200837103 九、發明說明: 【發明所屬之技術領域】 本發明係關於一種具高輝度與優異耐光性之聚矽氧粒 子、其製備方法、以及使用其之光擴散片。本發明尤其關 5 於一種具優異輝度與耐光性之聚矽氧粒子,並藉由表面處 理方式於該粒子表面上鍵結預定濃度之羥基,以提高其對 樹脂之可使用性與相容性;以及本發明有關於一種使用該 聚矽氧粒子之光擴散片。 【先前技術】BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polycrystalline oxygen particle having high luminance and excellent light resistance, a method for producing the same, and a light diffusion sheet using the same. The invention particularly relates to a polythene oxide particle having excellent brightness and light resistance, and bonding a predetermined concentration of hydroxyl groups on the surface of the particle by surface treatment to improve the usability and compatibility with the resin. And the present invention relates to a light diffusing sheet using the polysiloxane particles. [Prior Art]
聚石夕氧基粒子(例如聚倍半石夕氧烧(polysilsesquioxanQ 粒子與二氧化矽(silica)粒子)對於聚合物樹脂與有機物之 相容性通常相當優異,因此常應用於油漆、塑膠、橡膠、 、、、氏塗復’谷液用添加物、南畫質錄影帶用活化劑、以及類 15 似物。 尤其因為聚有機倍半石夕氧烧粒子為三維網狀分子锋 構,且其具有許多特性如光學折射率低、流動性佳以及對 樹脂之相容性。聚有機倍半矽氧烷粒子作為燈罩用擴散 劑、招牌、LCD背光以及光擴散片、或導光板用添加物月而 2〇 備受矚目。 此聚矽氧粒子之製備係經由使用甲基三烷氧基矽烷單 體之溶膠.凝膠法(其係由水解反應與縮合反應機構構成), 如日本早期公開專利號54-72300、63-077940、1〇_〇45914、 2〇〇〇-186148、以及類似專利所揭示。然而,當聚石夕氧粒子 5 200837103 用作為光擴散劑時會出現問 率差異造成其光擴散性良好 致聚矽氧粒子之輝度降低。 題’因為雖㈣與樹脂之折射 ,但是因為其光穿透性劣化導 ,…了解決上述問題,日本早期公開專利號 2006-10819、1-172801、1-269902、1〇_8咖乙及颛似專^Poly-stones (for example, polysilsesquioxan Q particles and silica particles) are generally excellent in compatibility with polymer resins and organic materials, and are therefore often used in paints, plastics, and rubbers. ,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,, It has many properties such as low optical refractive index, good fluidity and compatibility with resins. Polyorganopyquid siloxane particles are used as diffusers for lampshades, signs, LCD backlights and light diffusers, or additives for light guides. The preparation of the polyfluorene oxide particles is carried out by a sol. gel method using a methyltrialkoxydecane monomer (which is composed of a hydrolysis reaction and a condensation reaction mechanism), such as an early Japanese patent. No. 54-72300, 63-077940, 1〇_〇45914, 2〇〇〇-186148, and similar patents. However, there is a difference in the rate of question when polychlorinated particles 5 200837103 is used as a light diffusing agent. The light diffusibility is good, and the luminance of the polyoxynene particles is lowered. [Because (4) and the refraction of the resin, but because of the deterioration of the light transmittance, ... to solve the above problem, Japanese Early Patent No. 2006-10819, 1-172801, 1-269902, 1〇_8Cai B and 颛like special ^
揭不控制樹脂組成物之比例與成份以提高其輝度之方去 然而丄上述控制樹脂組成物之比例與成份的^有限^ 故目前亟需一種藉由控制擴散劑本身 光性的新方法。 “輝度與耐 因此,本發明之發明人研發出一種具有優異輝度 光性之聚秒氧粒子,並藉由表面處理方式於聚有機 表面ΐ鍵結預定濃度之經基,以提高其對樹脂之 二去 與相谷性;以及研發出一種製備該聚矽氧粒子之 15 【發明内容】 本發明之-目的為提供一種具有優異輝度以及耐光性 之聚石夕氧粒子。 本毛明之另-目的為提供一種藉由對粒子表面進行 2〇 =處理而製備具有優異輝度以及耐光性之聚石夕氧粒子的方 法0 本發明之又一目的為提供一種藉由對粒子表面進行表 2處理使其對樹脂之可使用性與相容性被改善的聚砍氧粒 子0 200837103 之光::Γ之再—目的為提供一種應用本發明聚石夕氧粒子 本發明之其他目 利範圍而了解。 的與優點將可從隨後之敘述與申請專 本lx月知:i、種聚矽氧粒子,其表面經處理而具有約 0.7至1.0之含羥基指數(〇Η 。 該聚石夕氧粒子之製備係經由對聚有機倍半石夕氧烧粉狀 粒子進打表面處理以控制粒子表面上的羥基濃度,使該粒 子具有約0·7至1.0之含羥基指數。 10 15 在本發明之一實施例中,該聚矽氧粒子之製備係經 由·乾蚝聚有機倍半矽氧烷⑽抓㊁)乳膠 以製成粉末狀聚矽氧粒子;以及藉由乾燥或燒結該粉末狀 聚矽氧粒子以控制該粉末狀聚矽氧粒子表面的羥基濃度。 以上述方法製備之聚矽氧粒子可用作為擴散劑,並可 於製造光擴散片時與熱塑性樹脂一起使用,因為該聚矽氧 粒子具有優異發光與耐光性並且具有優異地對其他樹脂之 可使用性與相容性。 