JP3710733B2 - Phosphorus elution prevention treatment method for beer lees forming coal, beer lees forming coal subjected to phosphorus elution prevention treatment, and water purification material comprising the beer lees forming coal - Google Patents
Phosphorus elution prevention treatment method for beer lees forming coal, beer lees forming coal subjected to phosphorus elution prevention treatment, and water purification material comprising the beer lees forming coal Download PDFInfo
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Description
【０００１】
【発明の属する技術分野】
本発明は、ビール粕成形炭のリン溶出防止処理法、リン溶出防止処理されたビール粕成形炭、及び該ビール粕成形炭からなる水質浄化材に関する。
【０００２】
【従来の技術】
環境に配慮して、ビール工場のゼロエミッションを推進し、安定したビール生産を保証するためには、ビール粕の有効利用の多様化が望まれる。
その対策の一つとして、ビール粕を炭化し、各種吸着材、土壌処理材、水質処理材などに利用することが検討されており、例えば特開平８−９９５４号公報には、ビール粕炭化物を吸着剤や濾過剤に用いることも記載されているが、下記のようなビール粕成形炭を水質浄化材として利用することは知られていない。
ビール粕成形炭は、本出願人の出願に係る特開２０００−３３４９６号公報に記載されているように、ビール粕を脱水乾燥した後、棒状などの適当な形状に加熱圧縮して成形物を作成し、次いで該成形物を適当な温度（通常５００℃以上）で焼成することにより得られる炭化物であって、特に６００℃以上の高温で焼成した場合には、硬度及び精煉度が備長炭並みの粉の発生が少ない白炭を得ることもできる。
また、ビール粕成形炭は、通常の炭に比べて灰分量（特にＰ、Ｍｇ）や窒素量が多く、土壌改良材などに用いる場合は好ましい。
しかし、水に浸漬すると、約２重量％含有されるリンの一部が溶出し、環境庁の富栄養化基準に抵触する可能性が高いため、水質浄化材として用いる場合にはリンの溶出を防止する必要がある。
【０００３】
【発明が解決しようとする課題】
本発明は、ビール粕成形炭のリン溶出防止処理法、リン溶出防止処理されたビール粕成形炭、及び該ビール粕成形炭からなる水質浄化材の提供を目的とする。
【０００４】
【課題を解決するための手段】
上記課題は、次の１）〜７）の発明によって解決される。
１） ビール粕を脱水乾燥したのち加熱圧縮して成形物を作成し、次いで該成形物を焼成することにより得られる炭化物（ビール粕成形炭）のリン溶出防止処理方法であって、リンと反応して難水溶性物質を生成する物質を成形前に添加することを特徴とするビール粕成形炭のリン溶出防止処理方法。
２） 前記リンと反応して難溶解性物質を生成する物質がカルシウム化合物であり、難溶解性物質がリン酸カルシウムである１）記載のビール粕成形炭のリン溶出防止処理方法。
３） 前記カルシウム化合物が消石灰であり、該消石灰の添加量が、ビール粕成形炭重量に対し５重量％以上である２）記載のビール粕成形炭のリン溶出防止処理方法。
４） 請求項１〜３の何れかに記載のリン溶出防止処理方法により処理されたビール粕成形炭。
５） 成形炭を純水と混合して静置した場合の、２４時間後のリンの溶出量が、成形炭１ｇ当り０．００５ｍｇ以下である４）記載のビール粕成形炭。
６） リン溶出防止処理により、リンをリン酸カルシウムの形態で含有する４）又は５）記載のビール粕成形炭。
７） ４）〜６）の何れかに記載のビール粕成形炭からなる水質浄化材。
【０００５】
