JP2021023917A - Metal replenisher obtainable from wood drying waste liquid, method of decolorizing wood drying waste liquid and method of recovering heartwood components - Google Patents
Metal replenisher obtainable from wood drying waste liquid, method of decolorizing wood drying waste liquid and method of recovering heartwood components Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 59
- 239000002023 wood Substances 0.000 title claims abstract description 53
- 239000002699 waste material Substances 0.000 title claims abstract description 46
- 239000002184 metal Substances 0.000 title claims abstract description 38
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 38
- 238000001035 drying Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000011282 treatment Methods 0.000 claims abstract description 57
- 239000013522 chelant Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 9
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 52
- 229910052742 iron Inorganic materials 0.000 claims description 28
- 238000001179 sorption measurement Methods 0.000 claims description 22
- 239000011162 core material Substances 0.000 claims description 21
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- 239000013589 supplement Substances 0.000 claims description 17
- 239000002738 chelating agent Substances 0.000 claims description 10
- 230000009920 chelation Effects 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- 238000004042 decolorization Methods 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 25
- 239000003463 adsorbent Substances 0.000 abstract description 4
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- -1 iron-EDTA compound Chemical class 0.000 description 6
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
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- DEFVIWRASFVYLL-UHFFFAOYSA-N ethylene glycol bis(2-aminoethyl)tetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)CCOCCOCCN(CC(O)=O)CC(O)=O DEFVIWRASFVYLL-UHFFFAOYSA-N 0.000 description 2
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- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 description 2
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical compound C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 description 1
- AGMNQPKGRCRYQP-UHFFFAOYSA-N 2-[2-[2-[bis(carboxymethyl)amino]ethylamino]ethyl-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)CCNCCN(CC(O)=O)CC(O)=O AGMNQPKGRCRYQP-UHFFFAOYSA-N 0.000 description 1
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 description 1
- QOPUBSBYMCLLKW-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]-4-hydroxybutanoic acid Chemical compound OCCC(C(O)=O)N(CC(O)=O)CCN(CC(O)=O)CC(O)=O QOPUBSBYMCLLKW-UHFFFAOYSA-N 0.000 description 1
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- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 1
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- 241000237852 Mollusca Species 0.000 description 1
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
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- 229930002875 chlorophyll Natural products 0.000 description 1
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- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 1
- 235000018417 cysteine Nutrition 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000002024 ethyl acetate extract Substances 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 235000003499 redwood Nutrition 0.000 description 1
- 229940056692 resinol Drugs 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229930004725 sesquiterpene Natural products 0.000 description 1
- 150000004354 sesquiterpene derivatives Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000003171 wood protecting agent Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Removal Of Specific Substances (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Water Treatment By Sorption (AREA)
Abstract
Description
本発明は、木材乾燥機から流出する廃液から得られる金属補給体、並びに木材乾燥機から流出する廃液を脱色する方法、及び木材乾燥機から流出する廃液から木材心材成分を回収する方法に関する。 The present invention relates to a metal supplement obtained from a waste liquid flowing out of a wood dryer, a method of decolorizing the waste liquid flowing out of the wood dryer, and a method of recovering a wood core material component from the waste liquid flowing out of the wood dryer.
木材は水分が含まれる生材の状態では変形や割れが生じるため、生材を乾燥して建築用製材などに利用される。生材の乾燥方法としては、天然乾燥のほか、人工的に加熱水蒸気を用いて乾燥させる蒸気式木材乾燥（以下、「蒸気式乾燥」という。）が広く用いられている。この蒸気式乾燥においては、木材中の水分が加熱水蒸気と共に蒸気式乾燥機の排気口から大気中へ排出され、また、蒸気式乾燥機底面から流出する液体（以下、「ドレーン」という。）が廃液として河川などに放出されている。このため蒸気式乾燥において環境中に排出される蒸気及びドレーンの有効利用に向けて各種研究がなされている。 Since wood is deformed and cracked in the state of raw wood containing moisture, the raw wood is dried and used for construction lumber. As a method for drying raw wood, in addition to natural drying, steam-type wood drying (hereinafter referred to as "steam-type drying"), which artificially dries using heated steam, is widely used. In this steam drying, the moisture in the wood is discharged to the atmosphere together with the heated steam from the exhaust port of the steam dryer, and the liquid (hereinafter referred to as "drain") flowing out from the bottom surface of the steam dryer is discharged. It is released into rivers as waste liquid. For this reason, various studies have been conducted toward the effective use of steam and drains discharged into the environment in steam drying.
蒸気式乾燥機から排出される蒸気の有効利用については、加熱温度９０℃〜１２０℃の蒸気式乾燥で排出される蒸気を自然冷却させて液体を補集し、上部に浮遊した木材精油を除去して消臭剤として利用することが開示されている（特許文献１）。また、このときの排出液は、白濁しており少量の有機層が含まれていることが開示されている（同特許文献１［００１３］段落参照）。 Regarding the effective use of steam discharged from the steam dryer, the steam discharged by steam drying at a heating temperature of 90 ° C to 120 ° C is naturally cooled to collect the liquid and remove the wood essential oil floating on the top. It is disclosed that it is used as a deodorant (Patent Document 1). Further, it is disclosed that the discharged liquid at this time is cloudy and contains a small amount of an organic layer (see paragraph 1 [0013] of the same patent document 1).