【實施方式】 本發明之聚矽氧粒子經過具有約〇·7至1·〇之如下式所 示之含羥基指數: 含羥基指數=[吸收位置於(3350〜3400〜3450 cnr1)] / [吸收峰位於(2920〜2970〜3020 cm-1)] 7 200837103 其中[吸收位置於(33 50〜3400〜3450 cm-b] : Si-OH吸收 峰,以及 [吸收位置於(2920〜2970〜3020 cnT1)] : Si-CH3吸收峰。 邊含备基指數等於Si-ΟΗ吸收峰數值(紅外線光譜範圍 3350〜3400〜3450 cm·1中)除以Si-CH3吸收峰數值(紅外線光 谱範圍2920〜2970〜3020 cm_1中)所獲得之數值。藉由ir(紅 外線)光5晋儀分析聚石夕氧粒子表面上的經基吸收濃度後,根 據上式即可獲得含羥基指數。此測量方法可測量與分析最 10 15It is not necessary to control the proportion and composition of the resin composition to increase the brightness thereof. However, there is a need for a new method for controlling the optical properties of the diffusing agent itself by controlling the ratio and composition of the above-mentioned controlling resin composition. "Thinness and Resistance" Therefore, the inventors of the present invention have developed a polysecond oxygen particle having excellent luminance lightness, and by surface treatment, a predetermined concentration of a warp group is bonded to a polyorganic surface to enhance the resin. And the development of a polyfluorene oxide particle. [Inventive] The present invention is directed to providing a polycrystalline oxygen particle having excellent luminance and light resistance. A further object of the present invention is to provide a method for preparing agglomerated particles having excellent luminance and light resistance by subjecting the surface of the particles to 2 〇 = treatment. Light-cut oxygen particles for improved usability and compatibility of resins 0 200837103 Light: Γ 再 — 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的 目的And the advantages will be known from the following description and application of the patent: i, polyoxynized particles, the surface of which has a hydroxyl group index of about 0.7 to 1.0 (〇Η. The preparation is carried out by surface treatment of polyorganopyquid oxynized powder particles to control the concentration of hydroxyl groups on the surface of the particles, so that the particles have a hydroxyl group index of about 0.77 to 1.0. 10 15 In the present invention In one embodiment, the poly-xylene particles are prepared by picking a latex from a polyorganopyquidoxane (10) to form powdered polysiloxane particles; and drying or sintering the powdered poly The oxygen-containing particles are used to control the concentration of the hydroxyl groups on the surface of the powdery polysiloxane particles. The polysiloxane particles prepared by the above method can be used as a diffusing agent, and can be used together with a thermoplastic resin in the manufacture of a light-diffusing sheet because of the polyoxyl The particles have excellent luminescence and light resistance and have excellent workability and compatibility with other resins. [Embodiment] The polyfluorene oxide particles of the present invention have the following formula having a formula of about 〇·7 to 1·〇. Hydroxyl index: hydroxyl group index = [absorption position at (3350~3400~3450 cnr1)] / [absorption peak at (2920~2970~3020 cm-1)] 7 200837103 where [absorption position at (33 50~3400~ 3450 cm-b] : S i-OH absorption peak, and [absorption position at (2920~2970~3020 cnT1)]: Si-CH3 absorption peak. The side-containing base index is equal to the Si-ΟΗ absorption peak value (infrared spectrum range 3350~3400~3450 cm· 1) Divided by the value of the Si-CH3 absorption peak value (infrared spectrum range 2920~2970~3020 cm_1). By ir (infrared) light 5 Jinyi analysis of the base absorption on the surface of the polysulfide oxide particles After the concentration, the hydroxyl group index can be obtained according to the above formula. This measurement method can measure and analyze the most 10 15