以下、上記本発明について詳しく説明する。
ビール工場から入手した機械脱水済みビール粕を乾燥し、加熱圧縮成形した後、低酸素雰囲気中で焼成してビール粕成形炭を作成した。焼成時の最終到達温度は６００℃と８００℃の２種類とし、それぞれサンプルを作成した。以後、６００℃のものを低温炭、８００℃のものを高温炭と呼ぶ。
また、ビール粕を事前に１Ｎ塩酸に浸漬させ、その後ｐＨが中性付近に戻るまで水洗処理したサンプルを使用して、焼成時の最終到達温度８００℃で炭化したビール粕成形炭も作成した。以後、このサンプルをリン除去炭と呼ぶ。
比較実験のため木炭水質浄化装置で採用されているマレーシア産木炭を入手した。
実験に用いた上記４種の炭の物性を表１に示す。
【０００６】
【表１】
上記４種の炭をそれぞれハンマーで粉砕後分級した。ＪＩＳ標準篩（目の開き：１９．０ｍｍ、ワイヤー径：３．１５ｍｍ、東洋スクリーン工業社製）の篩下、ＪＩＳ標準篩（目の開き：９．５ｍｍ、ワイヤー径：２．２４ｍｍ、東洋スクリーン工業社製）の篩上に分離された径が約１０〜２０ｍｍの粉砕炭を図１のフローシート中のカラム、具体的には図２のカラム（添付写真参照）に充填した。カラムの底部は円錐部となっており、底部から被処理原水（以下、原水という）を送入し、空気を円筒部と円錐部の接続箇所付近から水平方向に送気した。処理温度を均一にするため、カラムはジャケットを備えたものとし、ジャケット内には、恒温水循環装置（ＮＣＢ−２１００、東京理科器械社製）で常時２５℃の水を循環させた。
この種のカラムにおいて、塔径に対する充填物の径の比が８以下では液の分散が悪くなると言われており、前述のように粉砕炭の径が約１０〜２０ｍｍなので、カラムの直径を８０ｍｍとした。
カラムの総容積を３．８リットルに設計製作した上で、上記４種の炭を充填したところ、担体充填率は５０％であった。
【０００８】
滞留時間を８時間に調整するとして、原水流入量は４ｍｌ／ｍｉｎと計算した。原水流入量は当初４ｍｌ／ｍｉｎで開始したが、開始後９２日目に８ｍｌ／ｍｉｎに、開始後１２７日目に１６ｍｌ／ｍｉｎに、２度増加させて処理状況の経過を観察した。
通気量は、各カラムとも溢流部で溶存酸素が飽和状態となる１００〜２００ｍｌ／ｍｉｎに調整した。
上記４種の炭を用いたカラムの他に、通気効果だけで水質が浄化される効果を確認するため、炭を入れない対照カラムを用意した。
対照カラムにおいては、より低部のノズルから溢流させて滞留時間を調整したが、カラムの構造を統一した関係で、対照カラムの有効容積は２．０リットルとなり、滞留時間は他のカラムの場合よりも長い８．４となった（原水流入量４ｍｌ／ｍｉｎの場合）。
処理原水は霞ヶ浦から週に２回運搬した。全リンの測定には、全リン計（スミグラフＭｏｄｅｌ Ｐ−１５００、住化分析センター社製）を用いた。
以上のような条件で実験を行ったところ、リンの溶出量は、図３に示すような結果となった。図３の縦軸は処理水中の全リン濃度（ｍｇ／ｌ）、横軸は通水日数である。
図３から分るように、低温炭、高温炭共に長期間に亘り高濃度のリンが溶出したが、リン除去炭では、低温炭や高温炭に比べて、初期段階で全リン濃度が半分以下となり、４０日程度経過後にはほぼ原水に近い状態となった。
【０００９】
上記の結果をみると、リン除去炭、即ち酸によるリンの除去は、一応の効果が認められるものの、環境対策の観点からは十分とは言えない。
また、本発明者らは、ビール粕成形炭のリン含有量の高さ（約２重量％）から抽出除去も困難と判断し、何らかの安全な物質を添加してリンを含有する難溶解性物質を生成させることにより、リンの溶出を抑える方法について検討した。
リンの化合物の中では、リン酸カルシウムが、水に対する溶解度が極めて低く、かつ安全性も高いことから、消石灰や炭酸カルシウムを添加してリン酸カルシウムを生成させる手段について詳しく検討した。
その結果、ビール粕成形炭の成形前の原料に消石灰や炭酸カルシウムなどのカルシウム化合物を添加すれば、リンが難水溶性のリン酸カルシウムとして固定化できることを確認した。
ビール粕成形炭に含まれるリンの絶対量から当量計算した消石灰の必要最小添加量（理論値）は７重量％程度である。
