WO2018061915A1 - Procédé d'affinage de shungite - Google Patents

Procédé d'affinage de shungite Download PDF

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Publication number
WO2018061915A1
WO2018061915A1 PCT/JP2017/033846 JP2017033846W WO2018061915A1 WO 2018061915 A1 WO2018061915 A1 WO 2018061915A1 JP 2017033846 W JP2017033846 W JP 2017033846W WO 2018061915 A1 WO2018061915 A1 WO 2018061915A1
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WO
WIPO (PCT)
Prior art keywords
iron
purifying
water
powder
sulfur
Prior art date
Application number
PCT/JP2017/033846
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English (en)
Japanese (ja)
Inventor
藤田　豊久
ジョルジ ドドビバ
青木　太一
健太郎 鷹野
ヤナ ウシニナ
Original Assignee
国立大学法人 東京大学
株式会社アサボウ
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by 国立大学法人 東京大学, 株式会社アサボウ filed Critical 国立大学法人 東京大学
Publication of WO2018061915A1 publication Critical patent/WO2018061915A1/fr

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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
    • 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
    • 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
    • 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
    • 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
    • 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

Definitions

  • the present invention relates to a method for purifying sungite.
  • Shungite is said to have been deposited in the Precambrian period (about 2 billion years ago), is a black carbon ore containing natural fullerenes, and is produced in the Karelia region of Russia.
  • the main features of Sungaito are the following three points. (1) Carbon and silica in the ore are strongly bonded. (2) It has electrical conductivity. (3) Shows strong activity in redox reaction.
  • schungite is considered to be an important material for industrial use as a substitute for rubber fillers, water / soil cleaners, and silicon carbide, but is rarely used at present.
  • the reason is that the research is insufficient, the material composition ratio varies depending on the type (carbon content is greatly different), and impurities such as sulfur and iron exist.
  • Patent Document 1 discloses a desulfurization process.
  • metals such as iron, metal compounds, and sulfur from the shungaite ore.
  • An object of the present invention is to provide a method for refining shungait which can efficiently remove impurities such as metals such as iron, metal compounds, sulfur and the like from sungaiite ore and obtain high-pure sungite.
  • an embodiment of the present invention is a method for purifying a sungite, a dispersion step of dispersing the sungite powder in water, and a magnetic field acting on the sungite powder dispersed in the water to iron And an iron removal step of adsorbing and removing the iron compound.
  • a magnetic field is applied to a mesh of ferromagnetic stainless steel, and iron and an iron compound are attracted and removed by the mesh.
  • the iron removal step may be performed by chelate treatment instead of applying a magnetic field to the schungite powder dispersed in water.
  • the chelating agent used for the chelation treatment is preferably nitrilotriacetic acid.
  • the iron removal step may be performed by acid treatment instead of applying a magnetic field to the schungite powder dispersed in water.
  • the acid used for the acid treatment is preferably reverse aqua regia or a mixture of hydrochloric acid and hydrogen peroxide.
  • the sulfur removal step may be performed by chelate treatment instead of irradiating the schungite powder with microwaves in water or in air.
  • the chelating agent used for the chelation treatment is preferably nitrilotriacetic acid.
  • the sulfur removal step may be carried out by acid treatment instead of irradiating the sungite powder with water or in air.
  • the acid used for the acid treatment is preferably reverse aqua regia or a mixture of hydrochloric acid and hydrogen peroxide.
  • impurities such as metals such as iron, metal compounds, sulfur and the like can be efficiently removed from the ore of sungite, and high-purity sungite can be obtained.
  • the composition ratio of the shungaite ore is about 40% carbon, 43% silica, 3% sulfur, and about 7% iron.
  • Iron includes iron compounds such as iron sulfide.
  • FIG. 1 shows a configuration example for performing the iron removal step.
  • iron and iron compounds are removed from the sungite.
  • a shungaite dispersion 12 in which a shungait powder obtained by pulverizing shungaite ore is dispersed in water is placed in a beaker or other appropriate container 10 (dispersion step).
  • a mesh 14 made of a ferromagnetic material such as ferromagnetic stainless steel is disposed on the screen.
  • a magnetic field is applied by magnetic field generating means 16N, 16S such as magnets from both sides (directions facing each other) of the schungite dispersion liquid 12.
  • the net 14 in the shungait dispersion 12 is magnetized, and iron and iron compounds as impurities present in the shungait dispersion 12 are adsorbed and removed by the net 14.
  • iron sulfide etc. are mentioned as an iron compound.
  • iron and iron compounds may be adsorbed and removed by using a magnet directly in the schungite dispersion liquid 12 or schungite powder without using the net 14.
  • FIG. 2 shows a configuration example for performing the sulfur removal step.
  • sulfur is removed from the schungite.
  • a schungite powder 22 obtained by pulverizing schungite ore is placed on a saucer 20 disposed in the microwave generator 18, and microwaves are irradiated in the air by the microwave generator 18. Thereby, the sulfur in the schungite powder 22 is heated and vaporized and removed.
  • the sugagate dispersion 12 similar to the example of FIG. 1 may be placed on the saucer 20, and microwaves may be irradiated in water.
  • the sungite powder 22 or the shungait powder 12 in the shungait dispersion liquid 12 it is preferable to use the sungite powder after the iron removal step.
  • the microwave used in the sulfur removal process is an electromagnetic wave having a wavelength range of 1 m to 1 mm (frequency is 300 MHz to 300 GHz).
  • the microwave power used is preferably 800 to 1200 W and the irradiation time is preferably 1 to 10 minutes.
  • Modification 1 As modification 1 of an iron removal process and a sulfur removal process, iron, an iron compound, and sulfur can be removed by a chelate process instead of making a magnetic field act on the schungite dispersion liquid 12.
  • a chelating agent is placed in a container 10 shown in FIG. 1 together with a schungite dispersion 12 and stirred at a temperature of 70 to 90 ° C. for 1 to 10 minutes to remove iron, iron compounds and sulfur.
  • nitrilotriacetic acid NTA
  • EDTA ethylenediaminetetraacetate
  • EDTA.2Na ethylenediaminetetraacetate
  • nitrilotriacetic acid is particularly preferable.
  • Modification 2 As a second modification of the iron removal step and the sulfur removal step, iron, iron compounds, and sulfur can be removed by acid treatment instead of applying a magnetic field to the schungite dispersion 12.
  • the acid is preferably reverse 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 in a ratio of 3: 1 (concentrated nitric acid 3 to concentrated hydrochloric acid 1).
  • ⁇ Iron removal process> In a container 10 shown in FIG. 1, a sungite dispersion (concentration 1.25% by mass) in which sungite powder is dispersed in water is added, and hexametaphosphoric acid as a dispersant is added, and then a magnetic field of maximum 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 mesh 14.
  • the vertical axis represents the concentration of sulfur (such as SO 3 ) in the shungite powder
  • the horizontal axis represents the microwave irradiation time.
  • the sulfur concentration decreases with the irradiation time. Therefore, what is necessary is just to determine irradiation time suitably according to the target sulfur concentration.
  • sulfur concentration is falling because sulfur vaporizes. For example, when the microwave was irradiated for 9 minutes, 85% by mass of sulfur could be removed.
  • a shungaite dispersion (concentration: 0.6% by mass) in which shungait powder is dispersed in water is added, and after the temperature is raised to 80 ° C., nitrilotriacetic acid (NTA) as a chelating agent And stirred for 6 minutes, and then washed with water.
  • NTA nitrilotriacetic acid
  • the content of iron and iron compound was 10% by mass and sulfur was 5.2% by mass before the acid treatment, and the content of iron and iron compound was 2.0% by mass and sulfur was 0%. Reduced to 9 mass%.

