METHOD OF MAKING PELLETS FROM ALUMINOSILICATE RAW
MATERIALS
FIELD OF THE INVENTION The present invention relates generally to the processing of aluminosilicate raw materials \λ hen fabricating granulated materials intended to be used different branches of industry employing pellets, for example as propping agents m oil recovery
hydraulically fracturing the oil-beaπng bed.
BACKGROUND OF THE INVENTION
The closest pπor art with respect to a totality of essential features of the presently disclosed invention has been described m the Arup Khaund patent, U.S.
Pat. No. 4,668.645, m which, in order to manufacture granules, a mixture of milled bauxitic clay and corn starch is used. A calcined milled bauxitic clay
(about 450 kg) and starch grains (about 15 kg) are mixed dry m a standard pm type mixing tool at a low speed for about 15 seconds at which time about 135 kg of water is added. After the addition of water, the mixing is switched to high speed for proper compaction of the mixture. The high speed is continued for about 1-2 minutes at which time the mixing is switched to slow speed and about
180 kg of the calcined milled bauxitic clay is added to the mixture. After the addition is completed, mixing is continued for about 10-15 seconds and thus formed green spherical pellets are dumped from the mixer, dπed and fired at
1480° C. to 1500° C. for 45 minutes in a rotary kiln.
A drawback of this known method is associated with mixing of the blend and formation of the pellets at a time of supplying water at a constant mixer speed. Such pelletizmg conditions fail to provide a uniform compaction of the
moistened mass and, accordingly, a density-uniform structure of the calcined granules, nor the> provide a maximum output of predetermined fraction of pellets. In addition, the use of corn starch as a binding component requires that this component and v. ater be supplied separately during the mixing, since an aqueous starch solution can not be pre-fabπcated because of its quick coagulation. This circumstance complicates the pelletizmg process due to the fact that a uniform distribution of a dry component m a blend volume is more difficult than that of a liquid component
SUMMARY OF THE INVENTION
The proposed method of making pellets from aluminosilicate raw mateπals enables one to a\ oid shortcomings inherent m pπor art technical solutions such as described above
The pπncipal objects of the present invention are: to improve the strength of pellets and increase the yield of predetermined fraction of pellets while simplifying the process for distributing an organic binder by adding thereof m liquid form - m an aqueous solution.
The above and other objects and advantages of the present invention are achieved by the fact that m a method of making pellets from aluminosilicate raw mateπals, it is proposed to increase, duπng the process for feeding a moistener into a mixer-pelletizer, a rotational speed of a rotor agitator from 300 to 3,000 rpm directly proportionally to the amount of the moistener added. Thereupon, m order to increase the yield of properly pelletized granules of predetermined size and to improve their strength, the mixer-pelletizer is additionally loaded with milled aluminosilicate raw mateπals m a concentration of 10 to 50 % by weight, based on the total weight of the starting raw materials, at a constant rotational speed of the rotor agitator ranging from 300 to 1 ,500 rpm. It is proposed to use as the moistener an aqueous solution of an organic binder selected from the group consisting of carboxymethyl cellulose, methyl cellulose, industrial
lignosulphonates m a concentration of 10 to 30 % by weight, based on the total weight of the starting raw materials.
The present invention also embraces pellets prepared using the proposed method.
The formation of granulation nuclei is initiated upon increase m a moister content of the starting raw materials. The presence of a liquid component makes it possible for the particle mobility of the starting raw materials to be increased, thus enabling one to obtain a high density of the mass to be pelletized. With increase m a diameter of pellets to be formed, it is necessary to augment a force to compact the structure of pellets. Desired forces compacting the pellets are brought about with high linear velocities of particles following a vortex trajectory of the mass to be pelletized. Moreover, required structure and shape of a pellet derive at the expense of the pellet rotation about its own axis. In this way, velocity vector components dependent on the rotor agitator rotational speed define mam characteristics of resultant pellets and parameters of the pelletizmg process. Therefore, a possibility to vary a rotor agitator rotational speed m proportion to a blend moisture content and depending on a particular stage of the pelletizmg process is an important distinctive feature of the proposed method of making pellets from aluminosilicate raw materials.
Additional objects and advantages of the present invention will be set forth in the detailed description which follows, and m part will be obvious from the description, or may be learned by practice of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS To produce pellets, it is proposed to use bauxite containing (% by weight): A1203 - 65.0-75.0; Sι02 - 16.0-20.0; Fe- - 1.5-3.0, Tι02 - 2.5-5.0; Na20 + K20 - 0 5-3.0, CaO + MgO - 0.25-2.0, milled to an average particle size of 3-5 microns, having water absorption of 15-45 % and fired at a temperature not exceeding 1 150° C, that is, before start of the process for crystallizing the
structure which hampers bauxite milling and makes it less moldable. As established by pelletizing this bauxite in a laboratory-scale mixer-pelletizer EIRICH R02, just such a bauxite promotes a quick formation of pellet nuclei resulting in properly pelletized granules of predetermined size. The use as a moistener of an 1.0-5.0 % aqueous solution of carboxymethyl cellulose enables one to readily achieve a uniform binder distribution at a time of mixing in the mixer-pelletizer.
