JP5274892B2 - Method for producing fibrous basic magnesium sulfate particles - Google Patents
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- JP5274892B2 JP5274892B2 JP2008131979A JP2008131979A JP5274892B2 JP 5274892 B2 JP5274892 B2 JP 5274892B2 JP 2008131979 A JP2008131979 A JP 2008131979A JP 2008131979 A JP2008131979 A JP 2008131979A JP 5274892 B2 JP5274892 B2 JP 5274892B2
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- magnesium sulfate
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- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 title claims abstract description 178
- 229910052943 magnesium sulfate Inorganic materials 0.000 title claims abstract description 89
- 235000019341 magnesium sulphate Nutrition 0.000 title claims abstract description 89
- 239000002245 particle Substances 0.000 title claims abstract description 80
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000006185 dispersion Substances 0.000 claims abstract description 33
- 239000000835 fiber Substances 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 18
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000009835 boiling Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 abstract description 4
- 239000007787 solid Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000012779 reinforcing material Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- WRUGWIBCXHJTDG-UHFFFAOYSA-L magnesium sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Mg+2].[O-]S([O-])(=O)=O WRUGWIBCXHJTDG-UHFFFAOYSA-L 0.000 description 1
- 229940061634 magnesium sulfate heptahydrate Drugs 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
本発明は、繊維状塩基性硫酸マグネシウム粒子の製造方法に関するものである。 The present invention relates to a method for producing fibrous basic magnesium sulfate particles.
塩基性硫酸マグネシウム［ＭｇＳＯ4・５Ｍｇ（ＯＨ）2・３Ｈ2Ｏ］の繊維状粒子は、紙、樹脂及びゴムなどの強化材料、あるいはろ過材の原料として利用されている。 Fibrous particles of basic magnesium sulfate [MgSO 4 .5Mg (OH) 2 .3H 2 O] are used as reinforcing materials such as paper, resin and rubber, or as raw materials for filter media.
繊維状塩基性硫酸マグネシウム粒子の製造方法として、特許文献１には、硫酸マグネシウム水溶液に水酸化マグネシウムまたは酸化マグネシウムをその濃度が２５質量％以下になるように分散させた後、１００〜３００℃、好ましくは１２０〜３００℃の温度で水熱反応させる方法が開示されている。この特許文献の実施例では、平均繊維径が０．５〜１．０μｍの繊維状塩基性硫酸マグネシウム粒子が得られている。 As a method for producing fibrous basic magnesium sulfate particles, Patent Document 1 discloses that magnesium hydroxide or magnesium oxide is dispersed in a magnesium sulfate aqueous solution so that its concentration is 25% by mass or less, and then 100 to 300 ° C., A method of hydrothermal reaction at a temperature of preferably 120 to 300 ° C. is disclosed. In the examples of this patent document, fibrous basic magnesium sulfate particles having an average fiber diameter of 0.5 to 1.0 μm are obtained.
特許文献２には、水熱反応を特には必要としない繊維状塩基性硫酸マグネシウム粒子の製造方法として、可溶性硫酸塩含有水溶液に酸化マグネシウム粉末を分散させた分散液を、好ましくは常圧下６０℃以上、沸点以下の温度で、加熱反応させて、繭状塩基性硫酸マグネシウムを生成させ、次いで該繭状生成物に強力剪断力を作用させて解砕する方法が開示されている。この特許文献の実施例では、繊維径が最も細いもので０．２〜０．３μｍの繊維状塩基性硫酸マグネシウム粒子が得られている。
樹脂材料の補強材料として用いる繊維状塩基性硫酸マグネシウムは、細い繊維の方が、太い繊維よりも樹脂の弾性率を向上させる効果が大きく好ましい。しかしながら、前記特許文献１に記載されている水熱合成法を利用して繊維状塩基性硫酸マグネシウム粒子を製造すると、繊維径が０．４μｍ以下の細い繊維状粒子を得ることは難しい。一方、前記特許文献２には繊維径が０．２〜０．３μｍの繊維状塩基性硫酸マグネシウム粒子が開示されている。しかしながら、前記特許文献２に開示されている繊維状塩基性硫酸マグネシウム粒子の製造方法は、繭状塩基性硫酸マグネシウムを解砕する工程が必要となるという問題がある。
従って、本発明の目的は、解砕工程などの煩雑な工程を必要としないで繊維径が０．４μｍ以下の繊維状塩基性硫酸マグネシウム粒子を製造することができる方法を提供することにある。
In the case of fibrous basic magnesium sulfate used as a reinforcing material for a resin material, a thin fiber is preferable because it has a larger effect of improving the elastic modulus of the resin than a thick fiber. However, when fibrous basic magnesium sulfate particles are produced using the hydrothermal synthesis method described in Patent Document 1, it is difficult to obtain fine fibrous particles having a fiber diameter of 0.4 μm or less. On the other hand, Patent Document 2 discloses fibrous basic magnesium sulfate particles having a fiber diameter of 0.2 to 0.3 μm. However, the method for producing fibrous basic magnesium sulfate particles disclosed in Patent Document 2 has a problem in that a step of crushing caged basic magnesium sulfate is required.
