TW200823148A - Flame-retardant magnesium hydroxide compositions and associated methods of manufacture and use - Google Patents

Flame-retardant magnesium hydroxide compositions and associated methods of manufacture and use Download PDF

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Publication number
TW200823148A
TW200823148A TW096107056A TW96107056A TW200823148A TW 200823148 A TW200823148 A TW 200823148A TW 096107056 A TW096107056 A TW 096107056A TW 96107056 A TW96107056 A TW 96107056A TW 200823148 A TW200823148 A TW 200823148A
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Taiwan
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composition
magnesium hydroxide
resin
particles
distribution
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TW096107056A
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Chinese (zh)
Inventor
Lemuel O Granada Jr
James Innes
David Morgan Smith
Mark Wajer
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Martin Marietta Materials Inc
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Priority claimed from PCT/US2006/045421 external-priority patent/WO2007097795A2/en
Application filed by Martin Marietta Materials Inc filed Critical Martin Marietta Materials Inc
Publication of TW200823148A publication Critical patent/TW200823148A/en

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Abstract

The invention provides a submicron magnesium hydroxide particulate composition comprising a first distribution of magnesium hydroxide particles having a D50 of no more than about 0.30 μm, a D90 of no more than about 1.5 μm, and a BET surface area of at least about 35 m<sp>2</sp>/g, which can be used as a flame-retardant additive for synthetic polymers, optionally in combination with other flame-retardant additives such as nanoclays and larger-sized magnesium hydroxide particulate compositions. Polymeric resins comprising the submicron magnesium hydroxide particles and methods of manufacturing submicron magnesium hydroxide particles are also provided.

Description

200823148 九、發明說明: 【發明所屬之技術領域】 本發明係關於一種包含次微米粒子的氫氧化錤顆粒組 合物,此種組合物製造方法及併入此種組合物做為抗焰劑 的聚合物件。 【先前技術】200823148 IX. Description of the Invention: [Technical Field] The present invention relates to a cerium hydroxide particle composition comprising submicron particles, a method for producing such a composition, and a polymerization incorporating the composition as a flame retardant object. [Prior Art]

易於模製成各種形狀、大小及厚度的熱塑形聚合物事 貝上常用於每一類消費者及工業物件。雖然它們的用途已 變為到處存在的,此種聚合物的確存在必須注意的缺點, 伴隨塑膠品使用的火及煙霧的危險性之日益認知已產生塑 膠品配方關於抗焰性的立法及標準化。 有機鹵化物化合物,三氧化銻,及其組合物已用做塑 ,材料的抗關添加劑,然而,此種添加劑在暴露於火焰 日守產生顯著量的煙霧及有魏體。結果,企圖最小化它們 於贊成較少毒性替代物的使用已進行。 ▲ 風祕絲子錢氧化練子作為較安全 曰代物已變得日益普及的,在包含 塑膠品,氫氧化㈣师㉞4 1線電見應用的各種 氧化锘:主端性質,與煙霧抑制,氫 •體及塑膠化合 ==、_㈣加劑,及在較偏好抗焰及 煙務抑制的非_素溶液之場合其常併入彈性, 物0 氫氧化鎂根據 分解反應:Thermoformed polymers that are easily molded into a variety of shapes, sizes, and thicknesses are commonly used in every consumer and industrial item. Although their use has become ubiquitous, such polymers do have disadvantages that must be noted, and the increasing awareness of the dangers of fire and smoke associated with the use of plastics has led to legislation and standardization of flame resistance in plastic formulations. Organic halide compounds, antimony trioxide, and combinations thereof have been used as anti-offset additives for plastics and materials. However, such additives produce significant amounts of smoke and have a body upon exposure to the flame. As a result, attempts have been made to minimize their use in favor of less toxic alternatives. ▲ Feng Mizi Qian Oxidation as a safer progeny has become increasingly popular, in the inclusion of plastic products, Hydroxide (4) Division 344 1 line electricity see the application of various yttrium oxide: main end properties, with smoke suppression, hydrogen • Body and plastic compound ==, _ (four) additive, and in the case of non-sulphur solution that prefers anti-flame and smoke suppression, it often incorporates elasticity, material 0 magnesium hydroxide according to decomposition reaction:

下列反應式C0於約330°C 開始進行吸熱 5 200823148The following reaction formula C0 starts to absorb heat at about 330 ° C. 5 200823148

Mg(〇H)2 !S&gt; Mg0瑪ο (Ι) ^Mg(OH)2的吸熱分解反應,#在燃燒_發生,係為 幾構。在峨期間所釋出的水具有稀㈣燃氣體及做 二阻隔物、防止氧氣支援火焰之作用。咸信氫氧化鎮的煙 Γ: 霧抑制性貝係因為在易燃氣體上水蒸氣的稀釋作用或是因 為與聚合物形成焦炭。 儘官虱乳化鎂具有這些優點,在某些應用其用途可為 f問題的。例如’為得到非常高等級的抗·力(例如,UL94 =級)’抗焰劑添加劑必須大量添加,例如大於6〇重量百 刀比此έ負面地影響聚合樹脂的物理性質及使得其不合 適於一些應用例如電線及電纜絕緣。 雖然現有氫氧化鎮顆粒組合物提供一些抗焰及煙霧抑 =的方法,在該技藝仍存在能提供甚至更高等級防火而不 犧牲抗焰組合物所加至的聚合樹脂的有利物理性質的祖合 物之需求。 口 【發明内容】 本發明係提供_種適合用做聚合樹驗合物中抗 添加劑的錄傾顆綠合物,本發日歧氧傾組合物1 有次微米練及高粒子表簡,產生錢㈣抗焰性質: 本發明氫Α化_粒組合物的較健體纽儀由且有 超過約0.3微米的跡不超過約u微米的_歧 35平方公尺/公克的BET表面 、'、Ί 化。在沖靜奸W〜 子分布所特徵 在R具體貫補,風氣化鎂粒子係以表面活化劑例 6 200823148 或脂類塗佈,特佳表面活 如各種脂肪酸或是脂肪酸的鹽類 化劑包含硬脂酸_及硬脂酸。 β上述氫輪馳合物可與其他抗補添加雜合 別是由不雌子分布所特徵化的其他抗焰劑,例如^且八 物可與具註少約0.9微米的⑽及不超制%平方公尺 /公克的BET表面躺第二分布絲傾粒子混合。 在另方面,本發明係提供一種抗焰添加劑纟且合物, 其包含⑻錄化_子的―第—分布,該第—分布具有至 少約0.9微米的D50及不超過約3〇平方公尺/公克的㈣ 表面和,及(b)H合物,其包含①複數個奈米枯土粒 子’⑻氫氧傾粒子的m該第二分布具有不超 過約0.30微米的D50、不超過約15微米的D9〇及不超過 約35平方公尺/公克的BET表面;或是㈣①及⑼的一組 合。較佳奈米粘土係得自鋁碳酸鎂。 在本發明另一方面,提供一種聚合性樹脂組合物,該 ♦ δ性树爿曰組合物包含合成聚合物,例如熱塑性聚合物、 熱固性聚合物、或彈性體、及上述氳氧化鎂組合物或本發 明抗焰劑添加劑組合物的混合物。多種合成聚合物可用於 聚合樹脂組合物,例如烯烴(α-烯烴)聚合物及共聚物、烯 fe與一烯的共聚物、乙稀-丙烯酸g旨共聚物、聚苯乙浠及苯 乙烯共聚物、熱塑性聚烯烴(TPO)、乙烯基氯或醋酸乙烯酯 合物或共聚物、苯氧基樹脂、聚縮酸、聚醯胺樹脂、丙 烯基及甲基丙烯基樹脂、丁二烯、聚氨基曱酸酯、聚脂、 聚碳酸酯、聚酮、鄰苯二酸二烯丙酯樹脂、酚式樹脂、環 200823148 、醇咖旨、麟脂、及合成橡 膠的共聚物。 進—步—方面,本發明提供—種經模製聚合物件, 其包含具有本發明抗趋氫氧化鎂粒子或上文所指出上述抗 、則力▲且口物的上述聚合性樹脂組合物。該聚合物件依 據所欲終卿料_各伽Μ,示娜合餐包含電纜 及電線核、電子崎、汽輪件、及其類似物。 、在另;方面,本發明提供一種上述氫氧化鎂組合物製 造方法。該方法較佳地包含提供氫氧化鎮粒子(例如具有至 少約〇·9财的D5G粒徑的粒子),或是氧化雜子的水性 水液’該水性漿液較佳地包含不超過約62重量百分比固體 基於漿液總重量,該雜t液财餘不超過約〇·5 毫米的碾2介質進行礙製步驟,及在某些具體實施例不超 k、 力0.3笔米在礙製步驟期間,藉由添加水性溶液將固 體於生水液的重里百分比維持在或低於約幻%及/或藉由 添加水性减或黏度調節舰漿絲度_在不超過約 l, 000厘泊。 碾磨機的RPM較料轉在不超勒6,_及不低於 約2,000(例如3,〇00)。水性漿液的較佳固體含量為不超過約 重i/ο固體’更佳為不超過約5〇%,及最佳為不超過約 45%。碾製介質較佳實例包含氧化錯、石夕酸錯、及紀摻雜 四方晶錯多晶體。 【實施方式】 現在更详細敘述本發明於下文,然而,此發明可以許 200823148 夕不同形式具體化及不應建構為限制於此處所說明具體實 施例,·而是,這些具體實施例係提供使得此揭示滿足可應 用法規要求。當使用於此專利說明書及申請專利範圍,單 數形式”a”、’’an”、及”the”包含複數個所指參考物除非上下 文清楚指出。 ’ 當用於本文時名稱,,次微米,,係表示具有至少一個尺寸 在少於約1微米的範圍之粒子。 此處所參考的所有粒子尺寸參數,例如粒徑中央值, D90值,及其類似值,係使用由 通CR〇MERlTICS(I)Nc)rcr()ss5 GA 所製造的 SediGraph 5100 粒子尺寸分析儀測量。測試前,乾燥樣品及經由5〇網目篩 網(美國標準)磨平,之後,將3 〇公克置於乾淨的1〇〇毫升Mg(〇H)2 !S&gt; Mg0玛ο (Ι) ^Mg(OH)2 endothermic decomposition reaction, #在燃_, is a few structures. The water released during the sputum has a dilute (four) gas body and a second barrier to prevent oxygen from supporting the flame. Smoke from the salt water town of Xianxin: The fog-inhibiting shellfish is due to the dilution of water vapor on the flammable gas or the formation of coke with the polymer. Emulsified magnesium has these advantages, and in some applications its use can be problematic. For example, 'to obtain a very high level of resistance (for example, UL94 = grade)' flame retardant additive must be added in large amounts, for example, more than 6 〇 weight, which is a negative effect on the physical properties of the polymer resin and makes it inappropriate. For some applications such as wire and cable insulation. While existing oxidized granule compositions provide some resistance to flame and smoke, there are still ancestors in the art that provide even higher levels of fire protection without sacrificing the advantageous physical properties of the polymeric resin to which the flame resistant composition is added. The demand for the compound. Mouth [Invention] The present invention provides a pour green compound suitable for use as an anti-additive in a polymeric tree assay, and the present invention has a submicron process and a high particle form. (4) Anti-flame properties: The hydrazine-based composition of the present invention has a BET surface of more than about 0.3 micrometers and a trace of no more than about u micrometers of 35 square meters per gram of BET surface, ', Degenerate. In the smothering of the W~ sub-distribution, the characteristics of R in the specific complement, the volcanic magnesium particles are surfactants in the case of the example 6 200823148 or lipid coating, especially good surface activities such as various fatty acids or fatty acid salting agents Stearic acid _ and stearic acid. β The above-mentioned hydrogen-wheel-kneading compound can be mixed with other anti-complementing additives by other anti-flame agents characterized by non-female distribution, for example, and the eight objects can be less than about 0.9 micron (10) and not super-made. The BET surface of % square meters / gram is lying on the second distribution of silk particles mixed. In a further aspect, the present invention provides a flame-resistant additive composition comprising (8) a "first" distribution of recorded _ sub-distributions having a D50 of at least about 0.9 microns and no more than about 3 square meters / gram of (d) surface and, and (b) H compound, which comprises a plurality of nano-soil particles '(8) oxyhydrogenated particles of m. The second distribution has a D50 of no more than about 0.30 microns, no more than about 15 Micron D9 〇 and no more than about 35 square meters / gram of BET surface; or (d) a combination of 1 and (9). Preferred nanoclay is derived from magnesium aluminum carbonate. In another aspect of the present invention, there is provided a polymerizable resin composition comprising a synthetic polymer such as a thermoplastic polymer, a thermosetting polymer, or an elastomer, and the above magnesium antimony oxide composition or A mixture of the flame retardant additive compositions of the present invention. A variety of synthetic polymers can be used in polymer resin compositions, such as olefin (α-olefin) polymers and copolymers, copolymers of ene-ene and monoene, copolymers of ethylene-acrylic acid, copolymerization of polystyrene and styrene. , thermoplastic polyolefin (TPO), vinyl chloride or vinyl acetate or copolymer, phenoxy resin, polyacid, polyamide resin, propylene and methacryl resin, butadiene, poly A copolymer of amino phthalate, polyester, polycarbonate, polyketone, diallyl phthalate resin, phenolic resin, ring 200823148, alcohol, linoleum, and synthetic rubber. Further, the present invention provides a molded polymer member comprising the above-mentioned polymerizable resin composition having the anti-magnesium hydroxide particles of the present invention or the above-mentioned anti-resistance and ▲ and the above-mentioned mouth. The polymer parts are based on the desired materials. Each of the savoury meals consists of a cable and wire core, an electronic chip, a steam wheel, and the like. In another aspect, the present invention provides a method of producing the above magnesium hydroxide composition. The method preferably comprises providing oxidized granules (e.g., particles having a D5G particle size of at least about 10,000 Å), or an aqueous hydrate of oxidized impurities. The aqueous slurry preferably comprises no more than about 62 weights. The percentage solids are based on the total weight of the slurry, and the impurities are not more than about 〇5 mm of the mill 2 medium for the barrier step, and in some embodiments, not exceeding k, force 0.3 pens during the barrier step, The percentage of solids in the raw water liquid is maintained at or below about illusion % by adding an aqueous solution and/or the ship's silkness is adjusted by adding aqueous reduction or viscosity _ at no more than about 1,000 centipoise. The RPM of the mill is not more than 6 _ and not less than about 2,000 (for example, 3, 〇 00). Preferably, the aqueous slurry has a solids content of no more than about i/o solids, more preferably no more than about 5%, and most preferably no more than about 45%. Preferred examples of the milled media include oxidative, sulphuric acid, and doped tetragonal crystal polycrystals. [Embodiment] The present invention will now be described in more detail below, however, the invention may be embodied in various forms and should not be construed as being limited to the specific embodiments described herein. This disclosure makes it possible to meet applicable regulatory requirements. The singular forms "a", "an", and "the" are used in the <RTI ID=0.0> </ RTI> </ RTI> <RTIgt; </ RTI> <RTIgt; , means having at least one particle having a size in the range of less than about 1 micron. All particle size parameters referred to herein, such as the median diameter value, the D90 value, and the like, are used by the pass CR〇MERlTICS (I Nc)rcr()ss5 GA SediGraph 5100 particle size analyzer measurement. Before testing, dry the sample and smooth it through a 5〇 mesh screen (US standard), then place 3 〇g in a clean 1〇 〇ml

