JPS61227841A - Preparation of filter assistant - Google Patents

Preparation of filter assistant

Info

Publication number
JPS61227841A
JPS61227841A JP60067847A JP6784785A JPS61227841A JP S61227841 A JPS61227841 A JP S61227841A JP 60067847 A JP60067847 A JP 60067847A JP 6784785 A JP6784785 A JP 6784785A JP S61227841 A JPS61227841 A JP S61227841A
Authority
JP
Japan
Prior art keywords
coal ashes
coal ash
autoclave
weight
added
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.)
Granted
Application number
JP60067847A
Other languages
Japanese (ja)
Other versions
JPH0316176B2 (en
Inventor
Shuji Tsunematsu
修二 恒松
Hidekazu Abe
英一 安部
Naomichi Hara
尚道 原
Hideharu Hirosue
井上 憲弘
Norihiro Inoue
広末 英晴
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.)
National Institute of Advanced Industrial Science and Technology AIST
Original Assignee
Agency of Industrial Science and Technology
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 Agency of Industrial Science and Technology filed Critical Agency of Industrial Science and Technology
Priority to JP60067847A priority Critical patent/JPS61227841A/en
Publication of JPS61227841A publication Critical patent/JPS61227841A/en
Publication of JPH0316176B2 publication Critical patent/JPH0316176B2/ja
Granted legal-status Critical Current

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  • Filtering Materials (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

PURPOSE:To obtain a filter assistant consisting of a porous material wherein many holes are present by adding lime of the specified amount to the coal ashes, mixing the mixture and performing the hydrothermal reaction in an autoclave. CONSTITUTION:10-40pts.wt. is added to 100pts.wt. coal ashes and the mixture is mixed by adding water and the stirred slurry is heated in an autoclave to perform the hydrothermal reaction. Still more in this case, gypsum may be added to accelerate the reaction. A porous material wherein the many fine holes are present as shown in a figure is obtained by filtering, dehydrating and drying the obtained slurry of calcium silicate hydrate. The coal ashes to be used is preferably calcined at about 600 deg.C to remove the nonburned carbon as the pretreatment and furthermore it is more preferable that the degree of crystallization of coal ashes is increased by calcining them at about 1,000 deg.C. By such a method, the filter assistant exhibiting the same characteristics as diatom earth or above is obtained out of the coal ashes produced in great quantities.

Description

【発明の詳細な説明】 〈産業上の利用分野〉 本発明は、石炭灰を原料□として濾過助剤を製造する方
法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a method for producing a filter aid using coal ash as a raw material □.

〈従来の技術〉 近年のエネルギー事情に伴い火力発電所をはじめとする
石炭が再び多用される様になり、石炭灰が大量に産出さ
れる。しかるにこの石炭灰は現状としては有効な利用方
法は開発されておらず、未利用資源あるいは産業廃棄物
の域を脱していない。
<Conventional Technology> Due to the energy situation in recent years, coal is once again being used extensively in thermal power plants, and a large amount of coal ash is being produced. However, as of now, no effective method for using this coal ash has been developed, and it is still considered as an unused resource or industrial waste.

一方分散粒子がべ1・べl−1,た性質で濾材に目詰ま
りを起こさせる場合や、又は分散粒子が微細で、かつ濃
度が薄い場合等に用いる濾過助剤としては、従来からケ
イソウ上、パーライトが主として用いられ、その他木材
パルプから製造される繊維状濾過剤や炭素質濾過助剤も
若干用いられて来た。
On the other hand, as a filter aid used when the dispersed particles cause clogging of the filter medium due to their viscous nature, or when the dispersed particles are fine and have a low concentration, diatom-based filter aids have traditionally been used. Perlite has been mainly used, and fibrous filter agents made from wood pulp and carbonaceous filter aids have also been used to some extent.

〈発明が解決しようとする問題点〉 本発明は豊富に産出されているにも拘らず、そ1の有効
な利用法が見出されていない石炭灰から、産業上有用な
濾過助剤を製造しようとするものである。
<Problems to be solved by the invention> The present invention aims to produce an industrially useful filter aid from coal ash, which is abundantly produced but for which no effective use has been found. This is what I am trying to do.

〈問題点を解決する為の手段〉 本発明では、上記目的達成の為に、石炭灰に適量の石灰
を添加して出発原料となすものであり、その要旨は石炭
灰100重量部に対して、石灰10〜40重量部を添加
混合し、次いてオートクレーブによる水熱反応を行なわ
しめることを特徴とする濾過助剤の製造方法である。
<Means for Solving the Problems> In order to achieve the above-mentioned purpose, the present invention uses coal ash as a starting material by adding an appropriate amount of lime. , 10 to 40 parts by weight of lime are added and mixed, and then a hydrothermal reaction is carried out in an autoclave.

