JP2022537755A - 透明遮熱微粒子、微粒子分散体、その製法及び用途 - Google Patents
透明遮熱微粒子、微粒子分散体、その製法及び用途 Download PDFInfo
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- JP2022537755A JP2022537755A JP2021575521A JP2021575521A JP2022537755A JP 2022537755 A JP2022537755 A JP 2022537755A JP 2021575521 A JP2021575521 A JP 2021575521A JP 2021575521 A JP2021575521 A JP 2021575521A JP 2022537755 A JP2022537755 A JP 2022537755A
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- transparent heat
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Classifications
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C—CHEMISTRY; METALLURGY
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Abstract
Description
(1)タングステン源とM金属源の混合物を、窒素含有雰囲気を有する真空状態において450~750℃で2~8時間保温し、透明遮熱材料を取得し、得られた透明遮熱材料を透明遮熱微粒子に粉砕し、または、
ナノ酸化タングステン粉体とM金属源が均一に分散している溶液を撹拌して乾燥させ、前駆体を取得し、得られた前駆体を、窒素含有雰囲気を有する真空状態において400~700℃で1~8時間保温し、透明遮熱微粒子を得るステップと、
(2)透明遮熱微粒子と炭素源を120~180℃の温度下で1~24時間水熱反応させるステップと、を含む。
0.652kgの炭酸セシウムと、3.132kgのパラタングステン酸アンモニウムを混合し、容積が50Lの回転加熱炉に投入し、炉口を閉め、真空ユニットを用いて真空にした後、アンモニアガスを注入し、その流量を100SCCM(標準ミリリットル毎分)に保持し、かつ合成過程全体において一定の真空状態を保持する。炉の回転装置を起動させ、2時間以内に室温から750℃まで温度を上げ、その温度で4時間保温する。加熱を停止し、炉の温度を室温付近まで自然冷却する。回転炉の炉口を開けて材料を出し、所定のセシウムタングステンブロンズ粉体を得る。
(NH4)10(H2W12O42)・4H2O+Cs2CO3+NH3→Cs0.33WO3:N+NH3+H2O
反応過程で徐々に生成される水分などは、加熱の初期段階で徐々に真空から排出される。窒素含有原料及びアンモニア雰囲気中の窒素元素は、室温からセシウムタングステンブロンズ格子の形成反応プロセスに投入され、徐々に温度を上げて加熱処理した後、最終的に窒素ドープセシウムタングステンブロンズ結晶構造が形成される。
0.325kgの炭酸セシウムをメタノールに完全に溶かし、炭酸セシウムメタノール溶液を得る。1.391kgのナノ酸化タングステン(市販のWO3、平均粒径50nm)を該溶液に投入し、撹拌して乾燥させ、セシウムタングステンブロンズ前駆体を得る。得られたセシウムタングステンブロンズ前駆体を50Lの回転炉に投入し、炉口を閉め、真空ユニットで真空にしてから、窒素ガスと水素ガス(7:3)の混合ガスを注入し、その総流量を100SCCMに保ち、合成過程全体において炉内を一定の真空度に保持する。炉の回転装置を起動させ、2時間以内に室温から500℃まで温度を上げ、その温度下で8時間保温する。加熱を停止し、炉の温度を室温付近まで自然冷却する。回転炉の炉口を開けて材料を出し、所定の窒素ドープセシウムタングステンブロンズ粉体を得る。
Cs2CO3+CH3OH+WO3+N2+H2→Cs0.33WO3:N+N2+H2+CO2
実施例2で得られた窒素ドープセシウムタングステンブロンズナノ粉体200gと15kgの可塑剤(3G8)を撹拌機で均一に混合し、混合液を35kgのPVB粉末に漏斗で徐々に加え、横型混合機内で充分に混合した後、二軸式押出機によって160℃の温度下で可塑化させ、押出成形により窒素ドープセシウムタングステンブロンズナノ粒子を含むPVB遮熱中間膜(0.38mm×1m×100m)を得る。
実施例3で得られたPVB遮熱中間膜を適量取って、2枚のガラス(3mm×30mm×30mm)の間に配置し、加熱台上に置き、95℃の加圧条件下で一定時間保持し、温度が下がってからPVB遮熱合わせガラスを得る。
図5に示す2枚の遮熱合わせガラスを高温多湿(90℃/90%相対湿度)の実験箱に入れ、24時間ごとに取り出して、その透過率スペクトルを測定し、図5のもとのスペクトルと比較した。
