JP2021134278A - ポリビニルアルコール系樹脂及び地下処理用目止め剤 - Google Patents
ポリビニルアルコール系樹脂及び地下処理用目止め剤 Download PDFInfo
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- JP2021134278A JP2021134278A JP2020031395A JP2020031395A JP2021134278A JP 2021134278 A JP2021134278 A JP 2021134278A JP 2020031395 A JP2020031395 A JP 2020031395A JP 2020031395 A JP2020031395 A JP 2020031395A JP 2021134278 A JP2021134278 A JP 2021134278A
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- Prior art keywords
- based resin
- pva
- polyvinyl alcohol
- solubility
- underground
- 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
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- 239000011347 resin Substances 0.000 title claims abstract description 135
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- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 130
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- TZYULTYGSBAILI-UHFFFAOYSA-M trimethyl(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC=C TZYULTYGSBAILI-UHFFFAOYSA-M 0.000 description 1
- UPCXAARSWVHVLY-UHFFFAOYSA-N tris(2-hydroxyethyl)azanium;acetate Chemical compound CC(O)=O.OCCN(CCO)CCO UPCXAARSWVHVLY-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
-
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Abstract
Description
本開示は、特定の膨潤度と溶解度の関係を満たすポリビニルアルコール(以下、ポリビニルアルコールをPVAと称することがある。)系樹脂であり、該PVA系樹脂は、該PVA系樹脂を40℃の水に30分浸漬したときの膨潤度(%)を、該PVA系樹脂を65℃の水に5時間浸漬したときの溶解度(%)で割った値、すなわち膨潤度/溶解度が3.0以上である。
膨潤度(%)=(高さB/高さA)×100
固形分率(%)=(重量C/重量B)×100
溶解度(%)={6−(重量A×100/固形分率)}/6×100
酸ビニルが好ましい。
本開示の地下処理用目止め剤は、上記のPVA系樹脂を含む。PVA系樹脂の含有量は特に限定されないが、地下処理用目止め剤全体に対して50〜100質量%が好ましく、80〜100質量%がより好ましく、90〜100質量%がさらに好ましい。PVA系樹脂の含有量が上記範囲であることで、目止め効果により優れる傾向がある。
アクリル酸メチルを5モル%共重合させたポリ酢酸ビニルを原料として用いた。これを33%メタノール溶液として、反応槽に添加し、そこに無水ナトリウムメチラートのメタノール溶液を添加した。無水ナトリウムメチラートの量は、ポリ酢酸ビニルの0.5重量%とした。溶液を攪拌しながら反応槽を加温し、沸点で保持してけん化反応を行い、スラリー液を得た。得られたスラリー液を反応槽から取出し、中和処理を行わずにそのまま冷熱処理工程に送り、スラリー液の温度を50℃未満に冷却した。次いで、固液分離工程にて、該スラリー液をポリビニルアルコール系樹脂のウェットケーキと溶液とに分離した。その後、ウェットケーキのみを取出し、乾燥処理を行って、粉粒体の集合物であるPVA系樹脂(PVA1)を得た。PVA1の20℃における4%水溶液粘度は19mPa・sであり、けん化度は99.5モル%であり、比表面積は1.74m2/gであった。また、得られた粉粒体であるPVA1は、US100メッシュ(ASTM E11規格)を通過した。なお、US100メッシュを通過する粒子の粒子径は149μm以下である。
