JP2007217576A - Organic phosphorus treating agent and method for processing organic phosphorus-containing water using the same - Google Patents
Organic phosphorus treating agent and method for processing organic phosphorus-containing water using the same Download PDFInfo
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Abstract
Description
本発明は、主に、有機リン処理材およびそれを用いた有機リン含有水の処理方法に関する。 The present invention mainly relates to an organic phosphorus treatment material and a method for treating organic phosphorus-containing water using the same.
近年、環境問題が顕在化している。なかでも、農業や園芸等で世界中で使用されている、有機リン系殺虫剤に由来する有機リンの問題は大きくクローズアップされている。
有機リン系殺虫剤の主成分は、リン酸あるいはピロリン酸のエステル又はチオエステルで、構造がアセチルコリンと類似している。そのため、コリンエステラーゼと結合しやすい特性を有している。
In recent years, environmental problems have become apparent. In particular, the problem of organophosphorus derived from organophosphorus insecticides used around the world in agriculture and horticulture is greatly highlighted.
The main component of the organophosphorus insecticide is an ester or thioester of phosphoric acid or pyrophosphoric acid, and its structure is similar to acetylcholine. Therefore, it has the characteristic that it is easy to bind to cholinesterase.
人のからだは神経伝達によって活動をおこなっている。その伝達物質であるアセチルコリンはアセチルコリンエステラーゼという酵素によって分解される。有機リンはこのアセチルコリンエステラーゼの活性を阻害する。このため、神経末端にアセチルコリンが蓄積され、このたまったアセチルコリンによって有機リン中毒が引き起こされる。 The human body is active through nerve transmission. The transmitter acetylcholine is degraded by an enzyme called acetylcholinesterase. Organophosphorus inhibits the activity of this acetylcholinesterase. For this reason, acetylcholine accumulates at nerve endings, and organic phosphorus intoxication is caused by the accumulated acetylcholine.
水中や土壌からの有機リンの固定化・除去に関して、汎用性があって、効果的な処理材の開発が強く求められている。 There is a strong demand for the development of effective and effective treatment materials for fixing and removing organophosphorus from water and soil.
有機リンを含む廃水や土壌の処理方法としては、凝集剤や吸着剤を用いる方法や紫外線や酸化剤を用いて分解する方法等が提案されている（特許文献１〜特許文献６参照）。 As a method for treating waste water or soil containing organic phosphorus, a method using a flocculant or an adsorbent, a method of decomposing using an ultraviolet ray or an oxidizing agent, and the like have been proposed (see Patent Documents 1 to 6).
しかしながら、凝集剤や吸着剤を用いる方法では、その効果が充分でなく、また、処理時間を長く必要とするという問題もあった。
また、紫外線や酸化剤を用いて分解する方法では、高価な装置を必要とし、汎用的でないという課題があり、また、処理範囲が限定されるというデメリットもあった。
However, the method using a flocculant or an adsorbent has a problem that the effect is not sufficient and a long processing time is required.
In addition, the method of decomposing using ultraviolet rays or an oxidizing agent has a disadvantage that an expensive apparatus is required, is not versatile, and a processing range is limited.
このような背景に鑑み、有機リンの除去能力に優れ、その除去スピードも迅速であり、汎用的に、広範に利用できる有機リンの処理材の開発が強く求められている。 In view of such a background, there is a strong demand for the development of a treatment material for organic phosphorus that is excellent in organic phosphorus removal capability, has a rapid removal speed, and can be widely used widely.
そこで、本発明者は、鋭意努力を重ね、種々の実験検討を通して、特定の有機リン処理材を使用することで、前記課題が解決できることを知見し、本発明を完成するに至った。 Therefore, the present inventor has made extensive efforts, and through various experimental studies, has found that the above problem can be solved by using a specific organic phosphorus treatment material, and has completed the present invention.