20 25 理想之羥基濃度範圍,而本發明之含羥基指數較佳係介於 約0.7至1·〇之間。 S含羥基指數超過約丨·〇時,因為聚矽氧粒子表面上有 大$羥基使得聚矽氧粒子與水之親合力增加,聚矽氧粒子 與樹脂之姊丨生會劣化。並且,因為注入與擠壓成形製程 期間會有療氣產生,所以含經基指數超過約1〇會造成可 用性大幅降低。另外,當含經基指數小於約G·?時,聚 粒子之輝度降低。 Λ 乳 精由有效調整含羥基指數 石夕氧粒子,可改m二Γ: 1 經基給聚 士/右身之光學特性,從而提供路易 心 5,酸酸(Lewis/Br〇nsted acid)特性於 機倍㈣氧烧料氧粒子表面之間。 …有 聚有機倍半石夕氧燒之結構通常表示為肌〜, ΪΓ/具之有番經基。本發明之聚有機倍㈣氧燒具有二如: 式1表不之重複單元: 巧如下 [式1] RSi〇i.5-x (〇Η) 8 200837103 其中R為具有1至6個碳原子之烷基(alkyl以⑽p)、具有工 至6個碳原子之乙烯基(vinyl gr〇up)、具有6至2〇個碳原子之 芳香族羥基(aryl group)、或具有6至2〇個碳原子之經烷基取 代的芳香族羥基,以及〇 < X <丨.5。 5 在本發明之一代表性示例中,R為甲基、乙基或苯基。 在工業方面,R較佳為甲基。在式!中,χ範圍為〇<χ<ι·5。 聚矽氧粒子表面上之羥基的吸收濃度\係以IR分析,因此可 根據前述算式得到含羥基指數。 本發明之聚矽氧粒子係經由表面處理該些聚有機倍半 10矽氧烷粉狀粒子以控制該些粒子表面之羥基濃度,使得由 上述异式得到之含羥基指數約介於〇.7至1〇之間。 表面處理可為熱處理、化學處理、或類似方式。較佳 為該些粒子以200至400°c之間的溫度進行熱處理,更佳為 200至300°C之間。 15 該些聚有機倍半矽氧烷粉狀粒子可經由使用烷基有機 石夕烧(alkyl〇rganosilane)作為單體之溶膠-凝膠法進行製 備如日本早期公開專利號54-72300、63-077940、 1〇-〇45914、2000-186148、以及類似專利所揭示之技術。然 而,製備該些粒子之方法並非限定於一種特定方法。 在本發明之一實施態樣中,製備該些聚矽氧粒子之方 法包括下列步驟:乾燥聚有機倍半矽氧烷乳膠得到粉末狀 聚矽氧粒子、以及經由乾燥或燒結該些粉末狀聚矽氧粒子 以控制該些粉末狀聚矽氧粒子表面上之羥基濃度,使得該 些粉末狀聚矽氧粒子之含羥基指數約介於〇·7至1〇之間。 200837103 忒聚有機倍半矽氧烷乳膠之製備係經由使用有機烷氧 基石夕院之溶膠-凝膠法,但不限定於此。 使用噴務乾煉裝置(direct spray dryer)於8〇至2〇〇cc之 間的溫度乾燥上述聚有機倍半矽氧烷乳膠可得到白色的粉 5 末狀聚秒氧粒子。 在本發明之一實施態樣中,上述聚有機倍半矽氧烷乳 #可恢復成白色粉末狀聚石夕氧粒子,其係使用離心機、壓 濾機、震動篩(vibrating screen)或類似裝置將聚有機倍半矽 氧烷礼膠脫水以製備成泥狀物,接著清洗此脫水之泥狀物 10以去除雜質,接著使用旋轉閃蒸乾燥機(spin flash dryer)、 真空乾燥機、或類似裝置K8〇s20〇t:之間的溫度將此已去 除雜質之泥狀物乾燥。 所得到的粉末狀聚矽氧粒子具有之含水量約為5%或 以下,較佳為3%或以下,並且其經過第二次乾燥或燒結步 15 驟之後可製成本發明之聚石夕氧粒子。 聚矽氧粒子之羥基濃度係經由乾燥或燒結步驟來控 制’並且此乾燥或燒結步驟係於2〇〇至4〇〇〇Ci間進行。此 乾燥或燒結步驟約進行3〇分鐘至3小時,較佳約為小 時。 20 在本發明之一實施態樣中,藉由於鍛燒器如窯狀旋轉 乾燥的(kiln rotary dryer)或熱波爐(convecti〇n 〇ven)以 2〇〇 至400 C之間的溫度乾燥和燒結粉末狀聚矽氧粒子約3〇分 鐘至3小日守,使聚石夕氧粒子之含經基指數控制於約〇.7至1 ·〇 之間。 200837103 經表面處理而得到之聚有機倍半矽氧烷粒子的平均粒 徑約為0.1至20 μιη。 另一方面,本發明提供一種光擴散片,其使用上述聚 有機倍半矽氧烷粒子作為光擴散劑。此光擴散片可具有優 5 異輝度以及耐光性。 在本發明中,此光擴散片尤其適合作為LCD TV用之擴 散片。 在本發明之一實施態樣中,此光擴散片包括約0.1至10 重量份之該聚矽氧粒子以及約100重量份之熱塑性樹脂。 10 此光擴散片可以熟悉本發明技術領域之技藝者所周知 之方法製備。 該熱塑性樹脂可為氯乙稀樹脂(vinyl chloride resins)、苯乙稀樹脂(styrenic resins)、苯乙浠-丙稀腈基樹 月旨(styrene-acrylonitrile based resins)、丙:)# 酉曼才封月旨(acrylic 15 resins)、丙稀-苯乙稀基樹月旨(acryl-styrene based resins)、聚 酉旨樹脂(polyester resins)、ABS樹脂、聚破酸S旨樹脂 (polycarbonate resins)或其混合物。當本發明之聚有機倍半 矽氧烷粒子加入熱塑性樹脂時,此聚有機倍半矽氧烷粒子 會降低熱塑性樹脂的透光性。因此,使用此聚有機倍半石夕 20 氧烷粒子之LCD-TV用擴散板可具有優異輝度以及耐光性。 參考後敘實施例可進一步了解本發明,該些實施例之 目的為介紹本發明,並非限定本發明之申請專利範圍。 實施例 25 實施例1 200837103 將420g之曱基三甲氧矽烷(methyltrinieth〇xysilane)分 散於2580ml之蒸餾水中,並攪拌此溶液1小時。接著,於此 /合液中加入氨水調整其pH值至丨〇,並攪拌此調整過值之 溶液1小時。接著,將此攪拌過之溶液置於室溫中2小時以 5 ^成聚矽氧乳膠。接著,用離心機過濾和清洗此合成之乳 膠而得到約200§之白色細微粒子泥狀物。先用内部溫度 為16(TC外部溫度為8(rc之旋轉閃蒸乾燥機乾燥此聚甲氧 基L半石夕氧烧漿料,用以獲得 白色聚石夕氧粉末。#於200。〇用真空乾燥機二次乾燥此白色 10水秒氧物末2小日$,以提供有效且濃度經調整之經基於聚石夕 氧粉末表面。最後,得到含羥基指數為〇88之聚有機倍半矽 氧烧粒子。 實施例2 15 20 將37〇g”基三甲氧石夕烷以及,之甲基三氯石夕院 (methyhdch丨⑽silane)加入258_之離子交換水攪拌i小 時。將水性氨水加入此經授摔之溶液中以調整ph值至I 此經調整pH值之料靜置4小時進行反應。過濾、並清洗所得 到之產物後’再用喷霧乾燥機進行乾燥而得到細§之 著,於實施例1相同條件下先用旋轉閃蒸乾燥機乾 ^此白色粉末而得到白色㈣氧粉末。於窯狀旋轉乾燁号 中以2〇代二次乾燥此白色㈣氧粉末40分鐘,以提供有; 且浪度經調整之經基於聚%氧粉末表面。最後,^ 基指數為0.93之聚有機倍半矽氧烷粒子。 乙 12 25 200837103 實施例3 將 370g之 3- Μ 丙基三甲氧基矽烷 (3_mercaptopropyltrimethoxysilane)分散於 2580 ml之蒸顧水 中,再將50g 之3-氨基丙基曱氧基矽烷 5 (3-aminopropylmethoxysilane)此分散溶液中。接著,將此溶 液靜置於室溫中6小時。隨後,再用離心機攪拌以及清洗所 得到之溶液,而獲得200g之聚曱氧基倍半矽氧烷 (polymethoxysilsesquioxane)粒子漿料。將此聚石夕氧漿料注 入旋轉閃蒸乾燥機以160°C乾燥,得到白色聚矽氧粉末。