CN113087489A - Cordierite-based ultralow-density high-strength petroleum fracturing propping agent and preparation method thereof - Google Patents
Cordierite-based ultralow-density high-strength petroleum fracturing propping agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cordierite-based ultra-low density high-strength petroleum fracturing propping agent and a preparation method thereof, wherein talc, kaolin and high-plasticity clay are used as main raw materials, and the cordierite-based ultra-low density high-strength petroleum fracturing propping agent can be prepared into a product with good sphericity (the sphericity is more than 0.9) through a series of processes of wet ball milling, spray granulation, rolling ball granulation, green body screening, high-temperature firing and fired product screening, and the apparent density is 2.35-2.65g/cm3Interval, bulk density is 1.15-1.45g/cm3In the interval, the fracture rate of the proppant is less than 9 percent under the pressure of 69 MPa.
Description
Technical Field
The invention relates to a cordierite-based ultra-low density high-strength petroleum fracturing propping agent and a preparation method thereof, belonging to the technical field of petroleum fracturing propping agents.
Background
Fracturing techniques are widely used in the current field of oil and gas production. In the fracturing process, the fracturing fluid carrying the petroleum fracturing propping agent is introduced into rock fractures formed under high-pressure operation, and the fracturing propping agent propping fractures are not closed under the action of rock stratum closing pressure, so that a petroleum or natural gas channel with high flow conductivity is formed, and the beneficial effects of increasing the production of oil and gas field exploitation and prolonging the service life of an oil well are achieved. The petroleum fracturing propping agent plays a role in fracturing operation and is a key factor for the success and cost of the fracturing operation.
At present, the mainstream products of petroleum fracturing propping agents in China are composite materials which take alumina (or mullite) synthesized by taking aluminosilicate solid wastes or minerals as main raw materials as a main phase, such as: the invention patent CN 104371703B of Chinese authorization discloses a petroleum fracturing propping agent which takes high-alumina fly ash and clay as raw materials and takes mullite prepared by manganese ore powder as a sintering aid as a main phase; the invention patent CN 103525395B granted by China uses solid waste ceramsite sand and bauxite as raw materials, dolomite and manganese dioxide as sintering aids to prepare the petroleum fracturing propping agent, and the main phase of the petroleum fracturing propping agent is corundum, and the secondary crystal phase of the petroleum fracturing propping agent is mullite. The corundum density is 3.9g/cm3The density of the mullite is in the range of 3.0-3.1g/cm3, and the apparent density and the bulk density of the dense structure petroleum fracturing propping agent with corundum or mullite as a main phase are respectively 2.7-3.5g/cm3And 1.45-1.9g/cm3An interval. In corundum and mullite material systems, a strategy to further reduce proppant density is to make structural adjustments, such as changing the external morphology of the proppant or introducing a closed cell structure. The invention patent CN 105295889B granted by China prepares the spherical petroleum fracturing propping agent with concave-convex surface by a secondary granulation process, and reduces the bulk density of the propping agent to-1.35 g/cm3(ii) a The Chinese invention patent CN 110093149A prepares the low-density petroleum fracturing propping agent by introducing a certain proportion of pore structures into ceramsite, and the bulk density is 1.19g/cm3Apparent density 2.42g/cm3. Obviously, the secondary granulation process adds complexity to the product manufacturing process. The porosity (P) and the breaking strength (σ) are related as follows: sigma-sigma0exp(-nP)，σ0And n and P are respectively fracture strength, constant and porosity of the compact sample, and it can be seen that the fracture strength is exponentially reduced along with the increase of the porosity, and the increase of the pore structure obviously and rapidly weakens the mechanical strength of the proppant and influences the service performance of the proppant. The invention patent CN 102060562B granted by China prepares a ceramsite with a porous structure, and the ceramsite is difficult to be used as a petroleum fracturing propping agent due to low strength and is only used as a building ceramsite. The Chinese patent CN 106431349B adopts magnesite, fly ash and clayAnd the composite mineralizer is used for preparing the ultra-low density cordierite petroleum fracturing propping agent with the bulk density of 1.48g/cm3 and the apparent density of 2.58g/cm 3. The magnesite has large burning loss, high cost and relatively few sources, the main components of the light-burned magnesite, namely magnesium oxide and water, can generate hydration to bring difficulty to ball milling and slurry preparation, and the light-burned magnesite is not suitable for preparing the petroleum fracturing propping agent by a wet process, so that talc is considered to replace the magnesite to provide a magnesium source for preparing the cordierite-based petroleum fracturing propping agent. The greasy property of talc will make the rolling process difficult, so the key point to solve the forming problem is to select high-plasticity clay, adjust the clay dosage and optimize the preparation process parameters.