また、乾燥機排出口から出る排気を水冷式のコンデンサーを通して液体を回収し、その液体中の油分にセスキテルペンアルコールが含まれること及びこれを用いてナメクジなどの陸生軟体動物の忌避剤とすることが開示されている（特許文献２［００１０］段落参照）。 In addition, the liquid is recovered from the exhaust from the dryer outlet through a water-cooled condenser, and the oil in the liquid contains sesquiterpene alcohol, which is used as a repellent for terrestrial mollusks such as slugs. Is disclosed (see paragraph 2 [0010] of Patent Document).
一方、ドレーンの有効利用については殆ど研究がなされておらず、その成分については木材由来の水溶性抽出物が主であることから有害物質は含まれていないと考えられるものの、そのままドレーンを河川などへ廃棄すると、ドレーンが濃い黒色であることから景観を損ねることになり、黒色を呈する原因究明と景観を損なわないような色へ変換すること、あるいはその有効利用などの開発が求められていた。 On the other hand, little research has been done on the effective use of drains, and although it is thought that no harmful substances are contained in the components because water-soluble extracts derived from wood are the main components, drains can be used as they are in rivers, etc. If it is discarded, the drain will be dark black, which will spoil the landscape, and it has been required to investigate the cause of the black color, convert it to a color that does not spoil the landscape, or develop its effective use.
なお、ドレーンについての唯一の研究報告があるが、これはスギ柱材の木材乾燥機から排出されるドレーン発生量の経時変化及びｐＨを明らかにしたというものであり、ドレーンにオゾンを添加して黒色を多少淡色化できたこと及びドレーンを用いた微生物培養に利用する可能性が示唆されているのみである（非特許文献１）。このように、乾燥機排出口から排出される蒸気については消臭剤や忌避剤への利用がなされているものの、ドレーンについては有効利用されることもなく、黒色を呈したまま、現在も海洋や河川などへ投棄されているという問題があった。 In addition, there is the only research report on drains, which clarified the time course and pH of the amount of drainage generated from the wood dryer of cedar pillars, and added ozone to the drains. It is only suggested that the black color could be slightly lightened and that it could be used for culturing microorganisms using a drain (Non-Patent Document 1). In this way, although the steam discharged from the dryer outlet is used as a deodorant and repellent, the drain is not effectively used and remains black and is still in the ocean. There was a problem that it was dumped in rivers and rivers.
本発明は、このような問題点に着目してなされたもので、木材乾燥機から流出する廃液から産業上利用が可能となる物質を提供すると共に、ドレーンの黒色を脱色する方法と、その過程で分離回収される液体を有効利用することを目的とする。 The present invention has been made by paying attention to such a problem, and provides a substance that can be industrially used from the waste liquid flowing out from the wood dryer, and a method for decolorizing the black color of the drain and its process. The purpose is to make effective use of the liquid separated and recovered in.
本発明の第一の特徴である金属補給体は、木材の乾燥処理によって回収された廃液を原料とし、該廃液中の金属をキレート化したことである。 The metal supplement which is the first feature of the present invention is that the waste liquid recovered by the drying treatment of wood is used as a raw material and the metal in the waste liquid is chelated.
本発明の第二の特徴は、前記金属を鉄としたことである。 The second feature of the present invention is that the metal is iron.
本発明の第三の特徴は、前記金属のキレート化に利用されるキレート剤をＥＤＴＡとしたことである。 The third feature of the present invention is that the chelating agent used for chelating the metal is EDTA.
本発明の第四の特徴である木材乾燥廃液の脱色方法は、
木材の乾燥処理によって回収された廃液を、キレート処理、還元処理又はｐＨ処理の何れかによる方法で前処理を行う工程と、
前記前処理を行った前処理液を吸着担体に接触させる工程と、
により、前記廃液を脱色することである。
The method for decolorizing the dried wood waste liquid, which is the fourth feature of the present invention, is
A step of pretreating the waste liquid recovered by the drying treatment of wood by a method of either chelation treatment, reduction treatment or pH treatment, and
The step of bringing the pretreated liquid into contact with the adsorption carrier, and
This is to decolorize the waste liquid.
本発明の第五の特徴は、前記前処理がキレート処理又は還元処理であって、該キレート処理に利用されるキレート剤又は該還元処理に利用される還元剤は、鉄と強く結合するものとしたことである。 The fifth feature of the present invention is that the pretreatment is a chelate treatment or a reduction treatment, and the chelate agent used for the chelate treatment or the reducing agent used for the reduction treatment strongly binds to iron. That's what I did.