PVA1にポリエチレングリコールを1.5重量%添加して混錬した。次いで、二軸押出成形機を用いて、成形圧力1259psiでシート状に押出成形した。これを造粒機に投入し、6/8メッシュ(ASTM E11規格)に造粒し、PVA系樹脂(PVA2)を得た。PVA2の比表面積は1.18m2/gであった。なお、「6/8メッシュに造粒」とは、6メッシュを通過し、8メッシュを通過しない粒子サイズに造粒することを意味し、6/8メッシュに造粒した粒子の粒子径は2380μm以上3350μm以下である。
アクリル酸メチルを共重合させていないポリ酢酸ビニルを原料として使用した以外は、実施例1と同様の方法で、粉粒体の集合物であるPVA系樹脂(PVA3)を得た。PVA3の20℃での4%水溶液粘度は31mPa・s、けん化度は99.5モル%、比表面積は1.72m2/gであった。また、得られた粉粒体であるPVA3は、US100メッシュ(ASTM E11規格)を通過した。
PVA3にポリエチレングリコールを1.5重量%添加して混錬し、次いで、二軸押出成形機を用いて、成形圧力1250psiでシート状に押出成形した後、これを造粒機に投入し、6/8メッシュに造粒してPVA系樹脂(PVA4)を得た。PVA4の比表面積は1.10m2/gであった。
未変性のポリ酢酸ビニルのメタノール溶液(濃度32質量%)を、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%)と混合した。得られた混合物を、ベルト上に載置し、40℃の温度条件下で、均一系でのけん化反応を進行させた。その後、酢酸による中和処理、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)の篩を通し、PVA系樹脂(PVA5)を得た。得られたPVA5の20℃での4%水溶液粘度は22.5mPa・s、けん化度は88.0モル%であった。なおPVA5の比表面積は測定下限値(0.01m2/g)未満であった。また、PVA5は、US100メッシュ(ASTM E11規格)を通過した。
PVA5にポリエチレングリコールを1.5重量%添加して混錬し、次いで、二軸押出成形機を用いて、成形圧力1250psiでシート状に押出成形した後、これを造粒機に投入し、6/8メッシュに造粒してPVA系樹脂(PVA6)を得た。なおPVA6の比表面積は測定下限値(0.01m2/g)未満であった。
国際公開第2019/131952号の実施例1に記載のPVA系樹脂を再現したものをPVA7とした。なおPVA7の比表面積は測定下限値(0.01m2/g)未満であった。
PVA系樹脂0.5gを内径18mmの試験管に入れ、試験管内のPVA系樹脂が占める高さを測定した(高さA)。次いで、試験管内に蒸留水7mLを入れ、よく振り混ぜてPVAを分散させた。その後、40℃に設定したウォーターバスに試験管を浸し、試験管内の水温が40℃になってから30分間静置した後、試験管内のPVA系樹脂が占める高さを測定した(高さB)。得られた高さA及び高さBの数値から、下記式に従い、膨潤度(%)を算出した。
膨潤度(%)=(高さB/高さA)×100
200mLの蓋付きガラス容器に100gの蒸留水を入れ、PVA系樹脂6gを投入して、65℃の恒温槽にて5時間静置した。その後、ガラス容器の中味をナイロン製の120メッシュ(目開き125ミクロンの篩)に通し、篩上に残ったPVA系樹脂を140℃で3時間乾燥し、乾燥後の重量を測定した(重量A)。一方で、別途採取したPVA系樹脂を105℃で3時間乾燥させ、乾燥前の重量(重量B)と乾燥後の重量(重量C)を測定して、下記式に従いPVA系樹脂の溶解度(%)を算出した。
固形分率(%)=(重量C/重量B)×100
溶解度(%)={6−(重量A×100/固形分率)}/6×100
内径10mmのステンレスカラム中に120メッシュのステンレス製篩を設置し、上流側にPVA系樹脂5gを入れた。次に50℃に調整した温水をカラムに入れ、100psiの圧力を加えた。カラムを目視で観察し、15秒以内に温水の流出が止まった場合を「〇」、止まらなかった場合を「×」として目止め効果を評価した。
Claims (5)
- ポリビニルアルコール系樹脂であって、
該ポリビニルアルコール系樹脂を40℃の水に30分浸漬したときの膨潤度(%)と、
該ポリビニルアルコール系樹脂を65℃の水に5時間浸漬したときの溶解度(%)とが、
膨潤度/溶解度≧3.0を満たす、ポリビニルアルコール系樹脂。 - 膨潤度(%)が110%以上280%以下である、請求項1に記載のポリビニルアルコール系樹脂。
- 溶解度(%)が5%以上である、請求項1又は2に記載のポリビニルアルコール系樹脂。
- ポリビニルアルコール系樹脂がカルボン酸を含有する構成単位を含む、請求項1〜3のいずれか一項に記載のポリビニルアルコール系樹脂。
- 請求項1〜4のいずれか一項に記載のポリビニルアルコール系樹脂を含む地下処理用目止め剤。
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