Accordingly, an object of the present invention is to provide a method capable of producing fibrous basic magnesium sulfate particles having a fiber diameter of 0.4 μm or less without requiring complicated steps such as a crushing step.
本発明者は、硫酸マグネシウム水溶液に、繊維状塩基性硫酸マグネシウム種粒子と水酸化マグネシウム粒子とが分散されている分散液を、常圧下、５０℃以上、かつ該分散液の沸点以下の温度にて加熱反応させる事により、加圧条件下での反応と比較して細い繊維状塩基性硫酸マグネシウム粒子を解砕工程を必要とせずに製造することが可能となることを見出した。 The present inventor has prepared a dispersion in which fibrous basic magnesium sulfate seed particles and magnesium hydroxide particles are dispersed in an aqueous magnesium sulfate solution at a temperature not lower than 50 ° C. and not higher than the boiling point of the dispersion under normal pressure. It was found that, by heating and reacting, fine fibrous basic magnesium sulfate particles can be produced without the need for a crushing step as compared with the reaction under pressure.
従って、本発明は、硫酸マグネシウム水溶液に、繊維状塩基性硫酸マグネシウム種粒子と水酸化マグネシウム粒子とが分散されている分散液を、常圧下、５０℃以上、かつ該分散液の沸点以下の温度に加熱することによって、水の存在下での硫酸マグネシウムと水酸化マグネシウム粒子との反応で生成する塩基性硫酸マグネシウムを前記繊維状塩基性硫酸マグネシウム種粒子の表面に析出させ、次いで該分散液から繊維状塩基性硫酸マグネシウム粒子を取り出すことからなる平均繊維径が０．４μｍ以下である繊維状塩基性硫酸マグネシウム粒子の製造方法にある。 Accordingly, the present invention provides a dispersion in which fibrous basic magnesium sulfate seed particles and magnesium hydroxide particles are dispersed in an aqueous magnesium sulfate solution at a temperature not lower than 50 ° C. and not higher than the boiling point of the dispersion under normal pressure. Is heated to precipitate the basic magnesium sulfate produced by the reaction of magnesium sulfate and magnesium hydroxide particles in the presence of water on the surface of the fibrous basic magnesium sulfate seed particles. It exists in the manufacturing method of the fibrous basic magnesium sulfate particle | grains whose average fiber diameter which consists of taking out a fibrous basic magnesium sulfate particle | grain is 0.4 micrometer or less.
本発明の繊維状塩基性硫酸マグネシウム粒子の製造方法の好ましい態様は、次の通りである。
（１）分散液中の加熱前の繊維状塩基性硫酸マグネシウム種粒子量が、分散液中の硫酸マグネシウムと水酸化マグネシウム粒子との反応で生成する塩基性硫酸マグネシウムの理論量と繊維状塩基性硫酸マグネシウム種粒子量との合計量に対して１〜９０質量％の範囲となる量である。
（２）分散液中の加熱前の硫酸マグネシウム量が０．５〜４０質量％である。
（３）分散液中の加熱前の水酸化マグネシウム粒子量が、硫酸マグネシウム量１モルに対して０．０１〜５．０モルの範囲となる量である。
（４）分散液の加熱前のｐＨが６．９〜８．８の範囲にある。
The preferable aspect of the manufacturing method of the fibrous basic magnesium sulfate particle | grains of this invention is as follows.