リンの溶出量を減らす方法としては、前述のように原料であるビール粕を塩酸などの酸に浸漬した後、水洗処理する方法もあり、操作を繰り返すことにより前記環境庁の基準をクリヤーできる可能性はあるが、製造コストなどの点からみて実用的とは言えず、本発明の固定化法の方が、操作性、対環境特性などにおいて遥かに優れている。
【００１０】
【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より限定されるものではない。
【００１１】
実施例１
ビール工場から入手した機械脱水済みビール粕を乾燥した後、直径５０ｍｍの棒状に加熱圧縮して成形物を作成し、次いで、該成形物を低酸素雰囲気中で２４時間以上焼成（最高到達温度８００℃）することによりビール粕成形炭を得た。これとは別に、加熱圧縮工程直前に、消石灰（スーパー消石灰、協和株式会社製）を、２．５重量％、５重量％、１０重量％、２０重量％添加した点以外は、上記消石灰無添加の場合と全く同様にしてビール粕成形炭を作成した。
各成形炭５ｇを１００ｍｌの純水と混合し静置して、水中のリン濃度を全リン計（スミグラフMｏｄｅｌ Ｐ−１５００、住化分析センター社製）を用いて測定した。結果を図４に示す。図４の横軸は、消石灰添加率（重量％）であり、縦軸は２４時間後の成形炭１ｇ当りのリンの溶出量（ｍｇ）である。
図４から分るように、消石灰５重量％の添加で、リンの溶出量は５０分の１となり、１０重量％ではリンの溶出が認められなかった。
従って、リンの溶出を零にするために必要な消石灰の最小添加量は５重量％と１０重量％の間にあり、前述の当量計算による消石灰の必要最小添加量（理論値）の７重量％とよく整合している。
なお、リンの溶出防止の観点からは、特に消石灰の添加量に上限はないが、実質上１０重量％程度で十分である。
図５に、上記ビール粕成形炭のＸ線回折分析の結果を示す。図５（ａ）は消石灰無添加のもの、図５（ｂ）は消石灰を２．５重量％添加したもののチャートである。図５（ａ）、（ｂ）から、消石灰添加成形炭中にリン酸カルシウムが生成していることが確認された。
【００１２】
実施例２
実施例１における消石灰に代えて炭酸カルシウムを用いた点以外は、実施例１の場合と同様にしてビール粕成形炭を作成し、リンの溶出量を測定したところ、実施例１とほぼ同様の結果が得られた。
【００１３】
【発明の効果】
本発明によれば、ビール粕成形炭の簡便なリン溶出防止処理法、市販の水質浄化装置用木炭とほぼ同等の浄化能力を有し、環境基準を満足するリン溶出防止処理されたビール粕成形炭、及び該ビール粕成形炭からなる水質浄化材を提供できる。
【図面の簡単な説明】
【図１】実験用浄水装置のフローシート図。
【図２】図１の装置に用いたカラムの具体例を示す図（添付写真参照）。
【図３】低温炭、高温炭、リン除去炭、マレーシア産木炭を用いた場合の、処理水中の全リン濃度の測定結果を示す図。
【図４】消石灰を添加したビール粕成形炭を用いた場合の、処理水中の全リン濃度と、消石灰の添加量との関係に関する測定結果を示す図。
【図５】ビール粕成形炭のＸ線回折分析の結果を示す図。（ａ） 消石灰を添加しないビール粕成形炭。
（ｂ） 消石灰を添加したビール粕成形炭。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a phosphorus elution prevention treatment method for beer lees forming coal, beer lees forming coal subjected to phosphorus elution prevention treatment, and a water purification material comprising the beer lees forming coal.
[0002]
[Prior art]
Considering the environment, in order to promote zero emissions at beer factories and guarantee stable beer production, diversification of effective use of beer lees is desired.
