FR2657354A1 - Composite pigment containing titanium oxide and process for obtaining it - Google Patents

Composite pigment containing titanium oxide and process for obtaining it Download PDF

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Publication number
FR2657354A1
FR2657354A1 FR9001019A FR9001019A FR2657354A1 FR 2657354 A1 FR2657354 A1 FR 2657354A1 FR 9001019 A FR9001019 A FR 9001019A FR 9001019 A FR9001019 A FR 9001019A FR 2657354 A1 FR2657354 A1 FR 2657354A1
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Prior art keywords
adjuvant
powder
particle size
volume
group
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FR9001019A
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French (fr)
Inventor
Alary Jean-Andre
Greff Jerome
Dagrada Rene
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RECH EXPL MINIERES STE GLE
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RECH EXPL MINIERES STE GLE
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Priority to FR9001019A priority Critical patent/FR2657354A1/en
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    • 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
    • C09C1/0081—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound
    • C09C1/0084—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound containing titanium dioxide
    • C09C1/0087—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound containing titanium dioxide only containing titanium dioxide and silica or silicate
    • 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
    • C09C1/0081—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound
    • C09C1/0084—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound containing titanium dioxide

Abstract

Composite pigments containing titanium oxide and one (or more) mineral(s) and a process for obtaining the said composite pigments. The process consists: - in mixing submicronic TiO2 powders and adjuvant(s) with an adjuvant/TiO2 weight ratio of between 60/40 and 90/10 - in placing the whole in aqueous suspension with a solids content of up to 75 % - in spraying this suspension so as to obtain a final powder whose mean particle size D50 >/= 1 mu m (and preferably >/= 2 mu m) is such that not more than 10 % by volume is smaller than 1 mu m and not more than 10 % is larger than 30 mu m. Wetting agents, a silicon oil and/or silanes may be added to the initial mixture. The pigments obtained are used as fillers in the paper, paint, plastics and other industries.

Description

PIGMENT COMPOSITE CONTENANT DE L'OXYDE DE TITANE ET PROCEDE D'OBTENTION
L'invention concerne des pigments composites contenant de l'oxyde de titane, un (ou plusieurs) autre(s) minéral(aux) et un procédé d'obtention des pigments composites considérés.COMPOSITE PIGMENT CONTAINING TITANIUM OXIDE AND PROCESS FOR OBTAINING
The invention relates to composite pigments containing titanium oxide, one (or more) other mineral (s) and a process for obtaining the composite pigments under consideration.

Les produits de ce type sont connus et sont généralement obtenus par co-broyage intense de TiO2 et d'un (ou plusieurs) autre(s) minéral(aux) tels que feldspath, mica, talc, etc... Un tel procédé est décrit par exemple dans la demande de brevet français FR-A-2575170.Products of this type are known and are generally obtained by intense co-grinding of TiO2 and of one (or more) other mineral (s) such as feldspar, mica, talc, etc. Such a process is described for example in French patent application FR-A-2575170.

Cependant, ce procédé conduit à des produits pulvérulents ayant une prise d'huile trop élevée ( > 30 g/100 g suivant la norme AFNOR NF T30-022) et/ou une blancheur insuffisante ( < 90 suivant le norme NF Q-003-038).However, this process leads to powdery products having too high an oil uptake (> 30 g / 100 g according to the AFNOR standard NF T30-022) and / or insufficient whiteness (<90 according to the standard NF Q-003- 038).

Les produits selon l'invention possèdent une prise d'huile < 30 g/100 g et une blancheur }90. The products according to the invention have an oil uptake <30 g / 100 g and a whiteness} 90.

Les produits selon l'invention sont les pigments composites essentiellement constitués de Ti02 et d'un autre adjuvant minéral obtenu sous forme de poudre, dont la granulométrie moyenne est supérieure ou égale à 1 gm et de préférence k 2 Mm. The products according to the invention are the composite pigments essentially consisting of TiO 2 and of another mineral adjuvant obtained in the form of powder, the average particle size of which is greater than or equal to 1 gm and preferably k 2 Mm.

Par la granulométrie moyenne (D50) on entend la taille des particules pour laquelle 50% en volume possède une taille supérieure ou égale à cette dimension D50.By average particle size (D50) is meant the particle size for which 50% by volume has a size greater than or equal to this dimension D50.

