TW201343555A - 微細氫氧化鎂粒子 - Google Patents
微細氫氧化鎂粒子 Download PDFInfo
- Publication number
- TW201343555A TW201343555A TW102105181A TW102105181A TW201343555A TW 201343555 A TW201343555 A TW 201343555A TW 102105181 A TW102105181 A TW 102105181A TW 102105181 A TW102105181 A TW 102105181A TW 201343555 A TW201343555 A TW 201343555A
- Authority
- TW
- Taiwan
- Prior art keywords
- magnesium hydroxide
- hydroxide particles
- weight
- fine
- resin
- Prior art date
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 72
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 72
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 72
- 239000002245 particle Substances 0.000 title claims abstract description 71
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011163 secondary particle Substances 0.000 claims abstract description 19
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 17
- 238000004458 analytical method Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 48
- 239000002994 raw material Substances 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 17
- 239000011342 resin composition Substances 0.000 claims description 16
- 159000000003 magnesium salts Chemical class 0.000 claims description 10
- 229920003002 synthetic resin Polymers 0.000 claims description 10
- 239000000057 synthetic resin Substances 0.000 claims description 10
- 239000007822 coupling agent Substances 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 8
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 8
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 8
- 239000000194 fatty acid Substances 0.000 claims description 8
- 229930195729 fatty acid Natural products 0.000 claims description 8
- 150000004665 fatty acids Chemical class 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- 239000012756 surface treatment agent Substances 0.000 claims description 7
- 238000011282 treatment Methods 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229920000098 polyolefin Polymers 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 150000004645 aluminates Chemical class 0.000 claims description 3
- 235000021317 phosphate Nutrition 0.000 claims description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 2
- 238000004381 surface treatment Methods 0.000 claims description 2
