CN100535078C - Method for preparing acid-resistant pressing crack supporting agent - Google Patents
Method for preparing acid-resistant pressing crack supporting agent Download PDFInfo
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- CN100535078C CN100535078C CNB2007101680572A CN200710168057A CN100535078C CN 100535078 C CN100535078 C CN 100535078C CN B2007101680572 A CNB2007101680572 A CN B2007101680572A CN 200710168057 A CN200710168057 A CN 200710168057A CN 100535078 C CN100535078 C CN 100535078C
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- 239000002253 acid Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims description 6
- 239000003795 chemical substances by application Substances 0.000 title 1
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 239000002699 waste material Substances 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000004927 clay Substances 0.000 claims abstract description 8
- 239000008187 granular material Substances 0.000 claims abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001570 bauxite Inorganic materials 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims abstract 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract 2
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 abstract description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 abstract description 2
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000011819 refractory material Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910000831 Steel Chemical group 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000010959 steel Chemical group 0.000 description 3
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明公开了一种耐酸压裂支撑剂的制备方法。原料质量百分比为：Al2O3质量百分含量大于55%的铝矾土或耐火材料废料60-85%，粘土5-30%，碳酸钡5-20%，助烧剂0-10%；助烧剂为TiO2。具体步骤为：(1)将原料按配料比放入球磨装置中进行球磨；(2)将(1)步所得料经造粒制备成半成品颗粒；(3)将(2)步所得半成品颗粒在1300℃-1400℃进行烧结1-3小时，自然冷却到室温即可得到耐酸性能良好的压裂支撑剂。本发明立足于国内支撑剂生产行业普遍以铝矾土和高铝废料为主要原料的现状，通过改进配料特别是在原料中加入了碳酸钡使得压裂支撑剂成品的耐酸性能大大提高。The invention discloses a preparation method of an acid-resistant fracturing proppant. The mass percentage of raw materials is: 60-85% of bauxite or refractory material waste with Al 2 O 3 mass percentage greater than 55%, 5-30% of clay, 5-20% of barium carbonate, and 0-10% of sintering aid; The sintering aid is TiO 2 . The specific steps are: (1) put the raw materials into the ball milling device according to the batching ratio and carry out ball milling; (2) prepare the semi-finished granules by granulating the material obtained in the (1) step; (3) put the semi-finished granules obtained in the (2) step in the Sintering at 1300°C-1400°C for 1-3 hours, and naturally cooling to room temperature can obtain a fracturing proppant with good acid resistance. The present invention is based on the fact that bauxite and high-alumina waste are generally used as main raw materials in the domestic proppant production industry, and the acid resistance of the finished fracturing proppant is greatly improved by improving the ingredients, especially adding barium carbonate to the raw materials.
Description
技术领域 technical field
本发明涉及一种耐酸压裂支撑剂的制备方法。The invention relates to a preparation method of an acid-resistant fracturing proppant.
背景技术 Background technique
压裂支撑剂是石油、天然气工业重要的专用材料。耐酸性能是压裂支撑剂一个非常重要的指标，对压裂效果，压裂支撑剂使用的持久性和油、气的导流能力有重要的影响。我国生产的压裂支撑剂多以铝矾土或高铝的工业废料如高铝质耐火材料废料为主要原料，此类原料为Al2O3多孔矿石结构，生产出的压裂支撑剂耐酸性能普遍较差，因此2007年1月1日实施的石油天然气行业标准SY/T5108-2006对压裂支撑剂的耐酸性能有所降低，但是国内支撑剂的酸溶度仍普遍达不到该标准要求。Fracturing proppant is an important special material in petroleum and natural gas industry. Acid resistance is a very important indicator of fracturing proppant, which has an important impact on fracturing effect, durability of fracturing proppant and oil and gas conductivity. Most of the fracturing proppants produced in China use bauxite or high-aluminum industrial waste such as high-alumina refractory waste as the main raw material. Such raw materials are Al 2 O 3 porous ore structures, and the acid resistance of the produced fracturing proppants Generally poor, so the oil and gas industry standard SY/T5108-2006 implemented on January 1, 2007 has reduced the acid resistance of fracturing proppants, but the acid solubility of domestic proppants still generally does not meet the requirements of this standard .
发明内容 Contents of the invention
本发明的目的是针对目前国产压裂支撑剂的酸溶解度普遍偏高的现状，通过改进配料，来提高支撑剂的耐酸性能。The purpose of the invention is to improve the acid resistance of the proppant by improving the ingredients in view of the current situation that the acid solubility of the domestic fracturing proppant is generally high.
本发明的原料质量百分比为：Al2O3质量百分含量大于55％的铝矾土或耐火材料废料60-85％，粘土5-30％，碳酸钡5-20％，TiO20-10％。TiO2为助烧剂。The mass percent of raw materials in the present invention is: 60-85% of bauxite or refractory waste with Al2O3 mass percent greater than 55%, 5-30% of clay, 5-20% of barium carbonate, 0-10 % of TiO2 %. TiO2 is a burning aid.