La taille maximale (100% passant) sera désigné par D100.The maximum size (100% passing) will be designated by D100.

De façon plus précise, la granulométrie est telle qu' au plus 10% (en volume) des grains sont de taille inférieure à 1 gm et au plus 10% (en volume) sont de taille supérieure à 30 Mm. More precisely, the particle size is such that at most 10% (by volume) of the grains are of size less than 1 gm and at most 10% (by volume) are of size greater than 30 mm.

Ce produit est constitué de grains d'adjuvant minéral ayant leur surface tapissée de particules de Ti02 et agglomérés en particules individuelles dont la taille moyenne est k 1 Mm et de préférence k 2 Um. This product consists of grains of mineral additive having their surface lined with TiO 2 particles and agglomerated into individual particles whose average size is k 1 Mm and preferably k 2 Um.

Par "TiO2,, on entend le Ti02 pur, le TiO2 pour peintures (par ex. les références RL60 ou RL68 de THANN et MULHOUSE) et/ou le TiO2 pour plastiques (par ex. la référence RL90 de la même société). By "TiO2 ,, we mean pure Ti02, TiO2 for paints (eg the references RL60 or RL68 from THANN and MULHOUSE) and / or TiO2 for plastics (eg the reference RL90 from the same company).

Les adjuvants appartiennent au groupe des produits siliceux, de la famille des silicates, des carbonates ou de sulfates.Adjuvants belong to the group of siliceous products, of the family of silicates, carbonates or sulfates.

Les principaux représentants en sont le feldspath, le mica, le talc, la wollastonite, le silicate de Ca, la barytine, le calcin, utilisés seuls ou en mélange.The main representatives are feldspar, mica, talc, wollastonite, Ca silicate, barite, cullet, used alone or as a mixture.

Le rapport pondéral adjuvant/ "tu02" est compris entre 40/60 et 90/10.The adjuvant / "tu02" weight ratio is between 40/60 and 90/10.

Au-dessous de 40/60, le prix du pigment composite est trop élevé; en-dessous de 90/10, la blancheur obtenue est insuffisante.Below 40/60, the price of the composite pigment is too high; below 90/10, the whiteness obtained is insufficient.

La liaison entre les grains TiO2 et ceux de l'adjuvant est une liaison forte de type chimique.The bond between the TiO2 grains and those of the adjuvant is a strong bond of chemical type.

Le procédé consiste: a à mélanger des poudres de "tu02" (submicronique) et d'adjuvant(s) avec un rapport pondéral adjuvant/"TiO2" compris entre 60/40 et 90/10.The method consists in: a mixing powders of "tu02" (submicron) and of adjuvant (s) with an adjuvant / "TiO2" weight ratio of between 60/40 and 90/10.

2 . à mettre l'ensemble en suspension aqueuse, contenant jusqu'à 75% de matière sèche. 2. to put the whole in aqueous suspension, containing up to 75% of dry matter.

- à atomiser cette suspension de manière à obtenir une poudre finale dont la granulométrie moyenne D50 k 1 gm (et de préférence k 2 pm) est telle qu au plus 10% en volume soit inférieure 1 gm et au plus 10% > 30 Mm. - To atomize this suspension so as to obtain a final powder whose average particle size D50 k 1 gm (and preferably k 2 pm) is such that at most 10% by volume is less than 1 gm and at most 10%> 30 Mm.

On peut éventuellement ajouter au mélange initial un (ou des) agent(s) mouillant(s), dispersant(s) ou défloculant(s), de 0,1 à 1% (en poids) % par rapport à la matière sèche et/ou une huile de silicone ou un silane de préférence entre 1 et 10% en poids/matière sèche.It is optionally possible to add to the initial mixture a wetting agent (s), dispersant (s) or deflocculant (s), from 0.1 to 1% (by weight)% relative to the dry matter and / or a silicone oil or a silane preferably between 1 and 10% by weight / dry matter.

Au-delà des valeurs limites de 0,1% à 1%, la viscosité à fort taux de cisaillement (1000s .1) de la suspension est trop importante, ce qui interdit l'atomisation de suspension contenant plus de 75% de matières sèches.Beyond the limit values of 0.1% to 1%, the viscosity at high shear rate (1000s .1) of the suspension is too high, which prohibits the atomization of suspension containing more than 75% of dry matter .