- 239000013543 active substance Substances 0.000 claims 1
- 125000000129 anionic group Chemical group 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 239000002002 slurry Substances 0.000 description 20
- 239000010408 film Substances 0.000 description 18
- -1 alkali metal salts Chemical class 0.000 description 17
- 238000000034 method Methods 0.000 description 16
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 14
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 14
- 239000003063 flame retardant Substances 0.000 description 14
- 229920005989 resin Polymers 0.000 description 14
- 239000011347 resin Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000002105 nanoparticle Substances 0.000 description 10
- 238000009826 distribution Methods 0.000 description 9
- 238000005259 measurement Methods 0.000 description 9
- 239000010419 fine particle Substances 0.000 description 8
- 229910001629 magnesium chloride Inorganic materials 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 235000011121 sodium hydroxide Nutrition 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 239000000654 additive Substances 0.000 description 6
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- 238000001914 filtration Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
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- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 229920000459 Nitrile rubber Polymers 0.000 description 3
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000007983 Tris buffer Substances 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
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- QLZJUIZVJLSNDD-UHFFFAOYSA-N 2-(2-methylidenebutanoyloxy)ethyl 2-methylidenebutanoate Chemical compound CCC(=C)C(=O)OCCOC(=O)C(=C)CC QLZJUIZVJLSNDD-UHFFFAOYSA-N 0.000 description 2
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 2
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- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
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- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 2
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- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
