DE2153129C3 - Hexagonal plate-like white pigment and method of making the same - Google Patents

Hexagonal plate-like white pigment and method of making the same

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Publication number
DE2153129C3
DE2153129C3 DE19712153129 DE2153129A DE2153129C3 DE 2153129 C3 DE2153129 C3 DE 2153129C3 DE 19712153129 DE19712153129 DE 19712153129 DE 2153129 A DE2153129 A DE 2153129A DE 2153129 C3 DE2153129 C3 DE 2153129C3
Authority
DE
Germany
Prior art keywords
cao
white pigment
gel
pigment
integer
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.)
Expired - Lifetime
Application number
DE19712153129
Other languages
German (de)
Other versions
DE2153129B2 (en
DE2153129A1 (en
Inventor
Hirobumi Sendai Miyagi Tanaka
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
KOKUSAKU PULP INDUSTRY Co Ltd TOKYO JP
Original Assignee
KOKUSAKU PULP INDUSTRY Co Ltd TOKYO JP
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Filing date
Publication date
Application filed by KOKUSAKU PULP INDUSTRY Co Ltd TOKYO JP filed Critical KOKUSAKU PULP INDUSTRY Co Ltd TOKYO JP
Priority to DE19712153129 priority Critical patent/DE2153129C3/en
Priority to FR7142101A priority patent/FR2161409A5/en
Publication of DE2153129A1 publication Critical patent/DE2153129A1/en
Publication of DE2153129B2 publication Critical patent/DE2153129B2/en
Application granted granted Critical
Publication of DE2153129C3 publication Critical patent/DE2153129C3/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/36—Coatings with pigments
    • D21H19/38—Coatings with pigments characterised by the pigments
    • D21H19/385—Oxides, hydroxides or carbonates
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40—Compounds of aluminium
    • C09C1/402—Satin white, modifications thereof, e.g. carbonated or silicated; Calcium sulfoaluminates; Mixtures thereof, e.g. with calcium carbonate or kaolin
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Paper (AREA)

Description

Die Erfindung betrifft ein hexagonales, plattenartiges, weißes Pigment und ein Verfahren zur Herstellung desselben.The invention relates to a hexagonal, plate-like, white pigment and a method for its production same.

Kaolinit, der in hexagonaler, plattenartiger Kristallform auftritt, verleiht Papier hohen Glanz und gute «ι Bedruckbarkeit. Er wird deshalb bei der Papierherstellung in großem Ausmaß verwendet. Satinweiß ist für diesen Zweck ebenfalls verwendet worden, liegt jedoch in Form von Nadeln vor und ist deshalb bezüglich verschiedener Eigenschaften dem Kaolinit unterlegen. r>Kaolinite, which occurs in a hexagonal, plate-like crystal form, gives paper a high gloss and good quality Printability. It is therefore widely used in papermaking. Satin white is for has also been used for this purpose, but is in the form of needles and is therefore referred to various properties inferior to kaolinite. r>

Aufgabe der Erfindung ist es demgemäß, ein weiteres, für die Papierherstellung geeignetes, weißes Pigment, jedoch mit plattenartiger Kristallform, sowie ein Verfahren zur Herstellung desselben vorzusehen. Die erfindungsgemäße Lösung der Aufgabe ergibt sich aus 4n den Ansprüchen.The object of the invention is accordingly to provide a further, suitable for paper production, white pigment, but with a plate-like crystal shape, and a method for producing the same to be provided. the The solution to the problem according to the invention results from the claims.

Es ist somit gelungen, ein neuartiges, weißes Pigment herzustellen, dessen chemische Struktur derjenigen des Satinweiß ähnlich ist, das jedoch wie Graphit eine hexagonale, plattenartige Kristallform hat. -nIt has thus been possible to produce a new type of white pigment whose chemical structure is that of Satin white is similar, but like graphite, it has a hexagonal, plate-like crystal shape. -n

Das erfindungsgemäße Pigment hat die chemische Formel:The pigment according to the invention has the chemical formula:

3 CaO Al2O3Ca(X)nIvH2O,3 CaO Al 2 O 3 Ca (X) n IvH 2 O,

in der X ein einwertiges oder zweiwertiges Anion, w beispielsweise SO4-", SO3--, CO3--, CrO4--, MnO4-", Cl-, Br-, NO3-, NO2-, OH-, HCO3-, oder CH3-COO-, bedeutet, π die ganze Zahl 1 ist, wenn X ein zweiwertiges Anion ist, und η die ganze Zahl von 2 ist, wenn X ein einwertiges Anion ist, und wobei w eine v-, der ganzen Zahlen 10,12 oder 13 ist. Der Pigmentkristall hat Beugungswinkel (2Θ), die mit Röntgenstrahlen (Cu · Κλ), bei 9,95 (sehr stark), 19,90 (sehr stark) und 22,5 (stark) bestimmt wurden.in which X is a monovalent or divalent anion, w for example SO 4 - ", SO 3 -, CO 3 -, CrO 4 -, MnO 4 -", Cl-, Br-, NO 3 -, NO 2 -, OH-, HCO 3 -, or CH 3 -COO-, means π is the integer 1 when X is a divalent anion, and η is the integer of 2 when X is a monovalent anion, and where w is one v-, the integers 10, 12, or 13. The pigment crystal has diffraction angles (2Θ) which were determined with X-rays (Cu · Κλ) at 9.95 (very strong), 19.90 (very strong) and 22.5 (strong).

Das Pigment wird dadurch hergestellt, daß (a) «ι Calciumoxid oder Calciumhydroxid, (b) Aluminiumoxidgel und (c) wenigstens ein wasserlösliches Calciumsalz oder Aluminiumsalz in einer wäßrigen Suspension zur Reaktion gebracht werden. Falls erforderlich, kann das Reaktionssystem durchgemischt oder erhitzt werden. w> Die Durchmischung wird vorzugsweise durch Einleiten von Luft, die frei ist von Kohlendioxid, Sauerstoff oder Stickstoff, durchgeführt.The pigment is produced by reacting (a) calcium oxide or calcium hydroxide, (b) aluminum oxide gel and (c) at least one water-soluble calcium salt or aluminum salt in an aqueous suspension. If necessary, the reaction system can be mixed or heated. w> Mixing is preferably carried out by introducing air that is free from carbon dioxide, oxygen or nitrogen.

Die Reaktion zur Herstellung des Pigments wird beispielsweise mit folgenden Systemen durchgeführt:The reaction to produce the pigment is carried out, for example, with the following systems:

CaO -Al2O3 - Gel - H2OCaO -Al 2 O 3 - gel - H 2 O

CaO - Al2O3 - Gel - Al2(SO4)J - H2OCaO - Al 2 O 3 - Gel - Al 2 (SO 4 ) J - H 2 O

CaO - Al2O3 - Gel - CaCi2 - H2OCaO - Al 2 O 3 - Gel - CaCi 2 - H 2 O

CaO - Al2O3 - Gel - Ca(NO3)2 - H2OCaO - Al 2 O 3 - Gel - Ca (NO 3 ) 2 - H 2 O

CaO-AhO3-GeI-CaSO4 ■ 2 H2O-H2OCaO-AhO 3 -GeI-CaSO 4 ■ 2 H 2 OH 2 O

CaO - Al2O3 - Gel - AlCl3 - H2OCaO - Al 2 O 3 - Gel - AlCl 3 - H 2 O

CaO - Al2O3 - Gel - CaCrO4 - H2OCaO - Al 2 O 3 - Gel - CaCrO 4 - H 2 O

CaO - Al2O3 - Gel - Al(NO3J3 - H2OCaO - Al 2 O 3 - Gel - Al (NO 3 J 3 - H 2 O

CaO-Al2O3-GeI-CaBr2-H2OCaO-Al 2 O 3 -GeI-CaBr 2 -H 2 O

Im allgemeinen werden Reaktionstemperaturen bis zu ungefähr 120°C eingestellt. Je höher die Reaktionstemperatur ist, desto höher ist auch die Reaktionsgeschwindigkeit und desto größer werden die dabei gebildeten Kristalle. Wird jedoch das CaO -Al2O3- Gel -H2O-System verwendet, so entsteht das gewünschte Produkt mit hexagonalen, plattenartigen Kristallen in einem niedrigeren Temperaturbereich und es besteht bei Temperaturanstieg eine Tendenz zur Umwandlung in ein kubisches Hexahydrat 3 CaO · Al2O3 · 6 H2O. Im Anfangsstadium der Reaktion wird bei den SystemenIn general, reaction temperatures of up to about 120 ° C. are set. The higher the reaction temperature, the higher the reaction rate and the larger the crystals that are formed. If, however, the CaO-Al 2 O 3 -gel -H 2 O system is used, the desired product with hexagonal, plate-like crystals is formed in a lower temperature range and, when the temperature rises, there is a tendency to convert to a cubic hexahydrate 3 CaO · Al 2 O 3 · 6 H 2 O. In the initial stage of the reaction, the systems

CaO-Al2O3-GeI-CaSO4 · 2 H2O-H2O oderCaO-Al 2 O 3 -Gel-CaSO 4 · 2 H 2 OH 2 O or

Satinweiß gebildet, das in das gewünschte hexagonale, plattenartige Produkt umgewandelt wird.Satin white formed which is transformed into the desired hexagonal, plate-like product.

