DE568309C - Manufacture of titanium composition pigments - Google Patents

Manufacture of titanium composition pigments

Info

Publication number
DE568309C
DE568309C DEC39744D DEC0039744D DE568309C DE 568309 C DE568309 C DE 568309C DE C39744 D DEC39744 D DE C39744D DE C0039744 D DEC0039744 D DE C0039744D DE 568309 C DE568309 C DE 568309C
Authority
DE
Germany
Prior art keywords
solution
titanium
manufacture
acid
titanium oxide
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
Application number
DEC39744D
Other languages
German (de)
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.)
FR DU TITANE SOC
Original Assignee
FR DU TITANE SOC
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by FR DU TITANE SOC filed Critical FR DU TITANE SOC
Application granted granted Critical
Publication of DE568309C publication Critical patent/DE568309C/en
Expired legal-status Critical Current

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Classifications

    • 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
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3045—Treatment with inorganic compounds
    • C09C1/3054—Coating
    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Description

Die Erfindung bezieht sich auf ein Verfahren zur Herstellung eines weißen Farbstoffes, bei welchem Titanoxyd auf reine Infusorienerde oder kieselsaures Aluminium 5 oder auf ein Gemisch dieser beiden Stoffe in solcher Weise gefällt wird, daß das erhaltene Erzeugnis aus Teilchen von Infusorienerde oder kieselsaurem Aluminium besteht, die von Titanoxyd eingehüllt sind.The invention relates to a method for producing a white dye, at which titanium oxide on pure infusoric earth or silicate aluminum 5 or on a mixture of these two substances is precipitated in such a way that the product obtained consists of particles of infusor earth or siliceous aluminum, which are encased in titanium oxide.

Es sind bereits weiße Farbstoffe bekannt, die aus Titanoxyd bestehen, das mit Zinkoxyd, schwefelsaurem Baryt, Schwefelzink usw. gemischt ist.White dyes are already known which consist of titanium oxide, which is mixed with zinc oxide, barite sulphate, zinc sulphide, etc. is mixed.

Ferner ist bekannt, Titansäure in Gegenwart geeigneter Substrate, wie Erdalkalisulfate, Kieselsäure, Asbest, Kieselgur u. dgl., durch Kochen aus saurer oder alkalischer Lösung zu fällen.It is also known to use titanic acid in the presence of suitable substrates, such as alkaline earth sulfates, Silicic acid, asbestos, kieselguhr and the like, by boiling from acidic or alkaline Felling solution.

Es wurde auch schon vorgeschlagen, eine Lösung von Titanoxyd mit einem Gehalt von Schwefelsäure einzudampfen. Das hier anfallende Produkt enthält sämtliche Unreinheiten der Ausgangslösung, wie Eisenoxyd, Kieselsäure, Chlor und wasserfreie Schwefelsäure, die schädlich für Anstrichzwecke sind. Infolge dieser Unreinheiten ist dieses Produkt gelblichweiß.It has also been proposed to use a solution of titanium oxide containing Evaporate sulfuric acid. The resulting product contains all impurities the starting solution, such as iron oxide, silica, chlorine and anhydrous sulfuric acid, which are harmful for painting purposes. As a result of these impurities, this product is yellowish white.

Bei dem Verfahren gemäß der Erfindung wird von einer salzsauren Titanoxydlösung ausgegangen, die ungefähr 2 Atome Säure auf ein Titanatom enthält und aus der das Titanoxyd durch Kochen auf das kieselsaure Aluminium oder auf die Kieselerde bzw. auf ein Gemisch beider Stoffe, welche in der Lösung in der Schwebe gehalten werden, gefällt wird. Das Wesen, der Erfindung besteht darin, daß vor dem. Kochen das Gleichgewicht in der salzsauren Lösung durch Zugabe einer geringen Menge Schwefelsäure aufgehoben wird.In the method according to the invention, a hydrochloric acid titanium oxide solution is used assumed, which contains about 2 atoms of acid per titanium atom and from which the Titanium oxide by boiling on the silicic acid aluminum or on the silica or on a mixture of both substances, which are kept in suspension in the solution, is precipitated will. The essence of the invention is that before. Cooking the balance repealed in the hydrochloric acid solution by adding a small amount of sulfuric acid will.

Die bei der Hydrolyse des TiCl4 nach der GleichungThe hydrolysis of TiCl 4 according to the equation

TiCl4 + H2O = 4 HCl + Ti(OH)4 TiCl 4 + H 2 O = 4 HCl + Ti (OH) 4

entstehende Säure wird vor jeder Fällung durch Destillation unter Vakuum oder durch teilweise Neutralisation, z. B. durch 50- bis. 550/oige Natronlauge, ausgeschieden. Das nicht verbundene Hydrat bleibt dann in der klaren Lösung in einem labilen Gleichgewicht. Setzt man zu dieser Lösung eine geringe Menge von Schwefelsäure zu, so wird der Gleichgewichtszustand des in der Lösung befindlichen Salzes zerstört, so daß die Ausfällung begünstigt und die Bildung eines kolloidalen Hydrats verhindert wird. Hierdurch wird eine große Ausbeute erzielt, und der erhaltene Farbstoff ist vollkommen weiß und besitzt eine große Deckkraft, vor allen Dingen aus der Tatsache heraus, daß die in der ur-The resulting acid is before each precipitation by distillation under vacuum or by partial neutralization, e.g. B. by 50 to. 550% sodium hydroxide solution, excreted. That unconnected hydrate then remains in an unstable equilibrium in the clear solution. If a small amount of sulfuric acid is added to this solution, the The equilibrium state of the salt in the solution is destroyed, so that the precipitation and the formation of a colloidal hydrate is prevented. Through this a large yield is obtained and the dye obtained is perfectly white and possesses great opacity, above all from the fact that the

sprünglichen Lösung enthaltenen Unreinheiten beim Ausfällen des Titans in der Salzsäurelösung verbleiben.original solution contained impurities when the titanium precipitates in the hydrochloric acid solution remain.