將 10 此聚矽氧粉狀粒子置於窯狀旋轉乾燥器中用300°C乾燥40 分鐘來進行二次乾燥製程,用以表面處理此聚矽氧粉狀粒 子,使聚矽氧粉末表面具有有效且經控制之羥基。最後, 得到含羥基指數為0.80之聚有機倍半矽氧烷粒子。 15 實施例4 將 370g之 3-巯丙基三甲氧基矽烷 (3-mercaptopropyltrimethoxysilane)分散於2580 ml之蒸德水 中,再將50g 之3-氨基丙基甲氧基矽烷 (3-aminopropylmethoxysilane)此分散溶液中。接著,將此溶 20 液靜置於室溫中6小時。隨後,再用離心機攪拌以及清洗所 得到之溶液,而獲得200g之聚曱氧基倍半矽氧烷 (polymethoxysilsesquioxane)粒子漿料。將此聚石夕氧漿料注 入旋轉閃蒸乾燥機以160°C乾燥,得到白色聚矽氧粉末。將 此聚矽氧粉狀粒子置於窯狀旋轉乾燥器中用300°C乾燥2小 25 時來進行二次乾燥製程,用以表面處理此聚矽氧粉狀粒 13 200837103 子,使聚矽氧粉末表面具有有效且經控制之羥基。最後, 付到含基指數為〇 · 71之聚秒氧粒子。 比較例1 5 將42〇g之甲基三甲氧矽烷(methyltdmethoxysilane)分 散於2580ml之蒸餾水中,並攪拌此溶液丨小時。接著,於此 溶液中加入氨水調整其pH值至1〇,再攪拌此調整過pH值之 洛液1小時。接著,將此攪拌過之溶液置於室溫中2小時以 合成聚碎氧乳膠。接著,用離心機過濾和清洗此合成之乳 10膠,而得到約2〇〇g之白色細微粒子泥漿。用旋轉閃蒸乾燥 機以200 C之溫度乾燥此聚甲氧基倍半矽氧烷泥漿,而得到 白色聚石夕氧粉末。 比較例2 15 ^ 將 42〇g 之甲基三甲氧矽烷(methyltrimethoxysilane)分 散於2580ml之蒸餾水中,並攪拌此溶液丨小時。接著,於此 溶液中加入氨水調整其PH值至10,再攪拌此調整過pH值之 浴液1小時。接著,將此攪拌過之溶液置於室溫中2小時以 合成聚矽氧乳膠。接著,用離心機過濾和清洗此合成之乳 20膠,而得到約20〇g之白色細微粒子泥狀物。用真空乾燥機 以6〇〇°C之溫度乾燥此泥漿2小時。最後,得到含羥基指數 為〇·60之聚有機倍半矽氧烷粒子。 在上述實施例與比較例中,比較經過表面處理(改變溫 度與時間條件)之聚錢粒子之祕數量,並依據粒子表面 25之含經基指數而製備不同之聚石夕氧粒子。為了製備聚石夕氧 14 200837103 粒子加入母料(master batch)中用以射出成型擴散板,可藉 由孔徑為φ=45 mm之螺桿擠出機來製備粒子,而使聚矽氧 粒子、聚苯乙烯樹月旨、與EXL_5136(R〇hm&Haas製,usa) 以1 : 100: 1之比例混合。然後,於1〇 0z注射器中以21〇 5 °C之鑄造溫度可製得一厚度為1·5πππ之類板型樣品(簡易擴 散板)。羥基之最佳數量,也就是含羥基指數’可經由測量 所製得之類板型樣品的輝度而獲得。表丨列出各個實施例與 比較例中經過乾燥與表面處理製程之聚矽氧粒子經過讯分 析後,藉由上述含超基指數關係計算而得之含經基指數及 10 輝度。 經由上述製程得到之粒子的物理特性可由下述方法評 估’其結果列不於表1。 (1) 含經基指數之分析:藉由對聚矽氧粒子表面進行 IR分析’分析由上述含羥基指數關係所獲得之含羥基指數 15 後’比較彼此之經基數量。 (2) 輝度:經由擠壓和射出製程製備之五個擴散板樣 口口 之輝度可使用 Luminometer NL-1 (Nippon,Japan)連續測 ΐ °擴散板樣品上輝度之測量全部重複三次,採用平均值 來互相比較。 20 表1 含羥基指數 輝度 相對吸收度 實施例 1 0.88 2503 2 0.93 2891 15 200837103 3 T 0.80 〜------ 2596 ---—— - 0.71 2499 比較例 1 1.41 無法擠壓 2 0.60 ~___ 2400 ---------- 由表1可證實輝度會隨著經基數量減少而降低。因此, 反而適當濃度之經基(亦即最佳含經基指旬是必須的,而非 無限制地數量眾多的羥基(濃度)。 士比k例1所示’當聚石夕氧粒子表面存在數量眾多的經 基’也就是當X吸收増加時,聚石夕氧粒子與水之間的親合力 增加而使得其錢脂之相容性降低。並且,因為射出與擠 壓期間產生水②氣’使其可使用性降低,從而使擴散板射 出成型困難,而無法製得樣品。 因此’如表1所示,含羥基指數介於〇 7至1〇之間的實 施例1至4顯示出較佳輝度。 上文中,本發明係基於特定示例進行描述,然而熟悉 本發明技術領域之技藝者均知在不背離本發明之精神及後 文定義之申請專利範圍下可對本發進行各種改變與修飾。 【圖式簡單說明】 【主要元件符號說明】 1620 25 The desired hydroxyl concentration range, and the hydroxyl group index of the present invention is preferably between about 0.7 and 1 Torr. When the hydroxyl group index of S exceeds about 丨·〇, since the large amount of hydroxyl groups on the surface of the polyoxygen oxide particles increases the affinity of the polysiloxane particles with water, the twins of the polysiloxane particles and the resin deteriorate. Moreover, since the gas is generated during the injection and extrusion process, the warp index exceeding about 1 Å causes a significant decrease in usability. Further, when the warp-containing index is less than about G·?, the luminance of the polyparticles is lowered. Λ The milk essence can effectively adjust the hydroxyl-containing index of Shixi oxygen particles, which can be changed to m: 1 1 The optical properties of the base to the right/right body, thus providing the characteristics of Lewis/Br〇nsted acid In the machine (4) oxygen burning between the surface of the oxygen particles. ...the structure of polyorganic sesquitertes is usually expressed as muscle ~, ΪΓ / has a quilt. The polyorgano (tetra)oxygen of the present invention has the same as the following: The repeating unit of the formula 1 is as follows: [Formula 1] RSi〇i.5-x (〇Η) 8 200837103 wherein R is 1 to 6 carbon atoms An alkyl group (alkyl with (10) p), a vinyl group having 6 carbon