本発明の第六の特徴である木材心材成分の回収方法は、
木材の乾燥処理によって回収された廃液を、キレート処理、還元処理又はｐＨ処理の何れかによる方法で前処理を行う工程と、
前記前処理を行った前処理液を吸着担体に接触させる工程と、
前記吸着担体を有機溶媒で溶出させる工程と、
により、前記廃液から心材成分を回収することである。
The method for recovering the wood core material component, which is the sixth feature of the present invention, is
A step of pretreating the waste liquid recovered by the drying treatment of wood by a method of either chelation treatment, reduction treatment or pH treatment, and
The step of bringing the pretreated liquid into contact with the adsorption carrier, and
The step of eluting the adsorption carrier with an organic solvent and
This is to recover the core material component from the waste liquid.
本発明の第七の特徴である木材心材成分は、
前記本発明の第六の特徴である木材心材成分の回収方法によって回収された木材心材成分としたことである。
The wood core material component, which is the seventh feature of the present invention, is
The wood core material component recovered by the method for recovering the wood core material component, which is the sixth feature of the present invention.
本発明の第一の特徴により、黒色のドレーンとして利用されることのなかった廃液中の金属をキレート化し、該金属を必要とする産業分野において金属補給体として利用することが可能となる。また、キレート化された金属とキレート剤とが日光などの外的作用により徐々に解離することになり、長期間の間一定濃度の金属補給体を安定して供給することができる。
本発明の第二の特徴により、微量でありながらも植物の成長などに重要な成分である鉄を補給し、鉄成分の欠乏により生ずる生理障害を防ぐことができる。
本発明の第三の特徴により、金属、その中でも特に鉄と容易に、かつ強く結合することができる。また、被金属補給体に吸収され易くなると共に窒素源も付与することができる。
本発明の第四の特徴により、前処理を行って吸着担体に吸着されやすい物質に変換し、吸着担体に吸着された木材心材成分と懸濁のない略無色の液体とに分離することができる。
本発明の第五の特徴により、様々な物質から構成されるドレーンのうち、黒色の原因とされるノルリグナン類と鉄との錯体から鉄を解離させ、鉄とＥＤＴＡとの錯塩などのより安定した錯体を形成させることができる。
本発明の第六の特徴により、木材乾燥廃液を脱色することができると共に、有機溶媒中に溶出された木材心材成分を回収することができる。また、吸着担体を容易に再生することができる。
本発明の第七の特徴により、ドレーンから分離回収された木材心材成分を木材強化剤、抗菌剤、防腐剤又は害虫忌避剤などの有価物として利用できる。
The first feature of the present invention makes it possible to chelate a metal in a waste liquid that has not been used as a black drain and use it as a metal supplement in an industrial field that requires the metal. In addition, the chelated metal and the chelating agent are gradually dissociated by an external action such as sunlight, and a constant concentration of metal supplement can be stably supplied for a long period of time.
According to the second feature of the present invention, it is possible to supplement iron, which is an important component for plant growth and the like, although it is a trace amount, and prevent physiological disorders caused by deficiency of the iron component.
A third feature of the present invention allows for easy and strong binding to metals, especially iron. In addition, it can be easily absorbed by the metal supplement and a nitrogen source can be provided.
According to the fourth feature of the present invention, it is possible to perform pretreatment to convert it into a substance that is easily adsorbed on the adsorption carrier, and separate the wood core material component adsorbed on the adsorption carrier into a substantially colorless liquid without suspension. ..
According to the fifth feature of the present invention, among drains composed of various substances, iron is dissociated from a complex of norlignans and iron, which is a cause of black color, and more stable such as a complex salt of iron and EDTA. A complex can be formed.
According to the sixth feature of the present invention, the wood drying waste liquid can be decolorized and the wood core material component eluted in the organic solvent can be recovered. Moreover, the adsorption carrier can be easily regenerated.
According to the seventh feature of the present invention, the wood core material component separated and recovered from the drain can be used as a valuable resource such as a wood strengthening agent, an antibacterial agent, a preservative or a pest repellent.
以下に、本発明を実施するための形態について説明するが、本発明の範囲は、以下に示す実施例に限定されるものではない。 Hereinafter, embodiments for carrying out the present invention will be described, but the scope of the present invention is not limited to the examples shown below.
本発明は、木材の乾燥機から流出するドレーンを原料とし、この廃出されたドレーンから産業上利用が可能な物質を見いだすと共に、黒色に懸濁したドレーンを脱色する方法を見いだし、さらにその過程で有価物を回収するというものである。これらの発明は一連の分離技術において確立するものであり、下記にそのフローについて図を用いて詳述する。 The present invention uses a drain flowing out of a wood dryer as a raw material, finds a substance that can be industrially used from this waste drain, and finds a method for decolorizing a drain suspended in black, and further, the process. It is to collect valuable resources at. These inventions are established in a series of separation techniques, and the flow thereof will be described in detail below with reference to figures.
