DE2205126B2 - PROCESS FOR MANUFACTURING FINE PARTICLE SODIUM ALUMINUM SILICATE - Google Patents

PROCESS FOR MANUFACTURING FINE PARTICLE SODIUM ALUMINUM SILICATE

Info

Publication number
DE2205126B2
DE2205126B2 DE19722205126 DE2205126A DE2205126B2 DE 2205126 B2 DE2205126 B2 DE 2205126B2 DE 19722205126 DE19722205126 DE 19722205126 DE 2205126 A DE2205126 A DE 2205126A DE 2205126 B2 DE2205126 B2 DE 2205126B2
Authority
DE
Germany
Prior art keywords
silicate
sodium
reaction
sulfate
aluminum silicate
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.)
Granted
Application number
DE19722205126
Other languages
German (de)
Other versions
DE2205126C3 (en
DE2205126A1 (en
Inventor
Lowell Edwin Bei Air Md.; Crockett Joseph Thomas Auburn AIa.; Hackbarth (V.St.A.)
Original Assignee
J.M. Huber Corp, Locust, N.J. (V.St.A.)
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 J.M. Huber Corp, Locust, N.J. (V.St.A.) filed Critical J.M. Huber Corp, Locust, N.J. (V.St.A.)
Publication of DE2205126A1 publication Critical patent/DE2205126A1/en
Publication of DE2205126B2 publication Critical patent/DE2205126B2/en
Application granted granted Critical
Publication of DE2205126C3 publication Critical patent/DE2205126C3/en
Expired legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • 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
    • C09C1/405—Compounds of aluminium containing combined silica, e.g. mica
    • 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
    • D21H17/68—Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • 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
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • 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
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • 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
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Paper (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Silicon Compounds (AREA)

Description

Gegenstand des Hauptpatentes ist ein Verfahren zum Herstellen von feimeiligem Natriumaluminiumsilikat durch Umsetzen von Natriumsilikat und Aluminiumsulfat in einem wäßrigen Medium und anschließendem Waschen, Filtrieren und Trocknen, bei dem man Natriumsulfat der Reaktion in ihrem Verlauf in einer Menge von mindestens I Gew.-%, bezogen auf das Gewicht des Silikats, zuführt, wobei man mindestens etwa 0,1 Gew.-% des Sulfats in dem wäßrigen Reaktionsmedium von Reaktionsbeginn an bereitstelltThe subject of the main patent is a process for the production of finely divided sodium aluminum silicate by reacting sodium silicate and aluminum sulfate in an aqueous medium and then Washing, filtering and drying, in which one sodium sulfate of the reaction in its course in one An amount of at least 1% by weight, based on the weight of the silicate, is fed in, at least provides about 0.1% by weight of the sulfate in the aqueous reaction medium from the start of the reaction

Das so erhaltene einteilige Natriumsluminiumsilikat ist besonders geeignet als Füllstoff für vulkanisierte Kautschukmassen und Papiererzeugnisse.The one-part sodium aluminum silicate thus obtained is particularly suitable as a filler for vulcanized rubber compounds and paper products.

Die vorliegende Erfindung betrifft eine verbesserte Ausführungsform des im Patent 19 25 868 beschriebenen Verfahrens.The present invention relates to an improved embodiment of that described in US Pat. No. 1,925,868 Procedure.

Es wurde nämlich gefunden, daß man vorteilhaft das Aluminiumsulfat tier Reaktionszone als besonderen, praktisch konstarnen Strom während einer Zeitspanne zuführt, die um mindestens 10 Sekunden die normale Zeit beim diskontinuierlichen Betrieb für die Zufuhr von getrennten Strömen des genannten Aluminiumsulfats und des genannten Natriumsilikats zu dem Reaktionsmedium übersteigt. It has been found that it is advantageous to use the aluminum sulfate of the reaction zone as a special, practically you can see electricity for a period of time feeds, which is at least 10 seconds the normal time in discontinuous operation for the feed of separate streams of said aluminum sulfate and said sodium silicate to the reaction medium.

Wegen der allgemeinen und bevorzugten Verfahrensmerkmale wird in vollem Umfang auf das Hauptpatent 19 25 868 verwiesen.Because of the general and preferred process characteristics, reference is made in full to the main patent 19 25 868 referenced.