具体步骤为：The specific steps are:
(1)将原料按配料比放入球磨装置中进行球磨；(1) Put the raw materials into the ball milling device according to the batching ratio and carry out ball milling;
(2)将(1)步所得料经造粒制备成半成品颗粒；(2) Prepare the material obtained in step (1) into semi-finished granules through granulation;
(3)将(2)步所得半成品颗粒在1300℃-1400℃进行烧结1-3小时，自然冷却到室温即可得到耐酸性能良好的压裂支撑剂。(3) Sinter the semi-finished granules obtained in step (2) at 1300°C-1400°C for 1-3 hours, and cool naturally to room temperature to obtain a fracturing proppant with good acid resistance.
按照按SY/T5108-2006推荐方法进行测试，本发明成品酸溶解度在3.0％-6.0％之间，达到了行业标准的要求。Tested according to the method recommended by SY/T5108-2006, the acid solubility of the finished product of the invention is between 3.0% and 6.0%, which meets the requirement of the industry standard.
本发明立足于国内支撑剂生产行业普遍以铝矾土和高铝废料为主要原料的现状，通过改进配料特别是在原料中加入了碳酸钡使得压裂支撑剂成品的耐酸性能大大提高。The present invention is based on the fact that bauxite and high-alumina waste are generally used as main raw materials in the domestic proppant production industry, and the acid resistance of the finished fracturing proppant is greatly improved by improving the ingredients, especially adding barium carbonate to the raw materials.
具体实施方式 Detailed ways
实施例1：Example 1:
(1)原料质量百分比为：耐火材料废料(取自武汉钢铁集团)75％、粘土(采自广东湛江)14％、二氧化钛(化学纯)2％、碳酸钡(化学纯)9％；耐火材料废料和粘土的化学成分分别见见附表1和附表2；(1) The mass percentage of raw materials is: refractory waste (taken from Wuhan Iron and Steel Group) 75%, clay (taken from Zhanjiang, Guangdong) 14%, titanium dioxide (chemically pure) 2%, barium carbonate (chemically pure) 9%; refractory materials See Attached Table 1 and Attached Table 2 for the chemical composition of waste and clay, respectively;
(2)将原料按配料比放入球磨装置中进行球磨24小时；(2) Put the raw materials into the ball milling device according to the batching ratio and carry out ball milling for 24 hours;
(3)将(2)步所得料经造粒制备成半成品颗粒；(3) The material obtained in step (2) is prepared into semi-finished granules through granulation;
(4)将(3)步所得半成品颗粒在箱式电炉中1350℃进行烧结2小时，自然冷却到室温即可得到耐酸性能良好的压裂支撑剂。(4) Sinter the semi-finished particles obtained in step (3) in a box-type electric furnace at 1350° C. for 2 hours, and cool naturally to room temperature to obtain a fracturing proppant with good acid resistance.
筛取一定量的粒径范围为8/16目的成品，按SY/T5108-2006推荐方法进行测试，测得该成品酸溶解度为4.4％，抗酸溶性能达到SY/T5108-2006标准要求，优于所测试的同粒径范围的市场产品。Sieve a certain amount of finished product with a particle size range of 8/16 mesh, and test it according to the method recommended by SY/T5108-2006. The acid solubility of the finished product is measured to be 4.4%, and its anti-acid solubility meets the requirements of SY/T5108-2006 standard, excellent Market products in the same particle size range tested.
我们在实验室定性比较本发明成品和市场某厂家达标产品(8/16目，69Mpa闭合压力下破碎率为10.8％)的抗破碎能力：把相同质量、相同粒径范围的本发明成品和该厂家产品放入球磨罐中，在球磨机上用氧化铝瓷球打磨(击打)。结果表明本发明成品的抗破碎能力优于该厂家产品。We qualitatively compare the anti-fragmentation ability of the finished product of the present invention and the standard product (8/16 mesh, crushing rate 10.8% under 69Mpa closed pressure) of the finished product of the present invention and a certain manufacturer in the market in the laboratory: the finished product of the present invention with the same quality and the same particle size range and the finished product of the present invention The manufacturer's products are put into a ball mill jar and polished (beat) with alumina ceramic balls on a ball mill. The result shows that the crush resistance of the finished product of the present invention is better than that of the manufacturer's product.