なお出発原料として石灰と共に石膏をも添加混合した原
料を用いればオーl−クレープ中の反応が促進され、よ
り好ま1ツいものである。
It is more preferable to use a raw material in which gypsum is added and mixed together with lime as a starting raw material because the reaction in the ol-crepe is accelerated.

」1記方法に於いて、石灰の添加量を10〜40重量部
としたのは、10重量部未満の場合は石炭灰粒子表面に
濾過効果をもたらすケイ酸カルシウム水和物が十分に生
成されず、又40重量%を越えるとオートクレーブによ
る水熱反応の反応速度は大となるが、未反応の微細粒子
が残存し、濾過の際にこの未反応の微細粒子が濾材に付
着し濾過効果を阻害するからである。 次に反応促進の
為に添加する石膏は、その添加量が3重皿部より少ない
場合には添加の効果が殆んど見られず、逆に15重量部
を越えると未反応石膏として残存し濾過効果を阻害する
ので3〜15重量部とする。
In the method described in 1, the amount of lime added is set to 10 to 40 parts by weight because if it is less than 10 parts by weight, calcium silicate hydrate that provides a filtration effect on the surface of coal ash particles will not be sufficiently produced. Furthermore, if it exceeds 40% by weight, the reaction rate of the hydrothermal reaction in an autoclave will increase, but unreacted fine particles will remain, and during filtration, these unreacted fine particles will adhere to the filter medium and reduce the filtration effect. This is because it inhibits. Next, when gypsum is added to promote the reaction, if the amount added is less than the triple plate part, almost no effect will be seen; on the other hand, if it exceeds 15 parts by weight, it will remain as unreacted gypsum. Since it inhibits the filtration effect, the amount is set at 3 to 15 parts by weight.

又使用する石炭灰は、そのまま−の状態でも良いが、未
燃カーボンが含まれる場合には灰黒色を□呈しており、
乙の未燃カーボンが濾液に悪影響を与える事がある事が
あるので、前処理として400〜600℃で焼成すると
好ましい。更に前処理の焼成温度を1000℃位の高温
とすれば、石炭灰中に含よれる種々の不安定物質を固定
化する事が出来、濾液中への溶出が防Iト出来ると共に
、石炭灰粒子自体を局部的に結晶化せしめ、その後の4
−トクレープ中の反応で結晶化さ第1ていないガラス相
の部分のみが選択的に反応し結晶相はそのま5の形態で
残る結果石炭灰の内部から多孔質化が進行し、得られろ
製品がより望ましい形態となる。
The coal ash used may be used as is, but if it contains unburned carbon, it will take on a gray-black color.
Since the unburnt carbon (B) may have an adverse effect on the filtrate, it is preferable to calcinate it at 400 to 600°C as a pretreatment. Furthermore, by setting the pretreatment firing temperature to a high temperature of around 1000°C, various unstable substances contained in coal ash can be immobilized, preventing their elution into the filtrate, and reducing coal ash. The particles themselves are locally crystallized, and the subsequent 4
- Only the part of the glass phase that is not crystallized by the reaction in the tocrepe selectively reacts, and the crystalline phase remains in the form of 5. As a result, the coal ash becomes porous from the inside, resulting in the formation of porosity. The product takes on a more desirable form.

次に4−トクレープに於ける反応は、高温にする程圧力
も高くなり、反応速度は大となるが、本発明方法の場合
には220℃以下で十分てあり、又反応時間は最長でも
48時間あれば十分である。
Next, in the reaction in 4-tocrepe, the higher the temperature, the higher the pressure and the faster the reaction rate, but in the case of the method of the present invention, a temperature of 220°C or lower is sufficient, and the reaction time is at most 48°C. It's enough time.

〈実施例及び作用〉 以下本発明の実施例及び濾過試験結果を示す。<Examples and effects> Examples of the present invention and filtration test results are shown below.

】ε施−例」− 石炭灰10011i里部と、CaO18重量部とを添加
混合した混合粉末に対し、重量比で20倍相当の水を加
えて混合、攪拌したスラリーを、180℃で24時間オ
ートクレーブ中で攪拌し乍ら水熱反応を行いケイ酸カル
シウム水和物スラリーを得た。
】εExample - A slurry made by adding 20 times the weight of water to a mixed powder made by adding and mixing 10011 parts of coal ash and 18 parts by weight of CaO was mixed and stirred at 180°C for 24 hours. A hydrothermal reaction was carried out while stirring in an autoclave to obtain a calcium silicate hydrate slurry.

