USRE32320E - TiO2 pigment bearing a coating with cerium cations and sulfate-, phosphate- or silicate anions and laminate and coating containing same - Google Patents

TiO2 pigment bearing a coating with cerium cations and sulfate-, phosphate- or silicate anions and laminate and coating containing same Download PDF

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Publication number
USRE32320E
USRE32320E US06/737,501 US73750185A USRE32320E US RE32320 E USRE32320 E US RE32320E US 73750185 A US73750185 A US 73750185A US RE32320 E USRE32320 E US RE32320E
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United States
Prior art keywords
sulfate
pigment
tio
parts
slurry
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Expired - Lifetime
Application number
US06/737,501
Inventor
Howard W. Jacobson
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EIDP Inc
Original Assignee
EI Du Pont de Nemours and Co
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Filing date
Publication date
Priority claimed from US06/481,925 external-priority patent/US4461810A/en
Application filed by EI Du Pont de Nemours and Co filed Critical EI Du Pont de Nemours and Co
Priority to US06/737,501 priority Critical patent/USRE32320E/en
Assigned to E. I. DU PONT DE NEMOURS AND COMPANY, WILMINGTON, DELAWARE, A CORP OF DELAWARE reassignment E. I. DU PONT DE NEMOURS AND COMPANY, WILMINGTON, DELAWARE, A CORP OF DELAWARE ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: JACOBSON, HOWARD W.
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Publication of USRE32320E publication Critical patent/USRE32320E/en
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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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
    • 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
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3653—Treatment with inorganic compounds
    • C09C1/3661—Coating
    • 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
    • D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
    • D21H27/18—Paper- or board-based structures for surface covering
    • D21H27/22—Structures being applied on the surface by special manufacturing processes, e.g. in presses
    • D21H27/26—Structures being applied on the surface by special manufacturing processes, e.g. in presses characterised by the overlay sheet or the top layers of the structures
    • D21H27/28—Structures being applied on the surface by special manufacturing processes, e.g. in presses characterised by the overlay sheet or the top layers of the structures treated to obtain specific resistance properties, e.g. against wear or weather
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/256—Heavy metal or aluminum or compound thereof
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/27—Web or sheet containing structurally defined element or component, the element or component having a specified weight per unit area [e.g., gms/sq cm, lbs/sq ft, etc.]
    • Y10T428/273—Web or sheet containing structurally defined element or component, the element or component having a specified weight per unit area [e.g., gms/sq cm, lbs/sq ft, etc.] of coating
    • Y10T428/277—Cellulosic substrate
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31942—Of aldehyde or ketone condensation product
    • Y10T428/31949—Next to cellulosic
    • Y10T428/31964—Paper

