型の反応装置を使用して、鉱酸と珪酸ソーダ溶液を衝突させることによる混合と、得られる反応生成物の流速を早くすることによる反応系の混合との相乗効果によって得られる。
【００１５】
本発明において、該反応生成物を流速１．０ｍ／秒以上で流出させる態様は特に制限されることはないが、具体的には、絞り部４，４'から供給される液量の合計より、排出管内の流速が１．０ｍ／秒以上になるように、原料の供給量、排出口径等を決定してやればよい。
【００１６】
本発明において、原料供給管に各々供給される鉱酸と珪酸ソーダ溶液の流速は特に制限されるものではないが、絞り部の流速が鉱酸、珪酸ソーダ溶液ともに５ｍ／秒以上、好ましくは７ｍ／秒以上、更に好ましくは１０ｍ／秒以上であることが、合流部３にて、均一な反応を行うことができるため好ましい。なお、この方法においては、鉱酸と珪酸ソーダ溶液の両成分が上記の流速であることが均質なシリカゾルを得るためには好ましい。
【００１７】
本発明においては、均質なシリカゾルを得るために、Ｙ字型の反応装置の絞り部４、４’の流出口から合流部３までの距離Ｒは、絞り部径ｄ１、ｄ１’の１〜９倍（Ｒ／ｄ１またはｄ１’＝１〜９）である（ただし、絞り部４の流出口から合流部３までの距離と、絞り部４’の流出口から合流部３までの距離は等しい）。
【００１８】
本発明に用いるＹ字型の反応装置の材質は、鉱酸、珪酸ソーダ溶液等の耐薬品性に優れたものであれば例えばガラス、金属、プラスチック、ゴム等の公知のものが特に制限なく使用できる。
【００１９】
本発明において、Ｙ字型の反応装置を組み入れた工程を具体的に示せば、図2に示すように鉱酸と珪酸ソーダ溶液を原料供給管１、１’に供給するための原料貯槽５、５’及びポンプ６、６’等の原料移送手段が、一方シリカゾル排出管２の後には、得られたシリカゾルを貯蔵しておくためのシリカゾル貯槽７が接続したものが一般的である。
【００２０】
【実施例】
以下、実施例により本発明を具体的に説明するが、本発明はこれらの実施例に制限されるものではない。
【００２１】
実施例１
大きさ８０×８０ｍｍのＹ字型の反応装置を使用し、４．１６Ｎの硫酸を絞り部径４ｍｍに９．２Ｌ／ｍｉｎ．及びＳｉＯ２成分の含有量が２７１．４ｇ／Ｌの珪酸ソーダ水溶液を絞り部径（ｄ１）４．２ｍｍに１１．３４Ｌ／ｍｉｎ．で各々供給し、絞り部の流出口から合流部までの距離（Ｒ）と絞り部径（ｄ１）の比を２．５、排出口径１５ｍｍ，排出時の流速１．９ｍ／秒にして、１０分反応させ、２０５Ｌのゲル化物のない均質なシリカゾルを得た。
【００２２】
そのシリカゾル中のＳｉＯ２濃度は１４．９ｇ／１００ｍｌで、ｐＨは１．３９であった。その結果を表１に示す。
【００２３】
実施例２
実施例１と同じ濃度の硫酸、珪酸ソーダ水溶液を使用して、硫酸を９．５Ｌ／ｍｉｎ．、珪酸ソーダ溶液を１０．８Ｌ／ｍｉｎ．で各々供給し、排出口径１４ｍｍ、排出時の流速２．２ｍ／秒にした以外は実施例１と同様の操作を行った。その結果を表１に示す。
【００２４】
実施例３
大きさ４０×４０ｍｍのＹ字型の反応装置を使用して、４．０７Ｎの硫酸を絞り部径２．４ｍｍに３．０９Ｌ／ｍｉｎ．及びＳｉＯ２成分の含有量が２６５．８ｇ／Ｌの珪酸ソーダ水溶液を絞り部径（ｄ１）２．６ｍｍに３．７３Ｌ／ｍｉｎ．で各々供給し、絞り部の流出口から合流部までの距離（Ｒ）と絞り部径（ｄ１）の比を３．８、排出口径９ｍｍ，排出時の流速１．８ｍ／秒にして、２５分反応させ、１７０Ｌのゲル化物の無いシリカゾルを得た。その結果を表１に示す。
【００２５】
実施例４
４．２４Ｎの硫酸を絞り部径１．４ｍｍに１．０５Ｌ／ｍｉｎ．及びＳｉＯ２成分の含有量が２７１．７ｇ／Ｌの珪酸ソーダ水溶液を絞り部径（ｄ１）１．２ｍｍに１．２Ｌ／ｍｉｎ．で各々供給し、絞り部の流出口から合流部までの距離（Ｒ）と絞り部径（ｄ１）の比を８．３、排出口径６ｍｍ、排出時の流速１．３ｍ／秒にした以外は実施例３と同様の操作を行った。その結果を表１に示す。
比較例１
