CN111960807A - 一种中密度超高强度陶粒支撑剂的制备方法 - Google Patents

一种中密度超高强度陶粒支撑剂的制备方法 Download PDF

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CN111960807A
CN111960807A CN202010858407.3A CN202010858407A CN111960807A CN 111960807 A CN111960807 A CN 111960807A CN 202010858407 A CN202010858407 A CN 202010858407A CN 111960807 A CN111960807 A CN 111960807A
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bauxite
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唐珂
段虎生
徐美萍
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Yuanqu Corundum Proppants Corp
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Abstract

本发明涉及一种中密度超高强度陶粒支撑剂的制备方法，属于陶粒生产技术领域；解决用于石油压裂支撑剂的陶粒产品抗压强度低、稳定性低的问题；原料为按一定比例配合的两种铝矾土和矿化剂，具体步骤为：将铝矾土和矿化剂破碎粉磨；将粉磨后的原料加水湿磨成泥浆，在湿磨的同时加入添加剂；采用逆流式压力喷雾干燥塔对磨好的泥浆进行干燥，再进行造粒、筛分、煅烧、冷却，得到成品；本发明制备的陶粒支撑剂密度相对较低，抗压强度可达到103MPa，产品的性能优异，可满足深层油气井的压裂需求。

Description

一种中密度超高强度陶粒支撑剂的制备方法
技术领域
本发明属于陶粒生产技术领域，具体涉及一种中密度超高强度陶粒支撑剂的制备方法。
背景技术
石油支撑剂又叫石油压裂支撑剂。在石油天然气深井开采时，高闭合压力低渗透性矿床经压裂处理后，使含油气岩层裂开，油气从裂缝形成的通道中汇集而出，此时需要流体注入岩石基层，以超过地层破裂强度的压力，使井筒周围岩层产生裂缝，形成一个具有高层流能力的通道，为保持压裂后形成的裂缝开启，油气产物能顺畅通过。用石油支撑剂随同高压溶液进入地层充填在岩层裂隙中，起到支撑裂隙不因应力释放而闭合的作用，从而保持高导流能力，使油气畅通，增加产量。陶粒支撑剂是人造高强陶瓷颗粒，以铝矾土为原料，通过粉末制粒，烧结而成，具有耐高温、耐高压、耐腐蚀、高强度、高导流能力、低密度、低破碎率等特点，使用最为广泛，是压裂施工，油气井增产的关键材料。
随着压裂技术的不断发展，清水水平井体积压裂的技术日趋成熟，对陶粒支撑剂的规格及性能要求有了改变，要求低密度、高强度、小粒径，目的为了提高悬浮性，携砂能力，支撑裂缝能力，因此出现了很多低密、超低密高强度的陶粒支撑剂产品，可普遍用于油气井的压裂施工；但对于比较深的油气井（井深超过5000米），对于陶粒支撑剂的抗压强度要求较高，需要达到86MPa、103MPa，而低密度、超低密度陶粒支撑剂多适用52MPa、69MPa，因此对于深井用陶粒支撑剂则需要更高的强度。
目前陶粒支撑剂的主要原料是铝矾土（Al2O3含量大于55%），矿化剂为锰粉、铁粉、白云石、钾长石等。生产分为制粉、制粒和烧成三大工段，主要设备分别为干法球磨机、圆盘制粒机和回转窑。生产工艺流程为：将铝矾土和矿化剂按照配方比例加入球磨机混磨至325-400目，然后进入圆盘制粒机造粒，并根据生产规格进行筛分，筛下小颗粒作为引子继续造粒，筛上大颗粒经打散机打散后继续造粒，筛分好的半成品粒进入烘干窑烘干，然后进入回转窑高温煅烧，再进入冷却窑冷却，最后进行成品筛分包装。
存在问题：
1、噪音和粉尘较大；
2、产品密度大、强度相对较低；
3、圆球度、表面光洁度相对较差；
4、抗酸腐蚀能力一般；
适合生产粒径较大产品，比如30/50、20 /40目产品，生产小粒径40/70、70/140目产品时，产量明显降低。
发明内容
本发明克服了现有技术的不足，提出一种中密度超高强度陶粒支撑剂的制备方法。解决用于石油压裂支撑剂的陶粒产品抗压强度低、稳定性低的问题。
为了达到上述目的，本发明是通过如下技术方案实现的。
一种中密度超高强度陶粒支撑剂的制备方法，原料由质量百分比为：60%-80%的铝矾土A、20%-40%的铝矾土B、1%-3%的矿化剂；所述铝矾土A为含有质量百分比为68%的Al2O3，所述铝矾土B为含有质量百分比为63%的Al2O3；所述矿化剂为锰粉、硫酸钡、白云石和钾长石，具体包括以下步骤：
a）将铝矾土和矿化剂破碎粉磨至100-200目；
b）将粉磨后的原料加水湿磨成泥浆，在湿磨的同时加入添加剂；使得泥浆固含量为50-70%，泥浆的粒度达到800-2000目；
c）采用逆流式压力喷雾干燥塔对磨好的泥浆进行干燥，同时造粒；所述逆流式压力喷雾干燥塔的热风进口温度为250℃-350℃，出口温度为80℃-120℃；料浆压力为1.8-2.2MPa，喷片孔径为1.2-1.8mm。
如图1所示，泥浆从塔顶向下喷出，热风从塔底进入，从塔顶排出，热空气与雾滴的运动方向相反，由于热空气向上，雾滴向下，延缓了颗粒和雾滴的下降速度，在干燥室内停留时间长，有利于干燥；同时，泥浆在干燥成粒的过程中，所接触的热风温度由低到高，有利于形成致密的实心球形颗粒，不会因干燥温度过高，水分蒸发速率过快而形成表面硬壳、内部空心的颗粒。