实施例2：Example 2:
(1)原料质量百分比为耐火材料废料(取自武汉钢铁集团)60％、粘土(采自广东湛江)26％、碳酸钡(化学纯)14％；耐火材料废料和粘土的化学成分分别见见附表1和附表2；(1) The mass percentage of raw materials is 60% of refractory waste (taken from Wuhan Iron and Steel Group), 26% of clay (taken from Zhanjiang, Guangdong), and 14% of barium carbonate (chemically pure); see the chemical composition of refractory waste and clay respectively. Schedule 1 and Schedule 2;
(2)将原料按配料比放入球磨装置中进行球磨24小时；(2) Put the raw materials into the ball milling device according to the batching ratio and carry out ball milling for 24 hours;
(3)将(2)步所得原料经造粒制备成半成品颗粒；(3) preparing the raw materials obtained in step (2) into semi-finished granules through granulation;
(4)将(3)步所得半成品颗粒在箱式电炉中1350℃进行烧结2小时，自然冷却到室温即可得到耐酸性能良好的压裂支撑剂。(4) Sinter the semi-finished particles obtained in step (3) in a box-type electric furnace at 1350° C. for 2 hours, and cool naturally to room temperature to obtain a fracturing proppant with good acid resistance.
筛取一定量的粒径范围为0.85-1.18mm(16/20目)的成品，按SY/T5108-2006推荐方法进行测试，测得该成品酸溶解度为4.6％，抗酸溶性能达到SY/T5108-2006标准要求，优于所测试的同粒径范围的市场产品。Sieve a certain amount of finished product with a particle size range of 0.85-1.18mm (16/20 mesh), and test it according to the method recommended by SY/T5108-2006. The acid solubility of the finished product is measured to be 4.6%, and the acid solubility resistance reaches SY/T5108-2006. According to the T5108-2006 standard, it is better than the tested market products in the same particle size range.
我们在实验室定性比较本发明成品和市场某厂家达标产品(8/16目，69Mpa闭合压力下破碎率为10.8％)的抗破碎能力：把相同质量、相同粒径范围的本发明成品和该厂家产品放入球磨罐中，在球磨机上用氧化铝瓷球打磨(击打)。结果表明本发明成品的抗破碎能力优于该厂家产品。We qualitatively compare the anti-fragmentation ability of the finished product of the present invention and the standard product (8/16 mesh, crushing rate 10.8% under 69Mpa closed pressure) of the finished product of the present invention and a certain manufacturer in the market in the laboratory: the finished product of the present invention with the same quality and the same particle size range and the finished product of the present invention The manufacturer's products are put into a ball mill jar and polished (beat) with alumina ceramic balls on a ball mill. The result shows that the crush resistance of the finished product of the present invention is better than that of the manufacturer's product.
附表1 武汉钢铁集团耐火材料废料的化学组成(质量百分比)Attached Table 1 Chemical Composition of Refractory Waste from Wuhan Iron and Steel Group (Mass Percentage)
附表2 广东湛江粘土的化学组成(质量百分比)Attached Table 2 Chemical Composition of Clay in Zhanjiang, Guangdong (mass percentage)
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| CNB2007101680572A CN100535078C (en) | 2007-10-30 | 2007-10-30 | Method for preparing acid-resistant pressing crack supporting agent |
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| CNB2007101680572A CN100535078C (en) | 2007-10-30 | 2007-10-30 | Method for preparing acid-resistant pressing crack supporting agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786921A (en) * | 2012-08-03 | 2012-11-21 | 贵州林海陶粒制造有限公司 | Low-density oil fracturing propping agent and preparation method thereof |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575503B (en) * | 2009-06-11 | 2011-08-31 | 邹平金刚新材料有限公司 | High-strength fracturing propping agent for petroleum and preparation method thereof |
| CN101629075B (en) * | 2009-08-14 | 2012-09-05 | 陕西省轻工业研究设计院 | Oil fracturing proppant containing coal gangue |
| CN101717628B (en) * | 2009-11-20 | 2013-02-20 | 三门峡方圆实业股份有限公司 | Low-density ceramsite propping agent and preparation method thereof |
| CN101811873A (en) * | 2010-04-08 | 2010-08-25 | 桂林理工大学 | Method for preparing silicon-free or low-silicon acidproof ceramic fracturing propping agent |
| CN103288428B (en) * | 2013-05-16 | 2014-07-02 | 陕西科技大学 | A method for preparing proppant for shale gas fracturing by using poor bauxite |
| CN111454076B (en) * | 2020-04-30 | 2022-07-12 | 西安建筑科技大学 | Ceramsite proppant prepared from blast furnace tapping channel waste and preparation process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102786921A (en) * | 2012-08-03 | 2012-11-21 | 贵州林海陶粒制造有限公司 | Low-density oil fracturing propping agent and preparation method thereof |
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Assignee: China Ceramic Proppant (Guizhou) Ltd. Assignor: Guilin University of Technology Contract record no.: 2012520000011 Denomination of invention: Method for preparing acid-resistant pressing crack supporting agent Granted publication date: 20090902 License type: Exclusive License Open date: 20080319 Record date: 20120713 |
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