JP6791698B2 - Shungite purification method - Google Patents
Shungite purification method Download PDFInfo
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- JP6791698B2 JP6791698B2 JP2016188707A JP2016188707A JP6791698B2 JP 6791698 B2 JP6791698 B2 JP 6791698B2 JP 2016188707 A JP2016188707 A JP 2016188707A JP 2016188707 A JP2016188707 A JP 2016188707A JP 6791698 B2 JP6791698 B2 JP 6791698B2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/025—High gradient magnetic separators
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/025—High gradient magnetic separators
- B03C1/031—Component parts; Auxiliary operations
- B03C1/033—Component parts; Auxiliary operations characterised by the magnetic circuit
- B03C1/034—Component parts; Auxiliary operations characterised by the magnetic circuit characterised by the matrix elements
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
- C02F1/64—Heavy metal compounds of iron or manganese
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Description
本発明は、シュンガイトの精製方法に関する。 The present invention relates to a method for purifying shungite.
シュンガイト(Ｓｈｕｎｇｉｔｅ)は、先カンブリア期（約２０億年前）に堆積したとされ、天然のフラーレンを含む黒色の炭素鉱石であり、ロシアのカレリア地方で産出されている。シュンガイトの主要な特徴は次の三点である。
（１）鉱石中の炭素とシリカが強く結合している。
（２）電気伝導性を持つ。
（３）酸化還元反応において強い活性を示す。
Shungite is a black carbon ore containing natural fullerenes, which is said to have been deposited during the Precambrian period (about 2 billion years ago), and is produced in the Karelia region of Russia. The main features of Shungite are the following three points.
(1) Carbon and silica in the ore are strongly bonded.
(2) Has electrical conductivity.
(3) Shows strong activity in redox reaction.
これら特性から、シュンガイトはゴムフィラー、水質・土壌浄化剤、炭化ケイ素の代替品として、産業利用に於いて重要な材料であると考えられるが、現状では殆ど利用されていない。その理由としては、研究が不十分である事、種類によって物質構成比が異なる（炭素含有量が大幅に異なる）事、硫黄や鉄などの不純物が存在する事が挙げられる。 Based on these properties, shungite is considered to be an important material for industrial use as a substitute for rubber fillers, water / soil purifiers, and silicon carbide, but it is rarely used at present. The reasons for this are that the research is inadequate, that the substance composition ratio differs depending on the type (the carbon content differs significantly), and that impurities such as sulfur and iron are present.
以上を踏まえた上で、シュンガイトを産業利用するためには、シュンガイトを効率よく精製する技術が重要である。 Based on the above, in order to use Shungite industrially, a technology for efficiently refining Shungite is important.
炭素質材料を精製する方法としては、例えば下記特許文献１に脱硫プロセスが開示されている。しかし、この方法では、シュンガイトの鉱石から種々の不純物、特に鉄等の金属や金属化合物、硫黄を効率よく除去することが困難である。 As a method for purifying a carbonaceous material, for example, the desulfurization process is disclosed in Patent Document 1 below. However, with this method, it is difficult to efficiently remove various impurities, particularly metals such as iron, metal compounds, and sulfur from the ore of Shungite.
本発明の目的は、シュンガイトの鉱石から鉄等の金属や金属化合物、硫黄等の不純物を効率よく除去し、高純度のシュンガイトを得ることができるシュンガイトの精製方法を提供することにある。 An object of the present invention is to provide a method for purifying shungite capable of efficiently removing metals such as iron, metal compounds, and impurities such as sulfur from the ore of shungite to obtain high-purity shungite.
上記目的を達成するために、本発明の一実施形態は、シュンガイトの精製方法であって、シュンガイト粉末を水に分散させる分散工程と、前記水に分散されたシュンガイト粉末に磁場を作用させて鉄及び鉄化合物を吸着除去する鉄除去工程と、を備えることを特徴とする。 In order to achieve the above object, one embodiment of the present invention is a method for purifying shungite, which comprises a dispersion step of dispersing shungite powder in water and iron by applying a magnetic field to the shungite powder dispersed in water. It is characterized by comprising an iron removing step of adsorbing and removing an iron compound.
上記鉄除去工程は、強磁性ステンレス鋼の網に磁場を作用させ、前記網に鉄及び鉄化合物を吸引させて除去するのが好適である。 In the iron removing step, it is preferable that a magnetic field is applied to a ferromagnetic stainless steel net and iron and an iron compound are attracted to the net to remove the iron.
