JP6744589B2 - 製紙用歩留剤の希釈液の製造方法 - Google Patents
製紙用歩留剤の希釈液の製造方法 Download PDFInfo
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- JP6744589B2 JP6744589B2 JP2018133313A JP2018133313A JP6744589B2 JP 6744589 B2 JP6744589 B2 JP 6744589B2 JP 2018133313 A JP2018133313 A JP 2018133313A JP 2018133313 A JP2018133313 A JP 2018133313A JP 6744589 B2 JP6744589 B2 JP 6744589B2
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Description
前記製紙用歩留剤に電気伝導度0.1〜1mS/cmの水(B)を混合して1段階希釈液を調製する工程、次に、1段階希釈液に電気伝導度1〜50mS/cmの水(C)を混合して2段階希釈液を調製する工程を含む製紙用歩留剤の希釈液の製造方法。
条件(I):0.5規定NaCl水溶液で製紙用歩留剤中の(A)成分の濃度を0.5重量%に希釈した際の温度25℃における粘度をXmPa・s、
イオン交換水で製紙用歩留剤中の(A)成分の濃度を0.5重量%に希釈した際の温度25℃における粘度をYmPa・sとしたとき、
50≦X≦500、及び15≦Y/X≦100である。
条件(II):(A)成分の濃度が0.01〜1重量%のときの電気伝導度が1〜50mS/cm、及び温度25℃での粘度が1〜1,500mPa・sである。
撹拌機、還流冷却管、温度計および窒素導入管を備えた反応容器にイソパラフィン230.0gにソルビタンモノオレート17.5gを仕込んで希釈させた。別に50%アクリルアミド水溶液416.4g(80モル%)、80%アクリロイルオキシエチルトリメチルアンモニウムクロライド177.2g(20モル%)、イオン交換水105.9g、10%イソプロピルアルコール1.0gを混合した。油と水溶液を混合し、ホモジナイザーにて1000rpmで5分間撹拌乳化させた。得られた溶液の温度を40〜43℃に保ち、窒素置換を2時間行った後、1重量%の2,2‘−アゾビス(2−アミジノプロパン)塩酸塩(商品名:『V−50』、和光純薬工業(株)製)12.0gを加え、重合反応を開始させた。40±1℃で12時間重合させ反応を完了させた。生成した油中水型エマルションに転相剤としてポリオキシエチレンポリオキシプロピレンラウリルエーテル14.6gを添加して混合し、形態が油中水型エマルションである製紙用歩留剤を得た。組成及び物性を表1に示す(以下同様)。
製造例1において、重合温度、及び1重量%V−50水溶液の使用量等を変更して、形態が油中水型エマルションである製紙用歩留剤をそれぞれ得た。
表1に示す組成で、製造例1と同様の方法で行い、形態が油中水型エマルションである製紙用歩留剤をそれぞれ得た。
撹拌機、還流冷却管、温度計、窒素導入管および冷却装置を備えた反応容器に50%アクリルアミド水溶液416.4g(80モル%)、80%アクリロイルオキシエチルトリメチルアンモニウムクロライド177.2g(20モル%)及びイオン交換水102.5gを仕込んだ。フラスコ内部を十分に窒素置換した後、得られた溶液の温度を35℃に調整し、光重合開始剤として10重量%V−50水溶液3.5gを仕込み、全体を撹拌し均一にした。高圧水銀灯(400W、波長:365nm、光量:20mW/cm2)にて照射し、重合を開始し、窒素流入をさせながら2時間照射した。重合終了後、含水ゲル状の重合体を得た。得られた含水ゲル状の重合体を容器から取り出して細断し、80℃の送風乾燥機内で20時間乾燥した後、粉砕して、形態が粉末である製紙用歩留剤を得た。
表1に示す組成で、製造例12と同様の方法で合成し、形態が粉末である製紙用歩留剤を得た。
撹拌機を備えた容器に、0.5規定NaCl水溶液、またはイオン交換水を仕込み、撹拌機(600rpm)で撹拌しながら(A)成分の濃度が0.5%となるように製紙用歩留剤を加えた。製紙用歩留剤の形態が油中水型エマルションの場合は、室温下で1時間撹拌し、粉末の場合は溶解するまで室温下で撹拌した。
上記希釈液の温度が25℃となるように調節した後、B型粘度計(芝浦システム(株)製)を用いて測定した。なお、0.5規定NaCl水溶液で希釈した液の粘度(XmPa・s)は回転数を30rpm、イオン交換水で希釈した液の粘度(YmPa・s)は回転数を6rpmにして、それぞれ測定した。結果を表1に示す(以下同様)。