具有攪拌棒的燒杯中,及加入50毫升的A-ll SEDISPERSE 或水,攪拌樣品數分鐘,接著將樣品置於超聲清洗2〇分 知^接著擾拌樣品數分鐘及置於超聲清洗額外2〇分鐘,接 者授拌樣品數分触麵樣^完錢浮,樣品接著可用於 在粒子尺寸分析儀上測試。粒子尺寸測量係表示未塗覆粒 子。 、、當用於本文時,名稱,,DX值”,其中X為50或90,係 二、,別=在粒子分布的底部兄❽/❻或質量的粒子的所測 付直徑上限。例如,〇·3微米的D50值表示在分布中 質置的粒子具有直徑大於G.3微米及5G%質量的粒子 八 彳二】、於微米。此處D50值亦表示粒徑中央值。 名% bet表面積,,係表示根據本發明粒子的表面積, 9 200823148 單位為平方公尺/公克,及係使用表面積決定的bet方法計 算。由 MICROMERiTICS(g)N〇rcr〇ss,GA 所製造的 FIX)WSORB II 2300儀器係用於進行該測量。 本發明提供氫氧化鎂顆粒組合物,其係由具有小粒子 尺了及大表面積的次微米粒子之存在而特徵化,當用做聚 合樹脂的添加劑時其貢獻改善的阻焰及煙霧抑制性能。雖 然本發明並不受隨任何特定操作理論,雜本發明組合 物的較小的小粒子尺寸及增加表面積目為雜物質於聚合 f生树月曰内的更佳分佈❿貢獻車交佳的阻焰性能。本發明的阻 焰氫氧化餘合物亦基本上為不含_素的,及典型上包含 不超過約百萬分之2,5〇〇的氯(例如不超過約百萬分之2,⑻〇) 及不超過約百萬分之75〇的氟(例如不超過約百萬分之5〇〇 氟),本發_氫氧化難子典型上顯現六方棱形晶 狀。 7本發贱概難子組合物具有不超㈣微米的 粒控中央值_),車交佳為不超過約0.25微米,更佳為不超 3 0.22微米,及最佳為不鑛約_微米。在一些具體 實施例’粒針央值不超過約ai8微米,或甚至不超過約 =5或不超㈣〇.13微米,翻言之,本發财微米粒子 ^钟央值會在约㈣微米至約a25财,更佳為約 .8至約0.20微米’及最佳為約_至約㈣微米(例如 〇·11、0·12 ' 〇·13、〇·14、或 〇·ΐ5 微米)。 本發明次微米組合物的D90值較佳為不超過約6〇微 ” ’佳為不超蝴5.G齡’及最料不超勒4.0微米。 200823148 在—些具體實施例,D90值不超過約3.5微米或不超過約 3.0 Μ米。本發明特佳具體實施例特徵為不超過約I』微米 或不超過約1.0微米的D90值。In a beaker with a stir bar, add 50 ml of A-ll SEDISPERSE or water, stir the sample for a few minutes, then place the sample in ultrasonic cleaning for 2 minutes. Then discard the sample for a few minutes and place it in the ultrasonic cleaning for an additional 2 inches. In minutes, the picker samples the sample and the surface is sampled. The sample can then be used for testing on a particle size analyzer. Particle size measurement refers to uncoated particles. , as used herein, the name, the DX value, where X is 50 or 90, is the second, and is not the upper limit of the measured diameter of the particle at the bottom of the particle distribution. The D50 value of 〇·3 μm indicates that the particles in the distribution have particles larger than G.3 μm and 5 G% by mass. In the micrometer, the D50 value also indicates the central value of the particle size. The surface area, expressed as the surface area of the particles according to the present invention, 9 200823148 in square meters per gram, and calculated by the bet method determined by the surface area. FIX) WORRB manufactured by MICROMERITICS (g) N〇rcr〇ss, GA The II 2300 instrument is used to perform this measurement. The present invention provides a magnesium hydroxide particle composition characterized by the presence of submicron particles having a small particle size and a large surface area, when used as an additive for a polymeric resin Contributing to improved flame retardant and smoke suppression properties. Although the invention is not subject to any particular theory of operation, the smaller particle size and increased surface area of the compositions of the invention are intended to be heterogeneous within the polymeric f-tree more The flame retardant hydroxide of the present invention is also substantially free of _-, and typically contains no more than about 2, 5 parts per million chlorine. (for example, no more than about 2 parts per million, (8) 〇) and no more than about 75 parts per million of fluorine (for example, no more than about 5 parts per million of fluorine), this is a typical problem. The hexagonal prismatic crystal is formed. 7 The hairpin composition has a grain-control central value of not exceeding (four) micrometers, and the car is preferably no more than about 0.25 micrometers, more preferably no more than 3 0.22 micrometers, and most Preferably, it is not about _micron. In some embodiments, the central value of the granules does not exceed about ai8 microns, or even no more than about = 5 or not more than (four) 〇.13 microns, in other words, the present wealth micron particles ^ The clock center value will be in the range of about (four) micrometers to about a25, more preferably about .8 to about 0.20 micrometers, and most preferably about _ to about (four) micrometers (for example, 〇·11, 0·12 ' 〇·13, 〇· 14. Or 〇·ΐ5 μm) The D90 value of the submicron composition of the present invention is preferably no more than about 6 〇 micro" 'good for not exceeding 5. G age' and most preferably not exceeding 4.0 microns. 200823148 In some embodiments, the D90 value does not exceed about 3.5 microns or does not exceed about 3.0 microns. A particularly preferred embodiment of the invention is characterized by a D90 value of no more than about 1" micron or no more than about 1.0 micron.

本發明氫氧化鎂粒子組合物的ΒΕΤ表面積為至少約 35平方公尺/公克,較佳為至少約4〇平方公尺/公克,及最 佳為至少約50平方公尺/公克。在一些具體實施例,ΒΕΤ 表面積為約48平方公尺/公克至約8〇平方公尺/公克。某些 特佳具體實施讎徵為至少約55平方公尺/公克或至少約 6〇平方公尺/公克的ΒΕΤ表面積。本發明次微米氫氧化鎂 組合物的示例BET表面積包含約35、約38、約4〇、約42、 約44、約46、約48、約50、約52、約55、約58、約60、 約62、約65、約68、約7〇、約72、約乃、約%、 8〇平方公尺/公克。 、、本發明氫氧傾組合物可使用在馳藝巾已知的各種 式或乾式磨碎方法及設備製造。如在該技藝中所已知, 2於粒子尺寸減少的典型濕式_機包含以稱為礙製介 粒或珠粒填充的封_,這些介__生^ 圍入=册沾所作動,擾拌器的旋轉將能量施與周 將ΐ貝你及所產生力量作用於經由礙製室持續揚起的粒子 漿液中粒子的力量 保留二:機广法期間該雜介質係 速度、產品流速、體含量、餅器 式包含水平式盤式粉碎機、高能 200823148 型式。 、在本發明一個方面,本發明氫氧化鎂組合物係使用濕 式碾製技術及珠磨機製造,存在數種可用於執行本發明方 法的商業可提供珠磨機。在一個較佳具體實施例,珠磨機 為由 Willy A· Bachofen AG of Switzerland 製造及具有 6〇〇 毛升連續破璃内襯室及聚氨基甲酸酯葉輪的D出 水平式珠磨機(型式KDL)。用於本發明方法的礙製介質可 ,化。較佳碾製介質包含氧化鍅、矽酸錯(Zirc〇n)、及釔摻 雜四方晶鍅多晶體(YTZP)。然而,亦可制其他介質如不 銹鋼或碳化鎢。 、 、較佳礙製介質尺寸為不超過約0·5毫米,更佳為不超 過約〇·3毫米(例如約αι毫米至約〇·3毫米),及較佳碾製 介質材料為氧化鍅或具有密度為約3 〇至約6·8公克/立方 :刀的其他氧化鍅基介質。較佳為,流經珠磨機的流速為 、勺1至約3耄升/秒及在碾製操作期間礙磨機的rpm維持 在不赵過約6,000及不少於約2,〇〇〇(例如約2,5〇〇、約 3,〇〇〇、約 3,500、約 4,〇〇〇、約 4,500、約 5,_、或是約 5,5〇〇)。 典型碾製時間係在約i至約6小時的範圍。 單一碾磨機可用於實施本發明,在此種具體實施例, 被碾製的漿液可經由碾磨機循環直到達到所欲粒子尺寸。 或是,可使用串連連接的二或更多碾磨機,每一個連續碾 磨機包含較小尺寸的碾製介質或是每一個碾磨機包含相同 尺寸的碾製介質。 如在下文實例1所指出,已決定在注入碾磨機的氫氧 12 200823148 化鎂粒子水性漿液中固體百分比影響碾製方法產生所欲次 微綠子的能力。在難具體實闕,注人鶴機的起初 氫氧化鎂粒子水性漿液具有不超過約62重量%的固體含 畺基於水性漿液總重,更佳為不超過約55°/。,及最佳為 不超過約52%。在-個具體實施例,漿液中固體百分比不 超過約50%或不超過約45%。典型言之,在礙製步驟期間 固體含量係轉在介_ 25%及約62%之間的含量,更佳 為約40%至約62%。 土 在碾製方法期間可監測水性漿液的固體含量及黏度, 及需要時在碾製_可添加額外水溶液輯持所欲黏^範 圍或所欲固體含量,或是可加人減調_如各種表面活 化劑(例如陰離子表面活化劑)或是在該技藝中已知的聚人 物(例如㈣ymer Ve耐es提供㈣% _子胺聚合物^ 以在碾製丽及/或碾製期間調整黏度。The magnesium hydroxide particle compositions of the present invention have a ruthenium surface area of at least about 35 square meters per gram, preferably at least about 4 square meters per gram, and most preferably at least about 50 square meters per gram. In some embodiments, the 表面积 surface area is from about 48 square meters per gram to about 8 square meters per gram. Some particularly preferred implementations have a ruthenium surface area of at least about 55 square meters per gram or at least about 6 square meters per gram. An exemplary BET surface area of the submicron magnesium hydroxide compositions of the present invention comprises about 35, about 38, about 4, about 42, about 44, about 46, about 48, about 50, about 52, about 55, about 58, about 60. , about 62, about 65, about 68, about 7 〇, about 72, about, about %, 8 〇 square meters / gram. The oxyhydrogenated composition of the present invention can be produced by various methods or dry grinding methods and equipment known in the art. As is known in the art, a typical wet type machine having a reduced particle size comprises a seal _, which is referred to as a barrier to granule or bead filling, and these __生^ The rotation of the scrambler applies energy to the week. The force of the mussels and the forces generated by the particles in the slurry of the particles that are continuously raised through the barrier chamber are retained: the velocity of the hybrid medium, the product flow rate, Body content, cake type includes horizontal disc mill, high energy 200823148 type. In one aspect of the invention, the magnesium hydroxide compositions of the present invention are manufactured using wet milling techniques and bead mills, and there are several commercially available bead mills that can be used to carry out the process of the present invention. In a preferred embodiment, the bead mill is a D-out horizontal bead mill manufactured by Willy A. Bachofen AG of Switzerland and having a 6-inch hair continuous lining chamber and a polyurethane impeller ( Type KDL). The barrier medium used in the method of the present invention can be made. Preferred milling media comprise yttria, yttrium, and ytterbium doped tetragonal polycrystalline (YTZP). However, other media such as stainless steel or tungsten carbide can also be made. Preferably, the size of the medium is not more than about 0.5 mm, more preferably not more than about 〇3 mm (for example, about α1 mm to about 〇3 mm), and the preferred grinding medium is cerium oxide. Or other cerium oxide based media having a density of from about 3 Torr to about 6.8 gram per cubic: knife. Preferably, the flow rate through the bead mill is from 1 to about 3 liters per second and the rpm of the grinding machine is maintained at about 6,000 and not less than about 2 during the milling operation. (eg, about 2,5 〇〇, about 3, 〇〇〇, about 3,500, about 4, 〇〇〇, about 4,500, about 5, _, or about 5,5 〇〇). Typical milling times range from about i to about 6 hours. A single mill can be used to practice the invention. In this particular embodiment, the milled slurry can be circulated through the mill until the desired particle size is achieved. Alternatively, two or more mills can be used in series, each continuous mill containing a smaller size of milled media or each mill containing the same size of milled media. As indicated in Example 1 below, it has been decided that the percentage of solids in the aqueous slurry of magnesium oxide particles injected into the mill 12 200823148 affects the ability of the milling process to produce the desired sub-greens. In a difficult manner, the initial aqueous slurry of magnesium hydroxide particles having a solids content of no more than about 62% by weight, based on the total weight of the aqueous slurry, more preferably not more than about 55°/. , and the best is no more than about 52%. In a specific embodiment, the percentage of solids in the slurry does not exceed about 50% or does not exceed about 45%. Typically, the solids content during the barrier step is between about 25% and about 62%, more preferably from about 40% to about 62%. The soil can monitor the solid content and viscosity of the aqueous slurry during the milling process, and if necessary, add an additional aqueous solution to the desired viscosity or desired solid content, or add a reduction. Surfactants (e.g., anionic surfactants) or polyfoams known in the art (e.g., (iv) ymer Ve resistant es provide (d) _ s-amine polymer to adjust viscosity during milling and/or milling.

