JP2004244313A - Magnesium oxide - Google Patents
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Abstract
Description
本発明は、鉛または鉛化合物の含有量の少ない酸化マグネシウムに関する。 The present invention relates to magnesium oxide having a low content of lead or a lead compound.
酸化マグネシウムの製造法には、炭酸マグネシウム（マグネサイトともいう）を焼成する方法と、海水あるいは塩化マグネシウム水溶液（苦汁またはかん水）に水酸化カルシウムを加えて水酸化マグネシウムを生成させ、これをろ過、乾燥した後、焼成する方法とがある。 Magnesium oxide is produced by calcining magnesium carbonate (also called magnesite) or by adding calcium hydroxide to sea water or an aqueous solution of magnesium chloride (bitter or brine) to produce magnesium hydroxide, which is filtered, After drying, there is a method of firing.
上記の水酸化マグネシウムを焼成して製造される酸化マグネシウムは、その焼成温度でその性質や用途が異なる。水酸化マグネシウムを１５００℃以上の高温で焼成したものは硬焼（重焼、死焼ともいう）マグネシアまたはマグネシアクリンカーと呼ばれる。本酸化マグネシウムは活性がほとんどなく、高温耐火性能を有し、耐火物材料として塩基性耐火れんがや不定形耐火物の原料などに利用されている。 Magnesium oxide produced by calcining the above magnesium hydroxide has different properties and uses at the calcining temperature. A product obtained by firing magnesium hydroxide at a high temperature of 1500 ° C. or more is called hard-fired (also called heavy-fired or dead-fired) magnesia or magnesia clinker. The magnesium oxide has almost no activity, has high-temperature refractory performance, and is used as a material for basic refractory bricks and amorphous refractories as a refractory material.
また、水酸化マグネシウムを４５０〜１３００℃で焼成して得られる酸化マグネシウム（軽焼または仮焼マグネシアともいう。以下、単に酸化マグネシウムという）は、活性が比較的大きく、マグネシアセメント材料、あるいはミネラルの供給源として肥料、食品等の添加剤、制酸剤や下剤などの医薬品の原料、化粧品原料などに利用されている。
この酸化マグネシウムは肥料、食品等の添加剤、医薬品原料として、人体に直接あるいは間接的に摂取され、あるいは化粧品原料として人体に接触するものであるため、重金属の混入量がより少ないものが望まれている。
In addition, magnesium oxide obtained by calcining magnesium hydroxide at 450 to 1300 ° C. (also referred to as lightly calcined or calcined magnesia; hereinafter simply referred to as magnesium oxide) has relatively high activity and is a material of magnesia cement material or mineral. It is used as a supply source for additives such as fertilizers and foods, raw materials for pharmaceuticals such as antacids and laxatives, and raw materials for cosmetics.
Since this magnesium oxide is directly or indirectly taken into the human body as a fertilizer, an additive such as food, or a pharmaceutical raw material, or comes into contact with the human body as a cosmetic raw material, it is desired that the amount of the heavy metal mixed therein is smaller. ing.
一般的に海水中には、重金属はほとんど存在しない（例えば、鉛については１０-3〜１０-6ｐｐｍ程度）が、水酸化カルシウムの原料である石灰石（もしくは石灰岩）には、鉛または鉛化合物が鉛としておよそ０．２〜０．７ｐｐｍ程度存在している。なお、鉛は、例えば酵素阻害剤として人体に有害な作用を示すことが知られている金属である。
また、海水と水酸化カルシウムから生成される水酸化マグネシウムは、重金属の吸着剤としても知られている（例えば、特許文献１には水酸化マグネシウムを用いた鉱山排水の処理方法が提案されている）。
Generally, heavy metals hardly exist in seawater (for example, about 10 -3 to 10 -6 ppm for lead), but limestone (or limestone) as a raw material of calcium hydroxide contains lead or a lead compound. Is present as about 0.2 to 0.7 ppm as lead. Note that lead is a metal that is known to have a harmful effect on the human body, for example, as an enzyme inhibitor.