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- 229920006244 ethylene-ethyl acrylate Polymers 0.000 description 2
- 239000005042 ethylene-ethyl acrylate Substances 0.000 description 2
- 239000005043 ethylene-methyl acrylate Substances 0.000 description 2
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- 239000011521 glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 150000002484 inorganic compounds Chemical class 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
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- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
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- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
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- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
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Abstract
本發明之目的在於提供一種具有奈米粒子級之粒徑、碳含量較少而白度較高、透明性較高之微細氫氧化鎂粒子及其製造方法。本發明係一種微細氫氧化鎂粒子,其藉由頻率分析而測得之平均二次粒徑為1~100 nm,且碳含量未滿0.9重量%。
Description
本發明係關於一種微細氫氧化鎂粒子及其製造方法。又,關於一種包含該粒子之樹脂組成物及由其形成之成形品。
氫氧化鎂粒子自古以來便為人所知,用於醫藥用途、工業用途之廣泛領域。例如,作為醫藥用途,有制酸劑、瀉藥及動物用藥劑等,作為工業用途,有調配於熱塑性樹脂中而對該樹脂賦予難燃性之難燃劑、含油廢水用吸附劑、排煙脫硫劑、排水中和劑及土質改良劑等。
近年來,業界謀求藉由進行作為難燃劑之氫氧化鎂之微粒子化及高分散化而提高難燃效果之技術。其原因在於:越為微粒子、分散性越良好,難燃效率越上升,可以較少之添加量獲得較高之難燃性。又,由於電子機器等之應用之小型化、薄膜化等亦向前發展,因此需要可對應之微粒子難燃劑。作為微粒子難燃劑之微粒子氫氧化鎂,提出有平均粒徑為10~1000 nm之氫氧化鎂微粒子(專利文獻1)。然而,該氫氧化鎂微粒子含有0.9重量%以上之碳量,對於樹脂組成物中之調配,雖然存在有利之情況,但不適合無需有機處理之調配系或需要氫氧化鎂純度之用途(玻璃等陶瓷中之添加劑、作為鎂源之原料等)。
另一方面,已知利用微反應器而製造奈米粒子,微反應
器係定義為反應場為邊長小於1 mm或500 μm之規模之化學反應裝置,並且認為其與以更大規模進行反應之其他裝置相比,於能量效率、反應速度、產率、安全性、溫度控制、高速且均勻之混合、濃度均勻性之提昇、規模放大之類的部分細微條件之控制能力方面優異。較細之Y字管之微反應器較有名,已知可合成奈米粒子,但由於反應場為微小空間,故而若為如氫氧化鎂粒子等般之晶析反應,則會引起配管堵塞,存在僅可以非常稀之濃度進行合成之缺點,而不適合無機化合物之晶析反應。但是,例如關於專利文獻2所示之強制薄膜式微反應器,其反應場為1~30 μm之非常微小之空間,藉由使圖3所示之裝置圖之下表面圓盤旋轉,利用離心力將所生成之奈米粒子排出至裝置外,藉此奈米粒子不會堵塞在裝置內,而可容易地以高濃度合成無機化合物奈米粒子。
(專利文獻1)日本專利特開2009-62214號
(專利文獻2)日本專利特開2009-131831號
本發明之目的在於提供一種具有奈米粒子級之粒徑、碳含量較少而白度較高、透明性較高之微細氫氧化鎂粒子及其製造方法。
本發明者對獲得奈米粒子級之微細氫氧化鎂粒子之方法進行了研究。結果發現:若於強制薄膜式微反應器中使鎂鹽水溶液與鹼性物質原料進行反應,則可獲得奈米粒子級之微細氫氧化鎂粒子,又,所獲得之粒子之碳含量極少、純度優異而白度較高,從而完
成本發明。
即,本發明係一種微細氫氧化鎂粒子,其藉由頻率分析而測得之平均二次粒徑為1~100 nm,且碳含量未滿0.9重量%。又,本發明係一種樹脂組成物,其含有100重量份之合成樹脂及1~95重量份之藉由頻率分析而測得之平均粒徑為1~100 nm、且碳含量未滿0.9重量%之微細氫氧化鎂粒子。又,本發明係一種由上述樹脂組成物形成之成形品。又,本發明係一種上述氫氧化鎂粒子之製造方法,其特徵在於:於反應場之間隙為1~30 μm之強制薄膜式微反應器中,使鎂鹽水溶液與鹼性物質原料進行反應。