CsとWのモル比0.33に基づいて炭酸セシウム及びタングステン酸100gを計量し、自動乳鉢で充分に混合した後、還元雰囲気(Ar:H2=97:3体積比)中で、まず600℃で120分加熱し、反応物が室温まで冷却されてから、再び純Ar雰囲気中で800℃まで温度を上げ、60分保温して、セシウムタングステンブロンズ生成物を得る。XRD測定の結果、Cs0.33WO3六方晶構造を有しており、その27.8°付近に位置する(200)格子回折位置は理論値と一致している。
Cs2CO3+H2WO4+H2→Cs0 .33WO3+H2O+CO2
上記で得られた粉体を、流量500ミリリットル/分のNH3雰囲気中で、450℃の条件下で60分加熱し、セシウムタングステンブロンズ粉体生成物を得る。XRD測定によると、その27.8°付近に位置する(200)格子回折位置は、高角度の方にやや偏移しており、その偏移量は約0.05°であり、後続の熱処理後のセシウムタングステンブロンズに窒素ドープが生じていることを表しており、その反応式は以下の式で表すことができる。
Cs0.33WO3+NH3→Cs0.33WO3:N+NH3(加熱温度450℃)
但し、実施例1及び2で、反応物前駆体を窒素含有真空中で室温から加熱した情況と較べて、そのXRD回折ピークの偏移の度合いはかなり小さく、これは、比較例1の窒素のドープ量が実施例1及び2の窒素ドープ量よりはるかに少ないことを意味している。
実施例1で得られた炭素コーティング窒素ドープセシウムタングステンブロンズ粉体、分散剤及びポリマーマスターバッチキャリアを、高速混合機で充分に均一に撹拌した後、均一に撹拌した撹拌物を二軸式押出機によって250℃~280℃の温度下で混合し、溶融して押し出し、PETナノ遮熱マスターバッチを得る。
実施例2で得られた炭素コーティング窒素ドープセシウムタングステンブロンズナノ粉体100g、分散剤2g及びトルエン200gをサンドミルに投入し、回転速度2600r/分で5時間保持し、取り出して、炭素コーティング窒素ドープセシウムタングステンブロンズナノ分散液を得る。
実施例2で得られた炭素コーティング窒素ドープセシウムタングステンブロンズナノ粉体100g、分散剤(3-アミノプロピルトリエトキシシラン(APTES))、キャリアポリマーのポリアミド6樹脂(PA6)を、質量比1:0.1:8.9で配合し、高速混合機で充分に均一に撹拌した後、二軸式押出機によって220℃~250℃の温度下で混合し、溶融して押し出し、蓄熱保温マスターバッチを得る。
Claims (10)
- コアシェル構造の透明遮熱微粒子において、
前記微粒子は、コアと、前記コアを被覆するシェルを含み、
前記コアの材料は、化学式がMxWO3-δのタングステンブロンズ構造に窒素をドープして得られる透明遮熱材料であり、
そのうち、Mはアルカリ金属、アルカリ土類金属及び希土類元素の中のいずれか1種以上の元素であり、0.1≦x≦1であり、
Wはタングステン、Oは酸素で、0≦δ≦0.5であり、
前記シェルは炭素で、シェルの厚さが1nm~10nmであることを特徴とする、
コアシェル構造の透明遮熱微粒子。 - 前記透明遮熱材料の成分は一般式MxWOyNzで表され、
Nは窒素で、2.5≦y+z≦3であり、
zとyの比値は1/4以下であり、好適には1/10以下、より好適には1/20以下であることを特徴とする、請求項1に記載のコアシェル構造の透明遮熱微粒子。 - 前記コアの粒径が1nm~100nmであることを特徴とする、請求項1または2に記載のコアシェル構造の透明遮熱微粒子。
- (1)タングステン源とM金属源の混合物を、窒素含有雰囲気を有する真空状態において450~750℃で2~8時間保温し、透明遮熱材料を取得し、得られた透明遮熱材料を透明遮熱微粒子に粉砕し、または、
ナノ酸化タングステン粉体とM金属源が均一に分散している溶液を撹拌して乾燥させ、前駆体を取得し、得られた前駆体を、窒素含有雰囲気を有する真空状態において400~700℃で1~8時間保温し、透明遮熱微粒子を得るステップと、
(2)透明遮熱微粒子と炭素源を120~180℃の温度下で1~24時間水熱反応させるステップと、
を含むことを特徴とする、請求項1~3のいずれか1項に記載のコアシェル構造の透明遮熱微粒子の調製方法。 - 前記タングステン源は、酸化タングステン、タングステン酸、タングステン酸アンモニウムの中から選択される少なくとも1種で、好適にはタングステン酸アンモニウムであり、
前記M金属源は、M元素の炭酸塩で、好適には炭酸セシウムであることを特徴とする、
請求項4に記載の調製方法。 - 前記窒素含有雰囲気は、アンモニアガス、窒素ガスまたはその混合ガス、または上記のガスと水素ガスの混合ガスであることを特徴とする、請求項4または5に記載の調製方法。
- 前記炭素源が、ショ糖、ブドウ糖、グリコーゲン、及びビタミンCの中から選択される少なくとも1種であることを特徴とする、請求項4~6のいずれか1項に記載の調製方法。
- ステップ(2)において、炭素源と透明遮熱微粒子の質量比が(1~20):100であることを特徴とする、請求項4~7のいずれか1項に記載の調製方法。
- 請求項8に記載の透明遮熱微粒子が媒質中に分散して形成されることを特徴とする、透明遮熱微粒子分散体。
- 前記媒質が、樹脂を含む液体、透明樹脂フィルム、透明樹脂フィルム板材、ガラス基材、化学繊維、ファブリックの中から選択される任意の1種であることを特徴とする、請求項9に記載の透明遮熱微粒子分散体。
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