In addition, magnesium hydroxide generated from seawater and calcium hydroxide is also known as a heavy metal adsorbent (for example, Patent Document 1 proposes a method for treating mine drainage using magnesium hydroxide). ).
上記の理由により、海水と水酸化カルシウムから水酸化マグネシウムを生成させた場合、石灰石に含まれている鉛または鉛化合物が水酸化マグネシウムに吸着され、水酸化マグネシウムのＰｂ含有量（鉛含有量）が１．５ｐｐｍ以上になることがある。
なお、水酸化マグネシウムに吸着された鉛も水酸化マグネシウムの乾燥、焼成に伴って、水酸化鉛あるいは酸化鉛等の鉛化合物となる。
上述した酸化マグネシウムは水酸化マグネシウムを１３００℃以下で焼成して製造されるので、沸点が１３００℃以上の鉛化合物が一旦水酸化マグネシウムに混入すると、この鉛化合物を除去することが難しいという問題がある。
For the above reasons, when magnesium hydroxide is generated from seawater and calcium hydroxide, lead or a lead compound contained in limestone is adsorbed on magnesium hydroxide, and the Pb content of magnesium hydroxide (lead content) May be 1.5 ppm or more.
The lead adsorbed on the magnesium hydroxide also becomes a lead compound such as lead hydroxide or lead oxide with drying and firing of the magnesium hydroxide.
Since the above-described magnesium oxide is produced by firing magnesium hydroxide at 1300 ° C. or less, once a lead compound having a boiling point of 1300 ° C. or more is mixed with magnesium hydroxide, it is difficult to remove the lead compound. is there.
水酸化マグネシウムに混入する鉛または鉛化合物の量を低減させる方法として、水酸化マグネシウムに吸着された鉛または鉛化合物を洗浄除去することが考えられるが、水酸化マグネシウムは上述したように鉛または鉛化合物を吸着しやすく洗い流すことは難しい。
また、水酸化マグネシウムに吸着される鉛または鉛化合物の量を低減させる方法としては、Ｐｂ含有量の少ない石灰石から生成された水酸化カルシウムを用いて、海水から水酸化マグネシウムを生成させる方法が考えられるが、石灰石の産出量や輸送コストなどから量産化は難しい。
Further, as a method of reducing the amount of lead or a lead compound adsorbed on magnesium hydroxide, a method of generating magnesium hydroxide from seawater using calcium hydroxide generated from limestone having a low Pb content is considered. However, mass production is difficult due to limestone production and transportation costs.
本発明の目的は、肥料用、医薬品原料用又は化粧品原料用として有用なＰｂ含有量の少ない酸化マグネシウムを提供することにある。 An object of the present invention is to provide a magnesium oxide having a low Pb content, which is useful as a fertilizer, a pharmaceutical raw material, or a cosmetic raw material.
本発明者は、鉛または鉛化合物を含有する水酸化マグネシウムを、ハロゲン化物もしくはハロゲンガスであるハロゲン源の存在下に焼成すると、酸化マグネシウム１モル中のＰｂ含有量が２×１０-7モル以下（好ましくは１×１０-7モル以下、さらに好ましくは０．５×１０-7モル以下）の酸化マグネシウムを得ることができることを見出した。 The present inventors have found that when magnesium hydroxide containing lead or a lead compound is calcined in the presence of a halogen source, which is a halide or a halogen gas, the Pb content in 1 mol of magnesium oxide is 2 × 10 −7 mol or less. (Preferably 1 × 10 −7 mol or less, more preferably 0.5 × 10 −7 mol or less) magnesium oxide can be obtained.