実施例１と同じ大きさのＹ字管反応装置を用いて、４．１２Ｎの硫酸を絞り部径４ｍｍに１０Ｌ／ｍｉｎ．及びＳｉＯ２成分の含有量が２７０ｇ／Ｌの珪酸ソーダ水溶液を絞り部径（ｄ１）４ｍｍに１１．５Ｌ／ｍｉｎ．で各々供給し、絞り部の流出口から合流部までの距離（Ｒ）と絞り部径（ｄ１）の比を６．３、排出口径３０ｍｍ、排出時の流速０．５１ｍ／秒とした以外は実施例１と同様の操作を行った。得られた反応生成物は、反応開始時から白いゲル化物を含んでなり、そのゲル化物が反応液液面に浮かんだものであった。その結果を表１に示す。
【００２６】
比較例２
実施例１の大きさのＹ字管反応装置を用いて、４．０３Ｎの硫酸を絞り部径４ｍｍに９．３４Ｌ／ｍｉｎ．及びＳｉＯ２成分の含有量が２７５．７ｇ／Ｌの珪酸ソーダ水溶液を絞り部径（ｄ１）４．２ｍｍに１０．７Ｌ／ｍｉｎ．で各々供給し、絞り部の流出口から合流部までの距離（Ｒ）と絞り部径（ｄ１）の比を２．５、排出口径を３０ｍｍ、排出時の流速０．４７ｍ／秒とした以外は、実施例１と同様の操作を行った。得られた反応生成物は、反応開始時よりゲル化物を含んでいた。その結果を表１に示す。
【００２７】
比較例３
実施例３と同じ大きさのＹ字管反応装置を用いて、４．０３Ｎの硫酸を絞り部径２．４ｍｍに３．７５Ｌ／ｍｉｎ．及びＳｉＯ２成分の含有量が２７５．７ｇ／Ｌの珪酸ソーダ水溶液を絞り部径（ｄ１）２．６ｍｍに４．４８Ｌ／ｍｉｎ．で各々供給し、絞り部の流出口から合流部までの距離（Ｒ）と絞り部径（ｄ１）の比を３．８、排出口径を１４ｍｍ、排出時の流速を０．８９ｍ／秒とした以外は、実施例３と同様の操作を行った。得られた反応生成物は、反応開始時から白色のゲル化物を含んでいた。その結果を表１に示す。
【００２８】
比較例４
実施例４において、硫酸を０．９２Ｌ／min．珪酸ソーダ水溶液を１．０２Ｌ／ｍｉｎ．で各々供給し、排出口径９ｍｍにして排出時の流速を０．５１ｍ／秒とした以外は、実施例３と同様の操作を行った。得られた反応生成物は、反応開始時から白色のゲル化物を含んでいた。その結果を表１に示す。
【００２９】
【表１】
【発明の効果】
本発明の方法によれば、鉱酸と珪酸ソーダ溶液を接触させて得られたシリカゾルを特定の流速で取り出すことにより、高濃度であって均質なシリカゾルを簡便に生成することができる。また、本発明の方法により得られたシリカゾルは、土壌固化剤、水処理の凝集剤、紙のコーティング剤、鋳物の成形助剤、シリカゲル，合成石英等の原材料として使用することができる。
【００３１】
【図面の簡単な説明】
【図１】本発明に用いる反応装置の代表的な１例を示す概要図である。
【図２】本発明の代表的なフロー図である。
【符号の説明】
１、１’：原料供給管
２：排出管
３：合流部
４、４’：絞り部
Ｒ：絞り部の流出口から合流部までの距離
ｄ１、ｄ１’：絞り部径
ｄ２：排出口径
５、５’：原料貯槽
６、６’：ポンプ
７：シリカゾル貯槽[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a novel method for producing silica sol using a Y-shaped reactor. Specifically, in a method of obtaining a silica sol by supplying mineral acid and sodium silicate solution to a Y-shaped reactor and bringing them into contact with each other, the generation of a fine gelled product during the reaction product is prevented, and a homogeneous silica sol is efficiently produced. A method for producing a silica sol that can be produced is provided.