即ち、本発明は、カルシウムアルミネート系化合物を含有してなる有機リン処理材であり、カルシウムアルミネート系化合物の粉末度がブレーン比表面積で3,000cm2/g以上である該有機リン処理材であり、カルシウムアルミネート系化合物のCaO/Al2O3モル比が0.5〜３である該有機リン処理材であり、カルシウムアルミネート系化合物と水酸化カルシウムとを含有してなる有機リン処理材であり、該有機リン処理材を用いる有機リン含有水の処理方法である。 That is, the present invention is an organic phosphorus treatment material containing a calcium aluminate compound, and the organophosphorus treatment material having a fineness of calcium aluminate compound of 3,000 cm 2 / g or more in terms of Blaine specific surface area. Yes, the organophosphorus treatment material having a CaO / Al 2 O 3 molar ratio of calcium aluminate compound of 0.5-3, and an organophosphorus treatment material comprising a calcium aluminate compound and calcium hydroxide. There is a method for treating organic phosphorus-containing water using the organic phosphorus treatment material.
本発明の有機リン処理材（以下、本処理材という）は、あらゆる有機リンに有効で、効率良く有機リンを固定化などして除去することができ、また、その除去スピードも迅速であるなどの効果を奏する。 The organic phosphorus treatment material of the present invention (hereinafter referred to as the present treatment material) is effective for all organic phosphorus, can be efficiently removed by immobilizing organic phosphorus, and the removal speed thereof is also fast. The effect of.
以下、本発明を詳細に説明する。
なお、本発明における部や％は特に規定しない限り質量基準で示す。
Hereinafter, the present invention will be described in detail.
In the present invention, “parts” and “%” are based on mass unless otherwise specified.
本発明で使用するカルシウムアルミネート系化合物（以下、ＣＡ化合物という）とは、CaOとAl2O3からなる化合物を総称するものであり、特に限定されるものではない。
その具体例としては、CaOをC、Al2O3をA、及びアルカリ金属元素をRと表記すると、CA2（CaO・2Al2O3）、CA(CaO・Al2O3)、C12A7（12CaO・7Al2O3）、C11A7・CaF2（11CaO・7Al2O3・CaF2）、C3A（3CaO・Al2O3）、及び3CaO・3Al2O3・CaSO4などの結晶性の化合物、C8A3R（8CaO・3Al2O3・R2O）、C14A5R（14CaO・5Al2O3・R2O）、及びC3A5R2(3CaO・5Al2O3・2R2O)などのR2O成分を含む結晶性のCaO-Al2O3-R2O系化合物や、CaOとAl2O3を主成分とする非晶質の化合物等が挙げられる。
The calcium aluminate compound (hereinafter referred to as CA compound) used in the present invention is a general term for compounds composed of CaO and Al 2 O 3 and is not particularly limited.
As specific examples, when CaO is expressed as C, Al 2 O 3 as A, and an alkali metal element as R, CA 2 (CaO · 2Al 2 O 3 ), CA (CaO · Al 2 O 3 ), C 12 A 7 (12CaO · 7Al 2 O 3), C 11 A 7 · CaF 2 (11CaO · 7Al 2 O 3 · CaF 2), C 3 A (3CaO · Al 2 O 3), and 3CaO · 3Al 2 O 3 · crystalline compounds such as CaSO 4, C 8 a 3 R (8CaO · 3Al 2 O 3 · R 2 O), C 14 a 5 R (14CaO · 5Al 2 O 3 · R 2 O), and C 3 a 5 Crystalline CaO-Al 2 O 3 -R 2 O compounds containing R 2 O components such as R 2 (3CaO ・ 5Al 2 O 3・ 2R 2 O), and CaO and Al 2 O 3 as main components An amorphous compound etc. are mentioned.
ＣＡ化合物を工業的に得る場合、MgO、TiO2、Fe2O3、B2O3、SiO2、P2O5、及びClなどの不純物が含まれることがあるが、その種類や含有量は、本発明を阻害しない範囲内であれば特に制限されるものではない。
ＣＡ化合物にこのような不純物が含まれる場合の化合物としては、メルビナイト3CaO・MgO・2SiO2、アケルマナイト2CaO・MgO・2SiO2、及びモンチセライトCaO・MgO・SiO2などのカルシウムマグネシウムシリケートや、4CaO・Al2O3・Fe2O3、6CaO・2Al2O3・Fe2O3、及び6CaO・Al2O3・2Fe2O3などのカルシウムアルミノフェライトや、2CaO・Fe2O3、CaO・Fe2O3などのカルシウムフェライトや、ゲーレナイト2CaO・Al2O3・SiO2、アノーサイトCaO・Al2O3・2SiO2などのカルシウムアルミノシリケートや、トライカルシウムシリケート3CaO・SiO2、ダイカルシウムシリケート2CaO・SiO2、ランキナイト3CaO・2SiO2、及びワラストナイトCaO・SiO2などのカルシウムシリケートなどが混在する場合がある。
When CA compounds are obtained industrially, impurities such as MgO, TiO 2 , Fe 2 O 3 , B 2 O 3 , SiO 2 , P 2 O 5 , and Cl may be contained, but the type and content thereof Is not particularly limited as long as it does not inhibit the present invention.