本發明之微細氫氧化鎂粒子之平均二次粒徑(藉由頻率分析法而測定)為1~100 nm,較佳為10~90 nm,且不含碳,純度較高。本發明之微細氫氧化鎂粒子由於平均二次粒徑非常小,因此可期待應用於小型電子機器或薄膜等迄今為止次微米級之粒子無法適用之領域。又,由於粒子尺寸微細,故而透明性亦較高,亦可考慮用於需要透明性之領域。
又,本發明之微細氫氧化鎂粒子由於平均二次粒徑非常小,為100 nm以下,且白度較高(透明性較高),故而難燃效果高於先前之平均二次粒徑超過100 nm之氫氧化鎂,且可獲得透明性優異之成形品。
根據本發明之製造方法,可藉由使用鎂鹽水溶液與鹼性物質原料於強制薄膜式微反應器中進行反應而製造微細氫氧化鎂粒子。藉由粉碎而獲得之氫氧化鎂存在因與粉碎介質接觸而引起之污染,於添加包含有機物等之添加劑而獲得之氫氧化鎂中,此添加劑有
可能作為雜質而起作用,但由於本發明之微細氫氧化鎂粒子係由使用先前之氫氧化鎂原料之反應而合成,故而無污染,即便未添加添加劑,亦可獲得奈米粒子。又,於使用先前之反應容器之氫氧化鎂粒子的反應中,分散性較差而成為凝聚粒子,但於本發明之製造方法中,可獲得為微粒子且分散性良好之氫氧化鎂粒子。因此,於調配至樹脂中之情形時,亦顯示出較高之透明性。
1‧‧‧第1處理面
2‧‧‧第2處理面
3‧‧‧排出口
4‧‧‧旋轉圓盤
5‧‧‧固定圓盤
A‧‧‧鎂鹽水溶液
B‧‧‧鹼性物質
圖1係實施例2中所獲得之氫氧化鎂粒子之粒度分佈。
圖2係實施例2中所獲得之氫氧化鎂粒子之TEM圖像。
圖3係強制薄膜式微反應器之一例。
<微細氫氧化鎂粒子>
本發明之微細氫氧化鎂粒子之平均二次粒徑為1~100 nm,較佳為10~90 nm,更佳為15~90 nm。粒子之平均二次粒徑係藉由頻率分析進行測定。
本發明之微細氫氧化鎂粒子之碳含量未滿0.9重量%,較佳為未滿0.8重量%,更佳為未滿0.7重量%。
本發明之微細氫氧化鎂粒子可利用表面處理劑進行表面處理。作為表面處理劑,較佳為選自由高級脂肪酸類、鈦酸酯偶合劑、矽烷偶合劑、鋁酸酯偶合劑、多元醇與脂肪酸之磷酸酯類及陰離子系界面活性劑所組成之群中之至少一種。
作為高級脂肪酸類,可列舉:碳數10以上之脂肪酸、例如硬脂酸、油酸、芥子酸、棕櫚酸等及其鹼金屬鹽類。
作為鈦酸酯偶合劑,可列舉:三異硬脂醯基鈦酸異丙酯、三(二辛基焦磷醯氧基)鈦酸異丙酯、三(N-胺基乙基-胺基乙基)鈦酸異丙酯、十三烷基苯磺醯基鈦酸異丙酯等。
作為矽烷偶合劑,可列舉:乙烯基乙氧基矽烷、乙烯基-三(2-甲氧基)矽烷、γ-甲基丙烯醯氧丙基三甲氧基矽烷、γ-胺基丙基三甲氧基矽烷、β-(3,4-環氧環己基)乙基三甲氧基矽烷、γ-縮水甘油氧基-丙基三甲氧基矽烷、γ-巰基丙基三甲氧基矽烷等。
作為鋁酸酯偶合劑,可列舉乙醯烷氧基鋁酸二異丙酯等。
作為多元醇之磷酸酯類,可列舉硬脂醇與正磷酸之單酯或二酯或該等之混合物。
作為陰離子系界面活性劑,可列舉:醯胺鍵結脂肪族羧酸鹽、醯胺鍵結硫酸酯鹽、醯胺鍵結磺酸鹽、醯胺鍵結烷基芳基磺酸鹽、硬脂醇等高級醇之硫酸酯鹽、聚乙二醇醚之硫酸酯鹽、酯鍵結硫酸酯鹽、酯鍵結磺酸鹽、酯鍵結烷基芳基磺酸鹽、醚鍵結烷基芳基磺酸鹽等。
為了使用表面處理劑進行本發明之微細氫氧化鎂粒子之表面塗佈處理,可藉由本身公知之濕式法而實施。例如作為濕式法,只要於微細氫氧化鎂粒子之漿料中以液狀或乳膠狀添加該表面處理劑,並在約100℃為止之溫度下充分進行機械混合即可。作為乾式法,只要利用韓蘇混合機等混合機,於充分攪拌下以液狀、乳膠狀、固形狀添加表面處理劑,並於加熱或非加熱下充分地混合氫氧化鎂之粉末即可。表面處理劑之添加量可適當地選擇。
<樹脂組成物>
本發明之樹脂組成物相對於100重量份之合成樹脂,含有1~95重量份之藉由頻率分析而測得之平均粒徑為1~100 nm且碳含量未滿0.9重量%之微細氫氧化鎂粒子。
微細氫氧化鎂粒子之含量相對於100重量份之合成樹脂,較佳為5~90重量份,更佳為10~85重量份,進而較佳為15~85重量份。
合成樹脂只要為通常製成成形品而使用者即可,作為其例,可例示:聚乙烯、聚丙烯、乙烯/丙烯共聚合體、如聚丁烯、聚4-甲基-1-戊烯等C2~C8烯烴(α-烯烴)之聚合體或者共聚合體、該等烯烴與二烯之共聚合體類、乙烯-丙烯酸酯共聚合體、聚苯乙烯、ABS(Acrylonitrile-Butadiene-Styrene,丙烯腈-丁二烯-苯乙烯)樹脂、AAS(Acrylonitrile-Acrylic ester-Styrene,丙烯腈-丙烯酸酯-苯乙烯)樹脂、AS(Acrylonitrile-Styrene,丙烯腈-苯乙烯)樹脂、MBS(Methyl methacrylate-Butadiene-Styrene,甲基丙烯酸甲酯-丁二烯-苯乙烯)樹脂、乙烯/氯乙烯共聚合樹脂、乙烯乙酸乙烯酯共聚物樹脂、乙烯-氯乙烯-乙酸乙烯酯接枝聚合樹脂、偏二氯乙烯、聚氯乙烯、氯化聚乙烯、氯化聚丙烯、氯乙烯-丙烯共聚合體、乙酸乙烯酯樹脂、苯氧基樹脂、聚縮醛、聚醯胺、聚醯亞胺、聚碳酸酯、聚碸、聚苯醚、聚苯硫醚、聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯、甲基丙烯酸系樹脂等熱塑性樹脂。
作為該等熱塑性樹脂中之較佳例,有利用氫氧化鎂粒子之難燃效果、防熱劣化效果及機械強度保持特性優異之聚烯烴或其共聚合體。具體而言,為聚丙烯均聚物、乙烯丙烯共聚合體之類的聚丙烯系樹脂,高密度聚乙烯、低密度聚乙烯、直鏈狀低密度聚乙烯、超