Au-dessous de 1% d'huile de silicone ou silane, la tenue de TiO2 sur l'adjuvant est limitée.Below 1% of silicone or silane oil, the resistance of TiO2 on the adjuvant is limited.

Au-dessus de 10% d'huile de silicone ou silane, la blancheur n'est pas atteinte.Above 10% silicone or silane oil, the whiteness is not reached.

La granulométrie moyenne de l'adjuvant entrant dans le mélange (D50) est inférieure ou égale à 5 Mm; il comprend au plus 10% en volume de particules k 5 Mm. The average particle size of the adjuvant entering the mixture (D50) is less than or equal to 5 mm; it comprises at most 10% by volume of particles k 5 Mm.

L'invention sera mieux comprise à l'aide des exemples suivants:
EXEMPLE 1
Des échantillons ont été préparés dans les conditions suivantes: - mélange de:
feldspath EAL (SOGEREM) prébroyé mécaniquement et possédant la granulométrie suivante:
D50 = 3,20 Mm D100 = 20 Mm
50 . TiO2 "Rectapur" de PROLABO possédant la granulométrie suivante
D50 = 0,48 Mm D100 = 6 gm dans les proportions pondérales respectives 70/30.The invention will be better understood using the following examples:
EXAMPLE 1
Samples were prepared under the following conditions: - mixture of:
feldspar EAL (SOGEREM) mechanically pre-ground and having the following particle size:
D50 = 3.20 Mm D100 = 20 Mm
50. PROLABO TiO2 "Rectapur" with the following particle size
D50 = 0.48 Mm D100 = 6 gm in the respective weight proportions 70/30.

On a ajouté à ce mélange 0,2% en poids d'un agent dispersant nO 6768 de
STEPAN (polycarboxylate d'ammonium), ainsi que 5,5% en poids d'huile de silicone "RHODORSIL 10646" de RHONE-POULENC. 0.2% by weight of a dispersing agent No. 6768 of
STEPAN (ammonium polycarboxylate), as well as 5.5% by weight of silicone oil "RHODORSIL 10646" from RHONE-POULENC.

L'atomisation a été conduite sur atomiseur de laboratoire Mini Spray Dryer 5-90 de BUCHI dans les conditions suivantes:
Suspension à 60% en matière sèche
Température d'entrée: 2200C
Température de sortie: 1300C
Débit d'alimentation de la suspension : 0,8 1/h
Les résultats obtenus concernant la granulométrie finale (déterminée avec l'appareil Horiba Kappa 700) et les propriétés de prise d'huile et de blancheur selon les normes citées, sont les suivantes - D50 = 16,15 M m - D100= 40 gm - prise d'huile: 20g/lOOg - blancheur : 91
EXEMPLE 2
Mêmes caractéristiques que pour l'Exemple 1 sauf - EAL prébroyé mécaniquement et possédant la granulométrie D50=0,28 Mm
D100=2 gm - 1% par rapport à la matrice sèche d'huile de S; Rhodersil 10646.The atomization was carried out on a BUCHI Mini Spray Dryer 5-90 laboratory atomizer under the following conditions:
60% solids suspension
Inlet temperature: 2200C
Outlet temperature: 1300C
Suspension feed rate: 0.8 1 / h
The results obtained concerning the final particle size (determined with the Horiba Kappa 700 device) and the properties of oil setting and whiteness according to the standards cited, are as follows - D50 = 16.15 M m - D100 = 40 gm - oil intake: 20g / lOOg - whiteness: 91
EXAMPLE 2
Same characteristics as for Example 1 except - EAL mechanically pre-ground and having the particle size D50 = 0.28 mm
D100 = 2 gm - 1% relative to the dry matrix of S oil; Rhodersil 10646.

L'atomisation a été conduite dans les mêmes conditions que dans l'Exemple 1.The atomization was carried out under the same conditions as in Example 1.

Les caractéristiques de la poudre composite obtenue sont les suivantes - blancheur : 92 - prise d'huile : 34g/100 g - D50 = 3,5 gm - D100 = 10 Mn. The characteristics of the composite powder obtained are as follows - whiteness: 92 - oil setting: 34 g / 100 g - D50 = 3.5 gm - D100 = 10 Mn.