Disclosure of Invention
The invention overcomes the defects of the prior products and the prior art and provides a cordierite-based ultralow-density high-strength petroleum fracturing propping agent and a preparation method thereof, the method takes talc, kaolin and high-plasticity clay as main raw materials, and the cordierite-based ultralow-density high-strength petroleum fracturing propping agent can be prepared into a product with good sphericity (the sphericity is more than 0.9) and the apparent density of 2.35-2.65g/cm through a series of technological processes of wet ball milling, spray granulation, rolling ball granulation, blank screening, high-temperature firing and fired product screening3Interval, bulk density is 1.15-1.45g/cm3In the interval, the fracture rate of the proppant is less than 9 percent under the pressure of 69 MPa.
A cordierite-based ultra-low density high strength petroleum fracturing propping agent comprises the following raw materials in parts by weight:
25-35 parts of talc, 45-75 parts of kaolin and 5-30 parts of high-plasticity clay.
Furthermore, the talcum contains 25-35% of MgO and SiO by mass245-65% of Al2O30-15 percent of mass percentage and 3-15 percent of ignition loss.
Further, Al in the above kaolin2O330-50% of SiO240-55% of Fe by mass2O3The mass percentage content is 0-5%.
Further, Al in the above-mentioned high plasticity clay2O320-45 percent of SiO by mass percentage240-75% of Fe2O3The mass percentage content is 0-5%.
Further, the preparation method of the petroleum fracturing propping agent comprises the following steps:
1) weighing talc, kaolin and high-plasticity clay according to the weight parts, and carrying out wet ball milling to obtain grinding slurry, wherein the particle size of powder in the grinding slurry meets the requirement of being less than 50 microns;
2) introducing the grinding slurry obtained in the step 1) into a slurry tank, adding an organic additive into the slurry, stirring and ageing, and carrying out spray drying granulation after 12 hours to obtain granulation powder;
3) introducing the granulation powder obtained in the step 2) into a rotary sugar coating machine and adding atomized water to prepare a ball core; after the ball core is formed, introducing granulation powder and spraying atomized water at the same time, so that the ball core continuously grows up; stopping adding the granulation powder and the atomized water when the spherical core grows into spherical particles with the diameter of 0.1-1.5mm, continuously rotating the sugar coating machine, and polishing the surfaces of the spherical particles; sieving and grading the polished spherical particles to obtain a green body of the petroleum fracturing propping agent;
4) and (3) adding the proppant green compact obtained in the step 3) into a rotary kiln, sintering at 1300-1450 ℃ for 20-60min, and sieving and grading the sintered particles to obtain a petroleum fracturing proppant finished product.
Further, the organic additive in the step 2) is more than one of polyvinyl alcohol or ethyl cellulose.
Further, the addition amount of the organic additive in the step 2) is 0.2-1% of the total mass of the raw materials (talc, kaolin, high plasticity clay).
Has the advantages that:
(1) the talc replaces magnesite to prepare the low-density high-strength cordierite-based petroleum fracturing propping agent, so that the raw material cost of the cordierite-based petroleum fracturing propping agent can be reduced, and the high value-added utilization of talc resources is realized; meanwhile, the product with stable property and good performance can be obtained.
The magnesite is used as a magnesium source to prepare the cordierite-based propping agent, the calcination pretreatment is needed, and the talc replaces the magnesite to be used as the magnesium source without pretreatment, so that the pretreatment cost of the raw materials is reduced. The magnesite generates magnesium oxide after being lightly burned, the magnesium oxide is easy to hydrate with water, and the property of slurry is deteriorated, so that the cordierite-based petroleum fracturing propping agent is prepared by taking the magnesite as a raw material, and only a dry mixing ball milling process route can be adopted; the cordierite-based petroleum fracturing propping agent is prepared by using talc instead of magnesite as a raw material, and dry-method and wet-method mixed ball milling process routes can be adopted.
(2) The raw material formula ensures that the main crystal phase of the product is cordierite phase, and the low volume density and apparent density of the product are essentially ensured due to the low theoretical density of cordierite; the raw material formula introduces high-plasticity clay, and a small amount of ethyl cellulose or polyvinyl alcohol binder is added in the process, so that the defect that the talc raw material is difficult to form is overcome, and the green body of the petroleum fracturing propping agent with higher green body strength and good sphericity is easy to prepare.
(3) The petroleum fracturing propping agent prepared by the invention belongs to an ultralow-density high-strength petroleum fracturing propping agent, and can improve the sand carrying capacity and the migration efficiency of a fracturing fluid and reduce the fracturing cost.