この様にして得られtこケイ酸カルシウム水和物スラリ
ーを濾過、脱水して100℃で24時間乾燥した。得ら
れた粉体を電子顕微鏡で観、察した結果を第1図に示す
が、この写真から判る如く微細な空孔が多数存在する多
孔質体であった。
The calcium silicate hydrate slurry thus obtained was filtered, dehydrated, and dried at 100° C. for 24 hours. The obtained powder was observed under an electron microscope and the results are shown in FIG. 1. As can be seen from this photograph, it was a porous material containing many fine pores.

失血■又 石炭灰に混入している未燃カーボンを除去する為に60
0℃で4時間加熱処理を施した石炭灰を用い上記実施例
1と同様にしてケイ酸カルシウム水和物を得た。
Blood loss■Also, to remove unburned carbon mixed in coal ash, 60%
Calcium silicate hydrate was obtained in the same manner as in Example 1 using coal ash heat-treated at 0° C. for 4 hours.

111ユ 石炭灰に混入している未燃カーボンを除、去すると共に
、石炭灰の結晶化度を上げる為に1000℃で8時間加
熱処理を施した物100重量部に対し、CaOを20重
量部、Ca S 04・2 H20を5重量部添加混合
して混合粉末を得た。この混合粉末に対し、重量比で2
0倍の水を加えて混合、攪拌したスラリーを180℃で
24時間オートクレーブ中で攪拌し乍ら水熱反応1.を
行い、次いで上記実施例1と同様にして得た粉体を電子
顕微鏡で観察した結果を第2図に示すが、この写真から
判る如く外層のみならず、芯部まで微細な空孔が連通し
ている多孔質体であった。
20 parts by weight of CaO was added to 100 parts by weight of 111 parts of coal ash that was heated at 1000°C for 8 hours to remove unburned carbon mixed in and to increase the crystallinity of the coal ash. 5 parts by weight of Ca S 04.2 H20 were added and mixed to obtain a mixed powder. For this mixed powder, the weight ratio is 2
The slurry, which was mixed and stirred with 0 times the amount of water, was stirred in an autoclave at 180°C for 24 hours while undergoing a hydrothermal reaction. The powder obtained in the same manner as in Example 1 was then observed with an electron microscope, and the results are shown in Figure 2.As can be seen from this photograph, fine pores are connected not only to the outer layer but also to the core. It was a porous body.

このことは、この粉体を2NHC1で処理することによ
りケイ酸カルシウム水和物を除去した石炭灰自体を電子
顕微鏡により観察しtコ結果を第3図に示すが、乙の写
真から判る如くこの石炭灰自体も多孔質体となっている
事からも確頌された。なお比較の為に未処理の石炭灰の
電子顕微鏡写真を第4図に示すが、表面が凹凸粗面を呈
しているものの多孔質体とはなっていなかった。
This is confirmed by treating the powder with 2NHC1 to remove calcium silicate hydrate, and observing the coal ash itself using an electron microscope. The results are shown in Figure 3. It is also believed that coal ash itself is porous. For comparison, an electron micrograph of untreated coal ash is shown in FIG. 4, and although the surface was rough and uneven, it was not porous.

以上の実施例によって得られた試作濾過助剤と市販のケ
イソウ土を用い濾過実験を行った結果を以下に示す。
The results of a filtration experiment using the prototype filter aid obtained in the above examples and commercially available diatomaceous earth are shown below.

この実験は、濾過面積が63.6cdの加圧濾過器を用
い、蛙目粘土スラリーに各濾過助剤をボディフィードし
てルース(Ruth)の定圧濾過係数にに[cj/se
c〕(スラリ一温度20℃でのに値)を求めた。その際
の濾過圧力はI Kglcd 、スラリー濃度は01、
固形分中の濾過助剤の容積割合は05及び067で行な
った。
In this experiment, a pressure filter with a filtration area of 63.6 cd was used, and each filter aid was body-fed to the frog's eye clay slurry to reach Ruth's constant pressure filtration coefficient [cj/se
c] (value at slurry temperature of 20°C) was determined. At that time, the filtration pressure was I Kglcd, the slurry concentration was 01,
The volume ratio of the filter aid in the solid content was 05 and 067.

下記第1表に実験に用いt:試料の物性値を、又第2表
に定圧濾過速度係数に2oを示す。
Table 1 below shows t: the physical property values of the samples used in the experiment, and Table 2 shows 2o for the constant pressure filtration rate coefficient.

゛・。゛・.

\   パ。\  Pa.

□ ′□□、゛ 、 −,,、。□ ′□□、゛ 、 -,,,.