Definitions

  • This invention relates to pigment composed of coated TiO 2 particles. More particularly, it relates to a pigment of TiO 2 particles coated with alumina and having cerium cations and sulfate-, phosphate or silicate anions associated with them.
  • Paper laminates are products widely used in the construction industry for making counter tops and the like. They are ordinarily composed of paper impregnated with TiO 2 pigment and imbedded in a polymer matrix. Such laminates have an unfortunate tendency to discolor on exposure to ultraviolet light, and this detracts from their value because in many uses they are necessarily exposed to such radiation.
  • the pigment of the present invention is highly resistant to discoloration on exposure to ultraviolet light, and, when used in making a paper laminate, gives a product with significantly better lightfastness than one made with conventional TiO 2 pigment.
  • the pigment of the invention is composed of rutile TiO 2 particles conventionally coated with alumina or with alumina-silica.
  • the coating ordinarily constitutes 1-8%, by weight, of the pigment.
  • cerium cations preferably Ce +4 ions
  • Associated with the pigment particle surfaces are cerium cations (preferably Ce +4 ions), at a concentration of .[.0.5-2%,.]. .Iadd.about 0.17-2%, .Iaddend.by weight, and a stoichiometric amount of sulfate-, phosphate or silicate anions.
  • "Associated with the particle surfaces” means that the ions are bound to the TiO 2 particles by a chemical or physical attraction.
  • the ion content of the pigment may be determined by ion plasma chromatography.
  • the amount of alumina the TiO 2 particles bear as coatings is calculated by first determining, by ion plasma spectroscopy,
  • the cerium cations may be supplied by any water-soluble cerium salt, preferably cerium sulfate, and even more preferably ceric sulfate: when the anion is sulfate, this will also supply the sulfate ion.
  • the anion of choice is phosphate or silicate, it is supplied by using phosphoric acid or sodium silicate solution during preparation of the pigment, as will be described.
  • the TiO 2 used to prepare the pigment or the invention can be of the conventional rutile variety, prepared by either the chloride or the sulfate process.
  • the pigment of the invention can be made by first preparing an aqueous slurry containing 200-400 grams per liter of TiO 2 . This slurry is brought to 45°-70° C. and is held there during the rest of the preparation procedure. To the slurry is then added, with stirring, enough of a cerium salt to give a cerium ion concentration in the slurry of .[.0.5-2%,.]. .Iadd.0.05-2%, .Iaddend.by weight of the TiO 2 . If one desires a phosphate anion or a silicate anion to be associated with the pigment, he also adds a stoichiometric amount of phosphoric acid or sodium silicate. In any case, the slurry is then stirred for 1-15 minutes.
  • Alumina is then precipitated on the TiO 2 particles by slowly adding enough sodium aluminate to the slurry to give a concentration of about 2-8%, by weight of the TiO 2 .
  • Acid ordinarily sulfuric or hydrochloric, is added at the same time to maintain the pH of the slurry within the range 6-9 during the precipitation step.
  • the slurry is allowed to cure, with stirring, for 15-30 minutes.
  • the resulting pigment is then separated from the liquid by filtration or centrifugation, is washed with water and then dried.
  • the pigment thus prepared may be used to prepare a paper laminate in any of the customary ways typically by mixing the pigment with paper pulp and then making paper of it in the usual way, impregnating this paper with resin, ordinarily a melamine-formaldehyde or urea-formaldehyde resin, and then curing the mixture with heat.
  • resin ordinarily a melamine-formaldehyde or urea-formaldehyde resin
  • Coating compositions may be prepared with the pigments of the invention in any of the conventional ways, by blending the pigment with a film-forming component and a liquid carrier.
  • rutile TiO 2 Three thousand parts of rutile TiO 2 were dispersed in 7500 parts of distilled water, to give a slurry with a pH of 3.6. The slurry was then heated to and held at 50° C., and to it were added, over a 5-minute period, 145 parts of a solution of 85.5 parts of ceric sulfate in 1000 parts of water. The slurry at this point had a pH of 1.5. The slurry was then stirred for 10 minutes at 50° C.
  • the slurry was stirred for 30 minutes at 50° C.
  • the TiO 2 was then filtered off, washed with water, dried and micronized.
  • the resulting pigment was composed of TiO 2 particles coated with alumina and having cerium and sulfate anions associated with them.
  • the slurry was stirred for 30 minutes at 50° C.
  • the TiO 2 was then filtered off, washed with water, dried and micronized.
  • the resulting pigment was composed of TiO 2 particles coated with alumina and having cerium cations and phosphate anions associated with them.
  • the slurry was stirred for 30 minutes at 50° C.
  • the TiO 2 was then filtered off, washed with water, dried and micronized.
  • the resulting pigment was composed of TiO 2 particles coated with alumina and having cerium cations and silicate anions associated with them.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

A pigment of TiO2 particles coated with alumina, whose particle surfaces have associated with them cerium cations and sulfate-, phosphate or silicate anions, can be used to prepare paper laminates having a high degree of lightfastness.