また、上記鉄除去工程後のシュンガイト粉末に、水中または空気中でマイクロ波を照射し、硫黄を除去する硫黄除去工程をさらに備えるのが好適である。 Further, it is preferable to further include a sulfur removing step of irradiating the shungite powder after the iron removing step with microwaves in water or air to remove sulfur.
また、上記鉄除去工程を、水に分散されたシュンガイト粉末に磁場を作用させる代わりにキレート処理により行ってもよい。 Further, the iron removing step may be performed by a chelate treatment instead of applying a magnetic field to the shungite powder dispersed in water.
上記キレート処理に使用するキレート剤は、ニトリロ三酢酸であるのが好適である。 The chelating agent used for the chelating treatment is preferably nitrilotriacetic acid.
また、上記鉄除去工程を、水に分散されたシュンガイト粉末に磁場を作用させる代わりに酸処理により行ってもよい。 Further, the iron removing step may be carried out by acid treatment instead of applying a magnetic field to the shungite powder dispersed in water.
上記酸処理に使用する酸は、逆王水または塩酸と過酸化水素との混合物であるのが好適である。 The acid used for the acid treatment is preferably aqua regia or a mixture of hydrochloric acid and hydrogen peroxide.
また、上記硫黄除去工程を、シュンガイト粉末に水中または空気中でマイクロ波を照射する代わりにキレート処理により行ってもよい。 Further, the sulfur removing step may be performed by chelation treatment instead of irradiating the shungite powder with microwaves in water or air.
上記キレート処理に使用するキレート剤は、ニトリロ三酢酸であるのが好適である。 The chelating agent used for the chelating treatment is preferably nitrilotriacetic acid.
また、上記硫黄除去工程を、シュンガイト粉末に水中または空気中でマイクロ波を照射する代わりに酸処理により行ってもよい。 Further, the sulfur removing step may be performed by acid treatment instead of irradiating the shungite powder with microwaves in water or air.
上記酸処理に使用する酸は、逆王水または塩酸と過酸化水素との混合物であるのが好適である。 The acid used for the acid treatment is preferably aqua regia or a mixture of hydrochloric acid and hydrogen peroxide.
本発明によれば、シュンガイトの鉱石から鉄等の金属や金属化合物、硫黄等の不純物を効率よく除去し、高純度のシュンガイトを得ることができる。 According to the present invention, it is possible to efficiently remove metals such as iron, metal compounds, and impurities such as sulfur from the ore of Shungite to obtain high-purity Shungite.
以下、本発明を実施するための形態（以下、実施形態という）を、図面に従って説明する。 Hereinafter, embodiments for carrying out the present invention (hereinafter referred to as embodiments) will be described with reference to the drawings.
本発明者らの分析によると、シュンガイトの鉱石の構成比率は、炭素４０％、シリカ４３％、硫黄３％，鉄７％程度である。なお、鉄には硫化鉄等の鉄化合物も含まれる。 According to the analysis by the present inventors, the composition ratio of the ore of Shungite is about 40% carbon, 43% silica, 3% sulfur, and 7% iron. In addition, iron also includes iron compounds such as iron sulfide.
本実施形態においては、上記シュンガイト鉱石の構成元素の内、鉄及び鉄化合物と硫黄を不純物として除去する方法を示す。以後、鉄及び鉄化合物を除去する工程を鉄除去工程といい、硫黄を除去する工程を硫黄除去工程という。 In the present embodiment, a method for removing iron, an iron compound, and sulfur as impurities among the constituent elements of the Shungite ore is shown. Hereinafter, the step of removing iron and iron compounds is referred to as an iron removing step, and the step of removing sulfur is referred to as a sulfur removing step.