经过喷雾造粒得到表面光滑圆球度好的实心球形颗粒，水分含量6-8%，粒径大小集中在100目-35目之间，高达95%以上。如果生产40/70、70 /140目规格小粒径产品时，经过筛分取100-35目的颗粒作为半成品坯球进入烘干和烧成工段，筛余作为原料加入泥浆；如果30/50、20 /40目等粒径较大规格产品时，则需要将一部分颗粒作为引子，其余经打散机打成细粉，进入圆盘制粒机造粒。
d）将引子和细粉加入圆盘制粒机，同时喷入雾化水进行造粒，直至坯球达到相应规格粒径大小，然后进行筛分，筛分合格的进入半成品料仓，晒下做引子，晒上打散机打散成细粉循环使用；
将筛分合格的半成品坯球经烘干窑烘干后进入回转窑高温煅烧，然后进入冷却窑冷却，并对回转窑尾气进入脱硫脱硝塔进行处理；
冷却后的产品进行成品筛分、包装、入库。
优选的，所述添加剂为占原料总质量0.2%-0.6%的分散剂、0.2%-0.5%的悬浮剂和0.2%-0.5%的粘结剂。
更优的，所述分散剂为聚丙烯酸钠或聚丙烯酸氨。
更优的，所述悬浮剂是羧甲基纤维素钠。
更优的，所述粘结剂是聚乙烯醇。
优选的，所述步骤b中，每10分钟对泥浆取样用激光粒度仪检测粒度。
优选的，所述步骤d所述的煅烧的烧成温度为1350-1450℃。
本发明相对于现有技术所产生的有益效果为。
1、本发明产品密度相对较低，抗压强度可达到103MPa，可满足深层油气井的压裂需求，填补了现有产品的空白。
2、采用陶瓷球磨机湿法球磨，噪音小，无粉尘，混磨效果好，使多种原料充分混合均匀，产品质量稳定性好，同时可将原料加工至2000目，粒度远远小于现有干法球磨的400目，产品的性能优异。
3、采用喷雾干燥造粒技术，在干燥泥浆的同时，制成小粒径的半成品坯球，同时，采用喷雾干燥造粒技术，噪音小，粉尘少，自动化程度高，工人劳动强度低。
4、产品圆球度好，流动性好；
5、新加入硫酸钡（重晶石，常用于陶瓷增亮剂），在烧结过程中可形成钡长石，促进烧结同时，增加强度，同时改善陶粒表面光洁度。
6、酸溶解度较低。
附图说明
图1是本发明采用逆流式压力喷雾干燥塔对磨好的泥浆进行干燥的逆流流动示意图。
具体实施方式
为了使本发明所要解决的技术问题、技术方案及有益效果更加清楚明白，结合实施例和附图，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。下面结合实施例及附图详细说明本发明的技术方案，但保护范围不被此限制。
实施例1
原料配方：质量百分比：64%铝矾土A、30%铝矾土B和6%的矿化剂，其中矿化剂为2%锰粉、2%硫酸钡、1%白云石、1%钾长石。
制备方法如下：
1、将铝矾土和矿化剂破碎粉磨至100目；
2、将粉磨后的铝矾土和矿化剂按照配方比例加水进入陶瓷球磨机搅拌湿磨成泥浆，在湿磨的同时额外加入0.2%的聚丙烯酸氨、0.2%的CMC和0.3%的PVA；使得泥浆固含量为65%，粒度达到1200目；然后将磨好的浆料放入料浆池。
3、采用逆流式压力喷雾干燥塔对磨好的泥浆进行干燥同时造粒，其中，热风进口温度控制在350℃，出口温度控制在120℃；料浆压力为2.2MPa，喷片孔径为1.8mm。经过筛分取35目-100目的颗粒作为半成品。
4、将喷雾干燥造粒后的半成品坯球经烘干后进入回转窑高温煅烧，烧成温度为1400℃。
5、冷却后经过筛分可同时得到40/70和70/140目两种规格产品。
实施例2
原料配方：质量百分比：70%铝矾土A、24%铝矾土B和6%的矿化剂，其中矿化剂为1.5%锰粉、1.5%硫酸钡、1.5%白云石、1.5%钾长石。
制备方法如下：
1、将铝矾土和矿化剂破碎粉磨至100目；
2、将粉磨后的铝矾土和矿化剂按照配方比例加水进入陶瓷球磨机搅拌湿磨成泥浆，在湿磨的同时额外加入0.3%的聚丙烯酸氨、0.3%的CMC和0.3%的PVA；使得泥浆固含量为60%，粒度达到1500目；然后将磨好的浆料放入料浆池。
3、采用逆流式压力喷雾干燥塔对磨好的泥浆进行干燥同时造粒，其中，热风进口温度控制在300℃，出口温度控制在100℃；料浆压力为2MPa，喷片孔径为1.5mm。经过筛分取35目-100目的颗粒作为半成品。
4、将喷雾干燥造粒后的半成品坯球经烘干后进入回转窑高温煅烧，烧成温度为1380℃。
5、冷却后经过筛分可同时得到40/70和70/140目两种规格产品。
实施例3
原料配方：质量百分比：74%铝矾土A、20%铝矾土B和6%的矿化剂，其中矿化剂为1%锰粉、1%硫酸钡、2%白云石、2%钾长石。
制备方法如下：
1、将铝矾土和矿化剂破碎粉磨至100目；
2、将粉磨后的铝矾土和矿化剂按照配方比例加水进入陶瓷球磨机搅拌湿磨成泥浆，在湿磨的同时额外加入0.4%的聚丙烯酸氨、0.3%的CMC和0.2%的PVA；使得泥浆固含量为55%，粒度达到2000目；然后将磨好的浆料放入料浆池。
3、采用逆流式压力喷雾干燥塔对磨好的泥浆进行干燥同时造粒，其中，热风进口温度控制在280℃，出口温度控制在80℃；料浆压力为1.8MPa，喷片孔径为1.2mm。经过筛分取35目-100目的颗粒作为半成品。
4、将喷雾干燥造粒后的半成品坯球经烘干后进入回转窑高温煅烧，烧成温度为1400℃。
5、冷却后经过筛分可同时得到40/70和70/140目两种规格产品。
实施例1-3与现有40/70目低密陶粒性能对比见下表：
Figure DEST_PATH_IMAGE001
以上内容是结合具体的优选实施方式对本发明所做的进一步详细说明，不能认定本发明的具体实施方式仅限于此，对于本发明所属技术领域的普通技术人员来说，在不脱离本发明的前提下，还可以做出若干简单的推演或替换，都应当视为属于本发明由所提交的权利要求书确定专利保护范围。