低密度聚乙烯、EVA(Ethylene-Vinyl Acetate,乙烯-乙酸乙烯酯)樹脂、EEA(Ethylene-Ethyl Acrylate,乙烯-丙烯酸乙酯)樹脂、EMA(Ethylene-Methyl Acrylate,乙烯-丙烯酸甲酯)共聚合樹脂、EAA(Ethylene-Acrylic Acid,乙烯-丙烯酸)共聚合樹脂、超高分子量聚乙烯之類的聚乙烯系樹脂,及聚丁烯、聚4-甲基-1-戊烯等C2~C6之烯烴(α-乙烯)之聚合體或者共聚合體。
進而可例示:環氧樹脂、酚系樹脂、三聚氰胺樹脂、不飽和聚酯樹脂、醇酸樹脂、脲樹脂等熱硬化性樹脂及EPDM(Ethylene-Propylene-Diene Monomer,乙烯-丙烯-二烯單體)、丁基橡膠、異戊二烯橡膠、SBR(Styrene Butadiene Rubber,苯乙烯-丁二烯橡膠)、NBR(Nitrile Butadiene Rubber,丁腈橡膠)、氯磺化聚乙烯、NIR(Nitrile-Isoprene Rubber,丙烯腈-異戊二烯橡膠)、胺基甲酸酯橡膠、丁二烯橡膠、丙烯酸系橡膠、聚矽氧橡膠、氟橡膠等合成橡膠。合成樹脂較佳為聚烯烴或其共聚合體。
本發明之樹脂組成物實質上係由上述合成樹脂及微細氫氧化鎂粒子所形成,但可進一步調配難燃助劑。藉由調配該難燃助劑,可降低微細氫氧化鎂粒子之調配比例,又,可增大難燃效果。
作為難燃助劑,較佳為紅磷、碳粉末或該等之混合物。作為紅磷,除難燃劑用之通常之紅磷以外,例如可使用藉由熱硬化性樹脂、聚烯烴、羧酸聚合體、氧化鈦或鈦鋁縮合物進行表面被覆之紅磷。又,作為碳粉末,可列舉碳黑、活性碳或石墨,作為該碳黑,可為藉由油爐(oil furnace)法、煤氣爐(gas furnace)法、導槽法、熱法或乙炔法中之任一方法而製備者。
難燃助劑之含量相對於100重量份之合成樹脂,較佳為
0.1~20重量份,更佳為0.5~15重量份。
本發明之樹脂組成物可調配其他添加劑。例如可例示:抗氧化劑、防靜電劑、顏料、發泡劑、塑化劑、填充劑、補強材、有機鹵素難燃劑、交聯劑、光安定劑、紫外線吸收劑、滑劑等。
<成形品>
本發明包含由上述樹脂組成物所形成之成形品。作為成形品,可列舉:電線、電纜、散熱片材、印刷配線基板、半導體密封劑等電子電氣機器用零件、家電零件、汽車零件、玻璃製品、陶瓷製品等。
<微細氫氧化鎂粒子之製造方法>
本發明之微細氫氧化鎂粒子可於反應場之間隙為1~30 μm之強制薄膜式微反應器中,使鎂鹽水溶液與鹼性物質原料進行反應而製造。
本發明之微細氫氧化鎂粒子之製造可使用M-technique股份有限公司製造之微反應器ULREA SS-11。該裝置具備於反應場之間隙為1~30 μm之強制薄膜式微反應器中,藉由使圓盤旋轉而排出晶析之氫氧化鎂漿料之機構。其係於圓盤內進行晶析反應後,立即排出至裝置外之連續式之反應裝置。因此,即便為微細至1~30 μm之反應場間隙,所生成之晶析物亦不會堵塞在反應器內,可以高濃度進行反應,而可獲得奈米粒子。
將本發明中所使用之強制薄膜式微反應器之一例示於圖3。強制薄膜式微反應器係如下裝置:具有由相互對向之第1處理面(1)與第2處理面(2)所形成之反應場,可使第1處理面(1)與第2處理面(2)相對地旋轉,且可相對地接近或背離,藉由原料之供給壓於使兩個
處理用面背離之方向上產生力,且於使兩個處理用面接近之方向上另外施加使之移動之力,而將反應場維持為微小間隔。所謂第1處理面(1)與第2處理面(2),可使一者旋轉另一者靜止,又,亦可使兩者沿反方向旋轉。
原料之鎂鹽水溶液(A)係藉由既定之壓力自反應器之中央部供給至反應場。原料之鹼性物質(B)係自與鎂鹽水溶液(A)不同之供給口供給至反應場。含有藉由反應生成之微細氫氧化鎂的漿料係自排出口(3)排出。若使用強制薄膜式微反應器,則可於薄膜流體之狀態下進行反應。
圖3中,旋轉圓盤(4)旋轉,而固定圓盤(5)不旋轉。旋轉圓盤(4)之固定轉速較佳為300~3550 rpm,更佳為500~3000 rpm。
第1處理面(1)與第2處理面(2)之間隙、即反應場之間隙為1~30 μm,較佳為3~20 μm,更佳為5~15 μm。
第1處理面(1)為中空圓板狀,固定於圓板狀之固定圓盤(5)上。又,第2處理面(2)為中空圓板狀,固定於圓板狀之旋轉圓盤(4)上。
鎂鹽水溶液(A)於反應場中之流量較佳為10~250 ml/秒鐘,更佳為15~200 ml/秒鐘。鹼性物質(B)於反應場中之流量較佳為10~250 ml/秒鐘,更佳為15~200 ml/秒鐘。
作為原料之鎂鹽水溶液,係使用氯化鎂、硝酸鎂、硫酸鎂等之水溶液。又,作為鹼性物質原料,係使用苛性鈉、氨、氫氧化鉀等之水溶液。
反應之溫度較佳為5~90℃,更佳為5~60℃,進而較佳為5~50℃。
鎂與鹼之反應之比例較佳為相對於鎂1 mol,氫氧化物(OH)為0.2~12 mol,更佳為0.4~10 mol,進而較佳為0.6~8 mol。
於本發明之微細氫氧化鎂之製造方法中,如上所述,由於使用不含碳之原料,故而作為最終製品之微細氫氧化鎂粒子不含碳。又,若需要有機處理,則可進行作為先前技術之利用脂肪酸等之有機表面處理。
[實施例]
以下,藉由實施例及比較例詳細地說明本發明,但本發明並不僅限定於該等實施例。
再者,實施例中之氫氧化鎂粒子之(a)粒度分佈及平均二次粒徑、(b)TEM(Transmission Electron Microscope,穿透式電子顯微鏡)觀察直徑、(c)碳含量、(d)X射線構造解析,又,樹脂組成物之實施例中之(e)塗膜厚度、(f)霧度測定表示藉由以下所記載之測定法而測得之值。