＜鉄除去工程＞
図１には、鉄除去工程を実施するための構成例が示される。鉄除去工程では、シュンガイトから鉄及び鉄化合物を除去する。図１において、鉄除去工程は、ビーカーその他適宜な容器１０に、シュンガイトの鉱石を粉砕して得たシュンガイト粉末を水に分散させたシュンガイト分散液１２を入れ（分散工程）、シュンガイト分散液１２中に強磁性ステンレス鋼等の強磁性体で構成された網１４を配置する。次に、シュンガイト分散液１２の両側（互いに対向する方向）から磁石等の磁場発生手段１６Ｎ、１６Ｓにより磁場を作用させる。これにより、シュンガイト分散液１２中の網１４が磁化され、シュンガイト分散液１２中に存在する、不純物としての鉄及び鉄化合物が網１４に吸着されて除去される。ここで、鉄化合物としては、硫化鉄等が挙げられる。
<Iron removal process>
FIG. 1 shows a configuration example for carrying out the iron removing step. In the iron removal step, iron and iron compounds are removed from the shungite. In FIG. 1, in the iron removal step, a shungite dispersion liquid 12 in which shungite powder obtained by crushing shungite ore is dispersed in water is placed in a beaker or other appropriate container 10 (dispersion step), and the shungite dispersion liquid 12 is charged. A net 14 made of a ferromagnetic material such as ferromagnetic stainless steel is arranged therein. Next, a magnetic field is applied from both sides (directions facing each other) of the shungite dispersion liquid 12 by magnetic field generating means 16N and 16S such as magnets. As a result, the net 14 in the shungite dispersion liquid 12 is magnetized, and iron and iron compounds as impurities present in the shungite dispersion liquid 12 are adsorbed on the net 14 and removed. Here, examples of the iron compound include iron sulfide and the like.
なお、網１４を使用せず、シュンガイト分散液１２中、あるいはシュンガイト粉末に直接磁石を作用させて鉄及び鉄化合物を吸着除去してもよい。 In addition, iron and iron compound may be adsorbed and removed in the shungite dispersion liquid 12 or by directly acting a magnet on the shungite powder without using the net 14.
＜硫黄除去工程＞
図２には、硫黄除去工程を実施するための構成例が示される。硫黄除去工程では、シュンガイトから硫黄を除去する。図２において、マイクロ波発生装置１８内に配置した受け皿２０に、シュンガイトの鉱石を粉砕して得たシュンガイト粉末２２を載せ、マイクロ波発生装置１８により空気中でマイクロ波を照射する。これにより、シュンガイト粉末２２中の硫黄を加熱して気化し、除去する。
<Sulfur removal process>
FIG. 2 shows a configuration example for carrying out the sulfur removal step. In the sulfur removal step, sulfur is removed from the shungite. In FIG. 2, a shungite powder 22 obtained by crushing shungite ore is placed on a saucer 20 arranged in the microwave generator 18, and the microwave generator 18 irradiates microwaves in the air. As a result, the sulfur in the shungite powder 22 is heated, vaporized, and removed.
なお、受け皿２０には、シュンガイト粉末２２の代わりに、図１の例と同様のシュンガイト分散液１２を載せて、水中でマイクロ波を照射してもよい。また、シュンガイト粉末２２またはシュンガイト分散液１２中のシュンガイト粉末としては、上記鉄除去工程後のシュンガイト粉末を使用するのが好適である。 In addition, instead of the shungite powder 22, the shungite dispersion liquid 12 similar to the example of FIG. 1 may be placed on the saucer 20 and irradiated with microwaves in water. Further, as the shungite powder in the shungite powder 22 or the shungite dispersion liquid 12, it is preferable to use the shungite powder after the iron removing step.
硫黄除去工程で使用するマイクロ波は、波長範囲が１ｍ〜１ｍｍ（周波数が３００ＭＨｚ〜３００ＧＨｚ）の電磁波である。また、使用するマイクロ波の電力は８００〜１２００Ｗ、照射時間は１〜１０分間であるのが好適である。 The microwave used in the sulfur removal step is an electromagnetic wave having a wavelength range of 1 m to 1 mm (frequency is 300 MHz to 300 GHz). Further, it is preferable that the microwave power used is 800 to 1200 W and the irradiation time is 1 to 10 minutes.
＜鉄除去工程及び硫黄除去工程の変形例＞
変形例１．
鉄除去工程及び硫黄除去工程の変形例１として、シュンガイト分散液１２に磁場を作用させる代わりにキレート処理により鉄及び鉄化合物並びに硫黄を除去することができる。
<Modification example of iron removal process and sulfur removal process>
Modification example 1.
As a modification 1 of the iron removing step and the sulfur removing step, iron, an iron compound, and sulfur can be removed by a chelate treatment instead of applying a magnetic field to the shungite dispersion liquid 12.
図１に示された容器１０に、シュンガイト分散液１２と共にキレート剤を入れ、７０〜９０℃の温度で１〜１０分間攪拌することにより、鉄及び鉄化合物並びに硫黄を除去する。 Iron and iron compounds and sulfur are removed by putting a chelating agent together with the shungite dispersion 12 in the container 10 shown in FIG. 1 and stirring at a temperature of 70 to 90 ° C. for 1 to 10 minutes.