図１は、本発明を実施するためのフローを示したものである。原料は、木材の乾燥機から流出したものを回収した黒色のドレーンである。木材は、スギ、マツ、ヒノキなどの乾燥処理から回収され、乾燥処理は、例えばスギの蒸気式乾燥処理の場合、初期蒸煮工程、ドライングセット工程、乾燥工程及び冷却工程の４工程で行われる。スギの蒸気式乾燥処理で排出されるドレーンの量は、乾燥処理全工程１８３時間のうち、計５１時間で行われる初期蒸煮工程及びドライングセット工程において、庫内温度９６度から１２０度の環境で大量に回収される。なお、木材の乾燥処理においては、蒸気式乾燥や高周波減圧式乾燥などがあるが、木材乾燥処理において乾燥機底面から廃液として回収されるドレーンであれば本発明を利用することができる。 FIG. 1 shows a flow for carrying out the present invention. The raw material is a black drain that is collected from the wood dryer. The wood is recovered from the drying treatment of sugi, pine, cypress and the like, and the drying treatment is carried out in four steps of, for example, in the case of steam-type drying treatment of sugi, an initial steaming step, a drying set step, a drying step and a cooling step. The amount of drain discharged by the steam drying process of Sugi is the environment where the temperature inside the refrigerator is 96 to 120 degrees in the initial steaming process and the drying set process, which are performed in a total of 51 hours out of the total 183 hours of the drying process. Collected in large quantities. In the wood drying process, there are steam drying and high frequency vacuum drying, but the present invention can be used as long as the drain is recovered as waste liquid from the bottom surface of the dryer in the wood drying process.
ＳＴ１はこのドレーンをキレート処理、還元処理又はｐＨ処理の何れかによる方法で前処理を行う工程である。キレート処理の場合は、キレート剤として例えば、ＤＴＰＡ（ジエチレントリアミン五酢酸）、ＥＤＴＡ（エチレンジアミン四酢酸）、ＧＥＤＴＡ（グリコールエーテルジアミン四酢酸）、ＨＥＤＴＡ（ヒドロキシエチルエチレンジアミン三酢酸）、ＮＴＡ（ニトリロ三酢酸）などが挙げられる。還元処理の場合は、還元剤として例えば、ジチオトレイトール（ＤＴＴ）、ジチオエリトリトール（ＤＴＥ）、システイン、メルカプトエタノール（ＢＭＥ）などが挙げられる。また、これらのキレート剤及び還元剤は鉄と強く結合することができる。ｐＨ処理の場合は、例えばｐＨを酸性にするために硫酸、塩酸、クエン酸などを用いることができる。これらの前処理のうち少なくとも何れかを行うことによって、次のステップで説明する吸着担体通過工程で吸着担体に吸着されやすい物質に変換し、吸着担体に吸着された木材心材成分と懸濁のない略無色の液体とに分離することができる。 ST1 is a step of pretreating the drain by a method of either chelation treatment, reduction treatment or pH treatment. In the case of chelation treatment, as the chelating agent, for example, DTPA (diethylenetriaminetetraacetic acid), EDTA (ethylenediaminetetraacetic acid), GEDTA (glycol etherdiaminetetraacetic acid), HEDTA (hydroxyethylethylenediaminetetraacetic acid), NTA (nitrilotriacetic acid), etc. Can be mentioned. In the case of the reduction treatment, examples of the reducing agent include dithiothreitol (DTT), dithioerythritol (DTE), cysteine, mercaptoethanol (BME) and the like. In addition, these chelating agents and reducing agents can strongly bind to iron. In the case of pH treatment, for example, sulfuric acid, hydrochloric acid, citric acid or the like can be used to make the pH acidic. By performing at least one of these pretreatments, the substance is converted into a substance that is easily adsorbed on the adsorption carrier in the adsorption carrier passing step described in the next step, and the wood core material component adsorbed on the adsorption carrier is not suspended. It can be separated into a substantially colorless liquid.
ＳＴ１における前処理がキレート処理の場合、金属−キレート化合物が形成され、金属を必要とする産業分野において金属補給体として利用できる。例えば、植物の生育においてはＣａやＭｇのほか、Ｆｅ、Ｃｏ、Ｍｎ、Ｃｕ、Ｚｎなどの微量金属の役割が重要となっているが、本発明で得られる金属−キレート化合物を金属補給体として植物に供給することにより、木材乾燥処理から得られた成分を原料とする金属−キレート化合物を有効物質として土壌などに返還することができる。 When the pretreatment in ST1 is a chelate treatment, a metal-chelate compound is formed and can be used as a metal supplement in industrial fields requiring a metal. For example, in addition to Ca and Mg, the role of trace metals such as Fe, Co, Mn, Cu, and Zn is important in the growth of plants, and the metal-chelate compound obtained in the present invention is used as a metal supplement. By supplying to a plant, a metal-chelate compound made from a component obtained from a wood drying process can be returned to the soil or the like as an effective substance.