As one of the countermeasures, it has been studied to carbonize beer lees and use them for various adsorbents, soil treatment materials, water quality treatment materials, etc., for example, JP-A-8-9954 discloses beer lees carbide. Although it is also described that it is used as an adsorbent or a filter agent, it is not known to use beer lees forming charcoal as described below as a water purification material.
As described in Japanese Patent Application Laid-Open No. 2000-33496 related to the applicant's application, beer lees forming charcoal is dehydrated and dried from beer lees and then heated and compressed into an appropriate shape such as a rod shape. It is a carbide obtained by preparing and then firing the molded product at an appropriate temperature (usually 500 ° C. or higher), and particularly when calcined at a high temperature of 600 ° C. or higher, the hardness and refinement are comparable to Bincho charcoal. It is also possible to obtain white coal with less generation of powder.
In addition, beer lees forming coal has a larger amount of ash (particularly P, Mg) and nitrogen than normal charcoal, and is preferable when used as a soil conditioner.
However, when immersed in water, part of the phosphorus contained in about 2% by weight is eluted, and there is a high possibility that it will violate the eutrophication standards of the Environment Agency. There is a need to prevent.
[0003]
[Problems to be solved by the invention]
An object of the present invention is to provide a phosphorus elution prevention treatment method for beer lees forming coal, a beer lees forming coal subjected to phosphorus elution prevention treatment, and a water purification material comprising the beer lees forming coal.
[0004]
[Means for Solving the Problems]
The above problems are solved by the following inventions 1) to 7).
1) Phosphorus elution prevention treatment method for carbide (beer lees molding charcoal) obtained by dehydrating and drying beer lees and then heat-compressing to form the moldings and then firing the moldings to react with phosphorus And adding a substance that generates a poorly water-soluble substance before molding, a method for preventing phosphorus elution of beer lees forming charcoal.
2) The method for preventing phosphorus from leaching of beer lees formed coal according to 1), wherein the substance that reacts with phosphorus to produce a hardly soluble substance is a calcium compound, and the hardly soluble substance is calcium phosphate.
3) wherein a calcium compound is slaked lime, the amount of the slaked lime, a BSG coal briquettes by weight relative to 5 wt% or more 2) phosphorus elution prevention treatment method BSG briquette according.
4) Beer lees molding charcoal processed by the phosphorus elution prevention processing method in any one of Claims 1-3 .
5) The beer lees forming coal according to 4), wherein the amount of phosphorus eluted after 24 hours is 0.005 mg or less per 1 g of forming coal when the forming coal is mixed with pure water and allowed to stand.
6) The beer cake forming charcoal according to 4) or 5), which contains phosphorus in the form of calcium phosphate by a phosphorus elution prevention treatment.
7) A water purification material comprising the beer bran coal according to any one of 4) to 6).
[0005]
Hereinafter, the present invention will be described in detail.
A machine-dehydrated beer lees obtained from a beer factory was dried, compression-molded by heating, and then fired in a low oxygen atmosphere to produce beer lees forming charcoal. Two final temperatures of 600 ° C. and 800 ° C. were used during firing, and samples were prepared respectively. Hereinafter, the one with 600 ° C. is called low-temperature coal, and the one with 800 ° C. is called high-temperature coal.
Moreover, the beer lees forming charcoal which carbonized at the final reached temperature of 800 degreeC at the time of baking was also used using the sample which dipped beer lees beforehand in 1N hydrochloric acid, and then washed with water until pH returned to neutral vicinity. Hereinafter, this sample is referred to as phosphorus-removed charcoal.
For comparison experiments, we obtained Malaysian charcoal used in a charcoal water purification system.
Table 1 shows the physical properties of the four types of charcoal used in the experiment.