製紙用歩留剤を1規定NaCl水溶液で(A)成分の濃度(c)が0.02g/dl、0.04g/dl、0.06/dl、0.08g/dlとなるように希釈した液を25℃に調整し、オストワルド粘度計を用いてそれぞれの落下時間(t)を測定した。同様に、1規定NaCl水溶液の落下時間(t0)も測定し、(式2)より比粘度(ηsp)を算出した。
(式2)ηsp=(t/t0)−1
得られたηspを重合体濃度で除した値(ηsp/c)を縦軸に、重合体濃度(c)を横軸にしてプロットし、得られた直線の切片を固有粘度(単位:dl/g)とした。
*2:イオン交換水で(A)成分の濃度を0.5%に希釈した液の粘度
・AM:アクリルアミド
・Q :アクリロイルオキシエチルトリメチルアンモニウムクロライド
・BQ:N,N−ジメチルアミノエチルアクリレートベンジルクロライド
・AA・Na:アクリル酸ナトリウム
撹拌機を備えた容器に、(A)成分の濃度が0.5%となるように仕込んだ水道水(電気伝導度:0.2mS/cm)へ製造例1の製紙用歩留剤を加えて、撹拌機(600rpm)で室温下1時間撹拌させ、1段階希釈液を得た。次いで処理水(電気伝導度:3mS/cm)を(A)成分の濃度が0.1%となるように加えて、更に1時間撹拌し、製紙用歩留剤の2段階希釈液を得た。表2に組成及び物性を示す(以下同様)。
表2に示す処方で、実施例1と同様に行い、製紙用歩留剤の1段階希釈液、及び2段階希釈液をそれぞれ得た。
実施例1と同様の容器に、(A)成分の濃度が0.5%となるように仕込んだ水道水(電気伝導度:0.2mS/cm)へ製造例13の製紙用歩留剤を加えて、撹拌機(600rpm)で室温下溶解するまで撹拌させ、1段階希釈液を得た。次いで処理水(電気伝導度:3mS/cm)を(A)成分の濃度が0.1%となるように加えて、更に1時間撹拌し、製紙用歩留剤の2段階希釈液を得た。
表2に示す処方で、実施例27と同様に行い、製紙用歩留剤の1段階希釈液、及び2段階希釈液を得た。
pH/COND METER D−54((株)堀場製作所製)を用いて測定した。
各製紙用歩留剤の1段階希釈液、及び2段階希釈液の温度が25℃となるように調節した後、B型粘度計(芝浦システム(株)製)を用いて、回転数を30rpmにして測定した。結果を表2に示す(以下同様)。
(式1)OPR(%)={(Z1−Z2)/Z1}×100
(Z1:薬品添加後のパルプスラリーの濃度、Z2=下穴から採取した濾液の濃度)
Claims (6)
- 下記の条件(I)を満たす(メタ)アクリルアミド系ポリマー(A)を含む製紙用歩留剤を2段階希釈して、下記の条件(II)を満たす希釈液を得る製造方法であって、
前記製紙用歩留剤に電気伝導度0.1〜1mS/cmの水(B)を混合して1段階希釈液を調製する工程、次に、1段階希釈液に電気伝導度1〜50mS/cmの水(C)を混合して2段階希釈液を調製する工程を含む製紙用歩留剤の希釈液の製造方法。
条件(I):0.5規定NaCl水溶液で製紙用歩留剤中の(A)成分の濃度を0.5重量%に希釈した際の温度25℃における粘度をXmPa・s、
イオン交換水で製紙用歩留剤中の(A)成分の濃度を0.5重量%に希釈した際の温度25℃における粘度をYmPa・sとしたとき、
50≦X≦500、及び15≦Y/X≦100である。
条件(II):(A)成分の濃度が0.01〜1重量%のときの電気伝導度が1〜50mS/cm、及び温度25℃での粘度が1〜1,500mPa・sである。 - (A)成分が、(メタ)アクリルアミド(a1)、並びにカチオン性ビニルモノマー(a2)及び/又はアニオン性ビニルモノマー(a3)を含むモノマー成分のポリマーを含む、請求項1の製紙用歩留剤の希釈液の製造方法。
- (A)成分の1規定NaCl水溶液中での固有粘度(温度25℃)が5〜30dl/gである、請求項1又は2の製紙用歩留剤の希釈液の製造方法。
- 製紙用歩留剤の形態が、油中水型エマルション又は粉末である請求項1〜3のいずれかの製紙用歩留剤の希釈液の製造方法。
- (a2)成分が、第3級アミノ基含有(メタ)アクリレート及び/又は該(メタ)アクリレートの4級化塩である請求項2〜4のいずれかに記載の製紙用歩留剤の希釈液の製造方法。
- (a3)成分が、アクリル酸、イタコン酸及び無水イタコン酸からなる群より選ばれる少なくとも1種である、請求項2〜5のいずれかに記載の製紙用歩留剤の希釈液の製造方法。
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