また、多くの微量金属の中でも鉄は植物の必須元素であり、葉緑素の合成などに重要な役割を担っているが、鉄−キレート化合物を供給することによって植物の鉄成分欠乏症を防ぐことができる。キレート剤においては、特に鉄と強く結合するＥＤＴＡを用いて鉄−ＥＤＴＡ化合物とすることにより、植物に吸収され易くなると共に窒素源も付与することができる。 In addition, iron is an essential element of plants among many trace metals and plays an important role in the synthesis of chlorophyll. However, by supplying an iron-chelate compound, iron component deficiency in plants can be prevented. .. In the chelating agent, by using EDTA which strongly binds to iron to form an iron-EDTA compound, it becomes easy to be absorbed by plants and a nitrogen source can be provided.
また、従来から鉄の補給に利用されている塩化鉄や硫酸鉄を添加した場合、適当な補給濃度と補給回数が必要になるが、高濃度となれば薬害を起こすこととなり、低濃度となれば補給回数が増えるようになるところ、本発明による鉄−ＥＤＴＡ化合物であれば、日光などの外的作用により徐々に鉄がＥＤＴＡから解離することになり、長期間の間一定濃度の金属補給体を安定して供給することができる。 In addition, when iron chloride or iron sulfate, which has been used for iron supplementation, is added, an appropriate supplementation concentration and number of supplementations are required, but if the concentration is high, it will cause chemical damage and the concentration should be low. In the case of the iron-EDTA compound according to the present invention, iron gradually dissociates from EDTA due to an external action such as sunlight, and a constant concentration of metal supplement is provided for a long period of time. Can be stably supplied.
ＳＴ２は、ＳＴ１で前処理を行った廃液を吸着担体に通過させる工程である。吸着担体は、例えば疎水性吸着担体であればスチレン−ジビニルベンゼン系の合成吸着樹脂である、ダイヤイオンＨＰ２０（「ダイヤイオン」は登録商標、以下同じ。）、ダイヤイオンＨＰ２１などのダイヤイオンシリーズ（三菱ケミカル株式会社製）やポリスチレン樹脂であるデュオライトＳ８７８（住化ケムテックス株式会社製）を用いることができる。 ST2 is a step of passing the waste liquid pretreated in ST1 through the adsorption carrier. The adsorption carrier is, for example, a styrene-divinylbenzene-based synthetic adsorption resin in the case of a hydrophobic adsorption carrier, such as Diaion HP20 (“Diaion” is a registered trademark, the same applies hereinafter), Diaion HP21, and the like. Mitsubishi Chemical Co., Ltd.) and Duolite S878 (manufactured by Sumika Chemtex Co., Ltd.), which is a polystyrene resin, can be used.
ＳＴ３は、ＳＴ２の吸着処理により吸着担体を通過した略無色の廃液を河川などへ廃棄する脱色処理済廃液を廃棄する工程である。この廃液は鉄錯体から鉄が解離した鉄イオンとして存在している。 ST3 is a step of discarding the decolorized waste liquid that has passed through the adsorption carrier by the adsorption treatment of ST2 and is discarded into a river or the like. This waste liquid exists as iron ions in which iron is dissociated from the iron complex.
一方、ＳＴ４は、ＳＴ２により吸着担体に吸着された物質をエタノールやメタノールなどの有機溶媒で溶出させる工程である。この溶出工程により吸着担体を容易に再生し、繰り返し利用することができる。また、有機溶媒中に溶出された成分は、セクイリンＣやアガサレジノールを主成分とする赤色（「赤みの強い褐色」の色を「赤色」といい、以下同じである。）の木材心材成分であることから、これを用いた木材強化剤、抗菌剤、防腐剤又は害虫忌避剤などに利用できる。 On the other hand, ST4 is a step of eluting the substance adsorbed on the adsorption carrier by ST2 with an organic solvent such as ethanol or methanol. By this elution step, the adsorption carrier can be easily regenerated and used repeatedly. In addition, the component eluted in the organic solvent is a red wood core material component containing sequilin C or agasa resinol as a main component (the color of "reddish brown" is referred to as "red" and the same applies hereinafter). Therefore, it can be used as a wood strengthening agent, an antibacterial agent, a preservative, a pest repellent, etc. using this.
これらのＳＴ１〜ＳＴ４の処理により、木材乾燥機から流出するドレーンから産業上利用が可能となる金属補給体を得ると共に、黒色のドレーンを脱色し、さらにその過程で分離回収される木材心材成分を有価物として回収することができる。 By these treatments of ST1 to ST4, a metal supplement that can be industrially used is obtained from the drain flowing out from the wood dryer, the black drain is decolorized, and the wood core material component separated and recovered in the process is obtained. It can be recovered as a valuable resource.