當漿液的水性液體吸收於氫氧化鎂粒子的新露出表面 ,時(當粒子尺寸因礙製而降低時),漿液黏度會增加,當磨 W時’較佳為維持該減在不超過約W⑻厘泊㈣,更佳 =超過約_厘泊’及最佳為不超過約_厘泊。在礙 衣方法開始時,起始物質的黏度典型上低至觸_勘厘泊, 但碾製方法會使得黏度隨時間增加。 高及低黏度时_雜枝,雜賴得 因為在礙製期間增加的粒子表面積而升高,: ;交互:夜變得更_^ ” 、、減沙因為在粒子間的不足潤滑而 13 200823148 低^里想的’此潤滑為需要的以促進粒子緊壓。若黏度過 相t㈣稀釋的漿液,粒子分開過遠而不足以進行有 體人Ί。在某些具體實施例’在碾製期間可維持漿液的固 用=^或^液的黏度在所欲含量且不需在礙製期間採 溶液^=整&amp;些参數’例如藉由加入更多水性 r 有足體:質具 3里〆飞疋足夠回展度的黏度調節劑,則不 =步添加水性溶液或是黏度調_以在韻期間維 持水液於所欲黏度位準或是固體含量。 在礙製方法期間用於起始物質的氫氧化鎮粒子水性嘴 ;=τ藝中已知的水性溶液’更佳為,該水性溶 w、H t水包含各細b添加齡轉,例如黏度 == 主入礙製裝置的水性漿液中的氫氧化鎂粒子 := 提供氫氧化鎂產物,例如由M- 或mags諷卿氫氧化鎮 _EL_ 質的氯氧化鎂粒子具有不少於約0物9射=;,在進料物 超過約”方公尺 例,進料物質的D50粒徑為約】至約8微米。一體貫施 作:生=:=形二_,其會與水 /、丄mj a ’風化鎮進, 具雜上文針職魏鎂進料物= ·、、、負不的粒位為大的粒极。該氧化鎂可 二 化物形式或是氧输子裝液可進行賴 14 200823148 =本發明進-步具體實施例,氫氧化鎂粒子可使用表 :活性劑塗覆,較佳為使用陰離子表面活性劑,以減少粒When the aqueous liquid of the slurry is absorbed on the newly exposed surface of the magnesium hydroxide particles (when the particle size is lowered due to the hindrance), the viscosity of the slurry is increased, and when grinding W, it is preferable to maintain the reduction at no more than about W (8). PCT (4), better = more than about _ centipoise' and optimally no more than about _ centipoise. At the beginning of the barrier method, the viscosity of the starting material is typically as low as the exposure, but the milling method will increase the viscosity over time. High and low viscosity _ miscellaneous, the hybrid is increased due to the increased surface area of the particles during the obstruction:: interaction: the night becomes more _^ ”, and the sand is reduced due to insufficient lubrication between the particles 13 200823148 The low-thinking 'this lubrication is needed to promote particle compaction. If the viscosity is too much for the phase t(iv) diluted slurry, the particles are separated too far and not sufficient for human body cockroaches. In some specific examples ' during the milling period It can maintain the solidity of the slurry = ^ or ^ liquid viscosity at the desired level and does not need to take the solution during the control period ^ = whole &amp; some parameters 'for example by adding more aqueous r have a foot: quality 3黏 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋 疋More preferably, the water-soluble solution of the oxidized town particle of the starting material; = the aqueous solution known in the art of tau is more preferably, the aqueous solution w, H t water comprises the addition of each fine b, for example, the viscosity == the main barrier device Magnesium hydroxide particles in an aqueous slurry: = providing magnesium hydroxide product, for example by M- or mag s satiric oxidized town _EL_ qualitative magnesium oxychloride particles have not less than about 0 9 = =, in the feed more than about ” metric example, the D50 particle size of the feed material is about 】 to about 8 microns. Integrated application: raw =: = shape two _, it will be with water /, 丄mj a 'weathering town, with the above-mentioned needles Wei magnesium feeds = ·,,, negative grain size is large pole. The magnesium oxide dimerizable form or the oxygen transport liquid can be used to carry out the reaction. 14 200823148 = Further embodiments of the present invention, the magnesium hydroxide particles can be coated with an active agent, preferably an anionic surfactant. To reduce the grain

=附聚_献使錄子可紋合性翻旨更快速地分散。 曰肪酸及其鹽類或_為較佳的表面活 月旨職及其衍生物具有1G或更多碳原子。示例表面活性劑 :3硬脂酸、油酸、芥酸、月桂酸、二十二烷酸、及棕櫚 酉夂及其驗金屬雜(例如硬脂義、硬脂g_、硬脂酸妈、 -文納油自欠鉀、油酸j弓、棕櫚酸納、掠櫚酸钾、棕櫊酸 =月桂酸鈉、月桂酸卸、及月桂酸尚、硬脂酸銨、雙月 桂苯磺醯鈉、十八烷硫酸鉀、月桂磺醯鈉、及2_磺乙基_ α-石黃硬脂酸二鈉。 X可使用的其他類表面活性塗覆劑包含(i)矽烷耦合劑如 乙烯基乙氧基矽烷、乙烯基_三(2_甲氧基)矽烷、甲基丙 烯醯氧丙基三甲氧基矽烷、7_胺基丙基三甲氧基矽烷、冷 _(3,4-乙氧環己基)乙基三甲氧基矽烷、7_環氧丙氧基丙基 二甲氧基矽烷及氳硫基丙基三甲氧基矽烷;⑶)含鈦酸酯 耦合劑如異丙基三異硬脂醯鈦酸酯、異丙基參(焦磷酸二辛 酯)、異丙基三(N·胺乙基_胺乙基)鈦酸酯及異丙基三癸基苯 石貝基鈦酸酯,(iii)含紹躺合劑如乙醯石夕氧紹二異丙酯;(叫 磷酸酯類如正磷酸與硬脂醇的單或二脂類、這些酯類的混 合物或這些酯類的驗金屬鹽類或這些酯類的胺鹽類,及(v) 15 200823148 陰離子表面活性劑如醯胺_鍵結脂族羧酸酯、醯胺-鍵結硫酸 醋、sf胺-鍵結磺酸酯、醯胺·鍵結烷基烯丙基續酸醋、高級 醇如硬脂醇的硫酸酯、聚乙二醇醚的硫酸酯、酯_鍵結硫酸 酯、酯邀結磺酸酯、酯-鍵結烷基烯丙基磺酸§旨、及醚_鍵 結烷基烯丙基磺酸酯。這些表面活性塗覆劑可單獨使用或 是以二或更多的混合物使用。 當氫氧化鎂粒子以上述表面處理劑表面塗覆時,該表 面塗覆可使用在該技藝巾為已知的各種濕式或乾式塗覆方 法執行。在濕式方法中,例如將以液體或乳液形式的表面 處理劑加域氧賴好的綠,接著為機_拌。在乾 式f法中,將以液體、乳液、賴體形式的表面處理劑加 ^氫氧化齡子,且職氧傾粒子在_或不施用熱的 情況下於混合器,例如HENSCHEL⑧混合器中,完全擾拌。 在-些情況,在混合方法期間必需引人賴的熱以溶化表 面處理劑及,_,促進有效混合,熱可由外部來源供應 或是由混合ϋ杨職生的齡應。所使縣面活性塗覆 物二的里可魏’但典型上為約1G重量百分比或更少基於 氧氧化鎂粒子重量。 、 在本毛明某些替代具體實施例,本發明次微米氨氧化 ^組合物可與奈米枯土材料合併使用,或是以之取代。太 f枯土材料為該技藝中已知及係在由AkzoNobd所提^ =冉PERKAUTE彻奈米黏土所商業提供,此種材料一 =義為不米尺寸無機粒子,例如,在其至少一個尺寸具 T米尺寸圍的小片狀體粒子,—般此小片狀體粒子可 16 200823148 =為具有非常高縱橫比(物體長度與其厚度的比值)的姐 直二::長:是粒子亦可敘述為具有非常小的厚度或 如此處所_ U狀難子,,為具有兩個相當平的 相對面的粒子,其厚度為兩個面之間的距離,與面的大小 =料其:相當小的,小片狀體粒子包含經剝脫的層狀無 4有用的經剝脫無機材料包含衍生自包含天然戋人 ^例為⑯潤_ 土材料如蒙脫土、綠高嶺石、貝得石、 知潤土、鉻蒙脫石、合絲矣石、水輝石、矣石、辞合石、 、斜水_石、斯4石及其類似材料,及經:、多 二括=化物,碳_及其類似物。這些層狀材 科般包括含有以28埃或更少的層_隔緊密連 數個具有厚度約4]2埃的魏鹽小片狀體的粒子, =d交換陽離子或陰離子例如〇H、N(v、c〇32_、Na+、= Agglomeration _ Dedicated to the record can be more quickly dispersed. The fatty acid and its salts or _ are preferred surface actives and their derivatives have 1 or more carbon atoms. Exemplary surfactants: 3 stearic acid, oleic acid, erucic acid, lauric acid, behenic acid, and palm quinone and their metal (such as hard fat, stearic acid g_, stearic acid mother, - Wenna oil from potassium, oleic acid j, sodium palmitate, potassium palmitate, palmitic acid = sodium laurate, lauric acid, and lauric acid, ammonium stearate, sodium laurate Potassium octadecane sulfate, sodium lauryl sulfonate, and disodium 2-sulfoethyl _ a- tartaric acid. Other surface-active coating agents that can be used include (i) decane coupling agents such as vinyl B. Oxydecane, vinyl-tris(2-methoxy)decane, methacryloxypropyltrimethoxydecane, 7-aminopropyltrimethoxydecane, cold-(3,4-ethoxycyclohexane Hexyl)ethyltrimethoxydecane, 7-glycidoxypropyldimethoxydecane and decylpropyltrimethoxydecane; (3)) titanate-containing coupling agent such as isopropyl triiso-tear Barium titanate, isopropyl hydrazide (dioctyl pyrophosphate), isopropyl tris(N-amine ethyl-amine ethyl) titanate, and isopropyl trimethyl phthalite bet titanate, (iii) containing Shaoluo mixture such as acetaminophen Propyl ester; (called phosphates such as mono or dilipids of orthophosphoric acid and stearyl alcohol, mixtures of these esters or metal salts of these esters or amine salts of these esters, and (v) 15 200823148 Anionic surfactants such as guanamine _ bonded aliphatic carboxylic acid ester, guanamine-bonded sulphuric acid vinegar, sf amine-bonded sulfonate, guanamine-bonded alkyl allylic acid vinegar, higher alcohol Such as stearyl sulfate, polyglycol ether sulfate, ester-bonded sulfate, ester-inducing sulfonate, ester-bonded alkylallylsulfonic acid, and ether-bond The alkyl allyl sulfonate. These surface-active coating agents may be used singly or in combination of two or more. When the magnesium hydroxide particles are coated on the surface of the above surface treatment agent, the surface coating may be used. The technical towel is carried out in various wet or dry coating methods known in the art. In the wet process, for example, a surface treatment agent in the form of a liquid or an emulsion is added to the green oxygen, followed by machine-mixing. In the dry f method, a surface treatment agent in the form of a liquid, an emulsion, or a lysate is added to the oxidized age, and the oxygen oxidized particles are _ or in the absence of heat in a mixer, such as a HENSCHEL 8 mixer, completely disturbed. In some cases, during the mixing method must be inviting heat to dissolve the surface treatment agent and, to promote effective mixing, The heat may be supplied from an external source or from the age of the mixed eucalyptus. The granules of the county active coating 2 are typically about 1 G weight percent or less based on the weight of the oxymagnesia particles. In some alternative embodiments of the present invention, the submicron ammoxidation composition of the present invention may be used in combination with or substituted for the nano-sludge material. The too-f dry material is known and tied in the art. Commercially available from AkzoNobd's ^=冉PERKAUTE Chennai clay, this material is a non-meter-sized inorganic particle, for example, a small piece of particle with a T-meter size in at least one dimension. The small flake particles can be 16 200823148 = is a sister with a very high aspect ratio (the ratio of the length of the object to its thickness): long: the particles can also be described as having a very small thickness or as difficult as the U Child, for two A fairly flat opposite particle whose thickness is the distance between the two faces, and the size of the face = material: relatively small, the small piece of the particle contains the exfoliated layer without 4 useful exfoliation Inorganic materials are derived from natural 戋 ^ 为 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 16 Cifu stone, slanted water _ stone, Si 4 stone and similar materials, and the::, more than two = compound, carbon _ and its analogues. These laminates generally comprise particles having a layer of 28 angstroms or less and a plurality of Wei salt platelets having a thickness of about 4] 2 angstroms, =d exchange cations or anions such as 〇H, N (v, c〇32_, Na+,

Ca 、K或Mg+2存在於層間表面。 =此絲合物添加_小片狀難子具有個別層或 /、、複數層的厚度為小於、約10、較佳為小於約5、及更俨 為小於約3的層,及更佳為1或2層。較佳為,每一個^ 所有或基本上所有個別層^ 層層雜以形成個別小片狀體粒子 子:有小於約20埃的平均厚度:為 二=Γ 約3_6埃)’及範圍自約_至約1的縱 毛(長度.厚度),更典型為約300至約400。 ,、’ 17 200823148 存在許多方法產生包含奈米粘土的聚合性材料,且這 些方法可分為三類··(1)原位聚合;(2)溶液插層;及(3)溶化 剝落。在前兩種方法中,此種材料可由一種方法製備,其 中膨脹劑,如長鏈有機陽離子、及水溶性寡聚物或聚合物, 在相鄰層狀矽酸鹽層(例如膨潤性粘土)之間插入或合併,以 由此增加相鄰矽酸鹽層之間的層間間隔,使得聚合物鏈可 包含於矽酸鹽層之間當混合該層狀矽酸鹽與聚合物融溶 物。參考如,美國專利第5,552,469、WO 93/04117、日本 專利特♦公開申睛案弟8-151、449、7-207、134、、 762、7_33 卜 092、8-259、806、及 8_259、846。溶融剝落 或熔融插層係敘述於如p〇lymer Layered SilieateCa, K or Mg+2 is present on the interlayer surface. = 丝状状_小片状子 has a layer of individual layers or /, a plurality of layers having a thickness of less than, about 10, preferably less than about 5, and more preferably less than about 3, and more preferably 1 or 2 layers. Preferably, each of all or substantially all of the individual layers is intermingled to form individual platelet-shaped particles: having an average thickness of less than about 20 angstroms: two = 约 about 3-6 angstroms) and ranges from about The longitudinal hair (length. thickness) of _ to about 1, more typically from about 300 to about 400. , , ' 17 200823148 There are many methods for producing polymeric materials comprising nano-clay, and these methods can be divided into three categories: (1) in-situ polymerization; (2) solution intercalation; and (3) melting and spalling. In the first two methods, such materials can be prepared by a process in which a bulking agent, such as a long chain organic cation, and a water soluble oligomer or polymer, in an adjacent layered silicate layer (e.g., a swellable clay) Intercalation or combination is interposed to thereby increase the interlayer spacing between adjacent citrate layers such that the polymer chains can be included between the citrate layers when the layered citrate and polymer melt are mixed. For example, U.S. Patent No. 5,552,469, WO 93/04117, Japanese Patent Publication No. 8-151, 449, 7-207, 134, 762, 7-33, 092, 8-259, 806, and 8_259 846. Melt stripping or melt intercalation is described in p〇lymer Layered Silieate