atoms, an aryl group having 6 to 2 carbon atoms, or 6 to 2 An alkyl-substituted aromatic hydroxy group of a carbon atom, and 〇<X < X. 5 In a representative example of the invention, R is methyl, ethyl or phenyl. In industrial terms, R is preferably a methyl group. In style! In the middle, the range is 〇<χ<ι·5. The absorption concentration of the hydroxyl group on the surface of the polysiloxane particles is analyzed by IR, so that the hydroxyl group-containing index can be obtained according to the above formula. The polyfluorene oxide particles of the present invention are used to surface-treat the polyorganopyquioxalate powder particles to control the hydroxyl group concentration on the surface of the particles, so that the hydroxyl group index obtained by the above formula is about 〇.7 Between 1 。. The surface treatment can be heat treatment, chemical treatment, or the like. Preferably, the particles are heat-treated at a temperature between 200 and 400 ° C, more preferably between 200 and 300 ° C. 15 These polyorganosilsesquioxane powder particles can be prepared by a sol-gel method using an alkyl 〇rganosilane as a monomer, as disclosed in Japanese Laid-Open Patent Publication No. 54-72300, 63- Techniques disclosed in 077,940, 1 〇-45914, 2000-186148, and similar patents. However, the method of preparing the particles is not limited to a particular method. In one embodiment of the present invention, a method of preparing the poly-xonium oxide particles includes the steps of: drying a polyorganosilsesquioxane latex to obtain powdered polysiloxane particles, and drying or sintering the powdered poly The oxygen absorbing particles are used to control the concentration of the hydroxyl groups on the surface of the powdery polysiloxane particles such that the powdery polyoxynene particles have a hydroxyl group index of between about 至7 and 1 Torr. 200837103 The preparation of the ruthenium polysesquioxane latex is carried out by using a sol-gel method of an organic alkoxylate, but is not limited thereto. The above-mentioned polyorganosilsesquioxane latex was dried at a temperature between 8 Torr and 2 cc using a direct spray dryer to obtain white powder 5 terminal polysecond oxygen particles. In one embodiment of the present invention, the above polyorganopyoid sesquioxane # can be recovered into a white powdery polyoxoparticle, which is a centrifuge, a filter press, a vibrating screen or the like. The apparatus dehydrates the polyorganopyquioxane gum to prepare a sludge, and then washes the dehydrated sludge 10 to remove impurities, followed by a spin flash dryer, a vacuum dryer, or The temperature between the similar devices K8 〇 s20 〇 t: dries the mud from which the impurities have been removed. The obtained powdery polysiloxane particles have a water content of about 5% or less, preferably 3% or less, and can be formed into a polysulfide of the present invention after the second drying or sintering step 15 particle. The hydroxyl concentration of the polyoxynium particles is controlled via a drying or sintering step and the drying or sintering step is carried out between 2 Torr and 4 Torr. This drying or sintering step is carried out for about 3 minutes to 3 hours, preferably for about an hour. In one embodiment of the invention, the calciner is dried at a temperature between 2 Torr and 400 C by means of a calciner such as a kiln rotary dryer or a convecti〇n 〇ven. And sintering the powdery polyfluorene oxide particles for about 3 minutes to 3 hours, so that the inclusion base index of the poly-stone particles is controlled to be between about 77. 