CN109534740B - Preparation method of fracturing propping agent - Google Patents
Preparation method of fracturing propping agent Download PDFInfo
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- CN109534740B CN109534740B CN201910069383.0A CN201910069383A CN109534740B CN 109534740 B CN109534740 B CN 109534740B CN 201910069383 A CN201910069383 A CN 201910069383A CN 109534740 B CN109534740 B CN 109534740B
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- cement
- quartz
- water
- proppant
- quartz powder
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/48—Macromolecular compounds
- C04B41/4853—Epoxides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/62—Coating or impregnation with organic materials
- C04B41/63—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
- C09K8/805—Coated proppants
Abstract
A preparation method of a fracturing propping agent comprises the steps of firstly preparing modified quartz powder, then weighing 52.5 cement and the modified quartz powder, adding a cement mortar additive for mixing, uniformly stirring the raw materials, dissolving water-soluble resin in water, adding a polycarboxylic acid cement water reducing agent, uniformly mixing and stirring to prepare a granulated mixed solution, secondly, adding the uniformly stirred materials into a granulator, spraying the mixed solution for forming, finally, sieving the granulated cement quartz proppant, putting the sieved cement quartz proppant into a curing box, curing the cement quartz proppant by using the water-spraying epoxy resin solution, curing the obtained cement quartz proppant in an oven, the composite cement quartz fracturing propping agent can be obtained, and the prepared product has the characteristics of good sphericity, low density, excellent crushing resistance and corrosion resistance, simple process, low cost and easily obtained raw materials.
Description
Technical Field
The invention relates to the technical field of petroleum fracturing propping agents, in particular to a preparation method of a fracturing propping agent.
Background
The hydraulic fracturing technology is used as a main method for increasing the yield of oil and gas wells, and is widely applied to the development of various oil and gas fields, and a fracturing propping agent is a key for success of the hydraulic fracturing technology for petroleum. The proppant used in the present foreign fracturing technology mainly comprises quartz sand, ceramsite and resin coated sand proppant. The quartz sand proppant is widely distributed in China, is easy to obtain, has relatively low price, but has poor surface smoothness, poor sphericity and crushing resistance, is easy to crush, and is only suitable for shallow wells and low-sealed wells in hydraulic fracturing operation. The ceramsite has good sphericity, high strength and high compressive strength, and is not easy to break. However, their density is relatively high compared to quartz sand and, in the implementation of the work, they are extremely energy-intensive and expensive. The precoated sand proppant has the characteristics of poor sphericity, poor crushing resistance, easiness in crushing and the like although the performance of the precoated sand proppant is superior to that of a quartz sand proppant.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a fracturing propping agent, and the prepared product has the characteristics of good sphericity, low density, excellent crushing resistance and corrosion resistance, simple process, low cost and easily obtained raw materials.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a fracturing propping agent comprises the following steps:
step 1: adding quartz powder into a mixed solution of hydrogen peroxide and concentrated sulfuric acid, uniformly stirring, filtering with deionized water, washing to be neutral, drying, adding an ethanol solution of a silane coupling agent KH560, stirring overnight at room temperature, washing, and drying to obtain modified quartz powder;
step 2: weighing 52.5 mass percent of cement and modified quartz powder, adding a cement mortar additive, mixing, and uniformly stirring the raw materials for later use;
and step 3: preparing a granulating mixed solution: dissolving water-soluble resin in water, adding a polycarboxylic acid cement water reducing agent, and uniformly mixing and stirring to obtain a mixed solution;
and 4, step 4: adding the uniformly stirred materials in the step 2 into a granulator, and spraying the mixed solution obtained in the step 3 for forming;
and 5: sieving the granulated cement quartz proppant by a sieve with 20-40 meshes;
step 6: putting the cement quartz proppant sieved in the step 5 into a curing box, and curing for 18-24 hours by using a water-spraying epoxy resin solution;
and 7: and (3) curing the cement quartz proppant obtained in the step (6) in an oven at the temperature of 60-90 ℃ for 3-6h to obtain the composite cement quartz fracturing proppant.
In the step 1, the concentration of concentrated sulfuric acid is 98wt%, the concentration of hydrogen peroxide is 35-40wt%, and the mass ratio of hydrogen peroxide to concentrated sulfuric acid is 2 (1-2).
In the step 1, the stirring time is 30-40min, the drying temperature is 120-140 ℃, and the drying time is 4-6 h.
In the step 1, the concentration of the ethanol solution of the silane coupling agent KH560 is 50-70 wt%.
In the step 1, the mass volume ratio of the quartz powder to the ethanol solution of the silane coupling agent KH560 is 1 (0.2-0.5) g/ml.
In the step 2, the mass ratio of the 52.5 cement to the quartz powder is 2 (1-2).
In the step 2, the cement mortar additive accounts for 1-5% of the total mass of 52.5% of the cement and the quartz powder.
