Manufacturing method of ceramic proppant, and proppant itself

FIELD: oil and gas industry.

SUBSTANCE: in manufacturing method of ceramic proppant including grinding of initial charge components, preparation of ceramic slurry, introduction to the obtained ceramic slurry of water-soluble polymer binding agent, formation of granules, their drying and calcination, components of initial charge are crushed to the fraction size of not more than 30 mcm at fraction content of not more than 5 mcm - 60-70 wt %, and fraction of 5-30 mcm - 30-40 wt %, formation of granules is performed by dispersion of ceramic slurry at least through one gauged opening to water solution of fixing substance forming together with water-soluble polymer binding agent the water-nonsoluble compound providing the fixation of granule shape, to ceramic slurry there introduced in addition is phosphoric sodium salt in the quantity of 0.03 - 0.5 wt % of the weight of solid ceramic slurry component. Ceramic proppant is characterised by the fact that it has been obtained with the above method. Invention is developed in dependent claims.

EFFECT: improving proppant package permeability.

4 cl, 2 ex, 1 tbl, 3 dwg

 

The invention relates to the oil and gas industry, namely the technology of ceramic proppants for use as propping agents in the extraction of oil or gas by hydraulic fracturing - hydraulic fracturing.

The proppants - durable granules, holding the crack from closing under high pressure and providing the necessary productivity of oil and/or gas wells by creating in the formation of a conducting channel. As proppants using sand, grit, crushed walnut shells, steklosfera, ceramic granules, etc. Each of the common types of rasklinivanie has its advantages and disadvantages. For example, the use of hydraulic fracturing cheap natural organic materials or sand involves a preliminary drawing on their surface to make them more spherical protective and/or reinforcing polymer coating, which inevitably entails a rise in the production and manufacturing technology steklosfera with good strength and sphericity/roundness initially includes the high costs of melting of the charge, drying, sieving, re-annealing and classification of the final product. Currently, the most acceptable from the point of view of the ratio price/quality is drain the definition of the proppants, the raw material for the manufacture of which are clay, bauxite, sand, feldspar, serpentine, brucite, etc. For the production of ceramic proppants used two similar technological scheme, which can be divided into "dry" and "wet". Both technological schemes include preliminary heat treatment of raw materials, batching, grinding, granulation (spheroidization) on the plate granulator or pelletizer "Eirich", sintering firing, sieving and packaging of finished products. In "dry" production of proppant grinding is carried out in dry mills, where the material is fed to the granulation. In "wet" scheme is a two-stage grinding material, grinding the dry mills, then in the mills for wet grinding. The crushed material is sent for drying and partial spheroidization in tower spray dried (BRS) and further granulation.

The main operational characteristics of the propping agents regardless of their nature and technology are the conductivity and permeability of the proppant pack, which, in turn, depend on the strength of the surface shape of the granules and their fractional composition. It is believed that the spherical granules of uniform size are the most effective form of the body of the proppant, especiauy maximum values of conductivity and permeability by creating a predominantly laminar nature of the motion of the extracted hydrocarbons. Thus, ceteris paribus, spherical or solely spherical granules are the most preferable from the viewpoint of the mobility flow of oil and gas. In this regard, manufacturers of proppant are making significant efforts to search for technological solutions to get rasklinivanie with the maximum values of the roundness and sphericity of the pellets while maintaining acceptable strength characteristics.

A known method of manufacturing the proppant of glass spheres (RF patent No. 2336293), including the production of molten oxides with subsequent formation of spheres, their cooling and additional isothermal exposure for 8-25 minutes at a temperature 870-1100°C to obtain a glass-ceramic structure. In this way receive the proppant from sphericity 0.93-0.97 and roundness of 0.93-0.95. Fig.1 shows the General technological scheme of production of glass-ceramic proppants.

The disadvantages of this method include the need to install two high-temperature units - melting furnace for melting glass and a rotary kiln for further heat treatment of the granules, as well as the need for before annealing careful sieving of the granules due to the large variation in sizes of the spheres in diameter and the presence of the considerable amount of glass wool. Resulting in the output of commodity fractions of proppant does not exceed 60%. It should be noted that, despite the high strength characteristics of the glass-ceramic proppants in the air, when operating in a wet environment in the conditions of high pressures and temperatures, there is a significant loss of strength. This disadvantage is inherent in the vast majority of ceramic materials and is explained by the physico-chemical features of their structure, and therefore the proppants of this type it is recommended to use at pressures not exceeding 6000 psi. Use as a proppant glass and glass-ceramic spheres is limited also by the fact that unlike ceramic granules, these materials have low fracture toughness and their destruction when the critical pressure is fragile avalanche-like character.