Drawings
Figure 1 XRD pattern of petroleum fracturing proppant prepared in example 1.
Figure 2 appearance of the prepared oil fracturing proppant of example 1.
Detailed Description
In order to make the technical solutions in the present application better understood, the present invention is further described below with reference to examples, which are only a part of examples of the present application, but not all examples, and the present invention is not limited by the following examples.
Example 1
First, preparation process
A cordierite-based ultra-low density high strength petroleum fracturing propping agent and a preparation method thereof are disclosed, wherein the raw material formula is as follows: 25% of talcum, 65% of kaolin and 10% of high-plasticity clay, wherein the components are mass fractions. The talc comprises the following raw material chemical components: 35 percent of MgO by mass and SiO2Mass percentage of49％，Al2O3The mass percentage content is 10.8%; the ignition loss is 11%; chemical components of kaolin: al (Al)2O341.2% by mass of SiO245.7 percent of Fe by mass2O33.5 percent of mass percentage; high-plasticity clay raw material Al2O321.5 percent of SiO2The mass percentage content is 70.8 percent. The cordierite-based petroleum fracturing propping agent is prepared through the technical processes of wet ball milling, spray granulation, rolling ball granulation, green body screening, high-temperature sintering and the like.
1) Weighing talc, kaolin and high-plasticity clay according to the raw materials and the formula, and carrying out wet ball milling for 24-48h to obtain grinding slurry, wherein the particle size of powder in the grinding slurry is less than 20 microns;
2) introducing the grinding slurry obtained in the step 1) into a slurry tank, adding ethyl cellulose accounting for 0.5 percent of the total mass of the raw materials, stirring and ageing, and performing spray drying granulation after 12 hours to obtain granulation powder;
3) introducing the granulation powder obtained in the step 2) into a rotary sugar coating machine and adding atomized water to prepare a ball core; after the ball core is formed, introducing granulation powder and spraying atomized water at the same time, so that the ball core continuously grows up; stopping adding the granulation powder and the atomized water when the spherical core grows to form spherical particles with the size of 35-60 meshes, continuously rotating the sugar coating machine, and polishing the surfaces of the spherical particles; sieving and grading the polished spherical particles, and sieving by using screens with an upper sieve of 35 meshes and a lower sieve of 65 meshes to obtain a green body of the petroleum fracturing propping agent;
4) adding the proppant green body obtained in the step 3) into a rotary kiln for high-temperature sintering, wherein the sintering atmosphere is weak reducing atmosphere, the sintering temperature is 1380 ℃, the time is 60min, after the sintering is finished, sieving is carried out by adopting screens with 40 meshes of an upper sieve and 70 meshes of a lower sieve, and oversize products are petroleum fracturing proppants.
II, preparing the results
The phase composition of the petroleum fracturing proppant prepared in this example is shown in figure 1. From the XRD patterns, it can be seen that the main crystal phase of the product is cordierite, which has a lower theoretical density than the quartz and mullite phases, which is the essential reason why the example product is lighter and less dense than the A, B, C three low-density proppants currently on the market. The appearance and the appearance of the petroleum fracturing propping agent prepared by the embodiment are shown in figure 2. It can be seen from the figure that the prepared proppant has good sphericity and roundness.
The results of comparing the performance indexes of the petroleum fracturing propping agent prepared by the embodiment with three market product indexes are shown in table 1. As can be seen by comparison of table parameters: the product has lower bulk density and apparent density compared with the current A, B, C three low-density products; the product has a breakage rate of less than 7.3 percent under the pressure of a 69MPa barrel, and is only second to the product C; the sphericity/roundness, acid solubility and turbidity indexes of the product also reach or are higher than the average level of the products in the current market.
Table 1: the performance indexes of the petroleum fracturing propping agent prepared by the embodiment are compared with those of the low-density petroleum fracturing propping agent in the current market
Note: the index parameters are obtained by testing according to the China oil and gas industry standard (SY/T5018-2014).