Nanocomposites,Giannelis,Adv· Mater· 1996, 8, No· 1,29。不 像原位t合或&gt;谷液插層,熔融剝落僅涉及枯土礦物及聚合 物而不需私脹劑或分散介質。然而,可使用膨脹劑以藉由 特定聚合物增純土礦物的祕。在騎剝落,钻土礦物 及聚合物混合在-起’接著加熱至高於聚合錄化點的溫 度。 在奈米轴土 /聚合物奈米複合材料,兩種結獅式為可 能的。其中-個’結構為插人的,其中單—延伸聚合物鍵 插在層之$ i生具有父替聚合物/無機層的良好排序減 層。在另-個,稱之為非排序或層離的,無機層係以在聚 合物基ϊ的隨機位向基本均勻地分散於聚合物。 在較佳具體實施例,用於本發明的奈_土係自減 酸鎂、包含Mg及A1無機板的陰離子枯土得到,其一個具 18 =:==:=3 200823148 米米占土 在併入聚合樹脂之前’上述次微米氫氧化鎂組合物及/ 或奈米处材料(於本文其亦稱為”讀麵加们可與其 他抗焰材料’例如其他氫氧化齡子分佈,混合。例如, 次微米添加劑可與商業可提供氫氧傾組合物混合,例如 MAGSHIELD®S或MA_ELDOTp氫氧化鎮產物。若 本發明次微米添加劑鱗二氫氧傾粒子分佈掺合,該次 微米=触型上以至少約3重量百分喊於氫氧化鎮粒 子及次微f添加劑的總重量的量存在,更佳為以至少約汎 子在及敢it為以至少約J0%存在。在一個具體實施例, 本發明次微米添加劑係以約3%至約30%重量百分比基於 次微米添加敵其他抗崎·如其他錄傾粒子ς佈 的總重存在’更佳為以約3%至約I5%重量存在。 、曰與本發触微錢氧傾組合物(錢奈_ 土材料) 混合的較大尺寸氫氧化鎂粒子分佈典型上由至少約0.9微 米的D50(例如約1至約8微米的D5〇)及不超過約π平方 a尺/&amp;克,較佳為不超過約%平方公尺/公克,及最佳為 不超過約15 +方公尺/公細服表面積職徵化。適合 ^於與本發明組合物掺合的氳氧化鎂粒子分佈的形式亦適 δ用做在用於製造次微米氫氧化鎮組合物的進料漿液中的 ,粒物質。如可了解,自本發明次微米氫氧化鎂組合物與 第二粒子分佈的掺合物所產生的粒子組合物係由介於所掺 19 200823148 合的兩撕奸分_奸^錢b 子尺寸及BET表面積所特徵化。藉由掺合該 及較大尺寸氫氧化難子分佈,我們可潛在地齡在某^ 聚合物樹織騎f的抗_加_總量。 〜Nanocomposites, Giannilis, Adv· Mater·1996, 8, No. 1,29. Unlike in-situ t- or &gt; trough liquid intercalation, melt spalling involves only soil minerals and polymers without the need for a dilatant or dispersion medium. However, a swelling agent can be used to enhance the secret of the soil mineral by the specific polymer. On the ride, the mineral and polymer are mixed and heated to a temperature above the polymerized recording point. In the nano-alumina/polymer nanocomposite, two types of lions are possible. Wherein the structure is inserted, wherein the single-extended polymer bond is inserted into the layer to have a good ordering reduction of the parent polymer/inorganic layer. In another, termed non-sequential or delaminated, the inorganic layer is substantially uniformly dispersed in the polymer at random orientations in the polymer matrix. In a preferred embodiment, the nano-soil used in the present invention is obtained from magnesium sulfate, an anionic dry soil containing Mg and an inorganic plate of A1, one of which has 18 =:==:=3 200823148 m. The above-described sub-micron magnesium hydroxide composition and/or nano-material (which is also referred to herein as "reading surface can be mixed with other flame-resistant materials" such as other hydroxide ages before being incorporated into the polymeric resin. For example, the sub-micron additive can be mixed with a commercially available hydroxic acid tilting composition, such as MAGSHIELD® S or MA_ELDOTp hydrogenation product. If the submicron additive scale dihydrogen oxide particles are blended, the submicron = touch type The amount is present in an amount of at least about 3 weight percent of the total weight of the oxidized town particles and the sub-microf-additive, more preferably at least about ubiquinone and at least about J0%. In one embodiment The submicron additive of the present invention is present in an amount of from about 3% to about 30% by weight based on the total weight of the submicron additive to other anti-Sakis, such as other recorded particulate particles, preferably from about 3% to about I5% by weight. Exist, 曰, and this hair touch (Channai® soil material) The mixed larger size magnesium hydroxide particle distribution typically consists of a D50 of at least about 0.9 microns (e.g., D5 约 from about 1 to about 8 microns) and no more than about π square a ft. Preferably, it does not exceed about % square meters per gram, and most preferably does not exceed about 15 + square meters per square meter of surface area. Suitable for mixing magnesium oxide particles with the composition of the present invention. The form of the distribution is also suitable for use as a particulate material in the feed slurry used to make the submicron hydroxide hydride composition. As can be appreciated, the blend of the submicron magnesium hydroxide composition and the second particle distribution of the present invention is known. The particle composition produced by the composition is characterized by the two sub-sizes and the BET surface area of the blended smear and the BET surface area. We can potentially age in a certain polymer tree weaving f anti-plus_ total amount.