従って、本発明は、Ｐｂ含有量が２×１０-7モル／モル以下（質量基準に換算して１．０質量ｐｐｍ以下に相当する）である酸化マグネシウムにある。 Therefore, the present invention resides in magnesium oxide having a Pb content of 2 × 10 −7 mol / mol or less (corresponding to 1.0 mass ppm or less in terms of mass).
本発明はまた、肥料用、医薬品原料用又は化粧品原料用である酸化マグネシウム１モル中のＰｂ含有量が２×１０-7モル／モル以下の酸化マグネシウムにもある。 The present invention also resides in magnesium oxide having a Pb content of 2 × 10 −7 mol / mol or less per 1 mol of magnesium oxide for fertilizers, pharmaceutical raw materials, or cosmetic raw materials.
本発明の酸化マグネシウムの好ましい態様は、次の通りである。
（１）鉛または鉛化合物を含有する水酸化マグネシウムを、ハロゲン化物もしくはハロゲンガスであるハロゲン源の存在下に焼成して得たものである。
（２）Ｐｂ含有量が１×１０-7モル／モル以下（質量基準に換算して０．５質量ｐｐｍ以下に相当する）である。
（３）Ｐｂ含有量が０．５×１０-7モル／モル以下（質量基準に換算して０．２６質量ｐｐｍ以下に相当する）である。
Preferred embodiments of the magnesium oxide of the present invention are as follows.
(1) It is obtained by firing magnesium hydroxide containing lead or a lead compound in the presence of a halogen source, which is a halide or a halogen gas.
(2) The Pb content is 1 × 10 −7 mol / mol or less (corresponding to 0.5 mass ppm or less in terms of mass).
(3) The Pb content is 0.5 × 10 −7 mol / mol or less (corresponding to 0.26 mass ppm or less in terms of mass).
本発明の酸化マグネシウムは、Ｐｂ含有量が少ないので肥料用、医薬品原料用又は化粧品原料用として有用である。また、本発明の酸化マグネシウムは、鉛または鉛化合物を含有する水酸化マグネシウムをハロゲン源の存在下にて焼成することによって製造することができる。従って、本発明の酸化マグネシウムは工業的に容易に製造することができる。 Since the magnesium oxide of the present invention has a low Pb content, it is useful as a fertilizer, a pharmaceutical raw material, or a cosmetic raw material. The magnesium oxide of the present invention can be produced by firing magnesium hydroxide containing lead or a lead compound in the presence of a halogen source. Therefore, the magnesium oxide of the present invention can be easily produced industrially.
海水に水酸化カルシウムを加えて水酸化マグネシウムを生成させ、これをろ過、乾燥して、得られた水酸化マグネシウムには海水の主成分である塩化ナトリウムなどのハロゲン化物が存在する。
一般的に、ハロゲン化物が存在する水酸化マグネシウムを焼成すると、焼成炉が劣化しやすくなり、さらには得られた酸化マグネシウムはその純度が低くなったり、塩分が多くなりやすくなる。従って、通常水酸化マグネシウムを焼成して酸化マグネシウムを製造する場合、水酸化マグネシウムは重金属を含まない水で洗浄し、ハロゲン化物の存在量を低減した後焼成する。
Calcium hydroxide is added to seawater to produce magnesium hydroxide, which is filtered and dried, and the resulting magnesium hydroxide contains a halide, such as sodium chloride, which is a main component of seawater.
Generally, when magnesium hydroxide containing a halide is calcined, the calcining furnace is easily deteriorated, and the obtained magnesium oxide is liable to have a low purity or a high salt content. Therefore, in the case of producing magnesium oxide by calcination of magnesium hydroxide, the magnesium hydroxide is washed with water containing no heavy metal to reduce the amount of halides, and then calcined.