The compound where such contain impurities CA compound, and calcium magnesium silicate Merubinaito 3CaO · MgO · 2SiO 2, Akerumanaito 2CaO · MgO · 2SiO 2, and the like Monch Celite CaO · MgO · SiO 2, 4CaO · Calcium aluminoferites such as Al 2 O 3・ Fe 2 O 3 , 6CaO ・ 2Al 2 O 3・ Fe 2 O 3 , 6CaO ・ Al 2 O 3・ 2Fe 2 O 3 , 2CaO ・ Fe 2 O 3 , CaO ・Calcium ferrite such as Fe 2 O 3 , galenite 2CaO · Al 2 O 3 · SiO 2 , calcium aluminosilicate such as anorthite CaO · Al 2 O 3 · 2SiO 2 , tricalcium silicate 3CaO · SiO 2 , dicalcium silicate Calcium silicates such as 2CaO · SiO 2 , lanknite 3CaO · 2SiO 2 , and wollastonite CaO · SiO 2 may be mixed.
ＣＡ化合物のCaO／Al2O3のモル比は、0.5〜３が好ましく、１〜1.7がより好ましい。CaO／Al2O3のモル比が0.5未満では有機リンの除去スピードが充分でない場合があり、３を超えると液相中でのＣＡ化合物の分散が悪くなる傾向にあり、効率良く有機リンを除去できない場合がある。 The CA compound has a CaO / Al 2 O 3 molar ratio of preferably 0.5 to 3, more preferably 1 to 1.7. If the molar ratio of CaO / Al 2 O 3 is less than 0.5, the removal speed of organic phosphorus may not be sufficient, and if it exceeds 3, the dispersion of the CA compound in the liquid phase tends to deteriorate, and the organic phosphorus is efficiently removed. It may not be removed.
ＣＡ化合物の粉末度は特に限定されるものではないが、ブレーン比表面積値（以下、ブレーン値という）で3,000cm2/g以上が好ましく、4,000cm2/g以上がより好ましい。3,000cm2/g未満では、有機リンの除去スピードが遅くなり、効率が悪くなる場合がある。 While fineness of the CA compound is not particularly limited, Blaine specific surface area value (hereinafter, referred to as Blaine value) is preferably at least 3,000 cm 2 / g in, 4,000 cm 2 / g or more is more preferable. If it is less than 3,000 cm 2 / g, the removal rate of organic phosphorus is slow, and the efficiency may deteriorate.
本発明の水酸化カルシウムとは特に限定されるものではなく、Ca(OH)2と表される化合物を総称するものである。不純物としては、炭酸カルシウムや酸化カルシウムを含む場合があるが、環境に有害な不純物を含まなければ特に限定されるものではない。
水酸化カルシウムのCa(OH)2含有量は、80％以上が好ましく、90％以上がより好ましい。80％未満では有機リンの除去スピードが充分でない場合がある。
水酸化カルシウムの比表面積は特に限定されるものではないが、通常、BET比表面積（以下、ＢＥＴという）で２m2/g以上が好ましく、５m2/g以上がより好ましい。２m2/g未満ではカルシウムアルミネートとの相互作用が弱くなる傾向にあり、有機リンの除去スピードが充分でなくなる場合がある。
The calcium hydroxide of the present invention is not particularly limited, and is a general term for compounds represented as Ca (OH) 2 . Impurities may include calcium carbonate and calcium oxide, but are not particularly limited as long as they do not contain impurities harmful to the environment.
The Ca (OH) 2 content of calcium hydroxide is preferably 80% or more, and more preferably 90% or more. If it is less than 80%, the removal speed of organic phosphorus may not be sufficient.