[0002]
[Prior art]
Conventionally, the silica sol produced industrially is a method of adding a sodium silicate solution to a stirring mineral acid, a method of producing from a sodium silicate aqueous solution using an ion exchange resin, a method of hydrolyzing an alkyl silicate with an acid or an alkali. Etc. have been manufactured.
[0003]
Among them, in order to easily produce silica sol, we used a Y-shaped reactor in which two raw material supply pipes joined together and connected to a discharge pipe at the joining part, and high concentration A method for efficiently producing a high-concentration silica sol by contacting a mineral acid and a sodium silicate solution at a flow rate of 10 m / sec or more has been proposed (Japanese Patent Laid-Open No. 61-227915). The purpose of the above method is to obtain a homogeneous silica gel from the high concentration silica sol thus obtained.
[0004]
In recent years, applications of silica sol include water treatment agents, paper making, and the like using a solution diluted to a concentration lower than the concentration used as a raw material for silica gel. In these applications, it is a homogeneous silica sol that is substantially free of gelled material and does not gel in a few minutes, and the sol has a viscosity of 6 to 30 mPa.s. A silica sol controlled to about s is desired. Therefore, in order to obtain a silica sol applied to these uses, a raw material having a lower mineral acid concentration and a lower SiO 2 content in the sodium silicate solution than that of the embodiment of JP-A No. 61-227915 is used.
[0005]
Therefore, for the purpose of obtaining a silica sol applied to the above-mentioned application, we use the Y-shaped reactor to produce a silica sol using a raw material having a low mineral acid concentration and a low SiO 2 content of sodium silicate solution. Tried. However, since the obtained silica sol partially contains a fine gelled product, it cannot be used as it is as a raw material for the above applications, and development of a method for producing a homogeneous silica sol substantially free of the gelated product is desired. It was.
[0006]
[Problems to be solved by the invention]
Accordingly, an object of the present invention is to provide a method capable of efficiently producing a homogeneous silica sol substantially free from fine gelled products using a Y-shaped reactor.
[0007]
[Means for Solving the Problems]
The inventors of the present invention have continually studied to solve the above problems. As a result, in the Y-shaped reactor, after the mineral acid and sodium silicate solution collide and mix, the reaction liquid fills the discharge pipe and flows out as a liquid flow, but if the flow rate at that time is slow, mixing is sufficient It was not carried out and the knowledge that it will be in the state which becomes easy to produce | generate a fine gelled material was acquired. As a result of further research based on this finding, the reaction product obtained by bringing the mineral acid and sodium silicate solution into contact with each other is allowed to flow out at a specific flow rate or higher so that the mineral acid and sodium silicate solution are sufficiently mixed. As a result, the inventors have found that a homogeneous silica sol can be produced without generation of a gelled product, and the present invention has been proposed. That is, the present invention comprises two joined material supply pipe, Ri in name in conjunction with one of the discharge pipe confluence portion, the diaphragm portion of the diaphragm portion diameter Each of the raw material supply pipe respectively d1 and d1 ' provided, equal distance R to the merging section from the outlet of the throttle portion, and the distance R can use the reactor 1-9 Baidea Ru Y-shaped aperture portion diameter d1 and d1 ', supplying each mineral acids and sodium silicate solution from the raw material supply pipe of the reactor, discharging the reaction product obtained by contacting the both components Te in the merging portion, a discharge pipe at a flow rate of 1.0 m / sec or more A method for producing a silica sol.
[0008]
DETAILED DESCRIPTION OF THE INVENTION
The present invention will be described in detail below.