しかしながら、本発明者らは、水酸化マグネシウムを、ハロゲン化物もしくはハロゲンガスであるハロゲン源の存在下にて焼成することにより、酸化マグネシウムのＰｂ含有量が低減することを見出した。酸化マグネシウムのＰｂ含有量が低減する明確な理由は不明であるが、鉛化合物が沸点の低いハロゲン化鉛に変化して蒸発しやすくなる。あるいは、水酸化マグネシウムにハロゲン化物を存在させることにより鉛化合物自体の沸点が下がることなどが推定される。 However, the present inventors have found that calcining magnesium hydroxide in the presence of a halide or a halogen gas, which is a halogen gas, reduces the Pb content of magnesium oxide. Although the clear reason why the Pb content of magnesium oxide is reduced is unknown, the lead compound changes to lead halide having a low boiling point and is easily evaporated. Alternatively, it is estimated that the presence of a halide in magnesium hydroxide lowers the boiling point of the lead compound itself.
本発明において、ハロゲン源は、ハロゲン化物である塩化物、臭化物が好ましく、その例としては、塩化ナトリウム、塩化マグネシウム、臭化ナトリウム、臭化マグネシウムなどが挙げられる。ハロゲン化物は有機物であっても良い。
ハロゲン源は、ハロゲン化物の気体あるいはハロゲンガスであっても良く、ハロゲン化物の気体の例としては、塩化水素ガス、臭化水素ガスなどが挙げられる。また、ハロゲンガスの例としては、塩素ガス、臭素ガスが挙げられる。
In the present invention, the halogen source is preferably a halide such as chloride or bromide, and examples thereof include sodium chloride, magnesium chloride, sodium bromide, and magnesium bromide. The halide may be organic.
The halogen source may be a halide gas or a halogen gas, and examples of the halide gas include hydrogen chloride gas and hydrogen bromide gas. Examples of the halogen gas include chlorine gas and bromine gas.
ハロゲン源の存在量は、ハロゲン源としてハロゲン化物を用いた場合には、水酸化マグネシウム１モルに対して、２×１０-4〜４×１０-2モルの範囲内の量で存在させることが好ましく、より好ましくは、６×１０-4〜２×１０-2モルの範囲内の量である。ハロゲン源の量が少なすぎると、鉛または鉛化合物の除去が不十分になり、またハロゲン源の量が多すぎると、上述したように、焼成炉が劣化しやすくなり、さらには得られた酸化マグネシウムの純度が低くなったり、塩分が多くなる。 When a halide is used as the halogen source, the halogen source may be present in an amount within the range of 2 × 10 −4 to 4 × 10 −2 mol per mol of magnesium hydroxide. Preferably, the amount is in the range of 6 × 10 −4 to 2 × 10 −2 mol. If the amount of the halogen source is too small, the removal of lead or lead compounds will be insufficient, and if the amount of the halogen source is too large, as described above, the firing furnace tends to deteriorate, and further, the obtained oxidation Magnesium has low purity and high salt content.
本発明において、水酸化マグネシウムにハロゲン源を存在させる方法は、ハロゲン源としてハロゲン化物を用いた場合には、水酸化マグネシウムにハロゲン化物の固体を混合しても、互いに相対する量のハロゲン化物を含有する水酸化マグネシウムを混合しても、あるいは水酸化マグネシウムにハロゲン化物を含む溶液を混合しても良い。ハロゲン化物を含む溶液として、海水あるいは水酸化マグネシウムを生成させ、ろ過したときに発生するろ液を使用しても良い。 In the present invention, the method of causing the halogen source to be present in magnesium hydroxide is such that, when a halide is used as the halogen source, even if a solid of the halide is mixed with the magnesium hydroxide, the halides in opposite amounts to each other are mixed. The magnesium hydroxide contained therein may be mixed, or a solution containing a halide may be mixed with magnesium hydroxide. As a solution containing a halide, a filtrate generated when seawater or magnesium hydroxide is generated and filtered may be used.