200837103 The surface treated polyadipenoid particles have an average particle diameter of about 0.1 to 20 μm. In another aspect, the present invention provides a light-diffusing sheet using the above-mentioned polyorganosilsesquioxane particles as a light diffusing agent. This light diffusing sheet can have excellent brightness and light resistance. In the present invention, the light diffusing sheet is particularly suitable as a diffusing sheet for an LCD TV. In one embodiment of the invention, the light diffusing sheet comprises from about 0.1 to 10 parts by weight of the polyoxynene particles and about 100 parts by weight of the thermoplastic resin. 10 This light diffusing sheet can be prepared by a method well known to those skilled in the art of the present invention. The thermoplastic resin may be vinyl chloride resins, styrenic resins, styrene-acrylonitrile based resins, C:) #酉曼才封Acryl 15 resins, acryl-styrene based resins, polyester resins, ABS resins, polycarbonate resins, or mixtures thereof . When the polyorganosilsesquioxane particles of the present invention are added to a thermoplastic resin, the polyorganosilsesquioxane particles lower the light transmittance of the thermoplastic resin. Therefore, the diffusing plate for LCD-TV using the polyorganossesquioxane particles can have excellent luminance and light resistance. The invention may be further understood by reference to the following examples, which are intended to illustrate the invention and not to limit the scope of the invention. Example 25 Example 1 200837103 420 g of methyltrinieth〇xysilane was dispersed in 2580 ml of distilled water, and the solution was stirred for 1 hour. Next, ammonia water was added to the mixture to adjust the pH to hydrazine, and the adjusted solution was stirred for 1 hour. Next, the stirred solution was allowed to stand at room temperature for 2 hours to form a polyoxyl latex. Next, the synthetic latex was filtered and washed with a centrifuge to obtain a white fine particle slurry of about 200 §. First, the internal temperature was 16 (the external temperature of the TC was 8 (the rc rotary flash dryer was used to dry the polymethoxy L-semi-stone slurry to obtain white poly-stone powder. #200.〇 The white 10 water sec. oxygen was allowed to be twice dried with a vacuum dryer for 2 hours to provide an effective and concentration-adjusted surface based on the poly-stone powder. Finally, a poly-organic ratio having a hydroxyl group index of 〇88 was obtained. Semi-oxygenated particles. Example 2 15 20 37 〇g"-based methoxy sulphite and methyl sulphate (methyhdch 丨 (10) silane) were added to 258 _ ion-exchanged water for 1 hour. Ammonia water is added to the dropped solution to adjust the pH to I. The adjusted pH value is allowed to stand for 4 hours to carry out the reaction. After filtering and washing the obtained product, it is dried by a spray dryer to obtain fine §, under the same conditions as in Example 1, the white powder was dried by a rotary flash dryer to obtain a white (tetra) oxygen powder. The white (tetra) oxygen powder was twice dried in a kiln-like rotary dried mash. 40 minutes to