[0006]
[Table 1]
The above four types of charcoal were each crushed with a hammer and classified. Under the sieve of JIS standard sieve (opening: 19.0 mm, wire diameter: 3.15 mm, manufactured by Toyo Screen Industry Co., Ltd.), JIS standard sieve (opening: 9.5 mm, wire diameter: 2.24 mm, Toyo Screen) The pulverized charcoal having a diameter of about 10 to 20 mm separated on a sieve (manufactured by Kogyo Co., Ltd.) was packed into the column in the flow sheet of FIG. 1, specifically, the column of FIG. 2 (see attached photo). The bottom of the column was a conical portion, and raw water to be treated (hereinafter referred to as raw water) was fed from the bottom, and air was fed horizontally from the vicinity of the connection between the cylindrical portion and the conical portion. In order to make the treatment temperature uniform, the column was provided with a jacket, and water at 25 ° C. was constantly circulated in the jacket by a constant temperature water circulation device (NCB-2100, manufactured by Tokyo Science Instruments Co., Ltd.).
In this type of column, it is said that the dispersion of the liquid becomes worse when the ratio of the packing diameter to the tower diameter is 8 or less. As described above, the diameter of the pulverized coal is about 10 to 20 mm. It was.
The total volume of the column was designed and manufactured to 3.8 liters, and when the above four types of charcoal were packed, the carrier packing rate was 50%.
[0008]
Assuming that the residence time was adjusted to 8 hours, the raw water inflow was calculated to be 4 ml / min. The raw water inflow rate started initially at 4 ml / min, but was increased twice to 8 ml / min on the 92nd day after the start and 16 ml / min on the 127th day after the start, and the progress of the treatment state was observed.
The air flow rate was adjusted to 100 to 200 ml / min at which the dissolved oxygen was saturated at the overflow portion in each column.
In addition to the column using the above four types of charcoal, a control column without charcoal was prepared in order to confirm the effect of purifying water quality only by the ventilation effect.
In the control column, the residence time was adjusted by overflowing from the lower nozzle, but due to the unified structure of the column, the effective volume of the control column was 2.0 liters, and the residence time was that of other columns. It became 8.4 longer than the case (in the case of
The treated raw water was transported twice a week from Kasumigaura. For the measurement of total phosphorus, a total phosphorus meter (Sumigraph Model P-1500, manufactured by Sumika Chemical Analysis Co., Ltd.) was used.
When the experiment was conducted under the above conditions, the phosphorus elution amount was as shown in FIG. The vertical axis in FIG. 3 is the total phosphorus concentration (mg / l) in the treated water, and the horizontal axis is the number of days of water flow.
As can be seen from FIG. 3, high-concentration phosphorus was eluted over a long period of time for both low-temperature coal and high-temperature coal, but in the case of phosphorus-removed coal, the total phosphorus concentration is less than half in the initial stage compared to low-temperature coal and high-temperature coal. After about 40 days, it was almost in the state of raw water.
[0009]
From the above results, it can be said that removal of phosphorus with phosphorus-removed charcoal, that is, acid, is not sufficient from the viewpoint of environmental measures, although a temporary effect is recognized.
In addition, the present inventors determined that extraction removal is difficult due to the high phosphorus content (about 2% by weight) of beer bran coal, and added a safe substance to add a slightly soluble substance that contains phosphorus. The method for suppressing the elution of phosphorus by producing selenium was investigated.
Among the phosphorus compounds, calcium phosphate has extremely low solubility in water and high safety. Therefore, a means for generating calcium phosphate by adding slaked lime or calcium carbonate was examined in detail.
As a result, it was confirmed that if calcium compounds such as slaked lime and calcium carbonate were added to the raw material before forming beer lees forming coal, phosphorus could be immobilized as poorly water-soluble calcium phosphate.
The minimum required addition amount (theoretical value) of slaked lime calculated equivalently from the absolute amount of phosphorus contained in beer bran coal is about 7% by weight.
As described above, there is a method to reduce the amount of phosphorus elution. After immersing beer cake, which is a raw material, in an acid such as hydrochloric acid, it can be washed with water. By repeating the operation, it is possible to clear the standards of the Environment Agency. However, the immobilization method of the present invention is far superior in terms of operability and environmental characteristics.
[0010]
【Example】
EXAMPLES Hereinafter, although an Example demonstrates this invention concretely, this invention is not limited by these Examples.
[0011]
Example 1
After drying the machine-dehydrated beer cake obtained from a beer factory, it is heated and compressed into a rod shape having a diameter of 50 mm to form a molded product, and then the molded product is baked for 24 hours or more in a low oxygen atmosphere (maximum temperature 800 is reached). ℃)) to obtain beer koji forming charcoal. Apart from this, slaked lime (super slaked lime, manufactured by Kyowa Co., Ltd.) was added immediately before the heat compression step, except that 2.5% by weight, 5% by weight, 10% by weight and 20% by weight were added. In the same manner as in the above, beer lees coking coal was prepared.
5 g of each charcoal was mixed with 100 ml of pure water and allowed to stand, and the phosphorus concentration in the water was measured using a total phosphorus meter (Sumigraph Model P-1500, manufactured by Sumika Chemical Analysis Co., Ltd.). The results are shown in FIG. The horizontal axis in FIG. 4 is the slaked lime addition rate (% by weight), and the vertical axis is the phosphorus elution amount (mg) per gram of coal after 24 hours.
As can be seen from FIG. 4, when 5% by weight of slaked lime was added, the phosphorus elution amount became 1/50, and phosphorus elution was not observed at 10% by weight.
Therefore, the minimum amount of slaked lime required to make phosphorus elution zero is between 5% and 10% by weight, and 7% by weight of the minimum amount of slaked lime (theoretical value) calculated by the above-mentioned equivalent calculation. And is well aligned.
From the viewpoint of preventing phosphorus elution, there is no particular upper limit to the amount of slaked lime added, but about 10% by weight is sufficient.
In FIG. 5, the result of the X ray diffraction analysis of the said beer lees molding coal is shown. FIG. 5 (a) is a chart with no slaked lime added, and FIG. 5 (b) is a chart with 2.5% by weight of slaked lime added. 5 (a) and 5 (b), it was confirmed that calcium phosphate was generated in the slaked lime-added forming coal.
[0012]
Example 2
Except that calcium carbonate was used instead of slaked lime in Example 1, beer lees molding charcoal was prepared in the same manner as in Example 1 and the amount of phosphorus eluted was measured. Results were obtained.
[0013]
【The invention's effect】
According to the present invention, a simple phosphorus elution prevention treatment method for beer koji molding coal, a beer koji molding that has a purification capability substantially equivalent to charcoal for a commercially available water purification apparatus and that has been subjected to phosphorus elution prevention treatment that satisfies environmental standards. The water purification material which consists of charcoal and this beer bran forming charcoal can be provided.
[Brief description of the drawings]
FIG. 1 is a flow sheet diagram of an experimental water purifier.
FIG. 2 is a diagram showing a specific example of a column used in the apparatus of FIG. 1 (see attached photo).
FIG. 3 is a graph showing measurement results of total phosphorus concentration in treated water when low-temperature coal, high-temperature coal, phosphorus-removed coal, and Malaysian charcoal are used.
FIG. 4 is a diagram showing measurement results relating to the relationship between the total phosphorus concentration in the treated water and the amount of slaked lime added when using beer lees forming coal with slaked lime added.
FIG. 5 is a diagram showing the results of X-ray diffraction analysis of beer lees molding charcoal. (A) Coal-forming charcoal with no slaked lime added.
(B) Beer lees forming charcoal to which slaked lime is added.
Claims (7)
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| Application Number | Priority Date | Filing Date | Title |
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| JP2001230328A JP3710733B2 (en) | 2001-07-30 | 2001-07-30 | Phosphorus elution prevention treatment method for beer lees forming coal, beer lees forming coal subjected to phosphorus elution prevention treatment, and water purification material comprising the beer lees forming coal |
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| JP2001230328A JP3710733B2 (en) | 2001-07-30 | 2001-07-30 | Phosphorus elution prevention treatment method for beer lees forming coal, beer lees forming coal subjected to phosphorus elution prevention treatment, and water purification material comprising the beer lees forming coal |
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| JP2003041259A JP2003041259A (en) | 2003-02-13 |
| JP3710733B2 true JP3710733B2 (en) | 2005-10-26 |
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