There is also known a method of manufacturing a ceramic rasklinivanie oil wells (RF patent No. 2235702), which includes sequential grinding, granulation and sintering at a temperature of 1215-1290°C ceramic material, which is used as metasilicate magnesium and/or metasilicate calcium. Grinding of raw materials produced by the dry process to a fraction of less than 0.01 mm, and granulation - up fraction of 0.2 to 1.8 mm Crushed metasilicate before granulation is mixed with modifitsiruemoi and and sintering additives, for example, titanium oxide, zirconium silicate, iron oxide, clay and other

The disadvantage of this method is that the proppant pellets have low sphericity and roundness, consequently, reduced the permeability of the proppant pack. This is because when the spheroidizing material produced by the pelletizer disc type, there is a redistribution of the particles within the granules larger particles move to the surface of the granules, worsening indicators of roundness. In addition, the redistribution of the particles and the absence of the crushed material fractions larger than 10 μm causes a distortion of the geometric shape of the granules due to the large and non-uniform volumetric shrinkage during firing, which leads to the deterioration of their sphericity.

The closest to the technical nature of the claimed solution is a method for manufacturing products from aluminium dross (RF patent No. 2163227), in which ceramic rasklinivanie oil wells produced from cheaper aluminum-containing raw materials. The method includes the following steps: sintering raw material its crushing, compacting and sintering the obtained granules. Sintering of the feedstock is carried out in alocale when 1360-1650°C, and the firing of the pellets is carried out at 1180-1350°C. Grinding carry out wet grinding in a slightly acidic medium at a pH of 4.5-6.0 is about a specific surface area of more than 12000 cm 2/g, and the compacting of products is carried out by granulation of powders obtained by spray drying of the slip (PRS) in the presence of 0.01 to 0.3% of a hydrophobic surfactant. As the binder used CMC (carboxymethylcellulose) or liquid glass. This method of manufacture of proppant was implemented at the enterprises LLC PORES" (Russia, Ekaterinburg). Figure 2 presents the process flow diagram of production.

The complexity of the process by introducing in the technological chain wet grinding, and tower spray drying allows to some extent to improve the sphericity of the pellets due to the formation of embryos of the microspheres at the exit of the PRS, however, the performance of sphericity and roundness are not sufficiently high. In addition, complicates the technology and two-stage fractional sieving, requiring a large number rasinovo equipment.

Technical problem on which the invention is directed, is to increase the permeability of the proppant pack by producing granules with a total sphericity and roundness of 0.95 or more and fluctuations in the diameter of the granules is not more than 10%.

This result is achieved in that in the method of manufacturing a ceramic proppant, including the grinding of the components of the mixture, preparing the slurry, the introduction by the scientists of the slip water-soluble polymeric binder, the formation of granules, drying and firing, the components of the original mixture is crushed to a fraction of not more than 30 μm, when the content of the fraction is not more than 5 μm - 60-70 wt.% and fraction of 5-30 μm and 30-40 wt.%, and the formation of granules is carried out by dispersing the slurry through an orifice into an aqueous solution of fixing substances forming water-soluble polymer binder, water-insoluble compound, provide anchorage of the form of granules, and the slip before the dispersion is injected phosphate salts of sodium in the amount of 0.03-0.5 wt.% from the weight of the solid component of the slurry. In addition, water-soluble polymer binder is selected from Karaganov, pectins, gelatino, alginates, cellulose, karboksimetilirovaniya polysaccharides, agar, starch, guar resin, xanthan resin, acrylic acid derivatives, polyols. The dispersion is carried out by lateral or axial vibration impacts on laminar flow of the slurry. The result is also achieved by the fact that ceramic proppant obtained above.

Fig.3 shows the General technological scheme of production of proppant by the present method. In option "A" presents a scheme with sequential dry and wet grinding of raw materials, option "B" - dry. According to autorite large production option "A" is preferred because you immediately to prepare a slurry with a given humidity and enter all the necessary mineral supplements. In addition, if wet grinding is mechanochemical activation of the material, which has a positive effect on the passage of the sintering process of ceramics.