To manufacture pellets having a minimum internal porosity, a rotational speed of the rotor agitator is varied during pelletization. At the onset of pelletization, after the addition of a milled fired bauxite, a rotational speed of the rotor agitator is set to be preferably from 700 to 800 rpm (1 1.5-13.5 m/sec). Then the pelletizer is loaded with a binder in a preferred concentration of 12 to 15 % by weight, based on the total weight of the starting raw materials .At a time of supplying the binder, a rotational speed of the rotor agitator is increased preferably to 1 ,800-2,000 rpm (30-33 m/sec) while increasing the amount of the moistener added to the raw materials. Pelletization at a high speed of the rotor agitator is continued for 2-5 minutes and, when fine pellets having a 0.1-0.3 mm size appear, a rotational speed of the rotor agitator is decreased preferably to 700-
800 rpm (1 1.5-13.5 m sec). At that time the mixer is loaded with a milled bauxite for powdering at a rate of from 20 to 100 kg/min in a preferred concentration of
15 to 20 % by weight, based on the total weight of the starting raw materials, which is necessary to obtain pellets of predetermined size. In 1-5 minutes after powdering is completed, green pellets are dumped, dried at 1 10-320° C for 20-60 minutes to a residual moister of below 1.0 % and fired at 1350-1600° C for 30-70 minutes to water absorption of less than 1.5 %, density of 2.5-3.2 g/cm3 and bulk density of 1.3-1.85 g/cm3.
The following examples illustrate various embodiments of this invention, and are not to be interpreted as limiting the scope of the appended claims. In all these examples, bauxite having the same chemical composition is used.
EXAMPLE 1
For pelletization, bauxite containing (% by weight): A1203 - 71.3; Si02 - 16.9; Fe203 - 1.7; Ti02 - 4.2; Na20 + K20 - 1.1 ; CaO + MgO - 1.3 is used. Bauxite pre-crushed using a roll crusher to a grain size not exceeding 60 mm is fired to water absorption of 30 % at 1100° C. Thus fired bauxite is ground in a ball mill to a grain size of 2-3 mm. Fine-grinding of bauxite is carried out in a tube mill to an average grain size of from 3 to 5 microns. As a moistener, use is made of a 3 % aqueous solution of carboxymethyl cellulose prepared in the reaction vessel equipped with a central vertical agitator, at 65-75° C.
A mixer-pelletizer whose pan rotates at a constant speed of 20 rpm, is loaded with 300 kg of the milled bauxite and 50 kg of a 3 % aqueous solution of carboxymethyl cellulose for 80 seconds, while increasing a rotational speed of the rotor agitator from 300 rpm (5 m/sec) to 3,000 rpm (50 m/sec). Then an intense mixing is carried out for 1.5 minutes at a rotational speed of the rotor agitator of 3,000 rpm (50 m/sec) until formation of pellets having 0.1-0.3 mm in size. Thereafter, a rotational speed of the rotor agitator is decreased to 300 rpm (5 m/sec) and the mixer-pelletizer is loaded with 100 kg of the milled bauxite at a rate of 50 kg/min. Rotation of the mixer pan and rotor agitator is continued under these conditions for 4 minutes until formation of properly pelletized granules. The concentration of pellets thus formed with 0.4-1.4 mm in size amounts to 60-65 % by weight, based on the total weight of pellets.
Pellets thus obtained are screened, a 0.4-1.6 mm fraction is separated, dried in a rotary drier drum at 150-180° C for 50 minutes. Pellet fractions of +1.6 mm and -0.4 mm in size are recycled to milling in a ball mill. Dried pellets having a 0.6 % moister are fired at 1550° C for 45 minutes in a rotary kiln to water absorption of 0.6-0.8 %. Pellets so obtained are screened into commercial-grade fractions.
EXAMPLE 2. A method of making pellets similar to that described in Example 1 , characterized in that a rotational speed of the rotor agitator, when supplying a binding component, is increased from 800 rpm ( 13.3 m/sec) to 1 ,800 rpm (30 m/sec) at a rate of changing revolutions of 12.5 rpm per second.
EXAMPLE 3. A method of making pellets similar to that described in Example 1 , characterized in that a rotational speed of the rotor agitator, when supplying a binding component, is increased from 250 rpm (4.2 m/sec) to 3,050 rpm (50.8 m/sec j at a rate of changing revolutions of 35 rpm per second.
EXAMPLE 4. A method of making pellets similar to that described in Example 2, characterized in that a rotational speed of the rotor agitator, when additionally supplying a milled bauxite for powdering and until the termination of pelletization, is 1.500 rpm (25 m/sec).