(a)粒度分佈及平均二次粒徑:
使用日機裝之粒度分佈裝置UPA-UT151(動態光散射法,頻率分析)、日機裝之Microtrac MT3300EX II(雷射繞射法)進行測定。測定時之溶劑係於藉由超音波將離子交換水、氫氧化鎂漿料處理5分鐘後進行測定。合計進行2次測定,將各測定中所獲得之%50設為試樣之平均二次粒徑。
(b)TEM觀察直徑:
使用JEOL公司之JEM-2100。試樣係於藉由超音波將氫氧化鎂漿料處理5分鐘後,滴加至膠棉膜上而製作,並進行觀測。
(c)碳含量:
使用島津製作所之總有機碳計TOC-5000進行測定。
(d)X射線構造解析:
使用Rigaku公司之RINT2200V進行測定。
(e)塗膜厚度
使用高分子計器股份有限公司之試驗片測厚器SDA-25型進行測定。
(f)霧度測定
使用東京電色有限公司之AUTOMATIC HAZEMETER OPTICAL UNIT TC-HIIIDP而測定全光線透過率、霧度。
[實施例1]
使用M-technique股份有限公司製造之強制薄膜式微反應器ULREA SS-11作為反應器。原料係以30 ml/分鐘之流量供給1.409 mol/L之氯化鎂水溶液,以13.3 ml/分鐘之流量供給6.045 N之苛性鈉,並於反應溫度35℃、反應場間隙約10 μm、旋轉圓盤之轉速1700 rpm之條件下進行反應而獲得氫氧化鎂漿料。
利用離心分離機將所獲得之漿料過濾分離,並利用離子交換水洗淨。利用離子交換水將洗淨後之固形物成分乳化,藉由超音波處理5分鐘後,利用日機裝之粒度分佈裝置UPA-UT151(動態光散射法,頻率分析)進行測定,結果可獲得平均二次粒徑為15.8 nm之微細氫氧化鎂粒子。進行X射線解析,結果為氫氧化鎂。
[實施例2]
與實施例1相同地使用ULREA SS-11,原料係以10 ml/分鐘之流量供給0.764 mol/L之氯化鎂水溶液,以250 ml/分鐘之流量供給0.264 N之苛性鈉,並於反應溫度20℃、反應場間隙約10 μm、旋
轉圓盤之轉速1700 rpm之條件下進行反應而獲得氫氧化鎂漿料。
利用離心分離機將所獲得之漿料過濾分離,並利用離子交換水洗淨。利用離子交換水將洗淨後之固形物成分乳化,藉由超音波處理5分鐘後,利用日機裝之粒度分佈裝置UPA-UT151(動態光散射法,頻率分析)進行測定,結果可獲得平均二次粒徑為38.1 nm之微細氫氧化鎂粒子。進行X射線解析,結果為氫氧化鎂。利用穿透式電子顯微鏡(TEM)可觀察到50 nm以下之分散粒子。
[實施例3]
與實施例1相同地使用ULREA SS-11,原料係以10 ml/分鐘之流量供給0.764 mol/L之氯化鎂水溶液,以250 ml/分鐘之流量供給0.264 N之苛性鈉,並於反應溫度77℃、反應場間隙約10 μm、旋轉圓盤之轉速1700 rpm之條件下進行反應而獲得氫氧化鎂漿料。
利用離心分離機將所獲得之漿料過濾分離,並利用離子交換水洗淨。利用離子交換水將洗淨後之固形物成分乳化,藉由超音波處理5分鐘後,利用日機裝之粒度分佈裝置UPA-UT151(動態光散射法,頻率分析)進行測定,結果可獲得平均二次粒徑為60.1 nm之微細氫氧化鎂粒子。進行X射線解析,結果為氫氧化鎂。
[實施例4]
與實施例1相同地使用ULREA SS-11,原料係以100 ml/分鐘之流量供給0.7045 mol/L之氯化鎂水溶液,以44.3 ml/分鐘之流量供給3.023 N之苛性鈉,並於反應溫度35℃、反應場間隙約10 μm、旋轉圓盤之轉速1700 rpm之條件下進行反應而獲得氫氧化鎂漿料。
利用離心分離機將所獲得之漿料過濾分離,並利用離子交換水洗淨。利用離子交換水將洗淨後之固形物成分乳化,藉由超音
波處理5分鐘後,利用日機裝之粒度分佈裝置UPA-UT151(動態光散射法,頻率分析)進行測定,結果可獲得平均二次粒徑為69.4 nm之微細氫氧化鎂粒子。
[實施例5]
使用ULREA SS-11,原料係以100 ml/分鐘之流量供給1.409 mol/L之氯化鎂水溶液,以44.3 ml/分鐘之流量供給6.045 N之苛性鈉,並於反應溫度35℃、反應場間隙約10 μm、旋轉圓盤之轉速1700 rpm之條件下進行反應而獲得氫氧化鎂漿料。
利用離心分離機將所獲得之漿料過濾分離,並利用離子交換水洗淨。利用離子交換水將洗淨後之固形物成分乳化,藉由超音波處理5分鐘後,利用日機裝之粒度分佈裝置UPA-UT151(動態光散射法,頻率分析)進行測定,結果可獲得平均二次粒徑為89.4 nm之微細氫氧化鎂粒子。進行X射線解析,結果為氫氧化鎂。
[比較例1]
藉由於不鏽鋼製之反應容器中之分批反應,於溫度35℃攪拌下之1.409 mol/L之氯化鎂水溶液100 ml中,以5分鐘添加6.045 N之苛性鈉44.3 ml而獲得氫氧化鎂漿料。
利用離心分離機進行過濾分離,並利用離子交換水洗淨。利用離子交換水將洗淨後之固形物成分乳化,使用日機裝之Microtrac MT3300EX II,藉由雷射繞射散射法進行粒度測定,結果平均二次粒徑為1280 nm。
[實施例6]
(樹脂之調配例)
(樹脂組成物之製作)