、l ト1 □ (7)゛      、 :11 (q) ミニ’、、、4&’l  l’、:’−’+・  、、
111゛・、、′、         −八 −3≧、 〈発明の効果〉            ”−以上述べ
て来た如く、本発明方法によA1ばオートクレーブ中に
於ける水熱反応により、空孔が多く存在する多孔質体か
ら成る濾過助剤を得る事が出来、特にオートクレーブの
水熱反応前に石炭灰を高温(1000℃)焼成したもの
にあってはその空隙率がケイソウ十の08に対し09に
も達17ており、上記第2表に示す様に定圧濾過係数も
既存のケイソウ土濾過助剤と同等、ないしはそれ以上と
なり優れた濾過特性を奏するものである。
, l To1 □ (7)゛ , :11 (q) Mini',,,4 &'l l', :'-'+・,,
111゛・,,′, -8-3≧, <Effects of the invention> ”-As stated above, in the method of the present invention, A1 has many pores due to the hydrothermal reaction in the autoclave. It is possible to obtain a filter aid made of a porous material, and especially when coal ash is fired at a high temperature (1000°C) before the hydrothermal reaction in an autoclave, the porosity is as high as 0.09 compared to 0.08 for diatomaceous material. As shown in Table 2 above, the constant pressure filtration coefficient is equal to or higher than that of existing diatomaceous earth filter aids, demonstrating excellent filtration properties.

従って未利用資源の活用として工業−1二大きな効果を
有するものである。
Therefore, it has great effects on industry as a means of utilizing unused resources.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は本発明実施例1で得られた濾過助剤粒子の30
00倍の電子顕微鏡写真、第2図は同実施例3で得られ
た濾過助剤粒子の7000倍の電子顕微鏡写真、第3図
は同実施例3で処理した後の石炭灰粒子の7000倍の
電子顕微鏡写真、第4図は未処理石炭灰粒子の3000
倍の電子顕微鏡写14゜第1図 第2図 第3図 第4 図
Figure 1 shows 30% of the filter aid particles obtained in Example 1 of the present invention.
00x electron micrograph, Figure 2 is a 7000x electron micrograph of the filter aid particles obtained in Example 3, and Figure 3 is a 7000x electron micrograph of the coal ash particles treated in Example 3. Figure 4 is an electron micrograph of 3000 untreated coal ash particles.
Magnified electron micrograph 14° Fig. 1 Fig. 2 Fig. 3 Fig. 4

Claims (1)

【特許請求の範囲】 1、石炭灰100重量部に対して、石灰10〜40重量
部を添加混合し、次いでオートクレーブに、Lる水熱反
応を行なわしめる乙とを特徴とする濾過助剤の製造方法
。 2、石炭灰100重量部に対して、石灰10〜40重量
部及び石膏3〜15重量部を添加混合し、次いでオート
クレーブによる水熱反応を行なわしめることを特徴とす
る濾過助剤の製造方法。
[Claims] 1. A filter aid characterized in that 10 to 40 parts by weight of lime are added and mixed to 100 parts by weight of coal ash, and then a hydrothermal reaction is carried out in an autoclave. Production method. 2. A method for producing a filter aid, which comprises adding and mixing 10 to 40 parts by weight of lime and 3 to 15 parts by weight of gypsum to 100 parts by weight of coal ash, and then carrying out a hydrothermal reaction in an autoclave.
JP60067847A 1985-03-29 1985-03-29 Preparation of filter assistant Granted JPS61227841A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP60067847A JPS61227841A (en) 1985-03-29 1985-03-29 Preparation of filter assistant

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP60067847A JPS61227841A (en) 1985-03-29 1985-03-29 Preparation of filter assistant

Publications (2)

Publication Number Publication Date
JPS61227841A true JPS61227841A (en) 1986-10-09
JPH0316176B2 JPH0316176B2 (en) 1991-03-04

Family

ID=13356755

Family Applications (1)

Application Number Title Priority Date Filing Date
JP60067847A Granted JPS61227841A (en) 1985-03-29 1985-03-29 Preparation of filter assistant

Country Status (1)

Country Link
JP (1) JPS61227841A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013195369A (en) * 2012-03-22 2013-09-30 Taiheiyo Cement Corp Extracting method of coal ash particle, and estimation method of composition phase ratio of cement and manufacturing method of cement using extracting method concerned

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS49122889A (en) * 1973-03-29 1974-11-25

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS49122889A (en) * 1973-03-29 1974-11-25

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013195369A (en) * 2012-03-22 2013-09-30 Taiheiyo Cement Corp Extracting method of coal ash particle, and estimation method of composition phase ratio of cement and manufacturing method of cement using extracting method concerned

Also Published As

Publication number Publication date
JPH0316176B2 (en) 1991-03-04

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