また、ハロゲン源としてハロゲン化物の気体あるいはハロゲンガスを用いる場合には、焼成炉中にハロゲン化物の気体あるいはハロゲンガスを循環させても、加熱することによりハロゲン化物の気体あるいはハロゲンガスを発生する化合物の液体あるいは固体を焼成炉中に供給して、水酸化マグネシウムの焼成中に気化させても良い。加熱することによりハロゲン化物の気体を発生する化合物として、臭化エチレンなどを使用することができる。 When a halide gas or a halogen gas is used as a halogen source, a compound that generates a halide gas or a halogen gas by heating even if the halide gas or the halogen gas is circulated in a firing furnace. The liquid or solid may be supplied into a firing furnace to be vaporized during firing of magnesium hydroxide. Ethylene bromide or the like can be used as a compound that generates a halide gas by heating.
（水酸化マグネシウムケ−クの製造）
海水１ｍ3 に対し、水酸化カルシウムを３．５ｋｇ加えて、水酸化マグネシウムを生成させた後、これを水で洗浄した後、減圧ろ過して、含水率４０％の水酸化マグネシウムケークを作成した。得られた水酸化マグネシウムケークに含まれているＰｂ含有量を偏光ゼーマン型原子吸光分析法により定量したところ、Ｐｂ含有量は水酸化マグネシウム１モルに対して、２．８×１０-7モルであった。なお、得られた水酸化マグネシウムケークに含まれているハロゲン化物の量は水酸化マグネシウム１モルに対して１．５×１０-4モル以下であった。
(Production of magnesium hydroxide cake)
3.5 kg of calcium hydroxide was added to 1 m 3 of seawater to produce magnesium hydroxide, which was washed with water and filtered under reduced pressure to prepare a magnesium hydroxide cake having a water content of 40%. . When the Pb content contained in the obtained magnesium hydroxide cake was quantified by polarized Zeeman-type atomic absorption spectrometry, the Pb content was 2.8 × 10 -7 mol per 1 mol of magnesium hydroxide. there were. The amount of halide contained in the obtained magnesium hydroxide cake was 1.5 × 10 −4 mol or less per 1 mol of magnesium hydroxide.
（実施例１）
上記の水酸化マグネシウムケークに粉末の塩化ナトリウムを、水酸化マグネシウム（固形分）１モルに対して、塩化ナトリウムが３．３×１０-3モルになるように加えて、混合した後１２０℃で１２時間乾燥して、次いで９００℃で１時間焼成して、酸化マグネシウムを製造した。
(Example 1)
Powdered sodium chloride was added to the above magnesium hydroxide cake, and sodium chloride was added in an amount of 3.3 × 10 −3 mol with respect to 1 mol of magnesium hydroxide (solid content). It was dried for 12 hours and then calcined at 900 ° C. for 1 hour to produce magnesium oxide.
（実施例２）
実施例１において、塩化ナトリウムを水酸化マグネシウム１モルに対して、１．１×１０-2モルになるように加えた以外は、実施例１と同一の条件で、酸化マグネシウムを製造した。
(Example 2)
Magnesium oxide was produced under the same conditions as in Example 1 except that sodium chloride was added in an amount of 1.1 × 10 -2 mol per 1 mol of magnesium hydroxide.
（比較例１）
実施例１において、塩化ナトリウムを加えない以外は実施例１と同一の条件で、酸化マグネシウムを製造した。
(Comparative Example 1)
In Example 1, magnesium oxide was produced under the same conditions as in Example 1 except that sodium chloride was not added.
（比較例２）
実施例１において、焼成温度を５５０℃とした以外は実施例１と同一の条件で、酸化マグネシウムを製造した。
(Comparative Example 2)
In Example 1, magnesium oxide was produced under the same conditions as in Example 1 except that the firing temperature was 550 ° C.
（評価）
上記のようにして得た酸化マグネシウムのＰｂ含有量を、偏光ゼーマン型原子吸光分析法により定量した。その結果を表１に示す。
(Evaluation)
The Pb content of the magnesium oxide obtained as described above was quantified by polarized Zeeman-type atomic absorption spectrometry. Table 1 shows the results.