在另-方面,本翻提供—種聚餘組合物,及一種 由此製造的㈣,其包含本翻錢錢植馳合物及/ 或奈米枯土及合成縣合樹脂,該聚合觸可為如敎塑性 樹脂、熱樹脂、或彈性體。典型言之,該聚合物係落 在下列聚合物類別的其中—個:聚烯烴、聚驗(包含所有環 氧樹脂、聚縮酸、聚晴綱、聚_醯亞胺、及聚(二苯喊))、 聚醯胺(包含聚脲)、聚醯胺醯亞胺、聚芳香酯、聚苯咪唑、 ?«(包含聚碳酸醋)、聚氨基甲酸醋、聚醯亞胺、聚酿耕、 盼式樹鈿、聚石夕烧、聚;ε夕氧烧、聚礙化二亞胺、聚亞胺、 偶氮聚合物、多硫化合物、及聚石風。 要與本發明氳氧化鎂粒子(或奈米粘土)掺合的合成樹 脂較佳為一種一般用於產生模製物件的合成樹脂,如由烯 烴(α-烯烴)聚合物及共聚物所示例例如聚乙烯(如高密度 聚乙稀、低密度聚乙烯、線性低密度聚乙烯、及超低密度 聚乙烯)、聚丙烯、乙烯/丙烯共聚物、聚丁稀、及聚(4_甲 基小戊稀);浠烴與二烯的共聚物(例如乙烯_1_丁稀共聚 物、乙烯-4-曱基戊烯共聚物、丙烯小丁烯共聚物、及丙烯 -4-曱基-1-戊烯共聚物);乙烯-丙浠酸酯共聚物(例如乙烯丙 烯酸乙酯樹脂(ΕΕΑ)、乙烯丙烯酸甲酯共聚物樹脂(ΕΜΑ)、 及乙烯丙烯酸酯共聚物樹脂(ΕΑΑ));聚苯乙烯及苯乙烯共 20 200823148 聚物例如丙烯腈-丁二烯-苯乙烯(ABS)、丙烯腈-苯乙烯共聚 物(AS)、及丙烯腈-丙烯酸酯_苯乙烯(AAS);熱塑性聚烯烴 (TPO);乙烯基氯或醋酸乙烯酯聚合物或共聚物例如聚氯乙 烯、聚醋酸乙烯酯、聚偏二氯乙稀、乙烯_乙烯基氯共聚物、 及乙烯-醋酸乙烯酯共聚物(EVA);苯氧基樹脂;聚縮醛; 聚醯胺樹脂例如耐綸-6及耐綸-66 ;丙烯酸樹脂及甲基丙烯 酸樹脂,丁二烯;聚氨基甲酸酯;聚酯(例如聚對苯二曱酸 乙二醇酯(PET)及聚對苯二甲酸丁二醇酯(pBT);聚碳酸 酯;聚酮;鄰苯二酸二烯丙酯樹脂;酚式樹脂;環氧樹脂; 三聚氰醯胺樹脂;醇酸樹脂;尿素樹脂;及橡膠例如丁苯 橡膠(SBR)、乙烯-丙烯-雙烯單體(EpDM)、丁二烯橡膠 (BR)、氯丁二烯橡膠(CR)、氯化聚丁烯橡膠(CpE)、氯石黃化 ^^乙細(CSM)、丙細腈-丁二烯橡膠(nbr)、異戊橡膠(JR)、 丁基橡膠(IIR)、氨基曱酸甲酯橡膠、丙烯酯橡膠、矽酮橡 膠、及氟橡膠。 合成性♦合物可為任何前述聚合物的均聚物、無規則 共聚物、嵌段共聚物、交替共聚物、無酬三元聚合物、 嵌段三元聚合物、交替三元聚合物、其彳杜物(例如其接枝 共水物、自曰類、或_類)、及其類似物。在本發明不認 合物分子量是限制因子,及數量平均分子量典型上在^約 250至超過500,000Da的範圍,雖然可使用任何分子量且不 偏離本發明。 聚合物樹脂組合物進一步包含在該技藝中已知的一或 更多添加劑且不偏離本發明。示例進一步添加劑包含,但 21 200823148 :‘色Μ(例如,螢光染料及顏料)、氣 增塑劑、耐衝擊改質劑、填料、成核劑、潤_脫= 舌 2劑劑、除了本發明氫氧化鎂粒子之外的抗焰劑、 女疋以、抗氧化劑、殺菌劑、金屬減活劑、增稠劑、 麵㈣丨卜消沫劑、聚合物合金相容劑、触劑、乳化劑、 父聯&quot;式七丨、蝶、顆粒、助流劑、及添加以加強加工性或聚 f成份的終端使祕質的其他物質。此種添加劑可以習知 里使用,及典型上不會超過1〇%總組合物重量。 要添加至聚合樹脂的抗焰添加劑的總量,表示氫氧化 鎂所有粒子分似财本㈣讀米添加劑(例如次微米 氫氧化鎂或奈米粘土)的總量,可變化及依據各種因素而 定,包含所欲抗焰程度、聚合樹脂形式、所要形成 物件、及其類似因子。典型言之,抗焰添加劑的總量會在 約1至約80重量百分比基於聚合樹脂(具有添加劑)的總重 量,更佳為約35至約80重量百分比,及最佳為約5〇至約 80重里百分比,基於聚合樹脂及抗焰添加劑的總量。較佳 為加入足量的抗焰添加劑,例如足量的氫氧化鎂或奈米粘 土,以得到至少V2或更佳,較佳為V1或更佳及最佳為 V0的UL94(裝置及器具有中部件的塑膠材料之可燃性的測 試標準,第 5 版;Underwriters Laboratories Inc·)級。而且 較佳為加入足量的氫氧化鎂或奈米粘土以得到不超過約 270焦耳/公克·凱氏溫度、較佳為不超過約26〇焦耳/公克· 凱氏溫度、及最佳為不超過約250焦耳/公克·飢氏溫度的 熱釋放量(HRC)。 ^ 22 200823148 如上文所指出’抗焰添加劑可包含如此處所敘述的奈 米粘土材料或次微米氫氧化鎂組合物與其他抗焰添加劑如 車乂大尺寸氫氧化鎂粒子分佈的組合。此種組合包含較大尺 寸氫氧化鎂粒子分佈例如與奈米粘土合併的 MAGSHIELD(DS 或 MAGSHIELD®UF 氫氧化鎂產物、與 根據本發明次微米氳氧化鎂粒子分佈合併的較大尺寸氯氧 化鎂粒子分佈、及與奈料社及次微米氫氧化鎂粒子組合 物皆合併的較大尺寸氫氧化鎂粒子分佈。在添加至該聚合 物樹脂之前,該組合物可為緊密混合物形式,或是該二或 更多抗焰添加劑可分別地分散於聚合物樹脂,在此種組合 2中’較大尺寸氫氧化鎂粒子分佈係典型上以約5㈣; 1百分比的量存在’基於總聚合物樹脂重量(含添加劑),更 佳為約5〇至約65重量百分比’及次微米氫氧化鎂或夺米 枯土城份細約2簡3〇重量百分_量存在,較佳為約 4至約20重量百分比’及最佳為約6至約15重量百分比。 此種添加敝合物典型上為可使用該聽+已知的 合裝置製備的混合物形式。 σ /tb 包含本發明氫氧傾組合物或其他抗麵加劑的聚人 組合物可藉由使用在該技藝中已知的任何方法及裳置: 合、捏和、及難合成性聚合物樹脂及氫氧傾粒= 他添加劑以形成均勻混合物㈣成。例如,氫氧轉粒ς 及聚合樹脂的混合物可使用開放式報、單螺桿、或錐螺 擠壓機、班伯里混煉機、或類似裳置炫化捏和之。又3干 樹脂混合物可使用該技藝中已知的任何方法,例如7成 23 200823148 =、擠壓成型、吹塑成型、壓縮成型、迴轉加工成型、吹 袋成膜、及類似方法而模製成為最後所欲物件的形狀。 使用上文所敘述合成性聚合物樹脂/氳氧化鎂粒子混 合物所形成的聚合物件可用於各種應用及產品,例如電力 傳运及通訊的電規及電線護套、各種電子裝置、汽車組件、 商業建築及住宅賴產品、大眾運輸交通工具產品、或是 在各種航空/防禦應用。 本發明次微米氫氧化雜合物亦可賊—種添加劑以 防止燃油電力工廠中因礦物燃料燃燒而造成的灰逢形成。 為達此目的’氫氧化鎂組合物可赠末形式、水性浆液形 式、或是以分散於碳氫化合物流體(例如2號油、煤油、或 機油)的形式使用。無論形式,在概前將氳氧化鎂 加至燃料油(例如6號燃料油)。在—個具體實施例, 声^化输合物係以約25至約8G重量百分比的濃 =刀重2=料油,基於分散液總重量,更佳為約30至約 f本發㈣―方面,本發贱氧蝴組合物,例如氧 鎂或石反酸鎂(例如菱鎂確、驗式碳酸鎮 可用做其他鎂衍生物製造的反應 反鎮石專) 合物的次微米尺寸,伽本發贱氧轉所 =預期為亦顯示相同次微米尺寸,其在許多應用為 本發明由下列非限制實例進一步說明。 實驗 24 200823148 實例1 次微米氫氧化鎂粒子製造 使用不同尺寸氧化糾製介冑於 ==式叫進行研究,起始測試係= 駕未至0.8轉的尺寸範_铺介f, 礙製時間_晰,_糊_賴=下= 表1In another aspect, the present invention provides a composition of the remainder, and a (4) manufactured thereby, comprising the present money and planting compound and/or nano-sand and a synthetic resin. It is a plastic resin, a thermal resin, or an elastomer. Typically, the polymer falls into one of the following polymer classes: polyolefin, polyassay (including all epoxy resins, polyacids, polysapphire, poly-imine, and poly(diphenyl) Shout)), polyamine (including polyurea), polyamidoximine, polyaryl ester, polybenzimidazole, ?« (including polycarbonate), polyurethane, polyimine, poly-farming , Hope tree mites, Ju Shi Xia, poly; oxime oxygen, agglomerated diimine, polyimine, azo polymer, polysulfide, and poly石 wind. The synthetic resin to be blended with the niobium oxide particles (or nanoclay) of the present invention is preferably a synthetic resin generally used for producing molded articles, as exemplified by olefin (α-olefin) polymers and copolymers, for example. Polyethylene (such as high density polyethylene, low density polyethylene, linear low density polyethylene, and ultra low density polyethylene), polypropylene, ethylene/propylene copolymer, polybutylene, and poly (4_methyl small) Pentene); a copolymer of a terpene hydrocarbon and a diene (eg, ethylene-1_butylene copolymer, ethylene-4-mercaptopentene copolymer, propylene small butene copolymer, and propylene-4-mercapto-1) -pentene copolymer); ethylene-propionate copolymer (for example, ethylene ethyl acrylate resin, ethylene methyl acrylate copolymer resin, and ethylene acrylate copolymer resin (ΕΑΑ)); Styrene and styrene total 20 200823148 Polymers such as acrylonitrile-butadiene-styrene (ABS), acrylonitrile-styrene copolymer (AS), and acrylonitrile-acrylate-styrene (AAS); thermoplastic polymerization Olefins (TPO); vinyl chloride or vinyl acetate polymers or copolymers such as polyvinyl chloride, polyacetic acid Ester ester, polyvinylidene chloride, ethylene-vinyl chloride copolymer, and ethylene-vinyl acetate copolymer (EVA); phenoxy resin; polyacetal; polyamine resin such as nylon-6 and resistant Polyene-66; acrylic and methacrylic resins, butadiene; polyurethane; polyesters (eg polyethylene terephthalate (PET) and polybutylene terephthalate ( pBT);polycarbonate;polyketone; diallyl phthalate resin; phenolic resin; epoxy resin; melamine resin; alkyd resin; urea resin; and rubber such as styrene butadiene rubber (SBR) ), ethylene-propylene-diene monomer (EpDM), butadiene rubber (BR), chloroprene rubber (CR), chlorinated polybutene rubber (CpE), chlorite yellowing CSM), acrylonitrile-butadiene rubber (nbr), isoprene rubber (JR), butyl rubber (IIR), methyl amino decanoate rubber, propylene ester rubber, fluorenone rubber, and fluororubber. The compound may be a homopolymer, a random copolymer, a block copolymer, an alternating copolymer, an unpaid terpolymer, a block terpolymer, an alternating terpolymer of any of the foregoing polymers. a ruthenium (for example, a grafted hydrophile, a ruthenium, or a genus thereof), and the like. The molecular weight of the unidentified compound in the present invention is a limiting factor, and the number average molecular weight is typically about 250. It is in the range of more than 500,000 Da, although any molecular weight may be used without departing from the invention. The polymer resin composition further comprises one or more additives known in the art without departing from the invention. Exemplary further additives are included, but 21 200823148 : 'Color enamel (for example, fluorescent dyes and pigments), gas plasticizers, impact modifiers, fillers, nucleating agents, moisturizing agents, etc., in addition to the magnesium hydroxide particles of the present invention Flame Retardant, Nvwa, Antioxidant, Fungicide, Metal Deactivator, Thickener, Noodle (4) 丨 消 Defoaming Agent, Polymer Alloy Compatibilizer, Contact Agent, Emulsifier, Parent Union &quot;丨, butterfly, granules, glidants, and other substances added to enhance the processing properties or the terminal of the polyf component to make the secret. Such additives are conventionally used and typically do not exceed 1% by weight of the total composition. The total amount of the flame-resistant additive to be added to the polymeric resin, which means that the total amount of all the particles of magnesium hydroxide is similar to that of the four-dimensional reading additive (for example, sub-micron magnesium hydroxide or nano-clay), which can vary and according to various factors. It contains the desired degree of flame resistance, the form of the polymeric resin, the article to be formed, and the like. Typically, the total amount of flame resistant additive will range from about 1 to about 80 weight percent based on the total weight of the polymeric resin (with additives), more preferably from about 35 to about 80 weight percent, and most preferably from about 5 to about 80% by weight based on the total amount of polymeric resin and flame resistant additive. Preferably, a sufficient amount of flame resistant additive, such as a sufficient amount of magnesium hydroxide or nanoclay, is added to obtain a UL94 of at least V2 or better, preferably V1 or better and most preferably V0 (device and device have Test Standard for Flammability of Plastic Materials for Medium Parts, 5th Edition; Underwriters Laboratories Inc.). Further preferably, a sufficient amount of magnesium hydroxide or nanoclay is added to obtain a temperature of no more than about 270 Joules/gram Kelvin, preferably no more than about 26 FJ/kg Kelvin, and most preferably no. A heat release (HRC) of more than about 250 Joules per gram of hunger. ^ 22 200823148 As indicated above, the flame resistant additive may comprise a combination of a nanoclay material or a submicron magnesium hydroxide composition as described herein with other flame resistant additives such as ruthenium large size magnesium hydroxide particle distribution. Such a combination comprises a larger size magnesium hydroxide particle distribution such as MAGSHIELD (DS or MAGSHIELD® UF magnesium hydroxide product combined with nanoclay, larger size magnesium oxychloride combined with submicron strontium oxide particle distribution according to the invention) a particle distribution, and a distribution of larger size magnesium hydroxide particles combined with both the Nass and the submicron magnesium hydroxide particle composition. The composition may be in the form of an intimate mixture prior to addition to the polymer resin, or Two or more flame-resistant additives may be separately dispersed in the polymer resin, and in this combination 2 the 'larger size magnesium hydroxide particle distribution system is typically present in an amount of about 5 (four); 1 percentage by weight based on the total polymer resin weight More preferably, it is from about 5 to about 65 weight percent 'and sub-micron magnesium hydroxide or smectites, about 2% by weight, preferably about 4 to about 20% by weight 'and most preferably from about 6 to about 15% by weight. Such added chelates are typically in the form of a mixture which can be prepared using the hearing + known combination device. σ /tb comprises the hydrogen oxyhydroxide of the present invention The composition of the compound or other anti-additive additive can be carried out by any method known in the art and used: kneading, kneading, and difficult-to-synthesize polymer resins and hydroxide deuterium = other additives To form a homogeneous mixture (IV). For example, a mixture of oxyhydrogenated ruthenium and a polymeric resin can be kneaded using an open-ended, single-screw, or conical screw extruder, a Banbury mixer, or the like. Further, the dry resin mixture can be molded by any method known in the art, for example, 7 into 23 200823148 =, extrusion molding, blow molding, compression molding, rotary forming, blow bag forming, and the like. Made into the shape of the last desired object. The polymer parts formed using the synthetic polymer resin / magnesium strontium oxide particle mixture described above can be used in various applications and products, such as electric gauges and wire sheaths for power transmission and communication. , various electronic devices, automotive components, commercial buildings and residential products, mass transit vehicle products, or in a variety of aerospace / defense applications. The submicron hydroxide complex of the present invention may also be a thief - species Additives to prevent the formation of ash in the fuel-electricity plant due to the burning of fossil fuels. For this purpose, the magnesium hydroxide composition may be in the form of a final form, an aqueous slurry, or a dispersion of a hydrocarbon fluid (eg 2 In the form of oil, kerosene, or engine oil. Regardless of the form, magnesium strontium oxide is added to the fuel oil (for example, fuel oil No. 6). In a specific embodiment, the sounding compound is about 25 to about 8 G weight percent of concentration = knife weight 2 = oil, based on the total weight of the dispersion, more preferably from about 30 to about f (4) - aspects, the hair oxygenating composition, such as magnesium oxide or stone counter Magnesium sulphate (for example, magnesite, test carbonic acid can be used as a reaction for other magnesium derivatives). The submicron size of the compound, the gamma oxime oxygen transfer = expected to show the same submicron size, Its many applications are further illustrated by the following non-limiting examples. Experiment 24 200823148 Example 1 Submicron Magnesium Hydroxide Particles Manufactured using different sizes of oxidative rectifications in the == formula, the initial test system = the size range of driving to 0.8 revolutions _ paving f, hindering time _ Clear, _ paste_赖=下=表1

介質大小, RPM 毫米 0.6-0.8 3,000 0.6-0.8 3,000 0.6-0.8 4,500 0.6-0.8 4,500 0.6-0.8 6,000 時間 小時 1 2 2 3 1 漿液的5¾% 55.8 55.8 55.8 50.4 50.4 D50,微米 0.51 0.44 0.75 0.858 0.864Media Size, RPM mm 0.6-0.8 3,000 0.6-0.8 3,000 0.6-0.8 4,500 0.6-0.8 4,500 0.6-0.8 6,000 Time Hour 1 2 2 3 1 53⁄4% of the slurry 55.8 55.8 55.8 50.4 50.4 D50, micron 0.51 0.44 0.75 0.858 0.864