Claims (16)

REVENDICATIONS 1. Pigment composite contenant de l'oxyde de titane et un (ou plusieurs)1. Composite pigment containing titanium oxide and one (or more) autre(s) adjuvant(s) minéral(aux) caractérisé en ce qu'il est sous other mineral adjuvant (s) characterized in that it is under forme de poudre dont la granulométrie moyenne est supérieure ou égale à powder form with an average particle size greater than or equal to 1 Um et de préférence k 2 um 1 um and preferably k 2 um 2. Pigment composite selon la revendication 1 caractérisé en ce qu'il2. Composite pigment according to claim 1 characterized in that it comporte au plus 10% (en volume) des grains de taille I 1 gm et au plus contains at most 10% (by volume) of grain size I 1 gm and at most 10% (en volume) de grains de taille k 30 Um.  10% (by volume) of grain size k 30 Um. 3. Pigment selon l'une des revendications 1 ou 2 caractérisé en ce que3. Pigment according to one of claims 1 or 2 characterized in that 1 'adjuvant appartient au groupe constitué a un ou plusieurs produits The adjuvant belongs to the group made up of one or more products siliceux, carbonates, silicates ou sulfates. siliceous, carbonates, silicates or sulfates. 4. Produit selon la revendication 3 caractérisé en ce que l'adjuvant4. Product according to claim 3 characterized in that the adjuvant comporte un (ou plusieurs) des éléments de groupe constitué par le contains one (or more) group elements made up of the feldspath, le mica, le talc, la wollastonite, le silicate de Ca, la feldspar, mica, talc, wollastonite, Ca silicate, barytine, le calcin. barite, cullet. 5. Produit selon l'une des revendications 1 à 4 caractérisé en ce que le 5. Product according to one of claims 1 to 4 characterized in that the rapport pondéral adjuvant/"Ti0 " est compris entre 40/60 et 90/10. adjuvant weight ratio / "Ti0" is between 40/60 and 90/10. et agglomérés en particules individuelles. and agglomerated into individual particles. est consitué de grains d'adjuvant ayant leur surface tapissée de "Ti02"  is made up of additive grains having their surface covered with "Ti02" 2 2 6. Produit selon l'une des revendications 1 à 5 caractérisé en ce qu'il6. Product according to one of claims 1 to 5 characterized in that it 7. Procédé selon l'une des revendications 1 à 6 caractérisé en ce que la 7. Method according to one of claims 1 to 6 characterized in that the liaison "Ti02"/adjuvant est une liaison forte de type chimique. "Ti02" / adjuvant bond is a strong chemical bond. et de préférence k 2 pm.  and preferably k 2 pm. poudre finale dont la granulométrie D50 est supérieure ou égale à 1 Mm  final powder with a particle size D50 greater than or equal to 1 mm - on atomise le mélange aqueux ainsi obtenu de manière à obtenir une - The aqueous mixture thus obtained is atomized so as to obtain a - on réalise une suspension de ce mélange en milieu aqueux  - A suspension of this mixture is produced in an aqueous medium siliceux et/ou de la famille des silicates, carbonates,sulfates siliceous and / or of the family of silicates, carbonates, sulfates adjuvant(s) sous forme de poudre appartenant au groupe des minéraux powder adjuvant (s) belonging to the group of minerals - on mélange une poudre de Ti02 (submicronique) avec un (ou des) - a powder of Ti02 (submicron) is mixed with one (or more) une faible prise d'huile, une blancheur élevée caractérisé en ce que: low oil uptake, high whiteness characterized in that: 2 2 8. Procédé d'obtention de pigments composites contenant du tlTiO2" ayant8. Process for obtaining composite pigments containing tlTiO2 "having 9. Procédé selon la revendication 8 caractérisé en ce que l'atomisation9. Method according to claim 8 characterized in that the atomization conduit à une poudre dont au plus 10% (en volume) est 8 1 Mm et au plus leads to a powder of which at most 10% (by volume) is 8 1 Mm and at most 10% (en volume) est k 30 Mm.  10% (by volume) is k 30 mm. inférieure ou égale à 5 Mm.  less than or equal to 5 mm. moyenne D50 de l'adjuvant entrant dans le mélange initial est average D50 of the adjuvant entering the initial mixture is 10.Procédé selon la revendication 8 caractérisé en ce que la granulométrie 10. Method according to claim 8 characterized in that the particle size plusieurs) agent(s) mouillant(s), dispersant(s) ou défloculant(s). several) wetting agent (s), dispersant (s) or deflocculant (s). ajoute au mélange initial de 0,1 à 1% en poids au total d'un (ou add to the initial mixture 0.1 to 1% by weight in total of one (or 11.Procédé selon les revendications 8 ou 10 caractérisé en ce que l'on 11. Process according to claims 8 or 10 characterized in that one silane(s) à raison de 1 à 10% en poids au total. silane (s) at a rate of 1 to 10% by weight in total. on ajoute au mélange initial une huile de silicone ou un ou (des) a silicone oil or one or more is added to the initial mixture 12.Procédé selon l'une des revendications 8 ou 10, caractérisé en ce que 12. Method according to one of claims 8 or 10, characterized in that rapport pondéral adjuvant/TiO2 est compris entre 50/60 et 90/10. adjuvant / TiO2 weight ratio is between 50/60 and 90/10. 13.Procédé selon l'une des revendications 8 à 12 caractérisé en ce que le  13. Method according to one of claims 8 to 12 characterized in that the barytine. barite. feldspath, le mica, le talc, wollastonite, silicate de Ca, calcin, feldspar, mica, talc, wollastonite, Ca silicate, cullet, adjuvant(s) est (sont) choisi(s) dans le groupe constitué par le adjuvant (s) is (are) selected from the group consisting of 2 2 14.Procédé selon la revendication 13 caractérisé en ce que le (ou les)14. Method according to claim 13 characterized in that the (or them) 15.Procédé selon l'une des revendications 8 à 14 caractérisé en ce que le15. Method according to one of claims 8 to 14 characterized in that the (ou les) adjuvant(s) sont amenés à la granulométrie requise pour le (or the) adjuvant (s) are brought to the particle size required for the mélange par broyage mécanique, de manière à obtenir au plus 10% de la mixing by mechanical grinding, so as to obtain at most 10% of the poudre k 5 gm.  powder k 5 gm. 16.Procédé selon l'une des revendications 8 à 15 caractérisé en ce que la16. Method according to one of claims 8 to 15 characterized in that the suspension formée contient jusqu'à 75% de matière sèche.  suspension formed contains up to 75% dry matter.
FR9001019A 1990-01-19 1990-01-19 Composite pigment containing titanium oxide and process for obtaining it Withdrawn FR2657354A1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2678630A1 (en) * 1991-07-03 1993-01-08 Rech Expl Minieres Ste Gle Composite pigment containing titanium oxide and process of preparation
US5562763A (en) * 1992-04-07 1996-10-08 Merck Patent Gesellschaft Mit Beschrankter Haftung Process for the preparation of composite pigments