Claims (7)

1.一种中密度超高强度陶粒支撑剂的制备方法，其特征在于，原料由质量百分比为：60%-80%的铝矾土A、20%-40%的铝矾土B、1%-3%的矿化剂；所述铝矾土A为含有质量百分比为68%的Al2O3，所述铝矾土B为含有质量百分比为63%的Al2O3；所述矿化剂为锰粉、硫酸钡、白云石和钾长石，具体包括以下步骤：
a）将铝矾土和矿化剂破碎粉磨至100-200目；
b）将粉磨后的原料加水湿磨成泥浆，在湿磨的同时加入添加剂；使得泥浆固含量为50-70%，泥浆的粒度达到800-2000目；
c）采用逆流式压力喷雾干燥塔对磨好的泥浆进行干燥，同时造粒；所述逆流式压力喷雾干燥塔的热风进口温度为250℃-350℃，出口温度为80℃-120℃；料浆压力为1.8-2.2MPa，喷片孔径为1.2-1.8mm；经过喷雾造粒得到实心球形颗粒，所述实心球形颗粒的水分含量为6-8%；
d）将实心球形颗粒进行半成品筛分；将筛好的半成品进行煅烧、冷却得到成品。
2.根据权利要求1所述的一种中密度超高强度陶粒支撑剂的制备方法，其特征在于，所述添加剂为占原料总质量0.2%-0.6%的分散剂、0.2%-0.5%的悬浮剂和0.2%-0.5%的粘结剂。
3.根据权利要求2所述的一种中密度超高强度陶粒支撑剂的制备方法，其特征在于，所述分散剂为聚丙烯酸钠或聚丙烯酸氨。
4.根据权利要求2所述的一种中密度超高强度陶粒支撑剂的制备方法，其特征在于，所述悬浮剂是羧甲基纤维素钠。
5.根据权利要求2所述的一种中密度超高强度陶粒支撑剂的制备方法，其特征在于，所述粘结剂是聚乙烯醇。
6.根据权利要求1所述的一种中密度超高强度陶粒支撑剂的制备方法，其特征在于，所述步骤b中，每10分钟对泥浆取样用激光粒度仪检测粒度。
7.根据权利要求1所述的一种中密度超高强度陶粒支撑剂的制备方法，其特征在于，所述步骤d所述的煅烧的烧成温度为1350-1450℃。
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