EXAMPLE 5. A method of making pellets similar to that described in Example 2, characterized in that a rotational speed of the rotor agitator, when additionally supplying a milled bauxite for powdering and until the termination of pelletization, is 800 rpm (13.3 m/sec).
EXAMPLE 6. A method of making pellets similar to that described in Example 2, characterized in that a rotational speed of the rotor agitator, when additionally supplying a milled bauxite for powdering and until the termination of pelletization, is 1.550 rpm (25.8 m/sec).
EXAMPLE 7. A method of making pellets similar to that described in Example 2, characterized in that a rotational speed of the rotor agitator, when additionally supplying a milled bauxite for powdering and until the termination of pelletization, is 250 rpm (4.2 m/sec).
EXAMPLE 8. A method of making pellets similar to that described in Example 5, characterized in that the amount of a moistener added to the pelletizer is 30 kg (10 % by weight, based on the total weight of the starting raw materials).
EXAMPLE 9. A method of making pellets similar to that described in Example 5, characterized in that the amount of a moistener added to the pelletizer is 90 kg (30 % by weight, based on the total weight of the starting raw materials).
EXAMPLE 10. A method of making pellets similar to that described in Example 5, characterized in that the amount of a moistener added to the pelletizer is 25 kg (8.3 % by weight, based on the total weight of the starting raw materials), a rotational speed of the rotor agitator, when additionally supplying a milled bauxite and until the termination of pelletization, is 1 ,500 rpm (25 m/sec).
EXAMPLE 1 1. A method of making pellets similar to that described in Example 5, characterized in that the amount of a moistener added to the pelletizer is 95 kg (31.7 % by weight), a rotational speed of the rotor agitator, when additionally supplying a milled bauxite and until the termination of pelletization, is 1,500 rpm (25 m/sec).
EXAMPLE 12. A method of making pellets similar to that described in Example 5, characterized in that the amount of a milled bauxite additionally supplied to the pelletizer is 30 kg (10 % by weight, based on the total weight of the starting raw materials).
EXAMPLE 13. A method of making pellets similar to that described in Example 5, characterized in that the amount of a milled bauxite additionally supplied to the pelletizer is 150 kg (50 % by weight, based on the total weight of the starting raw materials).
EXAMPLE 14. A method of making pellets similar to that described in Example 5, characterized in that the amount of a milled bauxite additionally supplied to the pelletizer is 25 kg (8.3 % by weight, based on the total weight of the starting raw materials).
EXAMPLE 15. A method of making pellets similar to that described in Example 5, characterized in that the amount of a milled bauxite additionally supplied to the pelletizer is 155 kg (51.7 % by weight, based on the total weight of the starting raw materials).
Data with respect to all the above-described examples are summaπzed m the Table given below.
Pellets obtained under conditions described m Examples 1 -15 were studied with respect to mam quality indices. Compressive strength was tested employing four pressure values. Reactivity was determined by dissolving m a mixture of 12 % HCl and 3 % HF. To compare properties of pellets obtained in accordance with the present invention and that obtained under conditions of the prior art method, characteristics of these pellets are reported.
Table
Exam- Pycno- Bulk Roundness Sphericity Strength (number of destroyed particles), Solubility pie metric Density, t. %, under pressure, MPa in a density, g/cm mixture of g/cm3 acids
12 %
HC1/3 %
HF
52 70 88 105
0.4-0.8 mm fraction
1 2.97 1.85 0.8 0.8 3.2 4.4 7.8 - 4.9
2 2.86 1.74 0.8 0.9 3.1 4.2 7.5 10.8 4.9
3 3.05 1.92 0.8 0.8 4.5 7.6 9.3 - 5.0
4 2.85 1.77 0.8 0.9 3.8 4.2 7.6 9.8 4.4
5 2.89 1.80 0.9 0.9 2.7 3.8 7.1 9.4 3.6
6 2.91 1.84 0.8 0.8 5.2 7.3 9.6 - 4.5
7 2.88 1.79 0.8 0.8 5.4 7.7 9.3 - 4.4
8 2.78 1.73 0.7 0.7 5.7 8.0 10.2 - 4.8
9 2.87 1.79 0.7 0.7 6.3 8.8 12.3 - 4.9
10 2.70 1.71 0.7 0.7 7.9 10.5 - - 5.3
1 1 2.86 1.78 0.7 0.7 8.3 12.4 - - 5.2
12 2.82 1.75 0.7 0.7 6.1 8.3 14.2 - 4.9
13 2.85 1.77 0.7 0.9 5.0 7.2 9.6 - 4.4
14 2.77 1.70 0.6 0.7 5.2 8.4 12.1 - 4.1
15 3.05 1.85 0.9 0.9 4.9 7.8 9.7 13.1 4.0
Prior 3.05 1.85 0.9 0.8 5.1 7.9 9.5 12.1 3.9 art
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