JP6475352B2 - 炭酸カルシウム含有材料を含む懸濁液の製造方法 - Google Patents
炭酸カルシウム含有材料を含む懸濁液の製造方法 Download PDFInfo
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- JP6475352B2 JP6475352B2 JP2017542304A JP2017542304A JP6475352B2 JP 6475352 B2 JP6475352 B2 JP 6475352B2 JP 2017542304 A JP2017542304 A JP 2017542304A JP 2017542304 A JP2017542304 A JP 2017542304A JP 6475352 B2 JP6475352 B2 JP 6475352B2
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- Prior art keywords
- aqueous suspension
- calcium carbonate
- weight
- containing material
- aqueous
- Prior art date
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims description 312
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims description 146
- 239000000463 material Substances 0.000 title claims description 145
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- 238000000034 method Methods 0.000 claims description 98
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- 239000002270 dispersing agent Substances 0.000 claims description 33
- -1 primary amine salt Chemical class 0.000 claims description 32
- 125000001931 aliphatic group Chemical group 0.000 claims description 15
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000007795 chemical reaction product Substances 0.000 claims description 12
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- 229910019142 PO4 Inorganic materials 0.000 claims description 11
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- 229920003023 plastic Polymers 0.000 claims description 7
- 229940088417 precipitated calcium carbonate Drugs 0.000 claims description 7
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 6
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 6
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
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- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 3
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- 229920001577 copolymer Polymers 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- 235000019800 disodium phosphate Nutrition 0.000 claims description 3
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 3
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- 229920001519 homopolymer Polymers 0.000 claims description 3
- 229910003002 lithium salt Inorganic materials 0.000 claims description 3
- 159000000002 lithium salts Chemical class 0.000 claims description 3
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- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
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- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims description 3
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- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims 1