於Kanpe Hapio股份有限公司之水溶性拋光清漆(成分:合成樹脂(丙烯酸系)、有機溶劑、水)5.395 g(丙烯酸系樹脂含量2.460 g)中,混合製備為49.2 g/L之實施例4之氫氧化鎂粒子漿料10 ml,藉由超音波進行1分鐘分散處理而獲得無機有機複合漿料。於厚度為125 um之PET(Polyethylene Terephthalate,聚對苯二甲酸乙二酯)板上澆鑄無機有機複合漿料1 ml,使之自然乾燥一晚而獲得無機有機複合塗膜。塗膜之厚度為80~160 μm。
[比較例2]
使用平均二次粒徑0.8 μm之氫氧化鎂粒子漿料(49.2 g/L),於與實施例6相同條件下製作樹脂組成物。塗膜厚度為70~130 μm。
[實施例7]
進行實施例6與比較例2之塗膜之霧度測定。
[表2]
本發明之微細氫氧化鎂粒子可用作難燃劑、導熱劑、受酸劑、吸附劑、增黏劑、補強劑等。
Claims (8)
- 一種微細氫氧化鎂粒子,其藉由頻率分析而測得之平均二次粒徑為1~100 nm,且碳含量未滿0.9重量%。
- 如申請專利範圍第1項之氫氧化鎂粒子,其係利用選自由高級脂肪酸類、鈦酸酯偶合劑、矽烷偶合劑、鋁酸酯偶合劑、多元醇與脂肪酸之磷酸酯類及陰離子系界面活性劑所組成之群中之至少一種表面處理劑進行表面處理。
- 一種樹脂組成物,其含有100重量份之合成樹脂、及1~95重量份之藉由頻率分析而測得之平均粒徑為1~100 nm且碳含量未滿0.9重量%之微細氫氧化鎂粒子。
- 如申請專利範圍第3項之樹脂組成物,其中,合成樹脂為聚烯烴或其共聚合體。
- 一種成形品,其係由申請專利範圍第3項之樹脂組成物所形成。
- 如申請專利範圍第5項之成形品,其係電線或電纜。
- 一種申請專利範圍第1項之微細氫氧化鎂粒子之製造方法,其特徵在於:於反應場之間隙為1~30 μm之強制薄膜式微反應器中,使鎂鹽水溶液與鹼性物質原料進行反應。
- 如申請專利範圍第7項之製造方法,其中,強制薄膜式微反應器係具有由相互對向之第1處理面(1)與第2處理面(2)所形成之反應場,可使第1處理面(1)與第2處理面(2)相對地旋轉,且相對地接近或背離,藉由原料之供給壓於使兩個處理用面背離之方向上產生力,且於使兩個處理用面接近之方向上另外施加使之移動之力,而將反應場維持為微小間隔。
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EP (1) | EP2816011A4 (zh) |
JP (1) | JPWO2013122239A1 (zh) |
KR (1) | KR20140128997A (zh) |
CN (1) | CN104114492A (zh) |
RU (1) | RU2014137149A (zh) |
TW (1) | TW201343555A (zh) |
WO (1) | WO2013122239A1 (zh) |
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EP2535105A1 (en) * | 2011-06-14 | 2012-12-19 | Corning Incorporated | Systems and methods for scale-up of microreactors |
RU2561379C2 (ru) * | 2013-10-29 | 2015-08-27 | Открытое Акционерное Общество "Каустик" | Наночастицы антипирена гидроксида магния и способ их производства |
US10233305B2 (en) * | 2014-08-26 | 2019-03-19 | Kyowa Chemical Industry Co., Ltd. | Magnesium hydroxide-based solid solution, and resin composition and precursor for highly active magnesium oxide which include same |
KR102085040B1 (ko) | 2016-09-07 | 2020-03-05 | 교와 가가꾸고교 가부시키가이샤 | 미립자 복합 금속 수산화물, 그 소성물, 그 제조 방법 및 그 수지 조성물 |
JP7382643B2 (ja) * | 2019-08-02 | 2023-11-17 | 株式会社宮本製作所 | 水酸化マグネシウム懸濁液、その製造方法、水酸化マグネシウム飽和水溶液の製造方法およびpH上昇剤、ならびに、入浴剤、化粧品、医薬品、医薬部外品、除菌剤、防カビ剤およびそれらの製造方法 |
CN114573956B (zh) * | 2022-01-25 | 2023-11-24 | 浙江恒逸石化研究院有限公司 | 一种纳米氢氧化镁改性可降解共聚酯的制备方法 |
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JP3299921B2 (ja) * | 1997-10-17 | 2002-07-08 | 協和化学工業株式会社 | 水酸化マグネシウムを含有する耐酸性熱可塑性樹脂組成物 |