In the step 3, the mass ratio of water to the water-soluble epoxy resin is 1 (0.1-0.2).
In the step 3, the polycarboxylic acid cement water reducing agent accounts for 1-2% of the total mass of the mixed materials in the step 3.
In the step 4, the rotating speed of the granulator is 48r/min, and the water spraying amount of the granulator is 60-80 ml.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the surface of quartz powder is modified by the mixed liquid of hydrogen peroxide and concentrated sulfuric acid and the silane coupling agent KH560, so that the surface activity of quartz can be improved, the surface of quartz sand is provided with chemical bonds, and the bonding property between the quartz powder and cement and resin is improved by mixing and granulating the quartz powder and the cement, thereby improving the overall strength of the propping agent. The invention adopts cement, quartz powder and water-soluble epoxy resin to prepare the composite material with simple process, low cost, easily obtained raw materials, good sphericity (the sphericity is 0.9) and low density (1.46 g/cm)-3) The fracturing propping agent has excellent anti-crushing performance (the crushing rate is less than 3 percent), corrosion resistance (the solubility is less than 5 percent), good flow conductivity and high hydrophobic property.
Detailed Description
The present invention will be described in further detail with reference to examples.
The first embodiment is as follows:
step 1: adding quartz powder into hydrogen peroxide and concentrated sulfuric acid at a volume ratio of 3:1 to obtain a mixed solution, stirring for 30min, filtering, washing to neutrality, and drying at 120 deg.C for 4 h. Adding an ethanol solution (with the concentration of 50%) of a silane coupling agent KH560, stirring at room temperature for 12h, washing, and drying at 120 ℃ for 5h to obtain modified quartz powder.
Step 2: weighing 52.5 cement and quartz powder according to the mass ratio of 1:1, adding 2% of cement mortar additive, mixing, and uniformly stirring the raw materials.
And step 3: and (3) preparing a granulated mixed solution, dissolving the water-soluble resin in water according to the mass ratio of 1:10, adding a polycarboxylic acid cement water reducing agent (accounting for 1 percent of the total mass of the mixed raw materials), and uniformly mixing and stirring for later use.
And 4, step 4: and adding the uniformly stirred food into a granulator for forming.
And 5: sieving and screening the granulated cement quartz proppant, and selecting the proppant with 20-40 meshes.
Step 6: and (4) putting the cement quartz proppant sieved in the step (5) into a curing box, and curing for 24 hours by using a water-spraying epoxy resin solution.
And 7: and (4) curing the cement quartz proppant obtained in the step (6) in an oven at 60 ℃ for 5 hours to obtain the composite cement quartz fracturing proppant.
Example two:
step 1: adding quartz powder into hydrogen peroxide and concentrated sulfuric acid at a volume ratio of 2:1 to obtain a mixed solution, stirring for 20min, filtering, washing to neutrality, and drying at 130 deg.C for 4 h. Adding an ethanol solution (with the concentration of 55%) of a silane coupling agent KH560, stirring at room temperature for 12h, washing, and drying at 130 ℃ for 5h to obtain modified quartz powder.
Step 2: weighing 52.5 cement and quartz powder according to the mass ratio of 2:1, adding 3% of cement mortar additive, mixing, and uniformly stirring the raw materials.
And step 3: and (3) preparing a granulated mixed solution, dissolving the water-soluble resin in water according to the mass ratio of 1:9, adding a polycarboxylic acid cement water reducing agent (accounting for 1.2 percent of the total mass of the mixed raw materials), and uniformly mixing and stirring for later use.
And 4, step 4: and adding the uniformly stirred food into a granulator for forming.
And 5: sieving and screening the granulated cement quartz proppant, and selecting the proppant with 20-40 meshes.
Step 6: and (4) putting the cement quartz proppant sieved in the step (5) into a curing box, and curing for 24 hours by using a water-spraying epoxy resin solution.
And 7: and (4) curing the cement quartz proppant obtained in the step (6) in an oven at 65 ℃ for 5 hours to obtain the composite cement quartz fracturing proppant.
Example three:
step 1: adding quartz powder into hydrogen peroxide and concentrated sulfuric acid at a volume ratio of 1:1 to obtain a mixed solution, stirring for 15min, filtering, washing to neutrality, and drying at 140 deg.C for 4 h. Adding an ethanol solution (with the concentration of 60%) of a silane coupling agent KH560, stirring at room temperature for 12h, washing, and drying at 140 ℃ for 5h to obtain modified quartz powder.
Step 2: weighing 52.5 cement and quartz powder according to the mass ratio of 3:1, adding 4% of cement mortar additive, mixing, and uniformly stirring the raw materials.
And step 3: and (3) preparing a granulated mixed solution, dissolving the water-soluble resin in water according to the mass ratio of 1:8, adding a polycarboxylic acid cement water reducing agent (accounting for 1.5 percent of the total mass of the mixed raw materials), and uniformly mixing and stirring for later use.
And 4, step 4: and adding the uniformly stirred food into a granulator for forming.