provide; and the wave is adjusted based on poly% oxygen powder Finally, a poly-organopyloxane particle having a base index of 0.93. B 12 25 200837103 Example 3 370 g of 3-mercaptopropyltrimethoxysilane was dispersed in 2580 ml of steamed water, Further, 50 g of 3-aminopropylmethoxysilane was dispersed in the solution. Then, the solution was allowed to stand at room temperature for 6 hours, and then stirred and washed by a centrifuge. The solution was used to obtain 200 g of a polymethoxysilsesquioxane particle slurry. The polysulfide slurry was poured into a rotary flash dryer and dried at 160 ° C to obtain a white polyoxyn powder. 10 The polyfluorene powder particles are placed in a kiln rotary dryer and dried at 300 ° C for 40 minutes for a secondary drying process for surface treatment of the polyfluorene powder particles to make the surface of the polyoxygen oxide powder effective. And a controlled hydroxyl group. Finally, a polyorganosilsesquioxane particle having a hydroxyl group index of 0.80 was obtained. 15 Example 4 370 g of 3-mercaptopropyltrimethoxysilane was classified. Disperse in 2580 ml of distilled water, and then add 50 g of 3-aminopropylmethoxysilane to this dispersion solution. Then, the solution 20 was allowed to stand at room temperature for 6 hours. The resulting solution was further stirred and washed with a centrifuge to obtain 200 g of a polymethoxysilsesquioxane particle slurry. This polysulfide slurry was poured into a rotary flash dryer and dried at 160 ° C to obtain a white polyoxynium powder. The polyfluorene powder particles are placed in a kiln-like rotary drier and dried at 300 ° C for 2 hours and 25 hours to carry out a secondary drying process for surface treatment of the polyfluorinated powder particles 13 200837103 to make the polythene The oxygen powder surface has an effective and controlled hydroxyl group. Finally, a polysecond oxygen particle having a base index of 〇·71 is applied. Comparative Example 1 5 42 g of methyltdmethoxysilane was dispersed in 2580 ml of distilled water, and the solution was stirred for several hours. Next, ammonia water was added to the solution to adjust the pH to 1 Torr, and the pH-adjusted solution was stirred for 1 hour. Next, the stirred solution was allowed to stand at room temperature for 2 hours to synthesize a polyaluminum latex. Next, the synthetic milk 10 was filtered and washed with a centrifuge to obtain about 2 g of a white fine particle slurry. The polymethoxysilsesquioxane slurry was dried at a temperature of 200 C using a rotary flash dryer to obtain a white polysulfide powder. Comparative Example 2 15 ^ 42 〇g of methyltrimethoxysilane was dispersed in 2580 ml of distilled water, and the solution was stirred for a few hours. Next, ammonia water was added to the solution to adjust the pH to 10, and the pH-adjusted bath was stirred for 1 hour. Next, the stirred solution was allowed to stand at room temperature for 2 hours to synthesize a poly-xyloxy latex. Next, the synthetic milk 20 was filtered and washed with a centrifuge to obtain about 20 angstroms of white fine particle sludge. The slurry was dried with a vacuum dryer at a temperature of 6 ° C for 2 hours. Finally, polyorganosil sesquioxanes particles having a hydroxyl group index of 〇·60 were obtained. In the above examples and comparative examples, the number of the particles of the