US6376077B1 (en) * | 1998-04-10 | 2002-04-23 | Kyowa Chemical Industry Co., Ltd. | Process for the production of coupling agent-treated inorganic particles and use thereof |
US20080300342A1 (en) * | 2004-04-20 | 2008-12-04 | Yazaki Corporation | Polyolefin Resin Composition and Electric Wire Using the Same |
JP4997705B2 (ja) * | 2005-02-24 | 2012-08-08 | 富士ゼロックス株式会社 | 表面被覆難燃性粒子及びその製造方法、並びに難燃性樹脂組成物及びその製造方法 |
JP4458202B2 (ja) * | 2007-08-09 | 2010-04-28 | エム・テクニック株式会社 | 半導体微粒子の製造方法 |
JP5128882B2 (ja) | 2007-09-05 | 2013-01-23 | 関東電化工業株式会社 | 水酸化マグネシウム微粒子及びその製造方法 |
JP4986300B2 (ja) | 2007-11-09 | 2012-07-25 | エム・テクニック株式会社 | 微粒子の製造方法 |
MX2012010321A (es) * | 2010-03-09 | 2012-10-05 | Kyowa Chem Ind Co Ltd | Relleno para resina sintetica, composicion de resina sintetica, metodo de manufactura para la misma y objetos moldeados hechos a partir de la misma. |
JP5409461B2 (ja) * | 2010-03-19 | 2014-02-05 | 富士フイルム株式会社 | 金属水酸化物微粒子の製造方法 |
EP2578311B1 (en) * | 2010-05-25 | 2018-03-28 | M Technique Co., Ltd. | Method for producing precipitated substances with controlled amounts of dopant element |
JPWO2012008596A1 (ja) * | 2010-07-13 | 2013-09-09 | 協和化学工業株式会社 | 樹脂組成物の引張強度を向上させる方法 |
JP5598989B2 (ja) * | 2011-02-07 | 2014-10-01 | エム・テクニック株式会社 | ドープ元素量を制御された析出物質の製造方法 |
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- 2013-02-08 US US14/375,585 patent/US20150005429A1/en not_active Abandoned
- 2013-02-08 EP EP13748918.3A patent/EP2816011A4/en not_active Withdrawn
- 2013-02-08 WO PCT/JP2013/053776 patent/WO2013122239A1/ja active Application Filing
- 2013-02-08 KR KR1020147022100A patent/KR20140128997A/ko not_active Application Discontinuation
- 2013-02-08 RU RU2014137149A patent/RU2014137149A/ru not_active Application Discontinuation
- 2013-02-08 TW TW102105181A patent/TW201343555A/zh unknown
- 2013-02-08 JP JP2013558764A patent/JPWO2013122239A1/ja active Pending
- 2013-02-08 CN CN201380006920.8A patent/CN104114492A/zh active Pending
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EP2816011A1 (en) | 2014-12-24 |
US20150005429A1 (en) | 2015-01-01 |
JPWO2013122239A1 (ja) | 2015-05-18 |
EP2816011A4 (en) | 2015-11-04 |
RU2014137149A (ru) | 2016-04-10 |
CN104114492A (zh) | 2014-10-22 |
KR20140128997A (ko) | 2014-11-06 |
WO2013122239A1 (ja) | 2013-08-22 |
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