(1) The amount of fibrous basic magnesium sulfate seed particles before heating in the dispersion is the theoretical amount and basic basicity of basic magnesium sulfate produced by the reaction of magnesium sulfate and magnesium hydroxide particles in the dispersion. The amount is in the range of 1 to 90% by mass with respect to the total amount with the magnesium sulfate seed particle amount.
(2) The amount of magnesium sulfate before heating in the dispersion is 0.5 to 40% by mass.
(3) The amount of magnesium hydroxide particles before heating in the dispersion is an amount that is in the range of 0.01 to 5.0 mol with respect to 1 mol of magnesium sulfate.
(4) The pH of the dispersion before heating is in the range of 6.9 to 8.8.
本発明の製造方法を利用することによって、平均繊維径が０．４μｍ以下の繊維径が細い繊維状塩基性硫酸マグネシウム粒子を工業的に有利に製造することができる。 By using the production method of the present invention, fibrous basic magnesium sulfate particles having an average fiber diameter of 0.4 μm or less and a thin fiber diameter can be advantageously produced industrially.
本発明では、先ず、硫酸マグネシウム水溶液に、繊維状塩基性硫酸マグネシウム種粒子と水酸化マグネシウム粒子とが分散されている分散液を用意する。 In the present invention, first, a dispersion in which fibrous basic magnesium sulfate seed particles and magnesium hydroxide particles are dispersed in a magnesium sulfate aqueous solution is prepared.
上記分散液に分散されている繊維状塩基性硫酸マグネシウム種粒子は、平均繊維径が０．３０〜０．６０μｍの範囲にあって、平均繊維長さが８〜３０μｍの範囲にあることが好ましい。種粒子となる繊維状塩基性硫酸マグネシウム粒子は、従来の水熱法を利用して製造したものを使用することができる。また、水熱法を利用して製造した繊維状塩基性硫酸マグネシウム粒子を種粒子に用い、本発明の方法に従って、常圧で合成した繊維状塩基性硫酸マグネシウム粒子を種粒子に用いることもできる。種粒子の繊維径が細い方が、得られる繊維状塩基性硫酸マグネシウム粒子の繊維径は細くなる傾向にある。分散液中の種粒子量は、分散液中の硫酸マグネシウムと水酸化マグネシウム粒子との反応で生成する塩基性硫酸マグネシウムの理論量と繊維状塩基性硫酸マグネシウム種粒子量との合計量に対して１〜９０質量％の範囲となる量であることが好ましい。 The fibrous basic magnesium sulfate seed particles dispersed in the dispersion preferably have an average fiber diameter in the range of 0.30 to 0.60 μm and an average fiber length in the range of 8 to 30 μm. . What was manufactured using the conventional hydrothermal method can be used for the fibrous basic magnesium sulfate particle used as a seed particle. Further, fibrous basic magnesium sulfate particles produced using a hydrothermal method can be used as seed particles, and fibrous basic magnesium sulfate particles synthesized at normal pressure can be used as seed particles according to the method of the present invention. . The fiber diameter of the obtained fibrous basic magnesium sulfate particles tends to be narrower as the fiber diameter of the seed particles is smaller. The amount of seed particles in the dispersion is based on the total amount of the theoretical amount of basic magnesium sulfate produced by the reaction of magnesium sulfate and magnesium hydroxide particles in the dispersion and the amount of fibrous basic magnesium sulfate seed particles. It is preferable that it is the quantity used as the range of 1-90 mass%.
分散液中の硫酸マグネシウム量は０．５〜４０質量％にあることが好ましい。 The amount of magnesium sulfate in the dispersion is preferably 0.5 to 40% by mass.
水酸化マグネシウム粒子は、平均粒子径が０．１〜１０μｍの範囲にあることが好ましい。分散液中の水酸化マグネシウム粒子量は、硫酸マグネシウム量１モルに対して０．０１〜５．０モルの範囲となる量であることが好ましい。 The magnesium hydroxide particles preferably have an average particle diameter in the range of 0.1 to 10 μm. The amount of magnesium hydroxide particles in the dispersion is preferably in the range of 0.01 to 5.0 moles per mole of magnesium sulfate.