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
LU40959A1 (en) * 1961-12-14 1962-03-07
US3253939A (en) * 1962-02-19 1966-05-31 Laporte Titanium Ltd Titanium dioxide pigments
US3453131A (en) * 1966-01-05 1969-07-01 Oxford Paper Co Composite colloidal pigment particles,their formation and suspensions thereof
US3459574A (en) * 1964-11-20 1969-08-05 Du Pont Opacifying pigment glass composition
FR2386590A1 (en) * 1977-04-04 1978-11-03 Noranda Mines Ltd NEW CORROSION INHIBITOR PIGMENTS BASED ON ZINC MOLYBDATE COMPOUNDS

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
LU40959A1 (en) * 1961-12-14 1962-03-07
US3253939A (en) * 1962-02-19 1966-05-31 Laporte Titanium Ltd Titanium dioxide pigments
US3459574A (en) * 1964-11-20 1969-08-05 Du Pont Opacifying pigment glass composition
US3453131A (en) * 1966-01-05 1969-07-01 Oxford Paper Co Composite colloidal pigment particles,their formation and suspensions thereof
FR2386590A1 (en) * 1977-04-04 1978-11-03 Noranda Mines Ltd NEW CORROSION INHIBITOR PIGMENTS BASED ON ZINC MOLYBDATE COMPOUNDS

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2678630A1 (en) * 1991-07-03 1993-01-08 Rech Expl Minieres Ste Gle Composite pigment containing titanium oxide and process of preparation
US5562763A (en) * 1992-04-07 1996-10-08 Merck Patent Gesellschaft Mit Beschrankter Haftung Process for the preparation of composite pigments

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