JP2019137870A - ポリビニルアルコール粉体の製造方法 - Google Patents
ポリビニルアルコール粉体の製造方法 Download PDFInfo
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- JP2019137870A JP2019137870A JP2019085445A JP2019085445A JP2019137870A JP 2019137870 A JP2019137870 A JP 2019137870A JP 2019085445 A JP2019085445 A JP 2019085445A JP 2019085445 A JP2019085445 A JP 2019085445A JP 2019137870 A JP2019137870 A JP 2019137870A
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- JP
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- Prior art keywords
- saponification
- pva
- polyvinyl alcohol
- powder
- particle diameter
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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Abstract
Description
に関する。
P=([η]×10000/8.29)(1/0.62)
実施例および比較例の製造方法において、せん断速度は、ポリ酢酸ビニル(以下、「PVAc」と略記することがある)溶液のフィード量(m3/s)、スタティックミキサーの断面積(m2)およびスタティックミキサーの直径(m)から、次式により求められる。スタティックミキサーの直径を変更することによりせん断速度を制御することができる。
せん断速度(s−1)=PVAc溶液のフィード量/(スタティックミキサーの断面積×スタティックミキサーの直径)
実施例および比較例で用いられたPVA粉体を湿度65%RH、温度25℃の条件下で24時間静置した。次いで、光学顕微鏡(デジタルマイクロスコープKH−7700;株式会社ハイロックス社製)を用いて写真撮影をした。その写真から任意に50個のPVA粉体を選び、それぞれ実測し、その長径の平均値を平均粒子径(μm)とした。ただし、20μm未満のPVA微粉は、写真のコントラスト斑と区別がつかないため、測定の対象外とした。
実施例および比較例で用いられたPVA粉体300gについて、メッシュサイズの異なる4種類の篩い(メッシュサイズ:250μm、500μm、1000μm、1180μm)を用いて篩い分けした。得られた各粒子径を持つPVA粉体の質量を測定して、各々の質量%を計算した。
実施例および比較例で用いられたPVA粉体、および粒子径500〜1000μmに篩い分けしたPVAについて、JIS K6720−2に準じた方法により嵩比重を測定した。
D:50質量%未満
けん化原料溶液であるポリ酢酸ビニル(PVAc)のメタノール溶液(濃度32質量%)を4700L/h(=1.31×10−3m3/s)でフィードし、けん化触媒溶液である水酸化ナトリウムのメタノール溶液(濃度4質量%)を図2に示す流路中央部に165L/hでフィードした。フィードされたけん化原料溶液およびけん化触媒溶液をエレメント数22個(1エレメント当たりの圧力損失は0.035MPa)のスタティックミキサーを用いて、せん断速度10.6s−1の条件で混合した。得られた混合物を、ベルト上に載置し、40℃の温度条件下で18分保持して、けん化反応を進行させた。その後、予備粉砕、乾燥、本粉砕を行い、本粉砕時の粉砕機出口で12メッシュ(JIS規格)の篩いを通し、本発明のPVA粉体を得た。得られたPVAの粘度平均重合度は2400、けん化度は88.3モル%であった。得られたPVAの分析結果を表2に示す。
けん化反応、粉砕の製造条件を表1に示すように変更したこと以外は実施例1と同様にして、実施例2〜6および比較例1〜3のPVA粉体をそれぞれ得た。得られたPVAの分析結果を表2に示す。
けん化反応の条件を表1に示すように変更したこと以外は実施例1と同様に実施した。その結果、不均質な混合溶液の状態で鹸化反応が起こり、均質なPVA粉体が得られなかった。
2 スタティックミキサー
3 けん化原料溶液とけん化触媒混合物
4 ベルト型反応器
5 けん化触媒導入管
5a けん化触媒溶液
Claims (3)
- 湿度65%RH、温度25℃にて光学顕微鏡観察により測定した時の平均粒子径が100〜2000μmであり、粒子径500〜1000μmの部分における嵩比重(g/ml)が0.60を超えて0.80未満であり、かつ粒子径500〜1000μmの部分の割合が35〜70質量%であるポリビニルアルコール粉体。
- 粘度平均重合度が200〜5000であり、けん化度が50〜99.99モル%である請求項1に記載のポリビニルアルコール粉体。
- ポリビニルエステルおよび有機溶媒からなるけん化原料溶液が通流する流路中央部にけん化触媒を導入する導入工程と、前記けん化原料溶液と導入されたけん化触媒とをスタティックミキサーを用いてせん断速度5〜90s−1にて混合する混合工程と、
を有するポリビニルアルコール粉体の製造方法。
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