分散液のｐＨは６．９〜８．８の範囲にあることが好ましい。 The pH of the dispersion is preferably in the range of 6.9 to 8.8.
本発明では、上記の分散液を、常圧下、５０℃以上、かつ該分散液の沸点以下の温度に加熱する。この加熱によって、水の存在下での硫酸マグネシウムと水酸化マグネシウム粒子との反応により塩基性硫酸マグネシウムが生成し、繊維状塩基性硫酸マグネシウム種粒子の表面に析出して、種粒子は成長する。本発明の方法では従来の水熱法と比較して、種粒子が長さ方向に先細って成長するため、長く成長した粒子が折れるなどにより、繊維径の細い粒子が生成して、種粒子よりも平均粒子径の細い繊維状塩基性硫酸マグネシウム粒子が生成すると考えられる。 In the present invention, the above dispersion is heated to a temperature of 50 ° C. or higher and a boiling point or lower of the dispersion under normal pressure. By this heating, basic magnesium sulfate is generated by the reaction between magnesium sulfate and magnesium hydroxide particles in the presence of water, and is precipitated on the surface of the fibrous basic magnesium sulfate seed particles, so that the seed particles grow. In the method of the present invention, the seed particles grow in a taper direction in comparison with the conventional hydrothermal method, so that particles with a small fiber diameter are generated due to breakage of the long-grown particles, and so on. It is considered that fibrous basic magnesium sulfate particles having an average particle diameter smaller than that are formed.
分散液の加熱温度は、９０℃以上であることが好ましく、特に９５℃以上であることが好ましい。加熱は分散液を撹拌しながら行なうことが好ましい。加熱時間は、一般に０．５〜２０時間の範囲である。 The heating temperature of the dispersion is preferably 90 ° C. or higher, and particularly preferably 95 ° C. or higher. Heating is preferably performed while stirring the dispersion. The heating time is generally in the range of 0.5 to 20 hours.
加熱後の分散液中の繊維状塩基性硫酸マグネシウム粒子は、ろ過、デカンテーション及び遠心分離などの公知の固液分離法を用いて回収することができる。回収した繊維状塩基性硫酸マグネシウム粒子は、通常は水洗して、残留する硫酸マグネシウム分を除いた後に乾燥を行なう。 The fibrous basic magnesium sulfate particles in the dispersion after heating can be recovered using a known solid-liquid separation method such as filtration, decantation, and centrifugation. The recovered fibrous basic magnesium sulfate particles are usually washed with water to remove the remaining magnesium sulfate and then dried.
上記のようにして得られる繊維状塩基性硫酸マグネシウム粒子は、通常は、平均繊維径が０．１〜０．４μｍの範囲にあって、平均繊維長さが８〜３０μｍの範囲にある。この繊維状塩基性硫酸マグネシウム粒子は、樹脂及びゴムなどの強化材料、あるいはろ過材の原料として利用することができる。 The fibrous basic magnesium sulfate particles obtained as described above usually have an average fiber diameter in the range of 0.1 to 0.4 μm and an average fiber length in the range of 8 to 30 μm. The fibrous basic magnesium sulfate particles can be used as a reinforcing material such as resin and rubber, or a raw material for a filter medium.
［実施例１］
水道水６５５．８ｇに硫酸マグネシウム七水塩４９１．４ｇを溶解し、硫酸マグネシウム水溶液を１１４７ｇ調製した。次に、硫酸マグネシウム水溶液を撹拌しながら、該水溶液に平均繊維長が１５．８μｍ、平均繊維径が０．５０μｍの繊維状塩基性硫酸マグネシウム粒子（モスハイジ粉状物、宇部マテリアルズ（株）製）３．６ｇを種晶として加えた。さらに、該水溶液に宇部マテリアルズ製の水酸化マグネシウムスラリー（濃度：３４．６質量％）を６９．０ｇ加えて、ｐＨが８．４の混合物を調製した。
この混合物を、内容積１Ｌのヒータと撹拌機とを備えた反応容器に投入し、混合物を撹拌機で撹拌しながら、ヒータで混合物の温度を約１００℃に加熱した。混合物の加熱を開始してから混合物のｐＨは徐々に低下し、３００分経過後にはｐＨは７．０にまで低下した。
[Example 1]
491.4 g of magnesium sulfate heptahydrate was dissolved in 655.8 g of tap water to prepare 1147 g of an aqueous magnesium sulfate solution. Next, while stirring the magnesium sulfate aqueous solution, fibrous basic magnesium sulfate particles having an average fiber length of 15.8 μm and an average fiber diameter of 0.50 μm (Moss Heidi powder, manufactured by Ube Materials Co., Ltd.) ) 3.6 g was added as seed crystals. Furthermore, 69.0 g of magnesium hydroxide slurry (concentration: 34.6% by mass) manufactured by Ube Materials was added to the aqueous solution to prepare a mixture having a pH of 8.4.