surface-treated (changing the temperature and time conditions) was compared, and different poly-stone particles were prepared according to the basis index of the particle surface 25. In order to prepare the poly-stone oxygen 14 200837103 particles into the master batch for injection molding the diffusion plate, the particles can be prepared by a screw extruder with a pore diameter of φ=45 mm, and the poly-xonium particles are aggregated. The styrene tree was mixed with EXL_5136 (R〇hm & Haas, usa) in a ratio of 1:100:1. Then, a plate type sample (simple diffusion plate) having a thickness of 1.5 πππ can be obtained at a casting temperature of 21 〇 5 °C in a 1 〇 0z syringe. The optimum amount of hydroxyl groups, i.e., the hydroxyl group-containing index, can be obtained by measuring the luminance of a plate-like sample prepared. The table shows the warp-containing index and the 10-degree luminance calculated by the above-described superbase-based index relationship after the polysiloxane particles subjected to the drying and surface treatment processes in each of the examples and the comparative examples were subjected to signal analysis. The physical properties of the particles obtained through the above process can be evaluated by the following methods. The results are shown in Table 1. (1) Analysis of the warp-containing index: The number of the base groups of each other was compared by analyzing the surface of the polyoxynitride particles by IR analysis 'the hydroxyl group index 15 obtained from the above-mentioned hydroxyl group-containing index relationship. (2) Luminance: The luminance of the five diffuser-like mouths prepared through the extrusion and injection process can be continuously measured using Luminometer NL-1 (Nippon, Japan). The measurement of the luminance on the diffuser plate is repeated three times, using the average. Values are compared to each other. 20 Table 1 Hydroxyl index brightness relative absorbance Example 1 0.88 2503 2 0.93 2891 15 200837103 3 T 0.80 ~------ 2596 --- -- - 0.71 2499 Comparative example 1 1.41 Can not squeeze 2 0.60 ~___ 2400 ---------- It can be confirmed from Table 1 that the luminance decreases as the number of warp groups decreases. Therefore, instead of the appropriate concentration of the warp group (that is, the best contains the base of the base is necessary, rather than unlimited number of hydroxyl groups (concentration). The ratio of k is shown in Figure 1 'When the surface of the rock particles There are a large number of warp groups', that is, when X absorption increases, the affinity between the poly-stone particles and water increases, so that the compatibility of the money and fat is lowered. And, since the water is generated during the injection and extrusion 2 The gas 'is reduced in workability, making the diffusion plate injection molding difficult, and the sample cannot be produced. Therefore, as shown in Table 1, Examples 1 to 4 having a hydroxyl group index of between 〇7 and 1〇 show The present invention has been described above on the basis of specific examples, and it is to be understood by those skilled in the art that the present invention can be variously modified without departing from the spirit of the invention and the scope of the appended claims. And modification. [Simple description of the diagram] [Explanation of main component symbols] 16