US 3807704 A
This invention resides in apparatus and method for dispersing and mixing at least a first material with a liquid to form a composite material in the liquid by passing ultrasonic waves through the first material and liquid while rotating an element therein.
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United States Patent [1 1 Janzen et al.
[ DISPERSING AND MIXING APPARATUS  Inventors: Jay Janzen; Elton E. Rush, both of Bartlesville, Okla.
 Assignee: Phillips Petroleum Company,
22 Filed: Nev. 13, 1972  Appl. No.1 305,809
52 US. Cl 259/72, 259/1310. 44, 259/1310. 46 51 Int. Cl. B01r11/92,B01f13/0s  Field or'searchjl ....259/DIG. 41, DIG. 44,
[ 56] References Cited UNITED STATES PATENTS 2,673,81 l 3/1954 Tsunoda 259/DlG. 44
[111 3,807,704 [451 Apr. 30, 1974 4/1966 Steel 259/DlG. 46
Primary Examiner-Robert W. Jenkins .Assistant Examiner-Philip R. Coe
[5 7] ABSTRACT This invention resides in apparatus and method for dispersing and mixing at least a first material with a liquid to form a composite material in the liquid by passing ultrasonic waves through the first material and liquid while rotating an element therein. 7
4 Claims, 2 Drawing Figures DISPERSING AND MIXING APPARATUS It is desirable to provide apparatus which will disperse and mix at least a first material in a liquid for forming a composite material in the liquid. The invention is more particularly directed to apparatus which will disperse and mix a material, which has agglomerating properties, in a liquid and produce a composite material having a high uniformity perunit volume.
The invention therefore resides in apparatus for dispersing and mixing at least a first material with a liquid to form a composite material in the liquid by passing ultrasonic waves through the first material and liquid while rotating an element therein.
Other aspects, objects, and advantages of the present invention will become apparent from a study of the disclosure, the appended claims, and the drawings.
The drawings are diagrammatic views of the apparatus of this invention.
FIG. 1 shows a frontal view in partial section of the apparatus and I FIG. 2 shows a side view in partial section of the apparatus of FIG. 1.
Referring to thedrawings, a frame 2 has first and secend end portions 4,6 with the first end portion 4 adapted to receive pan 7 which in turn receives a vessel 8 containing materials to be mixed.
A power supply unit 12 (FIG. 2) is connected to preferably the lower portion of the frame 2 with an ultrasonic wave transmitting element 14 positioned at a lo cation adjacent and in wave transmitting relationship with the pan 7 and the vessel 8 in the installed position with a liquid 16, preferably water, positioned in the pan and in contact with the vessel 8.
The ultrasonic wave generating apparatus 12, 14 can be for example of the magnetostrictive or piezoelectric type. A small commerically available ultrasonic cleaning bath manufactured by Branson Instruments, Inc. has been found to contain a suitable generator for this purpose, for example.
A magnet 18 is positioned at a location adjacent the pan 7 and the vessel 8 in the installed position of the pan and vessel at the first end portion 4 of the frame 2. The magnet is rotatable about an axis 20 passing through the vessel 8 in the installed position of said vessel for rotating a magnetically attractable element 22 within the vessel in response to rotating the magnet 18.
An electric motor 24 for example is connected to the magnet 18 for rotating the magnet 18 and a power source (not shown) is connected to the wave generator 12 for operating said generator. 7
In orderto assure uniform mixing and dispersion, it is preferred that the magnet 18 be substantially coaxially positioned relative to the wave transmitter 14 and the vessel 8 in the installed position thereof.
In order to vary the mixing and dispersing action imparted to the composite material and liquid by the apparatus of this invention, control means 26, 28 can be provided with unit 12 and the magnet 18 for altering the waves emitted and the rate'of rotation of the magnet.
It is preferred that the ultrasonic waves be in a range of about 20,000 to about 100,000 cycles/second and the magnetic rotational rate be-controllable and be in a range of about 20 to about 3,000 rpm in order to match the frequency and shear speeds to the particular 2 materials being mixed and dispersed thereby reducing the time, labor, and expenditure requiredto obtain a high quality dispersion.
In the'methodof this invention, at least .a first material and a liquid,for example carbon'blackand chloroform, are placed in the vessel 8 and the vessel isposi- .tioned in the pan 7 which has liquid, preferably water,
together. Surprisingly, it has been discovered that the .qualityof mixing and dispersion of the one or more materials in aliquid is improved and the time for mixing and dispersion is greatly reduced where the mixing element 22 is utilized .to circulate the liquid and material within the vessel 8 for changing the position of the material relative to the vibrational wave fronts passing through the vessel. The material and liquid is thereby acted upon by the transmitted waves from a multiplicity of directions during .the mixing operations.
In one example, the specific surface area of carbon black is determined bymixing a weighed black sample and a solution containing a 'known quantity of a quaternary ammonium salt until equilibration is reached. At that time, the black is removed and the amount of quaternary salt remaining in the solution is determined by titration. From this information the specific surface of the :black in square meters per gram can be calculated. The time required to reach equilibration was reduced percent by using the method of the invention compared to using consecutive treatments with ultrasonic vibration and magneticstirring. The ultrasonic generator produced about 55,000 cycles per second and the stirrer was operated at about 300 rpm.
In another example, the primary aggregate size of carbon black particles suspended in chloroform was determined by light scattering means such as the dissymmetry method. G. Oster, Chemical Reviews 43, No. 2, Oct. 1948, pages 336-344; M. Kerker, The Scattering of Light and Other Electromagnetic Radiation," Academic Press, I969, Library of Congress Catalog Card Number: 69-26644, pages 432-433. Samples were prepared by mixing with ultrasonic agitation only and with simultaneous ultrasonic agitation and magnetic stirring. The same conditions were employed as in the previous example except that mixing times of 30, and 90 minutes were employed.
Invention Control Mixing Time Dissymmetry Mixing Time Dissymmetry 30 min. 2.41 30 min. 4.23 60 min. 2.36 60 min. 3.95 90 min. 2.3] 90 min. i 3.38
These results indicated that the dissymmetry values of the samples prepared using the device of the invention were all nearly the same showing that the secondary carbon black aggregates were essentially reduced to the primary structure. The dissymmetry valuesfor samthe primary aggregate particle size could not be reliably calculated.
Other modifications and alterations of this invention will become apparent to those skilled in the art from vessel, said magnet beingrotatable about an axis passing through the vessel in the installed position thereof for rotating a magnetically attractable element within the vessel; and
means for rotating the magnet.
2. An apparatus, as set forth in claim 1, wherein the magnet is substantially coaxially positioned relative to the transmitting element and the vessel in the installed position thereof.
3. An apparatus, as set forth in claim 1, including controlling means for altering the waves emitted from the wave transmitting element.
4, An apparatus, as set forth in claim 1,- including controlling means for altering the rate of rotation of the magnet.
Patent No 3,807,701; Jay Janzen and Dated: April 30, 197/ Attest:
UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Elton E. Rush It is certified that'error appears in the above-identified patent and that said letters Patent are hereby corrected as shown below:
Co'lunm 2, line 13, after "function", "of" should read to Column 3, line 1A, "a wave transmitting element" should read an ultrasonic wave generating means line 15, after "vessel", insert when the vessel is in its installed position in said frame Signed and sealed this 17th day of September 1974.
(SEAL) MCCOY M. GIBSON JR. 1 C. MARSHALL DANN Attesting Officer Commissionerof Patents
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