This mixture was put into a reaction vessel equipped with a 1 L heater and a stirrer, and the temperature of the mixture was heated to about 100 ° C. with a heater while stirring the mixture with a stirrer. The pH of the mixture gradually dropped after heating of the mixture was started, and after 300 minutes, the pH dropped to 7.0.
その後、反応容器から混合物を取り出して、ヌッチェにより吸引ろ過して固形分を回収した。固形物を該固形分に対して約６０質量倍の蒸留水で洗浄した。洗浄後、固形物を乾燥機にて１０５℃の温度で一晩乾燥した。得られた乾燥固形分のＸ線回折パターンを測定した結果、該Ｘ線回折パターンは塩基性硫酸マグネシウムのＸ線回折パターンと一致し、該乾燥固形分は塩基性硫酸マグネシウムであることが確認された。また、この塩基性硫酸マグネシウムを電子顕微鏡を用いて観察した結果、平均繊維長が１９．９μｍ、平均繊維径が０．３８μｍの繊維状塩基性硫酸マグネシウム粒子であり、原料の繊維状塩基性硫酸マグネシウム粒子よりも平均繊維径が細くなっていることが確認された。 Thereafter, the mixture was taken out from the reaction vessel, and suction filtered through a Nutsche to collect the solid content. The solid was washed with about 60 mass times distilled water with respect to the solid content. After washing, the solid was dried overnight at 105 ° C. in a dryer. As a result of measuring the X-ray diffraction pattern of the obtained dry solid, it was confirmed that the X-ray diffraction pattern coincided with the X-ray diffraction pattern of basic magnesium sulfate, and the dry solid was basic magnesium sulfate. It was. Further, as a result of observing the basic magnesium sulfate using an electron microscope, it was a fibrous basic magnesium sulfate particle having an average fiber length of 19.9 μm and an average fiber diameter of 0.38 μm. It was confirmed that the average fiber diameter was thinner than the magnesium particles.
［実施例２］
上記実施例１で得られた平均繊維長が１９．９μｍ、平均繊維径が０．３８μｍの繊維状塩基性硫酸マグネシウム粒子を種晶として用いたこと以外は、上記実施例１と同様の操作を行なって乾燥固形物を得た。
得られた乾燥固形分のＸ線回折パターンを測定した結果、該Ｘ線回折パターンは塩基性硫酸マグネシウムのＸ線回折パターンと一致し、該乾燥固形分は塩基性硫酸マグネシウムであることが確認された。また、この塩基性硫酸マグネシウム粒子を電子顕微鏡を用いて観察した結果、平均繊維長が２２．４μｍ、平均繊維径が０．３４μｍの繊維状塩基性硫酸マグネシウム粒子であり、原料の繊維状塩基性硫酸マグネシウム粒子よりも平均繊維径がさらに細くなっていることが確認された。
[Example 2]
The same operation as in Example 1 was performed except that fibrous basic magnesium sulfate particles having an average fiber length of 19.9 μm and an average fiber diameter of 0.38 μm obtained in Example 1 were used as seed crystals. And a dry solid was obtained.
As a result of measuring the X-ray diffraction pattern of the obtained dry solid, it was confirmed that the X-ray diffraction pattern coincided with the X-ray diffraction pattern of basic magnesium sulfate, and the dry solid was basic magnesium sulfate. It was. Moreover, as a result of observing the basic magnesium sulfate particles using an electron microscope, the basic magnesium sulfate particles are fibrous basic magnesium sulfate particles having an average fiber length of 22.4 μm and an average fiber diameter of 0.34 μm. It was confirmed that the average fiber diameter was thinner than that of the magnesium sulfate particles.
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