表１
─────────────────────────────
酸化マグネシウム１モル
に対するＰｂ含有量（モル）
─────────────────────────────
実施例１ ７．４×１０-8
実施例２ １．９×１０-8
─────────────────────────────
比較例１ ２．８×１０-7
比較例２ ２．８×１０-7
─────────────────────────────
Table 1
─────────────────────────────
1 mol of magnesium oxide
Pb content (mol) with respect to
─────────────────────────────
Example 1 7.4 × 10 −8
Example 2 1.9 × 10 −8
─────────────────────────────
Comparative Example 1 2.8 × 10 -7
Comparative Example 2 2.8 × 10 -7
─────────────────────────────
Claims (7)
7. The magnesium oxide according to claim 6, wherein the Pb content is 0.5 × 10 −7 mol / mol or less.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006036544A (en) * | 2004-07-22 | 2006-02-09 | National Institute For Materials Science | Method for producing cubic magnesia powder |
| WO2008093565A1 (en) * | 2007-01-30 | 2008-08-07 | Tateho Chemical Industries Co., Ltd. | Cubic magnesium oxide powder and method for producing the same |
| JP2009242165A (en) * | 2008-03-31 | 2009-10-22 | Tateho Chem Ind Co Ltd | High-purity magnesium hydroxide powder and high-purity magnesium oxide powder |
| JP2012211078A (en) * | 2012-06-15 | 2012-11-01 | Tateho Chemical Industries Co Ltd | Highly pure magnesium oxide powder |
| KR20190032624A (en) | 2017-02-24 | 2019-03-27 | 가부시키가이샤 미야모토 세이사쿠쇼 | Fertilizer for plant cultivation comprising laundry wastewater, plant cultivation method using the fertilizer, and method for using laundry wastewater as fertilizer for plant cultivation |
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| JP2012211078A (en) * | 2012-06-15 | 2012-11-01 | Tateho Chemical Industries Co Ltd | Highly pure magnesium oxide powder |
| KR20190032624A (en) | 2017-02-24 | 2019-03-27 | 가부시키가이샤 미야모토 세이사쿠쇼 | Fertilizer for plant cultivation comprising laundry wastewater, plant cultivation method using the fertilizer, and method for using laundry wastewater as fertilizer for plant cultivation |
| JP2021502941A (en) * | 2017-09-15 | 2021-02-04 | レフラテクニック ホルディング ゲゼルシャフト ミット ベシュレンクテル ハフツングＲＥＦＲＡＴＥＣＨＮＩＫ Ｈｏｌｄｉｎｇ ＧｍｂＨ | A method for producing a porous sintered magnesia, a batch for producing a crude ceramic (grobkeramisch) refractory product having a granulated product (Koernung) made of sintered magnesia, such a product, and a product. Method of manufacture, lining of industrial furnace (Zustellung), and industrial furnace |
| US11440847B2 (en) | 2017-09-15 | 2022-09-13 | Refratechnik Holding Gmbh | Method for producing a porous sintered magnesia, backfill for producing a heavy-clay refractory product with a granulation from the sintered magnesia, product of this type, and method for the production thereof, lining of an industrial furnace and industrial furnace |
| JP7299157B2 (en) | 2017-09-15 | 2023-06-27 | レフラテクニック ホルディング ゲゼルシャフト ミット ベシュレンクテル ハフツング | A method for producing porous sintered magnesia, a batch for producing a coarse ceramic refractory product with granules of sintered magnesia, such a product and the product Manufacturing method, industrial furnace lining (Zustellung) and industrial furnace |
| WO2023145548A1 (en) * | 2022-01-28 | 2023-08-03 | 宇部マテリアルズ株式会社 | Magnesium oxide particles and production method thereof |
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