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- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 6
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- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 4
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
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- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
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- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
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- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
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- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 229920005789 ACRONAL® acrylic binder Polymers 0.000 description 1
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- 235000021357 Behenic acid Nutrition 0.000 description 1
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- GONOPSZTUGRENK-UHFFFAOYSA-N benzyl(trichloro)silane Chemical compound Cl[Si](Cl)(Cl)CC1=CC=CC=C1 GONOPSZTUGRENK-UHFFFAOYSA-N 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
- YAQXGBBDJYBXKL-UHFFFAOYSA-N iron(2+);1,10-phenanthroline;dicyanide Chemical compound [Fe+2].N#[C-].N#[C-].C1=CN=C2C3=NC=CC=C3C=CC2=C1.C1=CN=C2C3=NC=CC=C3C=CC2=C1 YAQXGBBDJYBXKL-UHFFFAOYSA-N 0.000 description 1
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- 125000002469 tricosyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/185—After-treatment, e.g. grinding, purification, conversion of crystal morphology
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Description
a)炭酸カルシウム含有材料を含む少なくとも2つの水性懸濁液を提供する工程であって、
i)第1の水性懸濁液が、水性懸濁液の全重量に対して1.0から82.0重量%の固体含有量および1.0から30.0重量%の範囲の、2μm未満の粒径を有する粒子の含有量を有し、ならびに
ii)第2の水性懸濁液が、水性懸濁液の全重量に対して10.0から82.0重量%の固体含有量および30.0未満から100.0重量%の範囲の、2μm未満の粒径を有する粒子の含有量を有する工程、
b)工程a)で提供された少なくとも2つの水性懸濁液を混合して、水性懸濁液混合物を得る工程、
c)混合工程b)で得られた水性懸濁液混合物、および/または混合工程b)を行う前に工程a)で提供された少なくとも2つの水性懸濁液の少なくとも一方を粉砕する工程。
「炭酸カルシウム含有材料」という用語は、炭酸カルシウム含有材料の全乾燥重量に対して少なくとも50.0重量%の炭酸カルシウムを含む材料を示す。
本発明の方法の工程a)により、炭酸カルシウム含有材料を含む、少なくとも2つの水性懸濁液が提供される。
本発明の方法の工程b)により、少なくとも2つの水性懸濁液を混合して水性懸濁液混合物を得る。
本発明の方法の工程c)により、混合工程b)で得られた水性懸濁液混合物および/または混合工程b)を行う前の工程a)で提供された少なくとも2つの水性懸濁液のうちの少なくとも1つを粉砕する。
e)粉砕工程c)を混合工程b)の前に行うという条件で、工程b)で得られた水性懸濁液、もしくは粉砕工程c)を混合工程b)の後に行うという条件で、粉砕工程c)で得られた水性懸濁液混合物、もしくは濃縮工程d)で得られた水性懸濁液混合物を乾燥させて水の少なくとも一部を除去して、部分脱水炭酸カルシウム含有材料を得るもしくは乾燥炭酸カルシウム含有材料を得る工程、ならびに場合により
f)工程e)の後に得られた乾燥炭酸カルシウム含有材料を少なくとも1つの分散剤によって処理し、これを再希釈して分散炭酸カルシウム含有材料を含む水性懸濁液を得る工程、ならびに/または
g)工程e)の後に得られた乾燥炭酸カルシウム含有材料を少なくとも1つの飽和脂肪族直鎖もしくは分枝カルボン酸によって、ならびに/または少なくとも1つの一置換コハク酸無水物および/もしくは少なくとも1つの一置換コハク酸および/もしくは(1または複数の)塩反応生成物によって、ならびに/または1つ以上のリン酸モノエステルおよび/もしくはその反応生成物と、1つ以上のリン酸ジエステルおよび/もしくはその反応生成物との少なくとも1つのリン酸エステルブレンドによって処理して、疎水化炭酸カルシウム含有材料を得る工程