In contrast to the known technical solutions of the crushed material contains a relatively large particle size of 5-30 μm, which allow to reduce the amount of volumetric shrinkage of the material during firing and to increase thereby the measure of the sphericity of the pellets. When the content in the crushed feedstock fraction of 5-30 microns in more than 40 wt.% reduced strength characteristics of the sintered proppant. Reducing the number of coarse-grained component of less than 30 wt.% leads to the growth of firing shrinkage of the proppant granules of raw sugar during roasting and increase the degree of deformation of the sintered pellets.

In the slip obtained by sequentially performed dry and wet grinding or made from pre-crushed original material by adding water, introducing a solution of a binder, and phosphate salts of sodium. As a source of raw materials used as a natural aluminosilicate, minielite connection, Sands, and specially prepared oxygen-containing (Al2About3, ZrO2etc) or anoxic (silicon carbide, silicon nitride, boron carbide, etc.) ceramic materials. The amount of binder depends on its type, from the physico-chemical characteristics of the materials used for the manufacture of proppant, and is chosen individually in each case.

Introduction to the slip phosphate salts of sodium in the claimed amounts reduces water hardness and adjust the viscosity of the slip. In addition, phosphate salts of sodium are good sintering additive for most ceramic materials. The reduction in the content of phosphate salts of sodium below 0.03 wt.% makes the subtle influence of the additive, the increase in the content of phosphate salts of sodium above 0.5 wt.% narrows the temperature range of sintering ceramics. As phosphate salts of sodium can be used phosphates, polyphosphates, cyclophosphate sodium, preferably use digidrirovanny forms.

The slip containing all necessary additives, dispersed through an orifice into droplets of the desired diameter, which utverjdayut in the fixing solution of the substance, after which the spheres are dried and calcined at a temperature sufficient for maximum compaction of the granules. The diameter of the calibration of the holes is determined by the type of raw materials used and the chosen individual is real for each of the original slip. Preparation of the solution fixing substance is carried out depending on the type and amount of polymeric binder, and the concentration of the fixing solution is chosen individually for each pair of polymer binder/fixing stuff. As fixing agents may be used, for example, salts of Me2+Me3+B(OH)4-, SO42-etc.

The inventive method of spheroidizing allows you to get the proppant almost monofuctional particle size distribution, which cannot be achieved using other well known methods of granulation. Because of the rapid curing does not occur, the migration of large particles on the surface of the granules, the editor is able to obtain the ideal indicators of sphericity and roundness.

Production of proppant in the proposed method allows to reduce the requirements to the quality of screening and significantly reduce the number rasinovo equipment, as in this technical solution, the sieving is necessary only to separate fragments of granules, which may form during the process of movement, and drying and firing the proppant raw.

The proppant with improved sphericity and roundness provides predominantly laminar regime of movement of hydrocarbons inside PR is Pantai packs, and almost monofuctional material composition ensures education between the granules of highly large voids not filled with spheres of smaller diameter. The presence of homogeneous large pores between the granules shortens the path length of the extracted hydrocarbons inside layer of proppant and supports laminarinase flow of oil due to the absence of abrupt changes in cross section of the channels in the stack of rasklinivanie. It should also be emphasized that the proppant pack, consisting of granules with a defect-free surface, capable of withstanding without chipping significant compressive loads due to the sliding of the granules relative to each other. The combination of the above advantages of proppant produced by the claimed method allows to produce a product having high permeability.

Examples of carrying out the invention

Example 1

For the manufacture of proppant commodity fraction 12/18 mesh used prebaked natural minielite raw materials of the following composition, wt.%: MgO - 41, SiO2- 46, Fe2About37, and the impurities - the rest. The material was sequentially subjected to dry and wet milling to obtain slip humidity 35% of the next fractional composition: FR. 5 μm and less than 64 wt.%, fraction of 5-30 μm - 36 wt.%. Control of fractional composition was carried out on photoedit is ntegrate Horiba LA-300.

A. Part of the obtained slurry was dried and granulated in a laboratory disc granulator, the granules were dried, burned in a laboratory furnace with carbide electric heating elements at a temperature sufficient for maximum sealing ceramics, and subcultured to obtain marketable fractions 12/18 mesh.