Description

DESCRIPTION Technical Field
This invention relates to pigment composed of coated TiO2 particles. More particularly, it relates to a pigment of TiO2 particles coated with alumina and having cerium cations and sulfate-, phosphate or silicate anions associated with them.
BACKGROUND AND SUMMARY OF THE INVENTION
Paper laminates are products widely used in the construction industry for making counter tops and the like. They are ordinarily composed of paper impregnated with TiO2 pigment and imbedded in a polymer matrix. Such laminates have an unfortunate tendency to discolor on exposure to ultraviolet light, and this detracts from their value because in many uses they are necessarily exposed to such radiation.
The pigment of the present invention is highly resistant to discoloration on exposure to ultraviolet light, and, when used in making a paper laminate, gives a product with significantly better lightfastness than one made with conventional TiO2 pigment.
The pigment of the invention is composed of rutile TiO2 particles conventionally coated with alumina or with alumina-silica. The coating ordinarily constitutes 1-8%, by weight, of the pigment. Associated with the pigment particle surfaces are cerium cations (preferably Ce+4 ions), at a concentration of .[.0.5-2%,.]. .Iadd.about 0.17-2%, .Iaddend.by weight, and a stoichiometric amount of sulfate-, phosphate or silicate anions. "Associated with the particle surfaces" means that the ions are bound to the TiO2 particles by a chemical or physical attraction.
The ion content of the pigment may be determined by ion plasma chromatography.
The amount of alumina the TiO2 particles bear as coatings, expressed as percent by weight, is calculated by first determining, by ion plasma spectroscopy,
(a) the alumina content of a pigment of the invention, and
(b) the alumina content of the raw TiO2 from which the pigment is made,
and then computing the alumina coating content of the pigment by difference.
The cerium cations may be supplied by any water-soluble cerium salt, preferably cerium sulfate, and even more preferably ceric sulfate: when the anion is sulfate, this will also supply the sulfate ion. When the anion of choice is phosphate or silicate, it is supplied by using phosphoric acid or sodium silicate solution during preparation of the pigment, as will be described.
The TiO2 used to prepare the pigment or the invention can be of the conventional rutile variety, prepared by either the chloride or the sulfate process.
The pigment of the invention can be made by first preparing an aqueous slurry containing 200-400 grams per liter of TiO2. This slurry is brought to 45°-70° C. and is held there during the rest of the preparation procedure. To the slurry is then added, with stirring, enough of a cerium salt to give a cerium ion concentration in the slurry of .[.0.5-2%,.]. .Iadd.0.05-2%, .Iaddend.by weight of the TiO2. If one desires a phosphate anion or a silicate anion to be associated with the pigment, he also adds a stoichiometric amount of phosphoric acid or sodium silicate. In any case, the slurry is then stirred for 1-15 minutes.
Alumina is then precipitated on the TiO2 particles by slowly adding enough sodium aluminate to the slurry to give a concentration of about 2-8%, by weight of the TiO2. Acid, ordinarily sulfuric or hydrochloric, is added at the same time to maintain the pH of the slurry within the range 6-9 during the precipitation step. After addition of the aluminate is complete, the slurry is allowed to cure, with stirring, for 15-30 minutes.
The resulting pigment is then separated from the liquid by filtration or centrifugation, is washed with water and then dried.
The pigment thus prepared may be used to prepare a paper laminate in any of the customary ways typically by mixing the pigment with paper pulp and then making paper of it in the usual way, impregnating this paper with resin, ordinarily a melamine-formaldehyde or urea-formaldehyde resin, and then curing the mixture with heat. These procedures are set forth in greater detail in U.S. Pat. No. 4,239,548, which is incorporated into this specification to show such procedures.
Coating compositions may be prepared with the pigments of the invention in any of the conventional ways, by blending the pigment with a film-forming component and a liquid carrier.
EXAMPLES
In the following examples, all parts are by weight.
EXAMPLE 1
Three thousand parts of rutile TiO2 were dispersed in 7500 parts of distilled water, to give a slurry with a pH of 3.6. The slurry was then heated to and held at 50° C., and to it were added, over a 5-minute period, 145 parts of a solution of 85.5 parts of ceric sulfate in 1000 parts of water. The slurry at this point had a pH of 1.5. The slurry was then stirred for 10 minutes at 50° C.
To the slurry were then added, over a 30-minute period and with stirring at 50° C., 400 parts of an aqueous solution of sodium aluminate (containing an equivalent of 350 parts of Al2 O3 per 1000 parts of water). During this addition, the pH of the slurry was held at about 6.5 by adding sulfuric acid.
When addition of the sodium aluminate was finished, the slurry was stirred for 30 minutes at 50° C. The TiO2 was then filtered off, washed with water, dried and micronized.
The resulting pigment was composed of TiO2 particles coated with alumina and having cerium and sulfate anions associated with them.
EXAMPLE 2
Three thousand parts of rutile TiO2 were dispersed in 7500 parts of distilled water, to give a slurry with a pH of 3.6. The slurry was then heated to and held at 50° C., and to it were added, over a 5-minute period, 140 parts of a solution of 85.5 parts of ceric sulfate in 1000 parts of water.
When addition of the ceric sulfate was finished, 24 parts of concentrated H3 PO4 were added and the slurry stirred for 10 minutes at 50° C.
To the slurry were then added, over a 30-minute period and with stirring at 50° C., 343 parts of an aqueous solution of sodium aluminate (containing an equivalent of 350 parts of Al2 O3 per 100 parts of water). During this addition, the pH of the slurry was held at about 7.5 by adding sulfuric acid.
When the addition of the sodium aluminate was finished, the slurry was stirred for 30 minutes at 50° C. The TiO2 was then filtered off, washed with water, dried and micronized.
The resulting pigment was composed of TiO2 particles coated with alumina and having cerium cations and phosphate anions associated with them.
EXAMPLE 3
Two hundred parts of rutile TiO2 were dispersed in 500 parts of distilled water, to give a slurry with a pH of 3.8. The slurry was then heated to and held at 50° C., and to it were added, over a 5-minute period, 9.4 parts of a solution of 85.5 parts of ceric sulfate in 1000 parts of water.
When the addition of the ceric sulfate was finished, 5 parts of an aqueous sodium silicate solution (containing an equivalent of 400 parts of SiO2 per 1000 parts of water) were added and the slurry stirred for 10 minutes at 50° C.
To the slurry were then added, over a 10-minute period and with stirring at 50° C., 22.9 parts of an aqueous solution of sodium aluminate (containing an equivalent of 350 parts of Al2 O3 per 100 parts of water). During this addition, the pH of the slurry was held at about 7.5 by adding sulfuric acid.
When the addition of the sodium aluminate was finished, the slurry was stirred for 30 minutes at 50° C. The TiO2 was then filtered off, washed with water, dried and micronized.
The resulting pigment was composed of TiO2 particles coated with alumina and having cerium cations and silicate anions associated with them.