（実験例１）
以下に、木材乾燥廃液の黒色の原因と金属イオンとの関係を解明するために前処理を行った実験例について説明する。まず、ドレーンにキレート剤及び還元剤をそれぞれ加えた場合について検討した。図２は、右から順に、（１）何も加えていない状態のドレーン、（２）ドレーンにキレート剤としてＥＤＴＡを加えたもの、（３）ドレーンに還元剤としてＤＴＴを加えたものを示している。写真から明らかなように、（２）においては、懸濁した黒色が解消され、赤褐色の沈殿が確認できたことから３価の鉄がキレート化されて沈殿していると考えられる。また、（３）においては、懸濁した黒色が解消され、緑色の沈殿が確認できたことから２価の鉄が関与していることが考えられる。何れにしても、黒色の原因は金属イオンとフェノール性物質との錯体形成が関与し、その金属は鉄が主であることが強く疑われた。
(Experimental Example 1)
Below, an experimental example in which pretreatment was performed to clarify the relationship between the cause of the black color of the dried wood waste liquid and metal ions will be described. First, the case where a chelating agent and a reducing agent were added to the drain was examined. FIG. 2 shows, in order from the right, (1) a drain with nothing added, (2) a drain with EDTA added as a chelating agent, and (3) a drain with DTT added as a reducing agent. There is. As is clear from the photograph, in (2), the suspended black color was eliminated and a reddish brown precipitate was confirmed. Therefore, it is considered that trivalent iron was chelated and precipitated. Further, in (3), the suspended black color was eliminated and a green precipitate was confirmed, suggesting that divalent iron is involved. In any case, it was strongly suspected that the cause of the black color was the formation of a complex between a metal ion and a phenolic substance, and that the metal was mainly iron.
次に、これらの（１）〜（３）の各サンプルを酢酸エチルで抽出し、ＨＰＬＣを用いて分析を行った。その結果を図３に示す。（１）の原料ドレーンにおいては、保持時間９分においてのみアガサレジノールを示すピークを示した。（２）のＥＤＴＡ添加においては、保持時間３〜４．５分において僅かな複数のピークと、保持時間６〜６．５分においてセクイリンＣを示す強いピーク、保持時間９分においてアガサレジノールを示すピークを示した。（３）のＤＴＴ添加においては、保持時間５分付近で何らかの成分を示すピーク、保持時間６〜６．５分においてセクイリンＣを示す強いピーク、保持時間７．５分と９分付近で弱い何らかのピークを確認した。これらの分析結果より、黒色のドレーンをキレート処理もしくは還元処理することで、セクイリンＣやアガサレジノールなどを含むノルリグナン類（以下、単に「ノルリグナン類」という。）と金属との錯体から金属が解離し、ノルリグナン類が単体として存在することが明らかになった。 Next, each of these samples (1) to (3) was extracted with ethyl acetate and analyzed by HPLC. The result is shown in FIG. In the raw material drain of (1), a peak showing agasareginol was shown only at the holding time of 9 minutes. In the addition of EDTA in (2), a few peaks were added at a retention time of 3 to 4.5 minutes, a strong peak showing sequylin C at a retention time of 6 to 6.5 minutes, and agasaresinol at a retention time of 9 minutes. The peak shown was shown. In the addition of DTT in (3), a peak showing some component in the holding time of about 5 minutes, a strong peak showing sequylin C in the holding time of 6 to 6.5 minutes, and something weak in the holding time of 7.5 minutes and 9 minutes. The peak was confirmed. From these analysis results, by chelating or reducing the black drain, the metal is dissociated from the complex of the norlignans (hereinafter, simply referred to as "norlignans") containing sequylin C and agasaresinol and the metal. However, it became clear that norlignans exist as a single substance.
（実験例２）
さらに、金属の確定を行うため、キレート剤を用いて黒色物質の探索を行った結果について以下に詳述する。原料となる黒色のドレーンのサンプルは、スギの蒸気式乾燥処理にて９６度から１２０度で５１時間蒸煮処理し、乾燥機底面に流出したものを回収したものである（図５に示す左の写真）。このドレーンサンプル５００ｍＬにＥＤＴＡ−２Ｎａ（以下、単に「ＥＤＴＡ」という。）１０ｇを加えて攪拌したところ赤色を呈した（図５に示す右の写真）。
(Experimental Example 2)
Further, the results of searching for a black substance using a chelating agent in order to determine the metal will be described in detail below. The black drain sample used as a raw material was steam-dried at 96 to 120 degrees Celsius for 51 hours, and the one that flowed out to the bottom of the dryer was recovered (left in FIG. 5). Photo). When 10 g of EDTA-2Na (hereinafter, simply referred to as "EDTA") was added to 500 mL of this drain sample and stirred, it turned red (photograph on the right shown in FIG. 5).