由以上測試’發現增加的礙製機处施及增加的礙製 時間在碾磨Mg(OH)2顆粒的能力具有負面作用,觀察到保 持粒子在懸浮液的水因為贼方法的動能而吸收於新露出 的表面積上,及《絲度_,铺介f/Mg(卿接觸 面積的有效性降低。 為企圖修正此問題及進—步降低粒子大小,將礙製介 質尺寸減少至0.3毫米、藉由添加水將漿液的%固體減少至 少於抓、及齡雜機rpMs。儀製機進料聚液的⑽ 為1·70宅米,及這些試驗的結果示於下表2。 25 200823148 表2 毫米 RPM 時間,小時 漿液的 固體% D50,微 0.3 2,000 1 52.0 0.295 0.3 2,000 2 52.0 0.284 0.3 2,000 3 44.0 0.249 0,3 2,000 4 44.0 0.238 0.3 3,000 1 50.8 0.261 0.3 2,000 3 52.0 0.130 u 藉由進行這些改變,發現可在1小時碾製時間内,及 減少的碾製機RPMS產生具有胸小於〇·3毫米的Mg(〇H)2 顆粒。由14些結果賴增加的碾製時間絲幫助進一步的 粒子大小減少’ _是若%_保持在少於約55%及黏度 保持在少_ _厘泊。_有興趣的是在丨小時碾製時 間增加礙軸至3,_職3以纽⑽為咖微米的效 用,相較於在1小時時間間隔於2,000 RPM所產生的D50 為0.295¼米。然而’其他礙製機处^^及固體負载亦為有 效的。 . 實例2 人从米虱氧化鎂粒子製造的進一步實例 人併研ί 為G1至G.3微米的氫氧化餘子係藉由使用 ’丨貝研磨而產生。此雜機雄緒介質做 回流氣氧倾漿液喊作。持、_流該漿液直到得到戶= 26 200823148 介質粒子大小。研究許乡猶參數,包含介肢小 機馬達RPM、魏it概度、驗目體濃度、氣氧化錢^ 源、及添加劑的使用。產生標的產品的三種不同方法係 述於下文。 在此實例所使用的碾製設備係敘述如下·· 1·使用600毫升玻璃水冷卻碾製室的介質碾製 (DYNO⑧-Mill 型式 KDL)。 、 2·氨基甲酸甲酯葉輪。 3·漿液儲槽係為2公升體積的大漏斗或是4公升 鋼燒杯。、 4·頂置式電子攪拌器。 5·螺動式幫浦;Masterflex75l8_60揚程。 礙I 貝係為〇·3毫米氧化錯;比重為6 〇公克/毫升。 在此數據所敘述的測量係如下測量·· 1·使用 MICROMERITICSiDFLOWSORB II 2300 由 BET單點測量的表面積。 2·使用 MICR〇MERmCS®Sedigraph 5100 於水中(5〇 毫升水及3公克樣品)所測量的粒子大小。 3·由蒸發所決定的固體。 4·使用Brookfield黏度計型號RVDVII+3號針於1〇〇轉 每分鐘所測得的黏度。 A·產生0.17微米粒子大小及62.6平方公尺/公克表面 積的方法流程 FLOMAG⑧Η(得自 Martin Marietta Materials)漿液自 27 200823148 :固體含4開始,碾製機㈣以15GG毫升漿液填充至碾 衣機開始,接著在初始清洗期間500毫升漿液自碾製機除 ^碾裟械於3〇〇〇轉每分鐘啟動及將流動速度調整至μ 耄=/分鐘,將漿液排至儲槽,該儲槽為垂直接至碾製機進 料官線的2公升漏斗,此儲槽係在使用頂置式電子攪拌器 的固^攪拌下,漿液接著回流進人碾製機,總操作時間為 ^小時。在操作期間,在碾製期間以平均37.5毫升每ι7·5 分鐘將525毫升水加至產物,此產S 62·6平方公尺/公克表 面積及0·17微米介質粒子大小的最後產物。 在方法期間加入水,因為當FL〇MAG⑧Η的表面積增 加’漿液變得較稠。雖然未受限於任何特別理論,此係認 為是因為水於氫氧化鎂粒子及氯含量表面上的吸收。ι Β·產生0.103微米粒子大小及奶平方公尺/公克表面 積的方法流程 礙製水合 MAGCHEM⑧l〇-325Mg〇(得自 Martin Marietta Materials)產生此產物,MAGQjgM⑧ 1〇 325 係用 做不含氯物質的來源。測觸示氯含量為在碾製期間增加 漿液稠化的許多因素的其中一個。MAGCHEM(g)1〇_325在 25石旁/平方英吋於局壓鋼水合4小時,如在頒給·沈等的 RE36,369所敘述,其係以其全文併入做為參考。 燒失量(LOI)測試係用於決定Mg〇的水合程度,大於 30%的LOI典型上表* Mg0已轉化為氫氧化物形式。此測 試係由使用預先秤重量的氫氧化物樣品置於秤重掛禍而進 行,含有該樣品的坩堝置於&gt;85〇°C的爐子至少〗小時,將 28 200823148 掛禍及其内容物(現在轉細MgQ)於乾㈣冷卻,及之後 再秤重以決定《敏,其細百分比鱗報告,在此樣 口口的、水5產物的LOI為30.86%及表面積為5 49平方公 尺/公克。 25%漿液係在藉由蒸氣壓力水合 之後產生’將15〇〇 t升漿液填充至該碾製機,接著在初始 清洗期間5GG毫升漿液自礙製機除去。碾製機於3_轉每 分鐘啟動及職純度難至125毫升纷鐘,將漿液排至 儲槽,該儲槽域直接至賴機轉管、_ 2公升漏斗, 此儲槽係在使_置式電子游器_定攪拌下,裝液接 著回流進从雜,總操作_三小時。在操作期間或之 後未添加水,此產生49.5平方公尺/公克表面積及〇1〇3微 米介質粒子大小的最後產物。92%的產物小於1微米。 C.產生0.103微米粒子大小及54.5平方公尺/公克表面 積的方法流程 製備30%漿液的FLOMAG(DH,將百萬分之1〇〇〇的 POLYMER VENTURES⑧PC-546加入,其係以總漿液體積 為基準。POLYMER VENTURES(DPC-546為一種陰離子胺 聚合物,接著將漿液通過325網目篩網,此係進行以移除 可能已存在於該漿液的任何44微米以上的粒子。碾製機進 料係將3500毫升漿液填充至該碾製機開始,接著在初始清 洗期間500晕升漿液自碾製機除去。碾製機於3〇〇〇轉每分 鐘啟動及將流動速度調整至98毫升/分鐘,將漿液排至^ 槽,該儲槽為垂直接至碾製機進料管線的4公升不鏽鋼燒 29 200823148 杯,此儲槽係在使用頂置式電子攪拌器的固定擾拌下,漿 液接著回流進入碾製機,總操作時間六小時。在操作期間 或之後未添加水,加入P〇LYMERVENTURES(g)PC-546以 抵銷於黏度的氯化物影響,此產生54.5平方公尺/公克表面 積及0·103微米介質粒子大小的最後產物。92%的產物小於 1微米。From the above test, it was found that the increased resistance time at the machine was found to have a negative effect on the ability to grind Mg(OH)2 particles, and it was observed that the water holding the particles in the suspension was absorbed by the kinetic energy of the thief method. The newly exposed surface area, and the "filament _, paved f / Mg (the effectiveness of the contact area is reduced. In an attempt to correct this problem and further reduce the particle size, the media size will be reduced to 0.3 mm, borrow The % solids of the slurry was reduced by at least water and the rpMs of the grinder. The (10) of the machine feed liquid was 1.70 house meters, and the results of these tests are shown in Table 2 below. 25 200823148 Table 2 MM RPM time, hourly slurry solids % D50, micro 0.3 2,000 1 52.0 0.295 0.3 2,000 2 52.0 0.284 0.3 2,000 3 44.0 0.249 0,3 2,000 4 44.0 0.238 0.3 3,000 1 50.8 0.261 0.3 2,000 3 52.0 0.130 u by making these changes It was found that the RPMS of the mill can produce Mg(〇H)2 particles with a chest less than 〇3 mm within 1 hour of milling time. The results of 14 results increase the grinding time to help further particles. Size reduction ' _ is if %_ remains at less than about 55% and the viscosity remains less _ _ centipoise. _ Interested in the increase in the hour of grinding time to 3, _ job 3 to New Zealand (10) for coffee micron The utility model has a D50 of 0.2951⁄4 m compared to 2,000 RPM at 1 hour intervals. However, 'other machine resistances and solid loads are also effective. Example 2 Man made from rice bran magnesium oxide particles Further examples of human and research are as follows: G1 to G.3 micron hydroxide is produced by using 'mussel grinding. This machine is used to make reflux gas oxygen slurry. Slurry until the household = 26 200823148 media particle size. Study Xu Xiang Ju parameters, including the small machine motor RPM, Wei it, the concentration of the test body, gas oxidation source, and the use of additives. Three different methods are described below. The milling equipment used in this example is described below. 1. 1) Milling of the grinding chamber (DYNO8-Mill type KDL) using 600 ml of glass water. 2. Carbamate Methyl ester impeller. 3. The slurry storage tank is a large funnel with a volume of 2 liters. Or 4 liters of steel beakers. 4. 4 overhead electronic mixers. 5. Screw-type pump; Masterflex 75l8_60 head. Obstacle I is 〇·3 mm oxidization error; specific gravity is 6 〇 g/ml. The measurements described are as follows: 1. The surface area measured by the BET single point using the MICROMERITICSi DFLOWSORB II 2300. 2. Particle size measured using MICR®MERmCS®Sedigraph 5100 in water (5 mL water and 3 g sample). 3. Solids determined by evaporation. 4. Use the Brookfield viscometer model RVDVII+3 needle to measure the viscosity per minute at 1 turn. A. Method for producing 0.17 micron particle size and 62.6 square meters per gram surface area FLOMAG8(R) (from Martin Marietta Materials) slurry starting from 27 200823148: solids containing 4, the milling machine (4) filling with 15 GG ml of slurry to the grinder Then, during the initial cleaning, 500 ml of slurry is removed from the grinding machine at 3 rpm and the flow rate is adjusted to μ 耄 = / minute, and the slurry is discharged to the storage tank. Vertically connected to the 2 liter funnel of the mill feed line, the tank was held under the agitation of the overhead electronic stirrer, and the slurry was then returned to the human mill for a total operation time of ^ hours. During the operation, 525 ml of water was added to the product at an average of 37.5 ml per 1 7 5 minutes during the milling, which yielded a final product of S 62·6 m 2 /g surface area and a media particle size of 0.17 μm. Water was added during the process because the surface area of the FL 〇 MAG8 增 increased and the slurry became thicker. Although not limited to any particular theory, this is believed to be due to the absorption of water on the surface of the magnesium hydroxide particles and chlorine content. ι Β Process method for producing 0.103 micron particle size and milk square meters per gram surface area hydrated MAGCHEM 8l 〇-325Mg 〇 (available from Martin Marietta Materials) to produce this product, MAGQjgM8 1〇325 is used as a chlorine-free substance source. The measured chlorine content is one of many factors that increase the thickening of the slurry during milling. MAGCHEM(g)1〇_325 is hydrated at 25 stonesides/square inch for local pressure steel for 4 hours, as described in RE36,369, to Shen et al., which is incorporated by reference in its entirety. The loss on ignition (LOI) test is used to determine the degree of hydration of Mg ,. LOI greater than 30% is typically shown in the table * Mg0 has been converted to the hydroxide form. This test was carried out by using a pre-weighed weight of the hydroxide sample in a weighing hazard. The crucible containing the sample was placed in a furnace of > 85 ° C for at least 〖 hours, and 28 200823148 was hanged and its contents (Now turn fine MgQ) to dry (four) cooling, and then weigh to determine "min, its fine percentage scale report, in this mouth, water 5 product LOI is 30.86% and surface area is 5 49 square meters / gram. The 25% slurry was produced after hydration by vapor pressure to fill the 15 Torr slurry to the mill, followed by removal of 5 GG ml of slurry during the initial wash. The mill is started at 3 rpm and the purity is difficult to reach 125 ml. The slurry is discharged to the storage tank. The storage tank is directly connected to the turret, _ 2 liter funnel. Set electronic _ _ stirring, the liquid is then refluxed into the impurities, the total operation _ three hours. No water was added during or after the operation, which resulted in a final product of 49.5 square meters per gram of surface area and 介质1 〇 3 micrometers of media particle size. 92% of the product is less than 1 micron. C. Method for producing a 0.10 micron particle size and a surface area of 54.5 square meters per gram of FLOMAG (DH, 1 part per million of POLYMER VENTURES 8PC-546, with a total slurry volume of Benchmark. POLYMER VENTURES (DPC-546 is an anionic amine polymer which is then passed through a 325 mesh screen which is used to remove any particles above 44 microns that may already be present in the slurry. Mill Feeder System Filling 3500 ml of slurry to the start of the mill, followed by 500 halo slurry removal from the mill during the initial wash. The mill was started at 3 rpm and the flow rate was adjusted to 98 ml/min. The slurry is discharged to a tank which is a 4 liter stainless steel fired 29 200823148 cup that is vertically connected to the mill feed line. The tank is placed under a fixed stirrer using an overhead electronic stirrer, and the slurry is then refluxed. Milling machine, total operation time of six hours. No water was added during or after the operation, P〇LYMERVENTURES (g) PC-546 was added to offset the chloride influence of viscosity, which produced 54.5 m ^ 2 / g .92% of the product and the final product is product-0 103 micron medium particle size less than 1 micron.

此實例說明介質碾製機可製造具有粒徑中央值為〇1 微米的氫氧化鎂,此方法可使用多種不同進料來源進行, 例如類似於FLOMAG⑧Η的漿液或是經水合氧化鎂,該方 法可使用稀釋至30%或更低的漿液,此稀釋可在碾製方法 期間或是碾製方法之前進行。祕製前__藉由陰離 子聚合物的使用而有利地伴隨以產生·的最麵製:在 方法期間藉由持續地稀釋槳液以保持碾製作用進行,或是 藉由使用添加劑如polymer VENTURES(g)pc_546而抵= 具有顯著氯化物含量例如FL〇MAG⑧H的起始裝液物質的 氯化物含量為重要的。使驗水合低氣化物來源的氧化鎮 液進料有效地除去氯化物觸製及漿液特徵如黏度 V ’丫夕曰 實例3 聚合物/Mg(〇H)2掺合及可燃性測試 為決定本發明次微米Mg(〇H)2的抗焰能 聚丙烯樹脂配方的不同尺寸的綱2其他樣4= ί 種氫氣化糕揭口祖— 厂/、他像口口相較。各 夺3。㈣frf 個樣品列出贈表面積及⑽於下 ^ 人‘只虱氧化鎂係標示為,次微米,。 、 30 200823148 表3 樣品名稱 表面積,平方公尺/ 公克 D50,微米 MAGSHIELD®S* 13.3 4.44 MAGSHIELDOUF* 13.6 0.96 Brucite(天然) 12.6 1.67 次微米 39.6 0.223 50%UF&amp;50%次微米 22.4 0.35 掺合物 *由 Martin Marietta Magnesia Specialties Inc,所製造的 商業可提供氫氧化鎂產物。 有趣的是指出MAGSHIELD⑧S或UF產品可用做進料 物質以產生次微米產物。如同我們可發現,當氫氧化鎂碾 製成較小的粒子大小時,在次微米物質的BET表面積存在 顯著增加。 ' 以上樣品可與聚丙烯、硬脂酸約、及塑膠穩定劑於 BRABENI^ERd)流變儀掺合(5〇公克樣品)。樣品包含· 至65%重量的氫氧化鎂、〇·75重量百分比硬脂酸辦除了一 個樣品具有額外硬編_如下文所指出)、及Q2重量百分 ==劑_m(每—個掺合物進行三次重複)係於 〇〇c進仃及決定轉矩。結果說明於下表4。 31 200823148 表4 樣品 次微米 50%UF&amp;50%次微米 次微米This example illustrates that a media mill can produce magnesium hydroxide having a median particle size of 〇1 μm. This method can be performed using a variety of different feed sources, such as a slurry similar to FLOMAG8® or hydrated magnesium oxide. Using a slurry diluted to 30% or less, this dilution can be carried out during the milling process or prior to the milling process. Before the secret __ is advantageously accompanied by the use of an anionic polymer to produce the most complete: during the process by continuously diluting the paddle to keep the mill running, or by using additives such as polymer VENTURES (g) pc_546 ̄ = The chloride content of the starting liquid-containing material having a significant chloride content such as FL 〇 MAG8H is important. The oxidized town liquid feed of the hydrated low vapor source is effectively removed to remove chloride slip and slurry characteristics such as viscosity V '丫例3 Polymer/Mg(〇H)2 blending and flammability test Invented sub-micron Mg (〇H) 2 anti-flame energy polypropylene resin formula of different sizes of the other 2 4 = ί hydrogenated cake Jiekou ancestors - factory /, he is like mouth. Each wins 3. (d) The frf samples are listed for the surface area and (10) are listed below. , 30 200823148 Table 3 Sample name surface area, square meter / gram D50, micron MAGSHIELD® S* 13.3 4.44 MAGSHIELDOUF* 13.6 0.96 Brucite (natural) 12.6 1.67 submicron 39.6 0.223 50% UF &amp; 50% submicron 22.4 0.35 blend * Commercially available from Martin Marietta Magnesia Specialties Inc. to provide magnesium hydroxide products. It is interesting to note that MAGSHIELD8S or UF products can be used as feed materials to produce sub-micron products. As we have found, there is a significant increase in the BET surface area of sub-micron materials when magnesium hydroxide is milled to a smaller particle size. 'The above sample can be blended with polypropylene, stearic acid, and plastic stabilizer in BRABENI^ERd) rheometer (5 gram sample). The sample contains · up to 65% by weight of magnesium hydroxide, 〇·75 wt% stearic acid except one sample with additional hard coding _ as indicated below), and Q2 weight percent == agent _m (per-dosing The compound was repeated three times) and the torque was determined. The results are illustrated in Table 4 below. 31 200823148 Table 4 Samples Submicron 50% UF &amp; 50% submicron Submicron

轉矩,公尺-公各 340-360 340-360 320-330 320-330 280-300 240-260 次微米&amp;3 %硬脂酸鈣 MAGSHIELD®S MAGSHIELD0UF Brncite(天然)Torque, meter-gong 340-360 340-360 320-330 320-330 280-300 240-260 submicron &amp; 3% calcium stearate MAGSHIELD®S MAGSHIELD0UF Brncite (natural)