Claims (3)

I claim:
1. A pigment of rutile TiO2 particles bearing coatings consisting of alumina or alumina-silica, the particle surfaces having associated therewith .[.0.5-2%,.]. .Iadd.0.17-2%, .Iaddend.by weight of the TiO2, of cerium cations and a stoichiometric amount of sulfate-, phosphate or silicate anions.
2. A paper laminate comprising paper and a pigment according to claim 1, in a rigid matrix.
3. A coating composition comprising
(a) a pigment according to claim 1,
(b) a film-forming material, and
(c) a liquid carrier.
US06/737,501 1983-04-04 1985-05-24 TiO2 pigment bearing a coating with cerium cations and sulfate-, phosphate- or silicate anions and laminate and coating containing same Expired - Lifetime USRE32320E (en)

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US06/737,501 USRE32320E (en) 1983-04-04 1985-05-24 TiO2 pigment bearing a coating with cerium cations and sulfate-, phosphate- or silicate anions and laminate and coating containing same

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/481,925 US4461810A (en) 1983-04-04 1983-04-04 TiO2 Pigment bearing a coating with cerium cations and sulfate-, phosphate- or silicate anions and laminate and coating containing same
US06/737,501 USRE32320E (en) 1983-04-04 1985-05-24 TiO2 pigment bearing a coating with cerium cations and sulfate-, phosphate- or silicate anions and laminate and coating containing same

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5730796A (en) * 1995-06-01 1998-03-24 Kerr-Mcgee Chemical Corporation Durable pigmentary titanium dioxide and methods of producing the same
US5777001A (en) * 1997-08-04 1998-07-07 Kerr Mcgee Chemical Corp. Graft polymerized metal oxide compositions and methods
US5851652A (en) * 1992-10-09 1998-12-22 E. I. Du Pont De Nemours And Company Lightfast T102 pigment

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1023590A (en) * 1963-05-21 1966-03-23 British Titan Products Titanium dioxide pigments and compositions therefrom
US3513007A (en) * 1965-07-21 1970-05-19 British Titan Products Mixed coating process
US3767455A (en) * 1970-01-15 1973-10-23 Laporte Industries Ltd Treatment of oxide pigments
US3804655A (en) * 1971-04-07 1974-04-16 British Titan Ltd Pigments
US3960589A (en) * 1971-10-13 1976-06-01 Stanford Research Institute Stabilized pigment and method for producing the same
US4239548A (en) * 1978-12-21 1980-12-16 Tioxide Group Limited Titanium dioxide pigment

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1023590A (en) * 1963-05-21 1966-03-23 British Titan Products Titanium dioxide pigments and compositions therefrom
US3513007A (en) * 1965-07-21 1970-05-19 British Titan Products Mixed coating process
US3767455A (en) * 1970-01-15 1973-10-23 Laporte Industries Ltd Treatment of oxide pigments
US3804655A (en) * 1971-04-07 1974-04-16 British Titan Ltd Pigments
US3960589A (en) * 1971-10-13 1976-06-01 Stanford Research Institute Stabilized pigment and method for producing the same
US4239548A (en) * 1978-12-21 1980-12-16 Tioxide Group Limited Titanium dioxide pigment

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5851652A (en) * 1992-10-09 1998-12-22 E. I. Du Pont De Nemours And Company Lightfast T102 pigment
US5730796A (en) * 1995-06-01 1998-03-24 Kerr-Mcgee Chemical Corporation Durable pigmentary titanium dioxide and methods of producing the same
US5777001A (en) * 1997-08-04 1998-07-07 Kerr Mcgee Chemical Corp. Graft polymerized metal oxide compositions and methods

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