次に、図４（ａ）にＥＤＴＡによるキレート処理後のドレーンの抽出・分画手順を示す。黒色のドレーンにＥＤＴＡを加えた赤色の廃液をヘキサン２００ｍＬで３回抽出したところ、黄色い精油成分が６９．８ｍｇ得られた（図４（ａ）右上写真）。一方、ヘキサン不溶物を、酢酸エチル２００ｍＬで４回抽出したところ、７０３．９ｍｇの褐色物質が得られた（図４（ａ）右下写真）。この褐色物質をＨＰＬＣで分析したところ、図２（２）で示したピークと同じであった。以上より、黒色ドレーンにＥＤＴＡを加えた赤色の廃液のうち、精油を除く酢酸エチル抽出物は、単体のノルリグナン類２種が主要に含まれる物質であることが確認できた。 Next, FIG. 4A shows a drain extraction / fractionation procedure after chelation treatment with EDTA. When the red waste liquid obtained by adding EDTA to the black drain was extracted three times with 200 mL of hexane, 69.8 mg of a yellow essential oil component was obtained (Fig. 4 (a) upper right photograph). On the other hand, when the hexane insoluble matter was extracted four times with 200 mL of ethyl acetate, 703.9 mg of a brown substance was obtained (FIG. 4 (a) lower right photograph). When this brown substance was analyzed by HPLC, it was the same as the peak shown in FIG. 2 (2). From the above, it was confirmed that among the red waste liquid obtained by adding EDTA to the black drain, the ethyl acetate extract excluding the essential oil is a substance mainly containing two kinds of elemental norlignans.
次に、０．５％塩化鉄水溶液に上記の処理で得られた褐色物質１μＬ、即ち単体のノルリグナン類を加えて呈色を確認したところ、黒色に近い呈色を示すことが確認できた（図４（ｂ）の右の写真）。なお、水に上記の処理で得られた褐色物質１μＬを加えたものは、透明のまま色の変化は確認できなかった（図４（ｂ）左の写真）。このことから、スギの蒸気式乾燥処理によってスギの心材成分のノルリグナン類が溶出しており、ドレーンは該ノルリグナン類と金属とで錯体が形成されており、ドレーン即ち該錯体が黒色を呈しているのは「鉄」が原因であることが明らかとなった。 Next, when 1 μL of the brown substance obtained by the above treatment, that is, elemental norlignans was added to a 0.5% iron chloride aqueous solution and the coloration was confirmed, it was confirmed that the coloration was close to black (). Right photo of FIG. 4 (b)). In addition, when 1 μL of the brown substance obtained by the above treatment was added to water, no change in color could be confirmed while remaining transparent (Fig. 4 (b) left photo). From this, norlignans, which are the core material components of Sugi, have been eluted by the steam drying treatment of Sugi, and the drain has a complex formed by the norlignans and the metal, and the drain, that is, the complex has a black color. It became clear that the cause was "iron".
（実験例３）
次に、前処理としてキレート処理を行った場合における、ドレーンの色の変化及び心材成分を回収するスキームについて図５を用いて説明する。図５の左に示す黒色廃液は原料のドレーンであり、この中には多くの成分のうち、例えばセクイリンＣの一部を示した写真下の化学式のように、２価のフェノールのＯＨ基のＨ＋とＦｅ３＋が置換され、フェノール類と鉄との錯体となって存在していることが考えられる。このドレーンにＥＤＴＡを添加することによって、セクイリンＣを主成分とするノルリグナン類と３価の鉄イオンとによる鉄錯体から鉄が分離し、３価の鉄イオンはＥＤＴＡと結合してより安定な錯体を形成し、Ｆｅ−ＥＤＴＡ錯体となっていると考えられる。
(Experimental Example 3)
Next, a scheme for recovering the color change of the drain and the core material component when the chelate treatment is performed as the pretreatment will be described with reference to FIG. The black effluent shown on the left of FIG. 5 is a drain of the raw material, and among many components, for example, as shown in the chemical formula below showing a part of sequylin C, the OH group of divalent phenol It is considered that H + and Fe 3+ are substituted and exist as a complex of phenols and iron. By adding EDTA to this drain, iron is separated from the iron complex consisting of norlignans containing sequylin C as the main component and trivalent iron ions, and the trivalent iron ions are combined with EDTA to form a more stable complex. Is considered to be an Fe-EDTA complex.
なお、Ｆｅ−ＥＤＴＡ錯体は前述の金属補給体として利用できる。また、Ｆｅ−ＥＤＴＡ錯体だけでなく、このようにして得られた赤色の廃液そのもの、即ちノルリグナン類とＦｅ−ＥＤＴＡ錯体の混在する廃液そのものも金属補給体に含まれ、即ち木材の乾燥処理によって回収された廃液中の金属がキレート化された状態の物質が含まれる溶液全体を金属補給体として利用することが可能である。 The Fe-EDTA complex can be used as the above-mentioned metal supplement. Further, not only the Fe-EDTA complex but also the red waste liquid itself obtained in this manner, that is, the waste liquid itself in which the norlignans and the Fe-EDTA complex are mixed is contained in the metal supplement, that is, it is recovered by the drying treatment of wood. It is possible to use the entire solution containing the substance in which the metal in the waste liquid is chelated as a metal supplement.