[0009]
The Y-shaped reactor used in the present invention basically has a structure in which two raw material supply pipes are joined and connected to one discharge pipe at the joining part. FIG. 1 shows an example of a Y-shaped reactor used in the present invention. As shown in FIG. 1, this Y-shaped reactor is formed by joining raw
[0010]
Examples of the mineral acid used in the present invention include sulfuric acid, hydrochloric acid, nitric acid and the like, and sulfuric acid is particularly preferably used. Further, in order to obtain a silica sol that is homogeneous and does not gel in a short time, the concentration of the mineral acid is preferably 2 to 7N, particularly 3 to 6N.
[0011]
The sodium silicate solution used in the present invention is a water-soluble sodium silicate represented by the general formula SiO 2 / Na 2 O, and the molar ratio of SiO 2 and Na 2 O (SiO 2 / Na 2 O) of the solution is 2.5. ~ 4.0 are used. In order to obtain a silica sol that is homogeneous and does not gel in a short time, the content of the SiO 2 component is preferably 100 to 300 g / L, particularly preferably 200 to 290 g / L.
[0012]
Using a mineral acid and sodium silicate solution having the above concentrations as raw materials, a silica sol was produced under the conditions described in Examples of JP-A No. 61-227915. As a result, a fine gelled product was produced in the obtained silica sol, When used as a raw material for water treatment agents, papermaking, etc., not only the amount of effective silica was reduced, but also a separate step for removing the gelled product was required. For this reason, various studies were carried out using a Y-shaped reactor to obtain a homogeneous silica sol with no gelled product. In the present invention, a mineral acid and a sodium silicate solution were brought into contact with each other. The reaction product obtained was discharged from the discharge pipe at a flow rate of 1.0 m / second or more and sufficiently mixed at the junction, thereby solving the problem of forming a fine gelled product.
[0013]
That is, the greatest feature of the present invention is that a reaction product obtained by bringing a mineral acid and a sodium silicate solution into contact with each other using a Y-shaped reactor as shown in FIG. As described above, preferably, the discharge pipe is allowed to flow out at a rate of 1.3 m / second or more. When the flow rate of the reaction product is less than 1.0 m / sec, generation of fine gelled product cannot be suppressed even if the flow rate of the raw material to be supplied is increased and mixing by collision is performed strongly. On the other hand, the upper limit of the flow rate at which the reaction product is allowed to flow out is not limited, but generally 20 m / second, and making it faster requires a lot of energy from the pump, and the effect is the same. I can't get it.
[0014]
In the present invention, the effect of obtaining a homogeneous silica sol is that, by using a Y-shaped reactor, mixing by colliding the mineral acid and sodium silicate solution and increasing the flow rate of the resulting reaction product. It is obtained by a synergistic effect with the mixing of the reaction system.
[0015]
In the present invention, the aspect in which the reaction product is allowed to flow out at a flow rate of 1.0 m / sec or more is not particularly limited, but specifically, from the total amount of liquid supplied from the
[0016]
In the present invention, the flow rates of the mineral acid and sodium silicate solution respectively supplied to the raw material supply pipe are not particularly limited, but the flow rates of the throttle portions are 5 m / second or more, preferably 7 m for both the mineral acid and sodium silicate solution. / Second or more, more preferably 10 m / second or more, since a uniform reaction can be performed at the junction 3. In this method, it is preferable that both components of the mineral acid and the sodium silicate solution have the above flow rates in order to obtain a homogeneous silica sol.
[0017]
In the present invention, in order to obtain a homogeneous silica sol, the distance R from the outlet of the
[0018]
The material of the Y-shaped reactor used in the present invention may be any known material such as glass, metal, plastic, rubber, etc., as long as it has excellent chemical resistance such as mineral acid and sodium silicate solution. it can.
[0019]
In the present invention, if a process incorporating a Y-shaped reactor is specifically shown, a raw
[0020]
【Example】
EXAMPLES Hereinafter, although an Example demonstrates this invention concretely, this invention is not restrict | limited to these Examples.