Es wird bevorzugt, daß die Verhältnisse der Zusätze im wäßrigen Reaktionssystem der Produktzusammensetzung entsprechen. Das Produkt hat eine Teilchengröße von ungefähr 1 bis 20 μίτι. Es ist kein Wechsel in der Form des Produkts zu beobachten, wenn es erhitzt oder einer Kohlendioxidatmosphäre unter 1 bar und bei 40 bis 60% relativer Feuchtigkeit ausgesetzt wird. Wird das Produkt einer Kohlendioxidatmosphäre unter 1 bar und bei 100% relativer Feuchtigkeit ausgesetzt, so ist ein bemerkenswerter Wechsel in der Gestalt beobachtbar, der von der Bildung von CaCO3 herrührt. Das erfindungsgemäß hergestellte Produkt ist deshalb unter Normalbedingungen chemisch und thermisch stabil. Es ist deshalb als Pigment für die Papierherstellung geeignet.It is preferred that the proportions of the additives in the aqueous reaction system correspond to the product composition. The product has a particle size of approximately 1 to 20 μm. No change in the shape of the product is observed when heated or exposed to a carbon dioxide atmosphere below 1 bar and at 40 to 60% relative humidity. When the product is exposed to a carbon dioxide atmosphere below 1 bar and at 100% relative humidity, a remarkable change in shape can be observed, which results from the formation of CaCO 3 . The product produced according to the invention is therefore chemically and thermally stable under normal conditions. It is therefore suitable as a pigment for papermaking.

Beispiel 1example 1

In ein Reaktionsgefäß mit Rührer wurden 1380 Gewichtsteile Wasser gegeben und auf 700C erhitzt. Danach wurden ungefähr 100 Teile Calciumoxid unter Rühren und unter Bildung von Kalkmilch zugesetzt. Danach wurden ungefähr 330 Teile Aluminiumoxidgel (Wassergehalt 90%) und 100 Teile Aluminiumsulfat (A12(SO4)3 · 17H2O) zugegeben. Die Temperatur des Systems wurde erhöht und 10 Stunden lang auf 80 bis 10O0C gehalten, während die Reaktion zum Abschluß gebracht wurde.In a reaction vessel equipped with a stirrer 1380 parts by weight of water were charged and heated to 70 0 C. About 100 parts of calcium oxide were then added with stirring to form milk of lime. About 330 parts of aluminum oxide gel (water content 90%) and 100 parts of aluminum sulfate (A1 2 (SO 4 ) 3 · 17H 2 O) were then added. The temperature of the system was increased and held for 10 hours at 80 to 10O 0 C, while the reaction was brought to completion.

Das erhaltene Produkt bestand aus weißen, hexagonalen, plattenartigen Kristallen der chemischen Formel 3CaO ■ Al2O3CaSO4 · 12 H2O. Die Teilchengröße reichte von 1 bis 5 μιη.The product obtained consisted of white, hexagonal, plate-like crystals of the chemical formula 3CaO · Al 2 O 3 CaSO 4 · 12 H 2 O. The particle size ranged from 1 to 5 μm.

Beispiele 2 bis 7Examples 2 to 7

In der Tabelle sind die Reaktionsieilnehmer, die nach den Verfahren des Beispiels 1 umgesetzt wurden, und die Produkte aufgeführt.In the table are the respondents who after the procedures of Example 1 were implemented and the products listed.

TabelleTabel Beispielexample

H2OH 2 O

(Teile)(Parts)

CaO (Teile)CaO (parts)

Al2O3-GeI (Teile)Al 2 O 3 gel (parts)

Al- oder Ca-SaIz (Teile)Al- or Ca-SaIz (parts)