B ei s-p i elExample

Man setzt 30 bis 60 g Schwefelsäure von 66° Be 21 einer salzsauren Titanhydratlösung zu, welche ungefähr 150 g Titanoxyd entspricht und ungefähr 150 g konzentrierte30 to 60 g of sulfuric acid at 66 ° Be 21 are added to a hydrochloric acid titanium hydrate solution to, which corresponds to about 150 g of titanium oxide and concentrated about 150 g

«o Salzsäure je Liter enthält. Hierauf suspendiert man in dieser kalten; Lösung 700 g reines kieselsaures Aluminium oder sehr fein gemahlene reine Infusorienerde oder . 700 g einer Mischung dieser beiden Körper.«O contains hydrochloric acid per liter. Thereupon one suspends in this cold one; Solution 700 g pure siliceous aluminum or very finely ground pure infusor earth or. 700 g a mixture of these two bodies.

Die so erhaltene Mischung wird darauf gekocht, und das Titanhydrat setzt sich auf die suspendierenden Teilchen,. . die vollständig umhüllt werden. Die nach Abstehen an der Oberfläche schwimmende Flüssigkeit wirdThe mixture thus obtained is then boiled and the titanium hydrate settles on the suspending particles ,. . which are completely enveloped. The one after standing at the Surface becomes floating liquid

ao abgegossen und der so vorbereitete Teig mit reinem Wasser gewaschen, filtriert und in der Darrkammer getrocknet.ao poured off and the prepared dough washed with pure water, filtered and placed in the Dried kiln.

Nach der Trocknung wird das Erzeugnis mit einer schwachen alkalischen Lösung gemischt, deren Menge gerade ausreicht, um dem Enderzeugnis eine neutrale oder schwach alkalische Wirkung zu geben.After drying, the product is mixed with a weak alkaline solution, the amount of which is just sufficient to give the end product a neutral or slightly alkaline effect.

Das Erzeugnis wird von neuem gewaschen, getrocknet, dann 15 bis 30 Minuten auf Kirschrotglut erhitzt. Nach Erkaltung ist das erhaltene Erzeugnis vollständig weiß, und eine leicht vorzunehmende Mahlung gibt ein fettiges Pulver mit einer großen Deckkraft. The product is washed again, dried, then on for 15 to 30 minutes Cherry red embers heated. After cooling, the product obtained is completely white, and easy milling gives a fatty powder with great covering power.

Das zur Ausführung des Verfahrens benutzte kieselsaure Aluminium wird gemahlen und darauf mit heißer konzentrierter Salzsäure gewaschen. Nach dem Trocknen wird es in der Fällungslösung zur Suspension gebracht. ·The silicic acid aluminum used to carry out the process is ground and then washed with hot concentrated hydrochloric acid. After drying it will suspended it in the precipitation solution. ·

Findet der Niederschlag des Titanoxyds auf Infusorienerde statt, so wählt man vorzugsweise fossile Infusorienerde, welche infolge ihrer großen Feinheit, ihrer Fettigkeit und ihrer Undurchsichtigkeit nach Befeuchtung gewisse Vorteile bietet.If the titanium oxide is precipitated on infusor earth, the preferred choice is made fossil infusor earth, which due to its great fineness, its greasiness and its opacity after moistening offers certain advantages.

Claims (1)

Patentanspruch:Claim: Verfahren zur Herstellung eines Kompositionspigmentes aus Titandioxyd und Kieselerde (Infusorienerde) oder kieselsaurem Aluminium aus Titanchlorid durch Hydrolyse nach Zusatz von Schwefelsäure, dadurch gekennzeichnet, daß ein Titanchlorid als Ausgangsmaterial verwendet wird, das, auf Titanoxyd bezogen, nur die Hälfte der dem Tetrachlorid entsprechenden Salzsäure enthält.Process for the production of a composition pigment from titanium dioxide and Silica (infusion earth) or silicic acid aluminum from titanium chloride by hydrolysis after the addition of sulfuric acid, characterized in that a titanium chloride is used as the starting material that, based on titanium oxide, is only half of that corresponding to the tetrachloride Contains hydrochloric acid.
DEC39744D 1926-07-12 1927-05-04 Manufacture of titanium composition pigments Expired DE568309C (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR568309X 1926-07-12

Publications (1)

Publication Number Publication Date
DE568309C true DE568309C (en) 1933-01-17

Family

ID=8948428

Family Applications (1)

Application Number Title Priority Date Filing Date
DEC39744D Expired DE568309C (en) 1926-07-12 1927-05-04 Manufacture of titanium composition pigments

Country Status (5)

Country Link
BE (1) BE342706A (en)
DE (1) DE568309C (en)
FR (1) FR632087A (en)
GB (1) GB274072A (en)
NL (1) NL21503C (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE748015C (en) * 1936-09-16 1944-10-23 Manufacture of titanium dioxide pigments

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE532104A (en) * 1953-09-25

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE748015C (en) * 1936-09-16 1944-10-23 Manufacture of titanium dioxide pigments

Also Published As

Publication number Publication date
GB274072A (en) 1928-03-08
NL21503C (en)
FR632087A (en) 1927-12-31
BE342706A (en)

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