[0021]
Example 1
Using a Y-shaped reactor with a size of 80 × 80 mm, 4.16 N sulfuric acid was applied to a diameter of the throttle part of 4 mm and 9.2 L / min. And an aqueous solution of sodium silicate having a content of SiO 2 component of 271.4 g / L at a throttle part diameter (d1) of 4.2 mm of 11.34 L / min. The ratio of the distance (R) from the outlet of the throttle part to the converging part is 2.5, the ratio of the throttle part diameter (d1) is 2.5, the outlet diameter is 15 mm, and the flow rate during discharge is 1.9 m / sec. The reaction was allowed to proceed to obtain 205 L of a homogeneous silica sol without gelation.
[0022]
The SiO2 concentration in the silica sol was 14.9 g / 100 ml, and the pH was 1.39. The results are shown in Table 1.
[0023]
Example 2
Using sulfuric acid and sodium silicate aqueous solution having the same concentration as in Example 1, sulfuric acid was added at 9.5 L / min. The sodium silicate solution was 10.8 L / min. The same operation as in Example 1 was performed except that the discharge port diameter was 14 mm and the flow rate during discharge was 2.2 m / sec. The results are shown in Table 1.
[0024]
Example 3
Using a Y-shaped reactor having a size of 40 × 40 mm, 4.07 N sulfuric acid was added to the throttle part diameter of 2.4 mm and 3.09 L / min. And an aqueous solution of sodium silicate having a content of SiO 2 component of 265.8 g / L at a throttle part diameter (d1) of 2.6 mm, 3.73 L / min. The ratio of the distance (R) from the outlet of the throttle part to the converging part and the diameter of the throttle part (d1) is 3.8, the outlet diameter is 9 mm, and the discharge flow rate is 1.8 m / sec. The reaction was allowed to proceed to obtain 170 L of silica sol having no gelled product. The results are shown in Table 1.
[0025]
Example 4
4.24N sulfuric acid was added at a throttle diameter of 1.4 mm at 1.05 L / min. And an aqueous solution of sodium silicate having a content of SiO 2 component of 271.7 g / L, 1.2 L / min. Except that the ratio of the distance (R) from the outlet of the throttle part to the merging part and the diameter of the throttle part (d1) is 8.3, the outlet diameter is 6 mm, and the flow velocity during discharge is 1.3 m / sec. The same operation as in Example 3 was performed. The results are shown in Table 1.
Comparative Example 1
Using a Y-tube reactor of the same size as in Example 1, 4.12N sulfuric acid was applied at a throttle diameter of 4 mm at 10 L / min. And a SiO 2 component content of 270 g / L of sodium silicate aqueous solution at a squeeze part diameter (d1) of 4 mm at 11.5 L / min. Except that the ratio of the distance (R) from the outlet of the throttle part to the merging part and the diameter of the throttle part (d1) is 6.3, the outlet diameter is 30 mm, and the flow rate during discharge is 0.51 m / sec. The same operation as in Example 1 was performed. The obtained reaction product contained a white gelled product from the beginning of the reaction, and the gelled product floated on the reaction liquid surface. The results are shown in Table 1.
[0026]
Comparative Example 2
Using a Y-tube reactor having the same size as that of Example 1, 4.03N sulfuric acid was added to a throttle part diameter of 4 mm at 9.34 L / min. And a sodium silicate aqueous solution having a SiO 2 component content of 275.7 g / L at a throttle part diameter (d1) of 4.2 mm of 10.7 L / min. The ratio of the distance (R) from the outlet of the throttle part to the converging part is 2.5, the ratio of the throttle part diameter (d1) is 2.5, the discharge port diameter is 30 mm, and the discharge flow rate is 0.47 m / sec. The same operation as in Example 1 was performed. The obtained reaction product contained a gelled product from the start of the reaction. The results are shown in Table 1.
[0027]
Comparative Example 3
Using a Y-tube reactor of the same size as in Example 3, 4.03 N sulfuric acid was added to the throttle part diameter of 2.4 mm at 3.75 L / min. And a sodium silicate aqueous solution having a SiO 2 component content of 275.7 g / L and a squeezing part diameter (d1) of 2.6 mm of 4.48 L / min. The ratio of the distance (R) from the outlet of the throttle part to the converging part and the diameter of the throttle part (d1) was 3.8, the outlet diameter was 14 mm, and the flow rate during discharge was 0.89 m / sec. Except for the above, the same operation as in Example 3 was performed. The obtained reaction product contained a white gelled product from the start of the reaction. The results are shown in Table 1.