Produktproduct

1079
1213
1344
1310
1472
13681079
1213
1344
1310
1472
1368

UO 82 81 78UO 82 81 78

120 79120 79

664 498 492 471 360 480664 498 492 471 360 480

CaCl22H2O 95,6CaCl 2 2H 2 O 95.6

Ca(NO,)24H,O 11,5Ca (NO,) 2 4H, O 11.5

CaSO42H2O 83CaSO 4 2H 2 O 83

CaBr2OH2O 142CaBr 2 OH 2 O 142

AlCl3 48AlCl 3 48

CaCrO42H2OCaCrO 4 2H 2 O

3CaOAl2O3CaCl2 10H2O3CaOAl 2 O 3 CaCl 2 10H 2 O

3 CaOAl2O3Ca(NOO2IOH2O3 CaOAl 2 O 3 Ca (NOO 2 IOH 2 O

3CaO AI2O3 CaSO4IOH2O3CaO AI 2 O 3 CaSO 4 IOH 2 O

3CaOAl2O3CaBr2IOH2O3CaOAl 2 O 3 CaBr 2 IOH 2 O

3CaOAl2O3CaCl2IOH2O3CaOAl 2 O 3 CaCl 2 IOH 2 O

3CaO Al2O3 CaCrO4WH2O3CaO Al 2 O 3 CaCrO 4 WH 2 O

Claims (2)

Patentansprüche:Patent claims: 1. HexagonaJes, plattenartiges, weißes Pigment mit der chemischen Formel ~>1. HexagonaJes, platelike, white pigment with the chemical formula ~> 3 CaO Al2O3 Ca(X)nW H2O,3 CaO Al 2 O 3 Ca (X) n WH 2 O, in der X ein einwertiges Anion und η die ganze Zahl 2 oder X ein zweiwertiges Anion und η die ganze Zahl 1 und wdie ganze Zahl 10,12 oder 13 darstellt, dessen Kristall mit Röntgenstrahlen (Cu - Kx) bestimmte Beugungswinkel (20) von 9,95°, 19,90° und 22,5° aufweistin which X is a monovalent anion and η is the integer 2 or X is a divalent anion and η is the integer 1 and w is the integer 10, 12 or 13, its crystal with X-rays (Cu - Kx) of diffraction angles (20) of 9 , 95 °, 19.90 ° and 22.5 ° 2. Verfahren zur Herstellung des Pigments des Anspruchs 1, dadurch gekennzeichnet, daß (a) π Calciumoxid oder Calciumhydroxid, (b) Aluminiumoxidgel und (c) wenigstens ein wasserlösliches Aluminiumsalz oder Calciumsalz in wäßriger Suspension, gegebenenfalls unter Durchmischen oder Erhitzen, bei Temperaturen bis zu 12O0C zur 2i> Umsetzung gebracht werden.2. Process for the preparation of the pigment of claim 1, characterized in that (a) π calcium oxide or calcium hydroxide, (b) aluminum oxide gel and (c) at least one water-soluble aluminum salt or calcium salt in aqueous suspension, optionally with mixing or heating, at temperatures up to to 12O 0 C for 2i> implementation.
DE19712153129 1971-10-25 1971-10-25 Hexagonal plate-like white pigment and method of making the same Expired - Lifetime DE2153129C3 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE19712153129 DE2153129C3 (en) 1971-10-25 1971-10-25 Hexagonal plate-like white pigment and method of making the same
FR7142101A FR2161409A5 (en) 1971-10-25 1971-11-24 White satin pigment - contg calcium oxide, alumina and an aluminium/calcium salt

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19712153129 DE2153129C3 (en) 1971-10-25 1971-10-25 Hexagonal plate-like white pigment and method of making the same

Publications (3)

Publication Number Publication Date
DE2153129A1 DE2153129A1 (en) 1973-05-03
DE2153129B2 DE2153129B2 (en) 1980-07-10
DE2153129C3 true DE2153129C3 (en) 1981-11-05

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Family Applications (1)

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Country Status (2)

Country Link
DE (1) DE2153129C3 (en)
FR (1) FR2161409A5 (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2470820A1 (en) * 1979-11-30 1981-06-12 Lafarge Sa PROCESS FOR PRODUCING MINERAL FILLERS CONTAINING HYDRATED CALCIUM MONOCARBOALUMINATE
DE3225897A1 (en) * 1982-07-10 1984-01-12 Degussa Ag, 6000 Frankfurt INORGANIC PIGMENTS AND METHOD FOR THE PRODUCTION THEREOF
DE102006055214A1 (en) * 2006-11-21 2008-05-29 Nabaltec Gmbh Calcium carbonate hydroxodialuminates having hexagonal-plate crystal habit

Also Published As

Publication number Publication date
FR2161409A5 (en) 1973-07-06
DE2153129B2 (en) 1980-07-10
DE2153129A1 (en) 1973-05-03

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