Abstract

Le problème à résoudre dans le cadre de la présente invention consiste à fournir un procédé d'affinage de shungite qui permet d'éliminer de manière efficace des métaux tels que le fer, des composés métalliques et des impuretés telles que le soufre, d'un minerai de shungite, afin d'obtenir de la shungite très pure. La solution consiste en une poudre de shungite qui est dispersée dans de l'eau et un champ magnétique qui est appliqué à la poudre de shungite dispersée dans l'eau pour éliminer le fer et les composés de fer par adsorption. La poudre de shungite de laquelle le fer des composés de fer ont été éliminés par adsorption, est en outre bombardée avec des micro-ondes dans de l'eau ou dans de l'air pour éliminer le soufre, ce qui permet d'obtenir une purification plus élevée.
PCT/JP2017/033846 2016-09-27 2017-09-20 Procédé d'affinage de shungite WO2018061915A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2016-188707 2016-09-27
JP2016188707A JP6791698B2 (ja) 2016-09-27 2016-09-27 シュンガイトの精製方法

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WO2018061915A1 true WO2018061915A1 (fr) 2018-04-05

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WO (1) WO2018061915A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020112036A1 (fr) * 2018-11-26 2020-06-04 Sabuncu Abdulsamet Technique de pointage magnétique pour la valorisation de minerai

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2725233C1 (ru) * 2019-06-26 2020-06-30 Акционерное общество "СПЕЦХИММОНТАЖ" (АО "СПЕЦХИММОНТАЖ") Способ переработки шунгита

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58214361A (ja) * 1982-06-07 1983-12-13 Ube Ind Ltd 炭化水素質原料のガス化工程において得られる未反応炭素質粒子を含む水中懸濁液から炭素質物質以外の不純物を分離する方法
JPH02241557A (ja) * 1989-03-15 1990-09-26 Gakunan Koki Kk 粉体中の微細な鉄粉を除去する方法
JPH0639311A (ja) * 1992-07-23 1994-02-15 Sumitomo Chem Co Ltd アルミナ含有鉱石からの磁性物質の除去方法
JP2003243878A (ja) * 2002-02-15 2003-08-29 Hitachi Ltd 電磁波吸収材料及びそれを用いた各種製品
JP2006137907A (ja) * 2004-11-15 2006-06-01 Rusupuromuremonto Japan:Kk 鉄系金属部材の摩擦面改質材及び摩擦面改質方法
JP2014159004A (ja) * 2013-02-20 2014-09-04 Mitsubishi Paper Mills Ltd 半透膜支持体製造方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58214361A (ja) * 1982-06-07 1983-12-13 Ube Ind Ltd 炭化水素質原料のガス化工程において得られる未反応炭素質粒子を含む水中懸濁液から炭素質物質以外の不純物を分離する方法
JPH02241557A (ja) * 1989-03-15 1990-09-26 Gakunan Koki Kk 粉体中の微細な鉄粉を除去する方法
JPH0639311A (ja) * 1992-07-23 1994-02-15 Sumitomo Chem Co Ltd アルミナ含有鉱石からの磁性物質の除去方法
JP2003243878A (ja) * 2002-02-15 2003-08-29 Hitachi Ltd 電磁波吸収材料及びそれを用いた各種製品
JP2006137907A (ja) * 2004-11-15 2006-06-01 Rusupuromuremonto Japan:Kk 鉄系金属部材の摩擦面改質材及び摩擦面改質方法
JP2014159004A (ja) * 2013-02-20 2014-09-04 Mitsubishi Paper Mills Ltd 半透膜支持体製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020112036A1 (fr) * 2018-11-26 2020-06-04 Sabuncu Abdulsamet Technique de pointage magnétique pour la valorisation de minerai

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