Beispielexample

Das Reaktionsgefäß wird mit 3401 Wasser gefüllt und eine Natriumsilikat-Natriumsulfat-Lösung mit einer Silikat-Konzentration von 240 kg/m1 und einer Natriumsulfat-Konzentration von 2 bis 6 Gew.-% des Silikats wird dann mit einer Geschwindigkeit von 1162,6 ml/ Min. zugeführt Die Temperatur der sich ergebenden Reaktionslösung wird auf 71,1°C eingestellt und dort gehalten. Alaun wird in einer Konzentration von 360kg/mJ bei einer Temperatur von 71,1°C dem Reaktionsmedium, nachdem zunächst der Rührer angestellt worden ist, mit einer Geschwindigkeit von 0340 bis 4,15 l/Min, für 10 Sekunden oder länger vor dem Beginn der Nairiumsilikat-Natriumsulfat-Lösung-Zufuhr zugesetzt Zu diesem Zeitpunkt wird mit der Zufuhr der übrigen berechneten Menge der Natriumsilikat-Natriumsulfat-Lösung mit ihrer Geschwindigkeit von 1162,6 ml/Min, begonnen. Nach 25 Minuten wird der Silikat-Lösungsstrom abgestellt wenn der pH-Wert der Aufschlämmung oberhalb 8,0 ist Das Alaun wird weiter zugeführt, bis ein pH-Wert von 7,8 bis 8,0 erreicht worden ist. Wenn der pH-Wert unterhalb 8.0 ist, wird mit der Zufuhr der Silikat-Lösung fortgefahren, bis ein pH-Wert von 8,0 erreicht worden ist. Eine Absetz- oder Reifungsperiode von 15 Minuten wird eingehalten und der pH-Wert wird wiederum gemessen und wieder auf den Wert 7,8 bis 8,0 eingestellt; anschließend wird die Masse dem Filter zugeführt, wo sie zur Gewinnung des Natriumsulfats und. um ihren Restgehalt auf etwa 3% zu erniedrigen, mit Wasser gewaschen wird. Der erhaltene Kuchen, der fest (thixotrop) ist wird einem Schlagwerk zugeführt und verflüssigt worauf er bei einer Pigmenttemperatur am Auslaß von etwa 104,40C bis auf einen Feuchtigkeitsgehalt von 5% sprühgetrocknet wird. Das sich ergebende, trockene Pigment weist einen pH-Wert von 9,5 auf, und die Masse setzt sich aus äußerst feinen Teilchen zusammen, von denen verhältnismäßig wenige größer als 0,5 Mikron sind.The reaction vessel is filled with 3401 of water and a sodium silicate-sodium sulfate solution with a silicate concentration of 240 kg / m 1 and a sodium sulfate concentration of 2 to 6% by weight of the silicate is then added at a rate of 1162.6 ml / Min. The temperature of the resulting reaction solution is set to 71.1 ° C. and maintained there. Alum is added to the reaction medium in a concentration of 360 kg / m J at a temperature of 71.1 ° C. after the stirrer has first been turned on, at a rate of 0340 to 4.15 l / min, for 10 seconds or more before the Beginning of the sodium silicate-sodium sulfate solution feed added. At this point in time, the feed of the remaining calculated amount of the sodium silicate-sodium sulfate solution is started at its rate of 1162.6 ml / min. After 25 minutes, the silicate solution flow is shut off when the pH of the slurry is above 8.0. The alum continues to be added until a pH of 7.8 to 8.0 has been reached. If the pH is below 8.0, the addition of the silicate solution is continued until a pH of 8.0 has been reached. A settling or ripening period of 15 minutes is observed and the pH value is measured again and readjusted to the value 7.8 to 8.0; then the mass is fed to the filter, where it is used to obtain the sodium sulfate and. in order to reduce their residual content to about 3%, is washed with water. The cake obtained, the fixed (thixotropic) is a striking mechanism supplied to and liquefied whereupon it to a moisture content of 5% is spray-dried at a pigment temperature at the outlet of about 104,4 0 C. The resulting dry pigment has a pH of 9.5 and the mass is composed of extremely fine particles, relatively few of which are larger than 0.5 microns.