Although the specific surface area of calcium hydroxide is not particularly limited, it is usually preferably 2 m 2 / g or more and more preferably 5 m 2 / g or more in terms of BET specific surface area (hereinafter referred to as BET). If it is less than 2 m 2 / g, the interaction with calcium aluminate tends to be weak, and the removal speed of organic phosphorus may not be sufficient.
ＣＡ化合物と水酸化カルシウムの配合割合は特に限定されるものではないが、ＣＡ化合物と水酸化カルシウムからなる有機リン処理材のCaO／Al2O3のモル比が１〜６となるように配合することが好ましく、３〜５となるように配合することがより好ましい。この範囲外では充分な有機リン除去性能が得られない場合がある。 The blending ratio of the CA compound and calcium hydroxide is not particularly limited, but is blended so that the molar ratio of CaO / Al 2 O 3 of the organic phosphorus treatment material composed of the CA compound and calcium hydroxide is 1 to 6. It is preferable to mix, and it is more preferable to mix | blend so that it may become 3-5. Outside this range, sufficient organic phosphorus removal performance may not be obtained.
本発明では、本処理材の他に、モンモリロナイトとカオリナイトなどに代表される層状化合物であるベントナイト類や、クリノプチロライトとモルデナイトに代表されるゼオライト類や、セピオライトや、アパタイトとリン酸ジルコニウムなどのリン酸塩や、ハイドロタルサイト類や、活性炭や、多硫化物、硫化物、チオ硫酸塩類、及び亜硫酸塩類等のイオウ化合物や、アマルガムや、硫酸第一鉄、塩化第一鉄等の鉄化合物や、セルロース類や、ポリビニルアルコール、キトサンなどの水溶性高分子類や、ジアルキルジチオカルバミン酸類や、キノリン化合物類や、ポリアミン類や、糖類等の公知の有害物質低減材料の一種又は二種以上を併用することも可能である。 In the present invention, in addition to the treated material, bentonites which are layered compounds represented by montmorillonite and kaolinite, zeolites represented by clinoptilolite and mordenite, sepiolite, apatite and zirconium phosphate Such as phosphates, hydrotalcites, activated carbon, polysulfides, sulfides, thiosulfates, and sulfites such as sulfites, amalgam, ferrous sulfate, ferrous chloride, etc. One or more known materials for reducing harmful substances such as iron compounds, celluloses, water-soluble polymers such as polyvinyl alcohol and chitosan, dialkyldithiocarbamic acids, quinoline compounds, polyamines, and sugars It is also possible to use together.
本処理材の形態は特に限定されるものではなく、液状、粉末状、顆粒状、ペレット状、 カラム状、及びフィルター状等のいずれの形態でも使用可能である。液状、粉末状、及び顆粒状の本処理材を汚水中に投入して固液分離してもよく、水和物のカラムやフィルターとして、有機リン廃水等の有機リン含有水を通水させることも可能である。 The form of this treatment material is not particularly limited, and any form such as liquid, powder, granule, pellet, column, and filter can be used. Liquid, powder and granular treatment materials may be put into sewage for solid-liquid separation, and organic phosphorus-containing water such as organic phosphorus wastewater is passed through as hydrate columns and filters. Is also possible.
本処理材の使用量は、廃水等の有機リン含有水中の有機リンの濃度や有機リン含有水の種類によって異なるため、一義的に決定されるものではないが、通常、濃度１〜500mmol/lの有機リン含有水1,000cc当たり、0.5〜1,000ｇが好ましく、１〜500ｇがより好ましい。0.5ｇ未満では処理効果が充分でない場合があり、1,000ｇを超えて使用してもさらなる効果の増進が期待できず不経済である。 The amount of the treatment material used varies depending on the concentration of organic phosphorus in the organic phosphorus-containing water such as wastewater and the type of the organic phosphorus-containing water, and thus is not uniquely determined, but usually has a concentration of 1 to 500 mmol / l. Per 1,000 cc of organic phosphorus-containing water is preferably 0.5 to 1,000 g, more preferably 1 to 500 g. If it is less than 0.5 g, the treatment effect may not be sufficient, and even if it exceeds 1,000 g, further improvement of the effect cannot be expected, which is uneconomical.
本処理材は、例えば、いずれの有機リン廃水等の有機リン含有水にも有効であるが、廃水中に水が存在することが必要であり、廃水中の水の含有割合は多いほど好ましい。 This treatment material is effective for any organic phosphorus-containing water such as, for example, any organic phosphorus wastewater. However, it is necessary that water be present in the wastewater, and it is preferable that the content of water in the wastewater is large.
以下、本発明を実験例でさらに詳細に説明をするが、本発明はこれらに限定されるものではない。 Hereinafter, the present invention will be described in more detail with experimental examples, but the present invention is not limited thereto.
実験例１
表１に示すCaO/Al2O3モル比となるよう、ＣＡ化合物と水酸化カルシウムとを配合して本処理材を調製した。
調製した本処理材５ｇを、有機リン含有水1,000ccに入れて攪拌し、15分後と３時間後に有機リン含有水中の有機リン濃度減少度合を評価した。
なお、比較のために、市販の吸着材を用いた場合についても同様に行った。結果を表１に併記する。
Experimental example 1
This treatment material was prepared by blending a CA compound and calcium hydroxide so as to have a CaO / Al 2 O 3 molar ratio shown in Table 1.
5 g of the treated material thus prepared was put in 1,000 cc of organic phosphorus-containing water and stirred, and the degree of decrease in organic phosphorus concentration in the organic phosphorus-containing water was evaluated after 15 minutes and 3 hours.
In addition, it carried out similarly about the case where a commercially available adsorbent is used for the comparison. The results are also shown in Table 1.
＜使用材料＞
ＣＡ化合物ａ：１モルの炭酸カルシウムと２モルの酸化アルミニウムとを混合粉砕し、1,500℃で３時間焼成する工程を２回繰り返して合成、CaO・2Al2O3主体、ブレーン値5,000cm2/g
ＣＡ化合物ｂ：１モルの炭酸カルシウムと１モルの酸化アルミニウムを混合粉砕し、1,500℃で３時間焼成する工程を２回繰り返して合成、CaO・Al2O3主体、ブレーン値5,000cm2/g
ＣＡ化合物ｃ：12モルの炭酸カルシウムと７モルの酸化アルミニウムを混合粉砕し、1,350℃で３時間焼成する工程を２回繰り返して合成、結晶質の12CaO・7Al2O3主体、ブレーン値5,000cm2/g
ＣＡ化合物ｄ：３モルの炭酸カルシウムと１モルの酸化アルミニウムを混合粉砕し、1,350℃で３時間焼成する工程を２回繰り返して合成、3CaO・Al2O3主体、ブレーン値5,000cm2/g
ＣＡ化合物ｅ：非晶質のカルシウムアルミネート、ＣＡ化合物ｃにシリカを３％添加し、1,650℃で溶融した後、急冷して合成、ブレーン値5,000cm2/g
水酸化カルシウム：市販の消石灰、ＢＥＴ５m2/g、Ca(OH)2含有量90％
処理材イ ：市販の硫酸アルミニウム
処理材ロ ：市販のゼオライト
有機リン含有水：モノオクチルリン酸エステルの50mmol／l濃度の溶液
<Materials used>
CA compound a: 1 mol of calcium carbonate and 2 mol of aluminum oxide are mixed and pulverized and synthesized by repeating the process of firing at 1,500 ° C. for 3 hours twice, CaO · 2Al 2 O 3 mainly, brain value 5,000 cm 2 / g
CA compound b: 1 mol of calcium carbonate and 1 mol of aluminum oxide are mixed and pulverized and synthesized by repeating the process of firing at 1,500 ° C. for 3 hours twice, CaO · Al 2 O 3 mainly, brain value 5,000 cm 2 / g
CA compound c: 12 mol calcium carbonate and 7 mol aluminum oxide mixed and pulverized, and baked at 1,350 ° C. for 3 hours, synthesized twice, composed mainly of crystalline 12CaO · 7Al 2 O 3 , brain value 5,000 cm 2 / g
CA compound d: 3 mol of calcium carbonate and 1 mol of aluminum oxide are mixed and pulverized and synthesized by repeating the process of firing at 1,350 ° C. for 3 hours twice, 3CaO · Al 2 O 3 mainly, brain value 5,000 cm 2 / g
CA compound e: amorphous calcium aluminate, 3% silica added to CA compound c, melted at 1,650 ° C., then quenched and synthesized, brain value 5,000 cm 2 / g
Calcium hydroxide: Commercially available slaked lime, BET 5m 2 / g, Ca (OH) 2 content 90%
Treatment material A: Commercially available aluminum sulfate treatment material B: Commercially available zeolite organic phosphorus-containing water: 50 mmol / l concentration solution of monooctyl phosphate
＜測定方法＞
有機リン濃度減少度合：処理材で処理する前の液相の全炭素量と、処理材で処理後の液相の全炭素量を有機全炭素分析装置（ＴＯＣ）で定量し、処理前の液相の全炭素濃度を100％とした時の、処理後の液相の全炭素濃度の相対値から、有機リン分が99.9％以上低減されたと判断される場合は優、90％以上低減されたが99.9％まで低減できなかったと判断される場合を良、70％以上低減されたが89.9％まで低減できなかったと判断される場合を可、70％まで低減されなかったと判断される場合を不可とした。
<Measurement method>
Degree of decrease in organic phosphorus concentration: The total amount of carbon in the liquid phase before treatment with the treatment material and the total amount of carbon in the liquid phase after treatment with the treatment material are quantified with an organic total carbon analyzer (TOC). From the relative value of the total carbon concentration of the liquid phase after treatment when the total carbon concentration of the phase is 100%, the organic phosphorus content was judged to have been reduced by 99.9% or more, and it was reduced by 90% or more. If it is judged that it was not reduced to 99.9%, good if it was judged that it was reduced by 709.9% but could not be reduced to 89.9%, acceptable if it was judged that it was not reduced to 70% did.
表１から、本発明により、有機リン含有水中の有機リンが著しく低減することが判る。また、ＣＡ化合物と水酸化カルシウムを併用する場合、CaO/Al2O3モル比が１〜６にある本処理材は、有機リン含有水中の有機リン除去に有効で、特に、CaO/Al2O3モル比が３〜５にある処理材は効率良く有機リンを固定化して、除去できることが判る。 From Table 1, it can be seen that the present invention significantly reduces organic phosphorus in organic phosphorus-containing water. Further, when a CA compound and calcium hydroxide are used in combination, this treatment material having a CaO / Al 2 O 3 molar ratio of 1 to 6 is effective for removing organic phosphorus in organic phosphorus-containing water, and in particular, CaO / Al 2 It can be seen that the treatment material having an O 3 molar ratio of 3 to 5 can efficiently fix and remove organic phosphorus.
実験例２
表２に示すブレーン値のＣＡ化合物ｄからなる本処理材を使用したこと以外は、実験例１と同様に行った。結果を表２に併記する。
Experimental example 2
The experiment was performed in the same manner as in Experimental Example 1 except that this treatment material composed of the CA compound d having a brain value shown in Table 2 was used. The results are also shown in Table 2.
表２から、本発明により、有機リン含有水の有機リンが著しく低減することが判る。また、ＣＡ化合物のブレーン値は3,000cm2/g以上が好ましいことが判る。 From Table 2, it can be seen that the organic phosphorus in the organic phosphorus-containing water is significantly reduced by the present invention. It can also be seen that the brane value of the CA compound is preferably 3,000 cm 2 / g or more.
実験例３
有機リン含有水1,000ccに対して、表３に示すＣＡ化合物ｄからなる本処理材を使用したこと以外は、実験例１と同様に行った。結果を表３に併記する。
Experimental example 3
The test was conducted in the same manner as in Experimental Example 1 except that this treatment material consisting of the CA compound d shown in Table 3 was used for 1,000 cc of organic phosphorus-containing water. The results are also shown in Table 3.
表３から、本発明により、有機リン含有水中の有機リンが著しく低減することが判る。また、本処理材の使用量が所定量で効果が上がることが判る。 From Table 3, it can be seen that organic phosphorus in the organic phosphorus-containing water is significantly reduced by the present invention. Further, it can be seen that the effect increases when the amount of the treatment material used is a predetermined amount.
本発明の処理材および有機リン含有水の処理方法により、効果的に有機リンを固定化して除去でき、しかも、その除去スピードが迅速であるため、有機リン含有水の処理用途に好適である。 The treatment material and organic phosphorus-containing water treatment method of the present invention can effectively immobilize and remove organic phosphorus, and because the removal speed is rapid, it is suitable for organic phosphorus-containing water treatment.
Claims (5)
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