上記キレート剤としては、ニトリロ三酢酸（ＮＴＡ）、エチレンジアミン四酢酸塩（ＥＤＴＡ）、エチレンジアミン四酢酸塩（ＥＤＴＡ・２Ｎａ）等が好適であり、ニトリロ三酢酸が特に好適である。 As the chelating agent, nitrilotriacetic acid (NTA), ethylenediaminetetraacetic acid salt (EDTA), ethylenediaminetetraacetic acid salt (EDTA.2Na) and the like are suitable, and nitrilotriacetic acid is particularly preferable.
変形例２．
鉄除去工程及び硫黄除去工程の変形例２として、シュンガイト分散液１２に磁場を作用させる代わりに酸処理により鉄及び鉄化合物並びに硫黄を除去することができる。
Modification example 2.
As a modification 2 of the iron removing step and the sulfur removing step, iron, an iron compound, and sulfur can be removed by acid treatment instead of applying a magnetic field to the shungite dispersion liquid 12.
図２に示された受け皿２０に、シュンガイト粉末２２と共に酸を入れ、シュンガイト粉末２２に含まれる鉄及び鉄化合物並びに硫黄を溶解して除去する。なお、この操作は、マイクロ波発生装置１８内で行う必要はない。 Acid is added to the saucer 20 shown in FIG. 2 together with the shungite powder 22, and the iron and iron compounds and sulfur contained in the shungite powder 22 are dissolved and removed. It is not necessary to perform this operation in the microwave generator 18.
上記酸としては、逆王水または塩酸と過酸化水素との混合物であるのが好適である。逆王水は、濃硝酸と濃塩酸とを３対１（濃硝酸３に対して濃塩酸１）の割合で混合したものである。 The acid is preferably aqua regia or a mixture of hydrochloric acid and hydrogen peroxide. Reverse aqua regia is a mixture of concentrated nitric acid and concentrated hydrochloric acid at a ratio of 3: 1 (3 concentrated nitric acid to 1 concentrated hydrochloric acid).
以下、本発明の実施例を具体的に説明する。なお、以下の実施例は、本発明の理解を容易にするためのものであり、本発明はこれらの実施例に制限されるものではない。 Hereinafter, examples of the present invention will be specifically described. The following examples are for facilitating the understanding of the present invention, and the present invention is not limited to these examples.
＜鉄除去工程＞
図１に示した容器１０に、シュンガイト粉末を水に分散させたシュンガイト分散液（濃度１．２５質量％）を入れ、分散剤であるヘキサメタリン酸を加えた後、最大０．９８Ｔの磁場を作用させた。図１の例で説明したように、鉄及び鉄化合物は、網１４に吸引されて除去される。
<Iron removal process>
In the container 10 shown in FIG. 1, a shungite dispersion (concentration: 1.25% by mass) in which shungite powder is dispersed in water is placed, hexamethaphosphate as a dispersant is added, and then a magnetic field of up to 0.98 T is applied. I let you. As described in the example of FIG. 1, iron and iron compounds are sucked and removed by the net 14.
本実施例にかかる鉄除去工程の操作の結果、２３％の硫黄と１５％の鉄及び鉄化合物を除去することができた。 As a result of the operation of the iron removing step according to this example, 23% sulfur and 15% iron and iron compounds could be removed.
＜硫黄除去工程＞
図２に示したマイクロ波発生装置１８内に、受け皿２０としてのるつぼを配置し、このるつぼに入れたシュンガイト粉末３ｇに対して、２．４５ＧＨｚのマイクロ波１０００Ｗを３〜９分間照射した。空気中で照射した場合とるつぼに５０ｍｌの純水を加え水中で照射した場合の二つの操作を行った。この結果を図３に示す。
<Sulfur removal process>
A crucible as a saucer 20 was placed in the microwave generator 18 shown in FIG. 2, and 3 g of shungite powder placed in the crucible was irradiated with 1000 W of microwaves at 2.45 GHz for 3 to 9 minutes. When irradiated in air Two operations were performed when 50 ml of pure water was added to the crucible and irradiated in water. The result is shown in FIG.