Feinpapier- ErgebnisseFine paper results

TAPPl-Helligkeit bei 9%iger Füllung 893TAPPl brightness with 9% filling 893

TAPPl-Deckkraft bei 9%iger Füllung 87,8TAPPl opacity with 9% filling 87.8

Claims (1)

Patentanspruch:Claim: Verfahren zum Herstellen von {einteiligem Natriumaluminiumsilikat durch Umsetzen von Natri- S umsilikat und Aluminiumsulfat in einem wäßrigen Medium und anschließendem Waschen, Filtrieren und Trocknen, bei dem man Natriumsulfat der Reaktion in ihrem Verlauf in einer Menge von mindestens 1 Gew.-%, bezogen auf das Gewicht des Silicats, zuführt, wobei man mindestens etwa 0,1 Gew.-% des Sulfats in dem wäßrigen Reaktionsmedium von Reaktionsbeginn an bereitstellt gemäß Patent 19 25868. dadurch gekennzeichnet, daß man das genannte Aluminiumsulfat der Reaktionszone als besonderen, praktisch konstanten Strom während einer Zeitspanne zuführt, die um mindestens 10 Sekunden die normale Zeit beim diskontinuierlichen Betrieb für die Zufuhr von getrennten Strömen des genannten Aluminiumsulfats und des genannten Natriumsilikats zu dem Reaktionsmedium übersteigt.Process for the preparation of one-part sodium aluminum silicate by reacting sodium S umsilicate and aluminum sulfate in an aqueous medium followed by washing, filtering and drying, in which sodium sulfate of the reaction in its course in an amount of at least 1 wt .-%, based on the weight of the silicate, fed, at least about 0.1 % By weight of the sulfate in the aqueous reaction medium from the start of the reaction provided according to Patent 19 25868. characterized in that said aluminum sulfate of the reaction zone as a special, practically constant current during a period of time which is around at least 10 seconds, the normal time in the intermittent operation for the supply of separate streams of said aluminum sulfate and said sodium silicate to the Reaction medium exceeds.
DE2205126A 1971-02-03 1972-02-03 Process for the production of finely divided sodium aluminum silicate Expired DE2205126C3 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US11246971A 1971-02-03 1971-02-03

Publications (3)

Publication Number Publication Date
DE2205126A1 DE2205126A1 (en) 1972-08-31
DE2205126B2 true DE2205126B2 (en) 1977-07-07
DE2205126C3 DE2205126C3 (en) 1978-06-08

Family

ID=22344057

Family Applications (1)

Application Number Title Priority Date Filing Date
DE2205126A Expired DE2205126C3 (en) 1971-02-03 1972-02-03 Process for the production of finely divided sodium aluminum silicate

Country Status (11)

Country Link
BE (1) BE778862R (en)
CA (1) CA961210A (en)
DE (1) DE2205126C3 (en)
ES (1) ES399401A2 (en)
FI (1) FI58319C (en)
FR (1) FR2124335B2 (en)
GB (1) GB1385963A (en)
IT (1) IT998052B (en)
LU (1) LU64708A1 (en)
NL (1) NL7201290A (en)
NO (1) NO139120C (en)

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3228784A (en) * 1962-01-08 1966-01-11 Huber Corp J M Amorphous hydrogen alumino silicate pigments

Also Published As

Publication number Publication date
ES399401A2 (en) 1977-07-16
LU64708A1 (en) 1972-06-30
BE778862R (en) 1972-08-02
NO139120C (en) 1979-01-10
CA961210A (en) 1975-01-21
FR2124335A2 (en) 1972-09-22
GB1385963A (en) 1975-03-05
NO139120B (en) 1978-10-02
IT998052B (en) 1976-01-20
FR2124335B2 (en) 1977-06-17
FI58319B (en) 1980-09-30
NL7201290A (en) 1972-08-07
DE2205126C3 (en) 1978-06-08
FI58319C (en) 1981-01-12
DE2205126A1 (en) 1972-08-31

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C3 Grant after two publication steps (3rd publication)