をさらに含む。
本発明者らは驚くべきことに、本発明の方法により、第2の水性懸濁液の代わりに水を使用する従来方法と比べて、最終製品のBET比表面積が小さい炭酸カルシウム含有材料が得られることを見出した。
[1.測定方法]
以下では、実施例で行った測定方法について説明する。
微粒子材料の重量粒径および粒径質量分布は、沈降法、即ち重力場における沈降挙動の分析によって測定した。測定は、Micromeritics Instrument Corporation製のSedigraph(商標)5120またはSedigraph(商標)5100を用いて行った。
本文書を通じて、微粒子材料の比表面積(m2/g)は、当業者に周知である(吸着ガスとして窒素を使用する)BET法(ISO 9277:1995)を使用して求めた。次いで、微粒子材料の全表面積(m2)を比表面積と微粒子材料の質量(g)との積によって得る。方法および機器は当業者に公知であり、微粒子材料の比表面を求めるためによく使用されている。
懸濁液のpHは、メトラートレド(Mettler Toledo)セブンイージー(Seven Easy)pH計およびメトラートレドInLab(R)エキスパートプロ(Expert Pro)pH電極を使用して、25℃にて測定した。機器の3点較正(セグメント法による。)を、20℃にて4、7および10のpH値を有する市販の緩衝溶液(アルドリッチ(Aldrich))を使用して、最初に行う。報告したpH値は、機器によって検出した終点値である(終点は、測定した信号の平均からの差が最後の6秒間にわたって0.1mV未満である場合である。)。
本発明の目的のために、用語「粘度」または「ブルックフィールド粘度」は、ブルックフィールド粘度を示す。ブルックフィールド粘度はこの目的のために、ブルックフィールド(Type RVT)粘度計により25℃±1℃、100rpmにて、ブルックフィールド RVスピンドルセットの適切なスピンドルを使用して測定し、mPa・sで規定する。当業者は、自分の技術知識に基づいて、ブルックフィールド RVスピンドルセットから測定する粘度範囲に好適であるスピンドルを選択する。例えば、200から800mPa・sの間の粘度範囲では、スピンドル番号3が使用され得て、400から1600mPa・sの間の粘度範囲では、スピンドル番号4が使用され得て、800から3200mPa・sの間の粘度範囲では、スピンドル番号5が使用され得る。
固体含有量(「乾燥重量」としても公知)は、スイスのMettler−Toledo社製の水分分析装置HR73を以下の設定:温度120℃、自動スイッチオフ3、標準乾燥、生成物5から20gを使用して決定した。
顔料白色度R457は、Datacolor社製のELREPHO 3000を使用して、ISO 2469:1994(DIN 53145−2:2000およびDIN 53146:2000)に従って測定した。
光散乱係数「S」は、紙コーティングバインダであるBASF製Acronal(商標)S 360 D 10部(乾量基準)および炭酸カルシウム懸濁液90部(乾量基準)を使用して紙コーティングカラーを調製して、ドイツ、58675、HemerのEricksen製のラボラトリーコーターTypモデル624を使用してプラスチック支持体(Synteape、Argo Wiggins)に各種のコート重量の範囲でコーティングすることによって測定した。コーティングカラーはすべて、別途記載しない限り、45.0重量%の固体含有量を有していた。
以下の出発材料を実施例に使用した。
ノルウェー産大理石(40−48μm)を25重量%の固体含有量にて、W.Bachofen AG製のダイノーミルMultilab内で(粉砕チャンバの全容積=600cm3、ミル速度=2,500rpm、フロー=500cm3/分、融着粉砕ビーズであって、粉砕ビーズの全重量に対して68重量%のバデレアイトおよび32重量%のアモルファスシリカから成り、1.0から1.6mmの範囲の直径を有する融着粉砕ビーズ1,070gを充填)d50が8μmとなるまで粉砕した。
AS1からの上清を沈殿瓶に入れ、沈殿物が37%の固体含有量に達するまで数日放置した。上清の水をデカンテーションして、沈殿物をAS2として使用した。
AS1をAS2およびまたは水と混合した。さらに、下の表2に示す量の分散剤を添加した。混合物を激しく撹拌して、ミル内を圧送した。1バッチは、およそ5kgの(乾燥)炭酸カルシウムを含有していた。続いて、得られた炭酸カルシウム含有懸濁液を、炭酸カルシウム含有材料が所望の重量中央粒径d50を有するまで、即ち約60分間、室温にて粉砕した。粉砕には、W.Bachofen AG製のダイノーミルMultilab(粉砕チャンバの全容積=600cm3、ミル速度=2,500rpm、フロー=500cm3/分、融着粉砕ビーズであって、粉砕ビーズの全重量に対して68重量%のバデレアイトおよび32重量%のアモルファスシリカから成り、1.0から1.6mmの範囲の直径を有する融着粉砕ビーズ1,070gを充填)を使用した。得られた生成物の物理データを下の表2に示す。ΔSSAが本発明の実施例のBET比表面積の対応する比較例との差を示すことに留意すべきである。
Claims (14)
- 炭酸カルシウム含有材料の製造方法であって、
a)炭酸カルシウム含有材料を含む少なくとも2つの水性懸濁液を提供する工程であって、
i)第1の水性懸濁液が、前記水性懸濁液の全重量に対して1.0から82.0重量%の固体含有量および1.0から30.0重量%の範囲の、2μm未満の粒径を有する粒子の含有量を有し、ならびに
ii)第2の水性懸濁液が、前記水性懸濁液の全重量に対して10.0から82.0重量%の固体含有量および30.0を超え100.0重量%までの範囲の、2μm未満の粒径を有する粒子の含有量を有する工程、
b)工程a)で提供された前記少なくとも2つの水性懸濁液を混合して、水性懸濁液混合物を得る工程、
c)混合工程b)で得られた前記水性懸濁液混合物を粉砕する工程、