數據顯示包含樣品的次微米產生最高轉矩值,為減少 次微米/聚丙烯掺合物的轉矩,加入額外硬脂酸約至3%次 微米/聚丙雜合物重量的含量’此的癌減讀矩及產生粒 子於塑賴闕m散,使肢絲μ Bmdte樣品得 到最低轉矩值。為測試氫氧化鎂/聚丙烯掺合物的抗焰性, 提送上述樣品以進行微燃燒量熱儀分析,以三次重複測試 樣品及得到數據’測試職聚丙烯樣品以得到關於各種氳 氧化鎂於阻止樹脂燃燒的有效性之基線。 結果相關於尖峰熱釋出及係以熱釋放量(hrc)紀錄於 下表?:、有單位(焦耳/公克’凯氏溫度,得到HRC值及 此值自所選擇鮮的減少或增加顯示抗焰有效性。 E2_、極限氧心數’一般稱為氧指數,係根據AS™ -人二:Γ係為一種測量恰好維持氧氣及氮氣的流動 扣合物付靖細㈣氧濃度的火歧應峨。樣品暴 32 200823148 露於似躐燭狀位置及氧含量以氧百分比(體積)測量。不具有 抗焰劑的聚烯經具有約16%的氧指數,我們呼吸的空氣為 約21%的氧,高於21%氧的值顯示抗焰效果,L〇I結果亦 紀錄於下表5。 表5 樣品 熱釋放量 LOI 100%聚丙烯 1183 16 Brncite-天然 402 25 MAGSHIELD ⑧ S 300 28 MAGSfflELD®UF 288 28 次微米 261 29 次微米&amp;3 %硬脂酸妈 250 30 50%UF&amp;50°/。次微米 捧合物 254 30 如預』戶斤有氫氧化鎂提供抗焰性予樹脂,但是含有 樣品的次微米提供最低聰 MAGSHIELDWF具有0.96微米的 D50,其提供鲂呈古 了丨w的MAGSHIELTOS為佳的於樹脂的分 -欠值。但當使用具有G.223微米的⑽的 HRC^ 寺,得到較祖〇瞻LTOUF樣品為佳的 子於翁ΊΓ咸少,此改善極有可能幫助較小次微米粒 微求“的更佳3散^加=外硬脂酸辦更加強次 刀放因為硬月曰酸_用做潤滑劑當其炫化 33 200823148 時,其幫助更佳分佈次微米粒子,及產生HRC值更降低 Π單位(自261至250)。此外,次微米粒子於 MAGSHIELD⑧UF的50%添加,提供較1〇〇% MAGSHIELD(DUF配方降低34 HRC單位。雖然這些測試 係以聚丙烯樹脂進行,類似益處亦可預期於不同樹脂混合 物得到。 實例4 ♦ δ物/Mg(〇H)2及聚合物/紹碳酸鎂換合及可燃性測 試 、 圓錐量熱儀熱釋放決定係在包含聚丙烯及各種氫氧化 鎂或鋁碳酸鎂添加劑的五個不同10公分直徑圓形皿(3 2毫 米厚)上執行,圓錐量熱儀為一種根據ASTME 1354_〇如執 行的小型測試,及意欲顯示測試物質對可引起測試物質燃 燒的熱源之反應。在這些測試中,使用5〇千瓦/平方公尺 的入射熱,測試樣品受到此輻射能量,其模擬已良好發展 火的能量。此外,使用涉及將樣品置於檬檸爐及燒盡戶^有 機成份的灰化步驟評估該五個樣品以決定所存在填料的實 際量,所剩為金屬氧化物,金屬水合物量係由此氧化物二 餘物計算。 每一個樣品的配方係說明於下文: 控制組:此樣品係計晝為具有65%重量(基於總樣品重 量)magshield®uf氫氧化鎂且不具有任何進一步抗焰 添加劑,發現MAGSmELD®UF氫氧化鎂實際總量為 59.5%重量。 34 200823148 MM2 ·此樣品係計晝為具有6〇%重量 MAGSHIELD®UF氫氧化鎂及5%重量pERKALITETM銘石炭 酸鎂粒子(Akzo Nobel)。發現實際總填料含量為6〇·丨%(氫氧 化鎂及鋁碳酸鎂合併重量)。 MM3 ·此樣品係計晝為具有63%重量 MAGSHIELD®UF氫氧化鎂及2%重量pE跋ALITE™!呂碳 酸鎮粒子。發現實際總填料含量為重量。 ΜΜ5 ·此樣品係計晝為具有55%重量 MAGSHIELD®UF氫氧化鎂及10%重量根據本發明所製備 的-人破米Mg(OH)2 ,该次微米粒子具有o n微米粒子大小 及約44.4平方公尺/公克表面積。發現實際總填料含量為 64.3%重量。 ^ MM7 :此樣品係計晝為具有6〇%重量 MAGSHIELD(g)UF氫氧化鎂及5%重量根據本發明所製備 及用於樣品MM5的相同次微米Mg(〇H)2粒子。發現實際 總填料含量為64.9%重量。 、$ 因為在MAGSHIELD_氫氧化鎂及及其他抗焰添加 劑^存在總显差異,必須由圓錐量熱儀正規化結果。當變 化為小的(小於15%如同此處情況),正規化可經由簡單調 整技術完成,尖峰熱釋放值乘以所決定礦物填料量,將= 果除以原先所欲礦物填料量。 次微米氫氧化鎂粒子及鋁碳酸鎂粒子顯著減少尖峰熱 釋放及二分!邊釋放當與在目錐測試的控制組相較時。紹 石反酸鎂較次彳政米氫氧化鎂更為有效的。注意顯示顯 35 200823148 著差異(於重複測試)及所以可靠性為可質疑的。 大峰熱釋放(%PHR)減少及百分比3分鐘pHR減少結 果係示於下表6。 表6 %PHR減少 16.8The data shows that the submicron containing the sample produced the highest torque value, to reduce the torque of the submicron/polypropylene blend, adding additional stearic acid to the content of about 3% submicron/polypropylene hybrid weight' The subtraction of the moment and the generation of particles in the plastic 阙 阙 m scattered, so that the limb μ Bmdte sample to obtain the lowest torque value. To test the flame resistance of the magnesium hydroxide/polypropylene blend, the above samples were taken for micro-combustion calorimetry analysis, the test samples were repeated three times and the data 'test polypropylene samples were obtained to obtain various magnesium oxides. A baseline for preventing the effectiveness of resin burning. The results are related to the peak heat release and the heat release (hrc) recorded in the table below: :, there is a unit (Joules / gram 'Kelvin temperature, get the HRC value and this value from the selected fresh reduction or increase shows resistance Flame effectiveness. E2_, the number of limiting oxygen cores is generally referred to as the oxygen index, according to ASTM-Human 2: lanthanide is a kind of fire that should be used to measure the oxygen concentration of oxygen and nitrogen.样品.Sample storm 32 200823148 exposed in a candle-like position and oxygen content measured in percent oxygen (volume). Polyolefins without flame retardant have an oxygen index of about 16%, and we breathe about 21% of air. Oxygen, values above 21% oxygen showed anti-flame effect, and L〇I results were also recorded in Table 5 below. Table 5 Sample heat release LOI 100% polypropylene 1183 16 Brncite-natural 402 25 MAGSHIELD 8 S 300 28 MAGSfflELD® UF 288 28 times micron 261 29 times micron &amp; 3% stearic acid mother 250 30 50% UF &amp; 50 ° /. Submicron hand compound 254 30 If the pre- 』 斤 has magnesium hydroxide to provide flame resistance to the resin, But the submicron containing the sample provides the lowest Cong MAGSHIELDWF with 0.96 microns D50, which provides the MAGSHIELTOS of the ancient 丨w, is better than the sub-value of the resin. However, when using the HRC^ temple with G.223 micron (10), it is better to obtain the LTOUF sample. Weng Wei Xian Shao, this improvement is very likely to help the smaller sub-micron micro-seeking "more good 3 scattered ^ plus = external stearic acid to strengthen the secondary knife release because hard lunar acid _ used as a lubricant when it dazzles When it was 200823,148, it helped to better distribute submicron particles, and produced HRC values that were lower in Π units (from 261 to 250). In addition, submicron particles were added at 50% of MAGSHIELD8UF, providing more than 1% MAGSHIELD (DUF) The formulation reduces the 34 HRC units. Although these tests are carried out with polypropylene resin, similar benefits can be expected for different resin mixtures. Example 4 ♦ δ / Mg(〇H) 2 and polymer / magnesium sulphate blending and combustible The test, cone calorimeter heat release is performed on five different 10 cm diameter round dishes (32 mm thick) containing polypropylene and various magnesium hydroxide or aluminum magnesium carbonate additives. The cone calorimeter is a kind. Small tests performed in accordance with ASTM E 1354 It is intended to show the reaction of the test substance to a heat source that can cause the combustion of the test substance. In these tests, using 5 kW/m 2 of incident heat, the test sample is subjected to this radiant energy, which simulates the energy of a well developed fire. The five samples were evaluated using an ashing step involving placing the sample in a lemon broth and an organic component to determine the actual amount of filler present, leaving the metal oxide, the amount of metal hydrate being the oxide Remaining calculations. The formulation for each sample is described below: Control group: This sample is calculated to have 65% by weight (based on total sample weight) magshield®uf magnesium hydroxide and does not have any further flame resistant additives, found MAGSmELD® UF hydroxide The actual total amount of magnesium is 59.5% by weight. 34 200823148 MM2 · This sample is calculated to have 6〇% by weight of MAGSHIELD® UF magnesium hydroxide and 5% by weight of pERKALITETM Mingshi magnesium carbonate particles (Akzo Nobel). The actual total filler content was found to be 6 〇·丨% (magnesium hydroxide and aluminum magnesium carbonate combined weight). MM3 • This sample is calculated to have 63% by weight of MAGSHIELD® UF magnesium hydroxide and 2% by weight of pE跋ALITETM! The actual total filler content was found to be by weight. ΜΜ5 · This sample is calculated to have 55% by weight of MAGSHIELD® UF magnesium hydroxide and 10% by weight of the human broken rice Mg(OH)2 prepared according to the present invention, the submicron particles having on micro particle size and about 44.4 Square meter / gram surface area. The actual total filler content was found to be 64.3% by weight. ^ MM7 : This sample was calculated to have 6 % by weight of MAGSHIELD (g) UF magnesium hydroxide and 5% by weight of the same submicron Mg(〇H) 2 particles prepared according to the present invention and used for sample MM5. The actual total filler content was found to be 64.9% by weight. Because there is a general difference in MAGSHIELD_magnesium hydroxide and other anti-flame additives ^, the results must be normalized by a cone calorimeter. When the change is small (less than 15% as in this case), the normalization can be done by a simple adjustment technique, the peak heat release value multiplied by the determined amount of mineral filler, and the value = divided by the amount of mineral filler originally desired. Submicron magnesium hydroxide particles and aluminum magnesium carbonate particles significantly reduced peak heat release and binary release when compared to the control group tested in the eye cone. Shaoshi acid-reducing magnesium is more effective than Zizhengmi magnesium hydroxide. Note that the display shows the difference between 2008 and 200823 (and repeated tests) and so reliability is questionable. The Dafeng heat release (% PHR) reduction and the percentage 3 minute pHR reduction are shown in Table 6 below. Table 6 %PHR reduction 16.8

28.7 34.4 34.4 10.3 6.4 12.4 樣品 MM2 MM3 MM5 MM7 為支持這些物質提供顯著增加的可燃性保護之結論, 一種標準廣泛使用的可燃性測試,,於每—個樣品以 兩種厚度,3 2宅米及10毫米,操作。結果示於下表7, 及由對在測試中所評估的次微米氫氧化鎂及铭碳酸鎮物質 所進行的圓錐測试所顯示的確認了增加的可燃性保護。 表7 *^~刪 MM7 UL94 ~---—28.7 34.4 34.4 10.3 6.4 12.4 Sample MM2 MM3 MM5 MM7 provides a significant increase in flammability protection to support these substances, a standard widely used flammability test, in each sample in two thicknesses, 3 2 house meters and 10 mm, operation. The results are shown in Table 7, below, and the increased flammability protection was confirmed by the cone test performed on the submicron magnesium hydroxide and the carbonated material evaluated in the test. Table 7 *^~ Delete MM7 UL94 ~----

(3·2 毫米)V1 V〇 V0 VO VO UL94 (1·6 毫米)NR V1 V2 V2 V2 nr表示未評級。UL94V0結果因為測試方法的本質而 …、法正編匕’然而’此不會負面影響在此可燃性測試所有 36 200823148 測試樣品表現較控制組為佳的鈇认。 ==說明許多改善及‘二㈣體實施例會為熟 者所憶及關於擁有在先前敘述所呈現意旨的益 ’要了解本發明不限於所揭示特定具體實施例及 思各人已έ改善及其他具體實施例於所附申請專 寻疋名稱係於此處使用,它們係僅以一般及敘述觀點 使用及不為限制目的。 · 37 200823148 【圖式簡單說明】 無(3·2 mm) V1 V〇 V0 VO VO UL94 (1.6 mm) NR V1 V2 V2 V2 nr means unrated. The result of the UL94V0 is due to the nature of the test method..., the law is being compiled 'however' this will not adversely affect the flammability test in this 36 200823148 test sample performance is better than the control group. == </ RTI> </ RTI> <RTIgt; </ RTI> </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> </ RTI> <RTIgt; DETAILED DESCRIPTION OF THE INVENTION The specific names of the applications in the accompanying claims are used herein, and are intended to be · 37 200823148 [Simplified description] None

【主要元件符號說明】 無 38[Main component symbol description] None 38

Claims (1)