[0028]
Comparative Example 4
In Example 4, sulfuric acid was 0.92 L / min. Sodium silicate aqueous solution was added at 1.02 L / min. The same operation as in Example 3 was performed except that the discharge port diameter was 9 mm and the flow rate during discharge was 0.51 m / sec. The obtained reaction product contained a white gelled product from the start of the reaction. The results are shown in Table 1.
[0029]
[Table 1]
【The invention's effect】
According to the method of the present invention, a silica sol obtained by bringing a mineral acid and a sodium silicate solution into contact with each other can be taken out at a specific flow rate, whereby a high-concentration and homogeneous silica sol can be easily produced. The silica sol obtained by the method of the present invention can be used as a raw material for soil solidifying agents, water treatment flocculants, paper coating agents, casting molding aids, silica gel, synthetic quartz and the like.
[0031]
[Brief description of the drawings]
FIG. 1 is a schematic view showing a typical example of a reaction apparatus used in the present invention.
FIG. 2 is a representative flow diagram of the present invention.
[Explanation of symbols]
1, 1 ': Raw material supply pipe 2: Discharge pipe 3:
Claims (2)
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| JP2002021879A JP4014882B2 (en) | 2002-01-30 | 2002-01-30 | Method for producing silica sol |
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| JP2002021879A JP4014882B2 (en) | 2002-01-30 | 2002-01-30 | Method for producing silica sol |
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| JP4014882B2 true JP4014882B2 (en) | 2007-11-28 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005194463A (en) * | 2004-01-09 | 2005-07-21 | Tokuyama Corp | Method for preparing aqueous non-alkaline silicic acid solution for grouting chemical |
| JP5013683B2 (en) * | 2004-06-24 | 2012-08-29 | 株式会社トクヤマ | Method for producing surface-treated silica-based oxide, and method for producing surface-treated silica-based oxide slurry |
| CN101218179B (en) | 2005-08-24 | 2010-12-08 | 株式会社德山 | Method for treatment of wastewater containing fumed silica |
| CA2620058A1 (en) | 2005-08-24 | 2007-03-01 | Tokuyama Corporation | Method of treating silicon powder-containing drainage water |
| JP5200238B2 (en) * | 2006-07-20 | 2013-06-05 | 富士化学株式会社 | Method for producing silica sol |
| FR2910459B1 (en) * | 2006-12-22 | 2010-09-17 | Rhodia Recherches & Tech | NEW PROCESS FOR THE PREPARATION OF PRECIPITED SILICES BY IMPLEMENTING A RAPID MIXER |
| JP4897527B2 (en) * | 2007-03-23 | 2012-03-14 | 中国電力株式会社 | Soil improvement method |
| KR20090024711A (en) * | 2007-05-11 | 2009-03-09 | 가부시끼가이샤 도꾸야마 | Processes for production of iron-silica coagulants for water treatment |
| JP6204695B2 (en) * | 2013-05-15 | 2017-09-27 | 株式会社トクヤマ | Method for producing metal oxide sol |
| JP6161966B2 (en) * | 2013-06-11 | 2017-07-12 | 株式会社トクヤマ | Mixer and method for producing metal oxide sol using the same |
| KR101927277B1 (en) | 2014-01-14 | 2018-12-10 | 가부시끼가이샤 도꾸야마 | Hydrophobized spherical poly (alkyl silsesquioxane) microparticles, external additive for toner, dry electrophotography toner, and method for manufacturing hydrophobized spherical poly (alkyl silsesquioxane) microparticles |
| JP2017071740A (en) * | 2015-10-09 | 2017-04-13 | 信越化学工業株式会社 | Manufacturing method of spherical polyorganosilsesquioxane particle |
| JP7284167B2 (en) | 2018-07-03 | 2023-05-30 | 株式会社トクヤマ | spherical polymethylsilsesquioxane particles |
| TW202408934A (en) * | 2022-05-13 | 2024-03-01 | 日商多摩化學工業股份有限公司 | Colloidal silica and production method therefor |
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