この赤色の廃液を吸着樹脂により吸着させて３価もしくは２価の鉄イオン単体として脱色させた廃液を略無色の廃液として排出することができる。また、吸着樹脂に吸着された物質はアルコールなどの有機溶媒によって心材成分であるノルリグナン類を含む鮮やかな赤色溶液として回収することが可能である。 This red waste liquid is adsorbed by an adsorption resin and decolorized as a simple substance of trivalent or divalent iron ions, and the waste liquid can be discharged as a substantially colorless waste liquid. In addition, the substance adsorbed on the adsorbent resin can be recovered as a bright red solution containing norlignans which are core material components by an organic solvent such as alcohol.
（実験例４）
次に、前処理としてｐＨ処理を行った場合における、ドレーンの色の変化を示した実験例について図６を用いて説明する。まず、ｐＨ５．５〜６．０の黒色のドレーン１００ｍＬに、ｐＨが２になるまで硫酸を加えた。この時の溶液は褐色を呈した。次に吸着樹脂としてデュオライトＳ８７８を２０ｍＬ充填させたカラムを使用し、これに１００ｍＬの褐色溶液を通過させることで得られたフルースロー画分は、略無色の廃液として排水することができる。一方、カラムに吸着された物質をエタノールで溶出し、得られた吸着画分は、赤色の心材成分として回収することができると共に、カラムを水で平衡化することで再生し、同カラムを繰り返し利用することができる。また、得られた心材成分はＨＰＬＣの分析の結果図３の（２）と同じピークを示したことから、セクイリンＣやアガサレジノールが主要に回収されていることが確認された。よって、回収された赤色の心材成分からは、抗菌作用、抗蟻作用、害虫忌避作用などの様々な生理活性が期待されると共に、天然由来の木材防腐剤としての利用が期待できる。
(Experimental Example 4)
Next, an experimental example showing the change in the color of the drain when the pH treatment is performed as the pretreatment will be described with reference to FIG. First, sulfuric acid was added to 100 mL of a black drain having a pH of 5.5 to 6.0 until the pH reached 2. The solution at this time turned brown. Next, a column filled with 20 mL of Duolite S878 as an adsorption resin is used, and the fluthrow fraction obtained by passing 100 mL of a brown solution through the column can be drained as a substantially colorless waste liquid. On the other hand, the substance adsorbed on the column is eluted with ethanol, and the obtained adsorbed fraction can be recovered as a red core material component, and the column is regenerated by equilibrating with water, and the column is repeated. It can be used. In addition, the obtained core material component showed the same peak as (2) in FIG. 3 as a result of HPLC analysis, and it was confirmed that sequilin C and agasareginol were mainly recovered. Therefore, the recovered red heartwood component is expected to have various physiological activities such as antibacterial action, anti-ant action, and pest repellent action, and can be expected to be used as a naturally derived wood preservative.
以上、本発明の実施例を図面により説明してきたが、具体的な構成はこれら実施例に限られるものではなく、本発明の要旨を逸脱しない範囲における変更や追加があっても本発明に含まれる。 Although examples of the present invention have been described above with reference to the drawings, the specific configuration is not limited to these examples, and any changes or additions within the scope of the gist of the present invention are included in the present invention. Is done.
本発明は、木材乾燥機から流出するドレーンを原料とし、該ドレーンから金属補給体としての産業上の利用を見いだすと共に、黒色に懸濁したドレーンを略無色に脱色する方法と、その脱色過程において心材成分を回収する方法を見いだしたものである。 The present invention uses a drain flowing out of a wood dryer as a raw material, finds an industrial use as a metal supplement from the drain, and decolorizes a drain suspended in black to be substantially colorless, and in the decoloring process. We have found a way to recover the heartwood components.
Claims (7)
前記前処理を行った前処理液を吸着担体に接触させる工程と、
により、前記廃液を脱色することを特徴とする木材乾燥廃液の脱色方法。 A step of pretreating the waste liquid recovered by the drying treatment of wood by a method of either chelation treatment, reduction treatment or pH treatment, and
The step of bringing the pretreated liquid into contact with the adsorption carrier, and
A method for decolorizing a wood drying waste liquid, which comprises decolorizing the waste liquid.
前記前処理を行った前処理液を吸着担体に接触させる工程と、
前記吸着担体を有機溶媒で溶出させる工程と、
により、前記廃液から心材成分を回収することを特徴とする木材心材成分の回収方法。 A step of pretreating the waste liquid recovered by the drying treatment of wood by a method of either chelation treatment, reduction treatment or pH treatment, and
The step of bringing the pretreated liquid into contact with the adsorption carrier, and
The step of eluting the adsorption carrier with an organic solvent and
A method for recovering a wood core material component, which comprises recovering the heart material component from the waste liquid.
A wood core material component recovered by the method for recovering a wood core material component according to claim 6.
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