200823148 ^ 十、申請專利範圍: 1· 一種氫氧化鎂顆粒組合物,其包含氫氧化鎂粒子的一 第一分布,該第一分布具有不超過約0·30微米的 D50、不超過約1.5微米的D90及至少約35平方公尺/ 公克的BET表面積。 2.如申請專利範圍第1項的氫氧化鎂顆粒組合物,其中 該D50不超過約0.25微米。 3·如申請專利範圍第2項的氫氧化鎂顆粒組合物,其中 該D50不超過約0.22微米。 4·如申請專利範圍第1項的氫氧化鎂顆粒組合物,其中 該D90不超過約1.〇微米。 5·如申請專利範圍第1項的氫氧化鎂顆粒組合物,其中 該BET表面積至少約4〇平方公尺/公克。 6·如申請專利範圍第5項的氫氧化鎂顆粒組合物,其中 該BET表面積至少約5〇平方公尺/公克。 i; 7·如申明專利範圍第1項的氫氧化鎂顆粒組合物,其中 該顆粒以一表面活化劑塗佈。 &amp;如申請專利範圍第7項的氫氧化鎂顆粒組合物,其中 該表面活化_-跡酸或是其脑或脂類。 9·如申睛專利範圍第7項的氫氧化鎮顆粒組合物,其中 忒表面活化劑為硬脂酸約或硬脂酸。 10·如申清專利乾圍第i項的氫氧化鎂顆粒組合物,進一 步包含,該第-分布混合的氫氧化鎂粒子的一第二分 布4第一分布具有至少約〇·9微米的D5〇及不超過 39 200823148 約30平方公尺/公克的—3£丁表面積。 種抗焰添加劑組合物,其包含(a)氫氧化鎂粒子的一 第一分布,該第一分布具有至少約〇9微米的D5〇及 不超過約30平方公尺/公克的騰表面積;及⑼一第 二組合物,其包含①複數個奈米粘土粒子;(ii)氳氧化 鎮粒子的-第二分布,該第二分布具有不超過約〇3〇 微米的D50、不超過約〗.5微米的D9〇及不超過約% 平方公尺/公克的BET表面;或是㈣(〇及⑼的一組合。 A如申請專利範圍» 11項的抗焰添加劑組合物,其中該 第二組合物(b)包含氫氧化鎂粒子的該第二分布(切,及 該第二分布的D50不超過約0.22微米。 13·如申請專利範圍第11項的抗焰添加劑組合物,其中該 第二組合物(b)包含氫氧化鎂粒子的該第二分布⑴),及 該第二分布的D90不超過約ι 〇微米。 14·如申請專利範圍第11項的抗焰添加劑組合物,其中該 弟一組合物(扮包S虱氧化鎂粒子的該第二分布(丨丨),及 該第二分布的BET表面積至少約5〇平方公尺/公克。 15·如申請專利範圍第11項的抗焰添加劑組合物,其中該 弟一組合物(b)包含虱氧化鎂粒子的該第二分布(沿,及 该弟一分布的粒子係以一表面活性劑塗覆。 16·如申請專利範圍第15項的抗焰添加劑組合物,其中該 表面活性劑為一種脂肪酸或其鹽類或酯類。 17·如申請專利範圍f I5項的抗焰添加劑組合物,其中該 表面活性劑為硬脂酸詞或硬脂酸。 40 200823148 等 18.如申明專利範圍帛η項的抗焰添力口劑組合物,其中該 第二組合物(b)包含該奈米枯土粒子(〇,及該奈米社 粒子係得自紹碳酸鎂。 19· -種聚合性樹驗合物,其包含—合雜聚合物及如 申請專利範圍第1項的氫氧化鎂組合物的—混合物。 20·如申请專利範圍第19項的聚合性樹脂組合物,其中該 合成性聚合物係由烯烴(α_烯烴)聚合物及共聚物、烯 Γ ) 烴與二烯的共聚物、乙烯丙烯酸酯共聚物、聚苯乙烯 及苯乙烯共聚物、熱塑性聚烯烴(τρ〇)、乙烯基氣或醋 酸乙稀酯聚合物或共聚物、苯氧基樹脂、聚縮醛、聚 醢胺樹脂、丙稀基及曱基丙烯基樹脂、丁二烯、聚氨 基曱酸酯、聚脂、聚碳酸酯、聚酮、鄰苯二酸二烯丙 醋樹脂、齡式#f脂、環氧封脂、三聚氰醯胺;^脂、醇 酸樹脂、脲樹脂、及合成橡膠所組成族群選出。 21· —種經模製聚合物件,其包含如申請專利範圍第19項 I) 的聚合性樹脂組合物。 22·如申請專利範圍第21項的經模製聚合物件,其具有 VO、VI、或 V2 的一 UL94 等級。 23· —種聚合性樹脂組合物,其包含一合成性聚合物及如 申清專利範圍弟11項的抗焰添加劑組合物的一混合 物。 24·如申請專利範圍第23項的聚合性樹脂組合物,其中該 合成性聚合物係由烯烴(α-烯烴)聚合物及共聚物、烯 烴與二烯的共聚物、乙烯-丙烯酸酯共聚物、聚苯乙烯 41 200823148 及苯乙烯共聚物、熱塑性聚烯烴(ΤΡΟ)、乙烯基氯或酉普 酸乙烯酯聚合物或共聚物、苯氧基樹脂、聚縮醛、^ 醢胺樹脂、丙烯基及甲基丙烯基樹脂、丁二烯、聚氨 基甲酸酯、聚脂、聚碳酸酯、聚酮、鄰苯二酸二烯丙 酯樹脂、酚式樹脂、環氧樹脂、三聚氰醯胺樹脂、醇 酸樹脂、脲樹脂、及合成橡膠所組成族群選出。 25· —種經模製聚合物件,其包含如申請專利範圍第23項 的聚合性樹脂組合物。 26.如申請專利範圍第25項的經模製聚合物件,其具有 VO、V卜或V2的一 UL94等級。 27·如申請專利範圍第23項的聚合性樹脂組合物,其中該 抗焰添加劑組合物係以基於該聚合樹脂組合物的總量 的約50至約80重量百分比的量存在。 28·如申請專利範圍第27項的聚合性樹脂組合物,其中該 聚合性樹脂包含基於該聚合樹脂組合物的總量的50 至、、、勺70重里百分比的虱氧化鎮粒子的第一分布①,及 約2至約30重量百分比的第二組合物(ii)。 29· —種氳氧化鎂顆粒組合物製造方法,其包含·· (a) 提供氫氧化鎂粒子或是氧化鎂粒子的一水性漿液,· (b) 於一珠磨機以一碾製介質及在足以產生氫氧化鎂 粒子漿液的條件下碾製該水性漿液一段時間,其中該 碾製介質具有不超過約〇·5毫米的一直徑,該氫氧化鎂 粒子漿液具有不超過約〇·3微米的一 D50、不超過約 1.5微米的一!)90及至少約35平方公尺/公克的一 ΒΕτ 42 200823148 衣旬檟,·及 (0在韻步卿獨轉下順㈣至少 體含錄持於不超過約㈣重 (=亥水性漿液_度維持在不超過約⑽厘泊 3°.=:範圍第29項的方法,其中該礙製步驟持續 、习1主約6小時。 儿專利範圍第29項的方法, :田以水性漿液係維持於不超過約55%重量的一固體 含量。 兑如申請專利範圍第29項的方法,其中在礙製步驟期 間,该水性漿液的黏度係維持在不超過約800厘泊。 33·如申請專利範圍第四項的方法,其中維持該水性聚液 的黏度在不超過約1,〇〇〇厘泊的該步驟包含在該碾製 步驟之前或期間加入黏度調節劑於該水性漿液。 34·如申請專利範圍第Μ項的方法,其中該礙製介質具有 約0.1至約0.3毫米的直徑。 、/' 35·如申請專利範圍第29項的方法,其中該碾製介質由氧 化锆、矽酸锆、釔摻雜四方晶锆多晶體、不鏽鋼、及 碳化鎢所組成族群選出。 36·如申請專利範圍第29項的方法,其中該礙製介質為一 種具有密度約3·〇至約6.8公克/立方公分的氧化鍅基 介質。 43 200823148 37·如申請專利範圍第29項的方法,其中在該碾製步驟期 間該珠磨機的RPM維持在不超過約6,000及不低於約 2,000。 44200823148 ^ X. Patent Application Range: 1. A magnesium hydroxide particle composition comprising a first distribution of magnesium hydroxide particles having a D50 of no more than about 0.30 microns and no more than about 1.5 microns D90 and a BET surface area of at least about 35 square meters per gram. 2. The magnesium hydroxide particle composition of claim 1, wherein the D50 is no more than about 0.25 microns. 3. The magnesium hydroxide particle composition of claim 2, wherein the D50 does not exceed about 0.22 microns. 4. The magnesium hydroxide particle composition of claim 1, wherein the D90 does not exceed about 1. 〇 microns. 5. The magnesium hydroxide particle composition of claim 1, wherein the BET surface area is at least about 4 square meters per gram. 6. The magnesium hydroxide particle composition of claim 5, wherein the BET surface area is at least about 5 square meters per gram. The magnesium hydroxide particle composition of claim 1, wherein the particles are coated with a surface activator. &amp;A magnesium hydroxide granule composition according to claim 7, wherein the surface activation is - or a brain or a lipid thereof. 9. The oxidized granule composition of claim 7, wherein the cerium surfactant is stearic acid or stearic acid. 10. The magnesium hydroxide particle composition of claim i, wherein the second distribution 4 of the first distribution-mixed magnesium hydroxide particles has a first distribution of D5 of at least about 9 μm. 〇 and no more than 39 200823148 about 30 square meters / gram - 3 £ surface area. a flame resistant additive composition comprising (a) a first distribution of magnesium hydroxide particles having a D5 至少 of at least about 9 microns and a surface area of no more than about 30 square meters per gram; (9) a second composition comprising a plurality of nanoclay particles; (ii) a second distribution of oxidized oxidized particles, the second distribution having a D50 of not more than about 〇3 〇 microns, not more than about 〗. 5 micron D9 〇 and a BET surface of no more than about % square meters / gram; or (d) (a combination of 〇 and (9). A as claimed in the scope of the article » 11 flame resistant additive composition, wherein the second combination The material (b) comprises the second distribution of the magnesium hydroxide particles (cut, and the D50 of the second distribution does not exceed about 0.22 μm. 13) The flame resistant additive composition of claim 11 wherein the second The composition (b) comprises the second distribution (1)) of the magnesium hydroxide particles, and the D90 of the second distribution does not exceed about 1 μm. 14. The flame-resistant additive composition of claim 11, wherein The second distribution of the composition of the S-magnesium oxide particles (丨丨And the second distribution has a BET surface area of at least about 5 square meters per gram. 15. The flame resistant additive composition of claim 11, wherein the composition (b) comprises magnesium strontium oxide particles. The second distribution (the particles distributed along the same one is coated with a surfactant. The anti-flame additive composition of claim 15 wherein the surfactant is a fatty acid or a salt thereof. A flame-resistant additive composition as claimed in claim i, wherein the surfactant is a stearic acid or stearic acid. 40 200823148 et al. a flame-adding agent composition, wherein the second composition (b) comprises the nano-soil particles (〇, and the nano-particles are obtained from a magnesium carbonate. 19·-a polymeric tree complex And a polymerizable resin composition according to claim 19, wherein the synthetic polymer is composed of a polymerizable resin composition according to claim 19. Olefin (α-olefin) polymers and copolymers, Alkene 共聚物 ) a copolymer of a hydrocarbon and a diene, an ethylene acrylate copolymer, a polystyrene and styrene copolymer, a thermoplastic polyolefin (τρ〇), a vinyl or ethylene acetate polymer or copolymer, phenoxy Base resin, polyacetal, polyamide resin, acryl and mercapto propylene based resin, butadiene, polyamino phthalate, polyester, polycarbonate, polyketone, propylene terephthalate Resin, age-type #f grease, epoxy sealant, melamine, lipid, alkyd resin, urea resin, and synthetic rubber are selected from the group consisting of 21% - molded molded polymer parts, including The polymerizable resin composition of claim 19, wherein the molded polymer member of claim 21 has a UL94 rating of VO, VI, or V2. A polymerizable resin composition comprising a synthetic polymer and a mixture of a flame resistant additive composition as in the scope of the patent application. The polymerizable resin composition of claim 23, wherein the synthetic polymer is an olefin (α-olefin) polymer and copolymer, a copolymer of an olefin and a diene, and an ethylene-acrylate copolymer. , polystyrene 41 200823148 and styrene copolymer, thermoplastic polyolefin (ΤΡΟ), vinyl chloride or vinyl decanoate polymer or copolymer, phenoxy resin, polyacetal, phthalamide resin, propylene And methacryl-based resin, butadiene, polyurethane, polyester, polycarbonate, polyketone, diallyl phthalate resin, phenolic resin, epoxy resin, melamine A group consisting of a resin, an alkyd resin, a urea resin, and a synthetic rubber is selected. A molded polymer article comprising the polymerizable resin composition of claim 23 of the patent application. 26. The molded polymeric article of claim 25, which has a UL94 rating of VO, Vb or V2. The polymerizable resin composition of claim 23, wherein the flame-resistant additive composition is present in an amount of from about 50 to about 80% by weight based on the total amount of the polymer resin composition. [28] The polymerizable resin composition of claim 27, wherein the polymerizable resin contains a first distribution of cerium oxide granules of 50% by weight based on the total amount of the polymer resin composition. 1, and about 2 to about 30 weight percent of the second composition (ii). 29. A method for producing a bismuth magnesium oxide granule composition, comprising: (a) providing an aqueous slurry of magnesium hydroxide particles or magnesium oxide particles, (b) a grinding medium in a bead mill and The aqueous slurry is milled for a period of time sufficient to produce a slurry of magnesium hydroxide particles having a diameter of no more than about 〇5 mm, the slurry of magnesium hydroxide particles having no more than about 〇3 μm One D50, no more than about 1.5 microns! ) 90 and at least about 35 square meters / gram of a ΒΕ 42 4223 2323 衣 槚 · · · 衣 衣 韵 韵 韵 韵 韵 韵 韵 韵 韵 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四The method is maintained at a method of no more than about (10) centipoise 3°. =: range item 29, wherein the barrier step is continued, and the method of the first method is about 6 hours. The method of claim 29 of the patent scope, the field is an aqueous slurry system. Maintaining a solids content of no more than about 55% by weight. The method of claim 29, wherein the viscosity of the aqueous slurry is maintained at no more than about 800 centipoise during the barrier step. The method of claim 4, wherein the step of maintaining the viscosity of the aqueous polyliquid at no more than about 1, centipoise comprises adding a viscosity modifier to the aqueous slurry before or during the milling step. The method of claim 2, wherein the barrier medium has a diameter of from about 0.1 to about 0.3 mm. The method of claim 29, wherein the grinding medium is made of zirconium oxide or hafnium. Zirconium silicate, yttrium doped tetragonal zirconium polycrystal, 36. The method of claim 29, wherein the barrier medium is a cerium oxide-based medium having a density of from about 3 Å to about 6.8 gram per cubic centimeter. The method of claim 29, wherein the bead mill RPM is maintained at no more than about 6,000 and no less than about 2,000 during the milling step.
TW096107056A 2006-11-27 2007-03-01 Flame-retardant magnesium hydroxide compositions and associated methods of manufacture and use TW200823148A (en)

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CN105492579A (en) * 2013-09-05 2016-04-13 伊奎斯塔化学有限公司 Low-smoke, non-halogenated flame retardant composition and related power cable jackets
CN110573340A (en) * 2016-12-12 2019-12-13 汉华阿兹德尔股份有限公司 composite article including a surface layer providing enhanced formability

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103930373A (en) * 2011-11-11 2014-07-16 堺化学工业株式会社 Hydrotalcite and method for producing same
CN103930373B (en) * 2011-11-11 2016-06-01 堺化学工业株式会社 Hydrotalcite and manufacture method thereof
CN105492579A (en) * 2013-09-05 2016-04-13 伊奎斯塔化学有限公司 Low-smoke, non-halogenated flame retardant composition and related power cable jackets
CN105492579B (en) * 2013-09-05 2017-12-01 伊奎斯塔化学有限公司 The power cable sheath of low cigarette, non-halogenated flame-retarding composition and correlation
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