図３では、縦軸にシュンガイト粉末中の硫黄（ＳＯ３等）の濃度が、横軸にマイクロ波の照射時間がそれぞれ示されている。図３からわかるように、照射時間と共に硫黄濃度が低下していることがわかる。従って、目標とする硫黄濃度に応じて適宜照射時間を決定すればよい。なお、硫黄濃度は硫黄が気化することにより低下していると考えられる。例えば、９分間マイクロ波を照射した場合、硫黄を８５質量％除去することができた。 In Figure 3, the concentration of sulfur Shungaito powder on the vertical axis (SO 3, etc.), microwave irradiation time are shown respectively in the horizontal axis. As can be seen from FIG. 3, it can be seen that the sulfur concentration decreases with the irradiation time. Therefore, the irradiation time may be appropriately determined according to the target sulfur concentration. It is considered that the sulfur concentration is reduced by the vaporization of sulfur. For example, when microwave irradiation was performed for 9 minutes, 85% by mass of sulfur could be removed.
＜キレート処理による不純物除去＞
図１に示された容器１０に、シュンガイト粉末を水に分散させたシュンガイト分散液（濃度０．６質量％）を入れ、８０℃まで温度上昇させた後、キレート剤としてニトリロ三酢酸（ＮＴＡ）を加え６分間撹拌し、その後水により洗浄を行った。
<Impurity removal by chelation treatment>
In the container 10 shown in FIG. 1, a shungite dispersion (concentration: 0.6% by mass) in which shungite powder is dispersed in water is placed, the temperature is raised to 80 ° C., and then nitrilotriacetic acid (NTA) is used as a chelating agent. Was added, the mixture was stirred for 6 minutes, and then washed with water.
キレート処理の結果、硫黄が３６％、鉄び鉄化合物が６０％除去された。 As a result of the chelation treatment, 36% of sulfur and 60% of iron and iron compounds were removed.
＜酸処理による不純物除去＞
図２に示された受け皿２０としてのるつぼにシュンガイト粉末３ｇを入れ、これに対して逆王水または塩酸と過酸化水素との混合物を４０ｍｌ加え１２０分間撹拌した後、水により洗浄を行った。
<Remove impurities by acid treatment>
3 g of shungite powder was placed in a crucible as a saucer 20 shown in FIG. 2, 40 ml of reverse aqua regia or a mixture of hydrochloric acid and hydrogen peroxide was added thereto, and the mixture was stirred for 120 minutes and then washed with water.
逆王水を使用した場合には、酸処理前には鉄及び鉄化合物が１０質量％、硫黄５．２質量％あった含有量が、鉄及び鉄化合物が２．０質量％、硫黄が０．９質量％まで低減した。 When reverse royal water was used, the content of iron and iron compounds was 10% by mass and sulfur was 5.2% by mass before acid treatment, but iron and iron compounds were 2.0% by mass and sulfur was 0. It was reduced to 9.9% by mass.
また、塩酸と過酸化水素との混合物を使用した場合には、上記酸処理前の濃度が、鉄及び鉄化合物が１．８質量％、硫黄が１．３質量％まで低減した。 When a mixture of hydrochloric acid and hydrogen peroxide was used, the concentrations before the acid treatment were reduced to 1.8% by mass for iron and the iron compound and 1.3% by mass for sulfur.
１０ 容器、１２ シュンガイト分散液、１４ 網、１６Ｎ、１６Ｓ 磁場発生手段、１８ マイクロ波発生装置、２０ 受け皿、２２ シュンガイト粉末。
10 containers, 12 shungite dispersion, 14 nets, 16N, 16S magnetic field generating means, 18 microwave generator, 20 saucer, 22 shungite powder.
Claims (10)
前記水に分散されたシュンガイト粉末に磁場を作用させて鉄及び鉄化合物を吸着除去する鉄除去工程と、
を備える、シュンガイトの精製方法。 A dispersion process that disperses Shungite powder in water,
An iron removal step of adsorbing and removing iron and iron compounds by applying a magnetic field to the shungite powder dispersed in water.
A method for purifying shungite.
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| JP2016188707A JP6791698B2 (en) | 2016-09-27 | 2016-09-27 | Shungite purification method |
| PCT/JP2017/033846 WO2018061915A1 (en) | 2016-09-27 | 2017-09-20 | Shungite refinement method |
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| JPH02241557A (en) * | 1989-03-15 | 1990-09-26 | Gakunan Koki Kk | Removal of fine iron powder in powder |
| JPH0639311A (en) * | 1992-07-23 | 1994-02-15 | Sumitomo Chem Co Ltd | Method for removing magnetic substances from alumina-containing ores |
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