In conclusion, under the formula of the application, the cordierite petroleum fracturing propping agent with excellent performance can be obtained, the product quality and related performance can reach ideal conditions, and the product raw materials are optimized. The cordierite-based petroleum fracturing propping agent prepared by using the talc ore instead of the magnesite has the following advantages: a) the adaptability of the proppant preparation process is improved. The magnesite is lightly calcined to generate magnesium oxide, and the magnesium oxide is easy to generate hydration with water to destroy the property of slurry, so the magnesite is not suitable for wet ball milling mixing of raw materials. b) The talc ore has composition advantages in preparing cordierite products, and the formula composition is simplified. The standard composition of the talc is 3 MgO.4SiO2·H2O, only adding a proper amount of kaolin minerals (Al)2O3·2SiO2) The main phase of the synthesized cordierite (2 MgO.2Al)2O3·5SiO2) The product of (1). c) The price of the talc ore is usually lower than that of the magnesite, when the magnesite is used for preparing the petroleum fracturing propping agent, the magnesite needs to be subjected to light burning pretreatment, and the talc can be directly used. d) The talc ore has wide geographical distribution and easily obtained raw materials. The magnesite resource areas in China are not widely distributed, the magnesite resource areas are mainly concentrated in Liaoning areas and account for 85.6 percent of the whole country, and the talc is widely distributed and mainly distributed in 15 provinces of the whole country.
Claims (7)
1. A cordierite-based ultra-low density high strength petroleum fracturing propping agent is characterized by comprising the following raw materials in parts by weight:
25-35 parts of talc, 45-75 parts of kaolin and 5-30 parts of high-plasticity clay.
2. The oil fracturing proppant of claim 1, wherein the talc is 25-35% by weight MgO and SiO245-65% of Al2O30-15 percent of mass percentage and 3-15 percent of ignition loss.
3. The oil fracturing proppant of claim 1, wherein said kaolin Al is2O330-50% of SiO240-55% of Fe by mass2O3The mass percentage content is 0-5%.
4. The oil fracturing proppant of claim 1, wherein the Al of the high plasticity clay is Al2O320-45 percent of SiO by mass percentage240-75% of Fe2O3The mass percentage content is 0-5%.
5. The method of making a petroleum fracturing proppant of any one of claims 1-4, comprising the steps of:
1) weighing talc, kaolin and high-plasticity clay according to the weight part of claim 1, and performing wet ball milling to obtain grinding slurry, wherein the particle size of powder in the grinding slurry meets the requirement of being less than 50 μm;
2) introducing the grinding slurry obtained in the step 1) into a slurry tank, adding an organic additive into the slurry, stirring and ageing, and carrying out spray drying granulation after 12 hours;
3) introducing the granulation powder obtained in the step 2) into a rotary sugar coating machine and adding atomized water to prepare a ball core; after the ball core is formed, introducing granulation powder and spraying atomized water at the same time, so that the ball core continuously grows up; stopping adding the granulation powder and the atomized water when the spherical core grows into spherical particles with the diameter of 0.1-1.5mm, continuously rotating the sugar coating machine, and polishing the surfaces of the spherical particles; sieving and grading the polished spherical particles to obtain a green body of the petroleum fracturing propping agent;
4) and (3) adding the proppant green compact obtained in the step 3) into a rotary kiln, sintering at 1300-1450 ℃ for 20-60min, and sieving and grading the sintered particles to obtain a petroleum fracturing proppant finished product.
6. The method of claim 5, wherein the organic additive in step 2) is one or more of polyvinyl alcohol or ethyl cellulose.
7. The method according to claim 5, wherein the organic additive is added in the step 2) in an amount of 0.2 to 1% by mass based on the total mass of the raw materials.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696114A (en) * | 2009-10-23 | 2010-04-21 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing light fracturing propping agent for multi-hole oil and gas well |
| CN101823006A (en) * | 2010-04-08 | 2010-09-08 | 姚光纯 | Honeycomb nest proppant and process of applying same to fixed bed reactor |
| CN106431349A (en) * | 2016-09-30 | 2017-02-22 | 洛阳赛罗帕陶瓷科技有限公司 | Ultralow-density cordierite petroleum fracturing propping agent and preparation method thereof |
| KR20210045729A (en) * | 2019-10-17 | 2021-04-27 | 정 장 | A low-density high-strength ceramsite proppant |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696114A (en) * | 2009-10-23 | 2010-04-21 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing light fracturing propping agent for multi-hole oil and gas well |
| CN101823006A (en) * | 2010-04-08 | 2010-09-08 | 姚光纯 | Honeycomb nest proppant and process of applying same to fixed bed reactor |
| CN106431349A (en) * | 2016-09-30 | 2017-02-22 | 洛阳赛罗帕陶瓷科技有限公司 | Ultralow-density cordierite petroleum fracturing propping agent and preparation method thereof |
| KR20210045729A (en) * | 2019-10-17 | 2021-04-27 | 정 장 | A low-density high-strength ceramsite proppant |
Non-Patent Citations (1)
| Title |
|---|
| 张巍: "堇青石合成研究进展", 《岩石矿物学杂质》 * |
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Application publication date: 20210709 |