B. Another portion of the slurry by weight of 1 kg and a moisture content of 35% was placed into a laboratory propeller stirrer, which was added to the sodium tripolyphosphate in an amount of 0.03 wt.% (0.2 g) and sodium alginate in the amount of 1.1 wt.% (11 g). Thus prepared slurry was applied to a dispersant with a hole size 1.1 mm and broke into droplets with a diameter of about 2.1 mm, which was sent for curing tank with 6%solution of calcium chloride. For the formation of drops used source axial acoustic waves with a frequency of 550 Hz. Cured pellets were washed from the solution of calcium chloride under running water, dried to a moisture content of 1.5 - 2% and burned in a laboratory furnace with carbide electric heating elements at a temperature sufficient for maximum compaction of ceramics. After sintering were obtained granules fraction 12/14 mesh that does not require additional screening.

The granulated material obtained by rolling on a plate granulator and formed by dispersion, Regaleali roundness, the sphericity and conductivity by the method of ISO 13503 - 2:2006(E).

The measurement results are shown in table 1. Pictures of proppant shown in Fig.4, 5.

Example 2

For the manufacture of proppant commodity fraction 12/18 mesh used prebaked natural minielite raw materials of the following composition, wt.%: MgO - 41, SiO2- 46, Fe2About37, and the impurities - the rest. The material was subjected to dry grinding until the next fractional composition: FR. 5 μm and less than 64 wt.%, fraction of 5-30 μm - 36 wt.%. Control of fractional composition was carried out at photosedimentometer Horiba LA - 300. The crushed material in the amount of 650 g were placed in a laboratory propeller stirrer, which was added 350 g of water, then with constant stirring was added the sodium tripolyphosphate in the amount of 0.5 wt.% (3.25 g) and carboxymethyl cellulose in the amount of 1.4 wt.% (14 g). Thus prepared slurry was applied to a dispersant with a hole size of 1.1 mm when the total number of holes 300 pieces and smashed into droplets with a diameter of about 2.1 mm, which was sent for curing tank with 7%solution Fl3. For the formation of drops used the source side of the acoustic oscillation frequency of 550 Hz. Cured pellets were washed from the ferric chloride solution flowing water, was dried to a moisture content of 1.5-2% and burned in a laboratory C carbide electric heating elements at a temperature sufficient for maximum compaction of ceramics. After sintering were obtained granules fraction 12/14 mesh that does not require additional screening.

The resulting pellet was determined roundness, sphericity and conductivity by the method of ISO 13503 - 2:2006(E). The measurement results are shown in table 1.

holes
Table 1.
Properties of the proppant
N p/pMethod of compactingThe sphericity/ roundnessLoad, psiConductivity, mDft
1PRS + disc0.85/0.8200035517
granulator400025783
(patent RF № 2163227)600013734
8000 6954
100003545
2Disc granulator0.8/0.75200033978
(example 1 (a)400017077
60007694
80003322
10000849
3The dispersion through0.98/0.96200045245
calibrated400028940
600014323
(example 1 b)80007773
100004256
4The dispersion through0.98/0.95200044235
calibrated400028243
holes600014122
(example 2)80007433
100003845

Data analysis the table shows that the proppant produced by the claimed method (No. 3, Tablitsy), has elevated indices of sphericity and roundness, as well as the conductivity of the proppant pack in comparison with the known analogues. The authors confirm that each of the following types of water-soluble polymeric binders, fixing agents and phosphate salts of sodium to achieve the technical result.

1. A method of manufacturing a ceramic proppant, comprising grinding the starting components of the mixture, preparing the slurry, introducing the resulting slurry a water-soluble polymeric binder, the formation of granules, drying and firing, characterized in that the components of the original mixture is crushed to a fraction of not more than 30 μm, when the content of the fraction is not more than 5 μm - 60-70 wt.% and faction 5-30 μm - 30-40 wt.%, and the formation of granules is carried out by dispersing the slurry through at least one calibrated orifice into an aqueous solution of fixing substances forming water-soluble polymer binder, water-insoluble compound, provide anchorage of the form of granules, and the slip impose additional phosphate salt sodium in the amount of 0.03 - 0.5 wt.% from the weight of the solid component of the slurry.

2. The method according to claim 1, characterized in that the water-soluble polymer binder is selected from the groups is of Karaganov, pectins, gelatino, alginates, cellulose, karboksimetilirovaniya polysaccharides, agar, starch, guar resin, xanthan resin, acrylic acid derivatives, polyols.

3. The method according to claim 1, characterized in that the dispersion is carried out by lateral or axial vibration impacts on laminar flow of the slip.

4. Ceramic proppant, characterized in that it is obtained by the method according to claim 1.



 

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