を含む方法。 - 請求項1に記載の方法であって、少なくとも1つの分散剤を、工程a)で提供された少なくとも2つの水性懸濁液のうちの少なくとも一方、および/または混合工程b)で得られた水性懸濁液混合物に添加することを特徴とする方法。
- 請求項2に記載の方法であって、少なくとも1つの分散剤が、(メタ)アクリル酸、マレイン酸、フマル酸、イタコン酸およびこれらの酸の誘導体の少なくとも部分的に中和されたホモポリマーまたはコポリマーのナトリウム塩、カリウム塩、カルシウム塩、マグネシウム塩、リチウム塩、ストロンチウム塩、第1級アミン塩、第2級アミン塩、第3級アミン塩および/もしくはアンモニウム塩(ここで、アミン塩は直鎖または環式である。)、リン酸水素ナトリウムまたはポリホスフェート、カルボキシメチルセルロース、櫛形ポリマーならびに/またはこれの混合物から成る群から選択されることを特徴とする方法。
- 請求項1から3のいずれか一項に記載の方法であって、
i)粉砕工程c)で得られた水性懸濁液混合物中の炭酸カルシウム含有材料のBET比表面積が、窒素およびISO 9277によるBET法を使用して測定される場合、0.1から30.0m2/gの間であり、ならびに/または
ii)粉砕工程c)で得られた前記水性懸濁液混合物中の炭酸カルシウム含有材料のBET比表面積が、第2の水性懸濁液の代わりに水を使用する方法で製造された炭酸カルシウム含有材料のBET比表面積よりも0.1から2.0m2/gの間だけ小さいことを特徴とする方法。 - 請求項1から4のいずれか一項に記載の方法であって、粉砕工程c)で得られた水性懸濁液混合物のブルックフィールド粘度が、50から5,000mPa・sの間であることを特徴とする方法。
- 請求項1から5のいずれか一項に記載の方法であって、粉砕工程c)で得られた水性懸濁液混合物中の炭酸カルシウム含有材料が、
i)50.0μm以下のトップカット粒径d98を有すること、ならびに/または
ii)0.1から10.0μmの間の重量中央粒径d50を有すること
を特徴とする方法。 - 請求項1から6のいずれか一項に記載の方法であって、
i)第1の水性懸濁液の固体含有量が、前記水性懸濁液の全重量に対して、30.0から78.0重量%であり、ならびに/または
ii)第2の水性懸濁液の固体含有量が、前記水性懸濁液の全重量に対して、30.0から40.0重量%であり、ならびに/または
iii)粉砕工程c)で得られた水性懸濁液混合物の固体含有量が、前記水性懸濁液の全重量に対して、20.0から80.0重量%である
ことを特徴とする方法。 - 請求項1から7のいずれか一項に記載の方法であって、工程a)で提供された少なくとも2つの水性懸濁液のうちの少なくとも一方を、濃縮工程に供することを特徴とする方法。
- 請求項1から8のいずれか一項に記載の方法であって、炭酸カルシウム含有材料が、天然炭酸カルシウム、沈降炭酸カルシウム、ドロマイトおよびこれらの混合物から選択されることを特徴とする方法。
- 請求項1から9のいずれか一項に記載の方法であって、工程a)で提供された少なくとも2つの水性懸濁液が、第1および第2の水性懸濁液を、10.0重量%を超える量で含むことを特徴とする方法。
- 請求項1から10のいずれか一項に記載の方法であって、工程a)で提供された少なくとも2つの水性懸濁液が、第1および第2の水性懸濁液から成ることを特徴とする方法。
- 請求項1から11のいずれか一項に記載の方法であって、粉砕工程c)で得られた水性懸濁液混合物を濃縮して、水の少なくとも一部を機械的手段および/または熱的手段によって除去する、少なくとも1つの工程d)をさらに含むことを特徴とする方法。
- 請求項1から12のいずれか一項に記載の方法であって、
e)粉砕工程c)で得られた水性懸濁液混合物、もしくは濃縮工程d)で得られた水性懸濁液混合物を乾燥させて水の少なくとも一部を除去して、部分脱水炭酸カルシウム含有材料を得るもしくは乾燥炭酸カルシウム含有材料を得る工程、ならびに場合により
f)工程e)の後に得られた前記乾燥炭酸カルシウム含有材料を少なくとも1つの分散剤によって処理し、これを再希釈して分散炭酸カルシウム含有材料を含む水性懸濁液を得る工程、ならびに/または
g)工程e)の後に得られた前記乾燥炭酸カルシウム含有材料を少なくとも1つの飽和脂肪族直鎖もしくは分枝カルボン酸によって、ならびに/または少なくとも1つの一置換コハク酸無水物および/もしくは少なくとも1つの一置換コハク酸および/もしくは(1または複数の)塩反応生成物によって、ならびに/または1つ以上のリン酸モノエステルおよび/もしくはその反応生成物と、1つ以上のリン酸ジエステルおよび/もしくはその反応生成物との少なくとも1つのリン酸エステルブレンドによって処理して、疎水化炭酸カルシウム含有材料を得る工程
をさらに含むことを特徴とする方法。 - 請求項1から13のいずれか一項に記載の方法によって炭酸カルシウム含有材料を製造し、炭酸カルシウム含有材料を、紙用フィラーおよび紙用コーティング用途のために、プラスチック用途、塗料、接着剤、封止剤、コンクリート、農業用途、食品用途、化粧品用途または医薬用途において使用することを含む、炭酸カルシウム含有材料の使用方法。
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US6569527B1 (en) * | 1998-05-22 | 2003-05-27 | Imerys Minerals, Limited | Particulate carbonates and their preparation and use in thermoplastic film compositions |
FR2818165B1 (fr) | 2000-12-20 | 2003-10-31 | Coatex Sas | Agent d'aide au broyage de materiaux mineraux en suspension aqueuse. suspensions aqueuses obtenues et leurs utilisations |
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