And 5: sieving and screening the granulated cement quartz proppant, and selecting the proppant with 20-40 meshes.
Step 6: and (4) putting the cement quartz proppant sieved in the step (5) into a curing box, and curing for 24 hours by using a water-spraying epoxy resin solution.
And 7: and (4) curing the cement quartz proppant obtained in the step (6) in an oven at 70 ℃ for 5 hours to obtain the composite cement quartz fracturing proppant.
Claims (6)
1. The preparation method of the fracturing propping agent is characterized by comprising the following steps:
step 1: adding quartz powder into a mixed solution of hydrogen peroxide and concentrated sulfuric acid, uniformly stirring, filtering with deionized water, washing to be neutral, drying, adding an ethanol solution of a silane coupling agent KH560, stirring overnight at room temperature, washing, and drying to obtain modified quartz powder;
step 2: weighing 52.5 mass percent of cement and modified quartz powder, adding a cement mortar additive, mixing, and uniformly stirring the raw materials for later use;
and step 3: preparing a granulating mixed solution: dissolving water-soluble resin in water, adding a polycarboxylic acid cement water reducing agent, and uniformly mixing and stirring to obtain a mixed solution;
and 4, step 4: adding the uniformly stirred materials in the step 2 into a granulator, and spraying the mixed solution obtained in the step 3 for forming;
and 5: sieving the granulated cement quartz proppant by a sieve with 20-40 meshes;
step 6: putting the cement quartz proppant sieved in the step 5 into a curing box, and curing for 18-24 hours by using a water-spraying epoxy resin solution;
and 7: curing the cement quartz proppant obtained in the step 6 in an oven at the temperature of 60-90 ℃ for 3-6h to obtain a composite cement quartz fracturing proppant;
in the step 1, the concentration of the ethanol solution of the silane coupling agent KH560 is 50-70 wt%;
in the step 1, the mass volume ratio of the quartz powder to the ethanol solution of the silane coupling agent KH560 is 1 (0.2-0.5) g/ml;
in the step 2, the mass ratio of the 52.5 cement to the quartz powder is 2 (1-2);
in the step 3, the mass ratio of water to the water-soluble resin is 1 (0.1-0.2).
2. The preparation method of the fracturing propping agent according to claim 1, wherein in the step 1, the concentration of concentrated sulfuric acid is 98wt%, the concentration of hydrogen peroxide is 35-40wt%, and the mass ratio of hydrogen peroxide to concentrated sulfuric acid is 2 (1-2).
3. The method as claimed in claim 1, wherein the quartz powder is added into the mixture of hydrogen peroxide and concentrated sulfuric acid in step 1, the stirring time is 30-40min, the drying temperature is 120-140 ℃, and the drying time is 4-6 h.
4. The method for preparing a fracturing propping agent according to claim 1, wherein in the step 2, the cement mortar additive accounts for 1-5% of the total mass of 52.5 cement and quartz powder.
5. The method for preparing a fracturing propping agent according to claim 1, wherein in step 3, the polycarboxylic acid cement water reducing agent accounts for 1-2% of the total mass of the mixed liquor in step 3.
6. The method for preparing the fracturing propping agent according to claim 1, wherein in the step 4, the rotating speed of a granulator is 48r/min, and the water injection quantity of the granulator is 60-80 ml.
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| CN201910069383.0A CN109534740B (en) | 2019-01-24 | 2019-01-24 | Preparation method of fracturing propping agent |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101464927B1 (en) * | 2013-05-03 | 2014-11-28 | 새턴바이오텍 주식회사 | Silicic acid fertilizer pill and manufacturing method thereof |
| CN104893707A (en) * | 2015-05-22 | 2015-09-09 | 巩义市天祥耐材有限公司 | Self-suspension proppant for hydraulic fracturing and preparation method thereof |
| CN104962276A (en) * | 2015-06-26 | 2015-10-07 | 西安理工大学 | Modified carbon nano-tube touching resin pre-coated-sand propping agent and preparing method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101464927B1 (en) * | 2013-05-03 | 2014-11-28 | 새턴바이오텍 주식회사 | Silicic acid fertilizer pill and manufacturing method thereof |
| CN104893707A (en) * | 2015-05-22 | 2015-09-09 | 巩义市天祥耐材有限公司 | Self-suspension proppant for hydraulic fracturing and preparation method thereof |
| CN104962276A (en) * | 2015-06-26 | 2015-10-07 | 西安理工大学 | Modified carbon nano-tube touching resin pre-coated-sand propping agent and preparing method thereof |
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Effective date of registration: 20221227 Address after: 257100 West of Xisi Road and South of Lingpai Road, Dongying District, Dongying City, Shandong Province Patentee after: Shengli Oilfield Fangyuan Ceramics Co.,Ltd. Address before: 710021 Shaanxi province Xi'an Weiyang university campus of Shaanxi University of Science and Technology Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY |