CN107266045A - 一种刚玉–莫来石陶粒支撑剂及其制备方法 - Google Patents

一种刚玉–莫来石陶粒支撑剂及其制备方法 Download PDF

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CN107266045A
CN107266045A CN201710456280.0A CN201710456280A CN107266045A CN 107266045 A CN107266045 A CN 107266045A CN 201710456280 A CN201710456280 A CN 201710456280A CN 107266045 A CN107266045 A CN 107266045A
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mullite
propping agent
corundum
bauxite
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力国民
马海强
田玉明
王凯悦
邹欣伟
周毅
武雅乔
梁丽萍
郝建英
柴跃生
白频波
李占刚
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Taiyuan University of Science and Technology
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Abstract

一种刚玉–莫来石陶粒支撑剂及其制备方法，属于油气压裂支撑剂技术领域，特征是该陶粒支撑剂是按质量比92~99%的铝矾土和1~8%的钙长石。其制备方法是首先将铝矾土和钙长石分别进行破碎、筛分、干燥，接着按质量比92~99%铝矾土和1~8%钙长石进行混合后加入14~19wt%水在混合机内制粒，然后在烘干箱内30~50℃下干燥、筛选出半成品生料球，最后将生料球置于烧结炉内经1300~1450℃烧结3~5h后空冷至室温，并经20/40目标准筛筛分，即得到刚玉–莫来石陶粒支撑剂。优点是制备的刚玉–莫来石陶粒支撑剂成本低廉，质量优良，适于广泛应用。

Description

一种刚玉–莫来石陶粒支撑剂及其制备方法
技术领域
本发明属于油气压裂支撑剂技术领域，具体涉及一种刚玉–莫来石陶粒支撑剂及其制备方法。
背景技术
支撑剂是一类应用于石油、天然气开采的重要关键材料。目前，支撑剂主要分为三类：石英砂、树脂包覆陶粒和陶粒支撑剂。由于石英砂强度低，圆球度差，因此只能应用于浅井中；而树脂包覆陶粒在强度和圆球度方面虽然有了极大地提高，但在制造过程中成本较高，不适合大规模生产。相比之下，陶粒支撑剂具有明显的优势，陶粒支撑剂不但强度高，圆球度好，而且在制造过程中成本较低，所以被广泛应用于油气开采施工作业中。
目前，陶粒支撑剂以铝矾土为主要原料，添加一些碱金属氧化物烧结而成。但是，陶粒支撑剂在制备过程中存在两方面问题：一是原料成本高，不利于工业化大规模生产。如：（1）如中国专利申请号为02157202.X公开了一种陶粒支撑剂的制备方法，以高品位铝矾土（Al2O3含量65~75wt%）为主要原料，添加6~10wt%的二氧化锰细矿粉在1320~1350℃温度区间烧结1.5小时制备而成；（2）中国专利申请号为201210352728.1公开了一种中密度陶粒支撑剂，以87~95wt%的铝矾土（Al2O3含量65~78wt%）为主要原料，通过添加4~10wt%的MnO2及0.5~3wt%粘结剂在1280~1340℃烧结2~4h制备。二是在烧结过程中温度高，耗能大。如：（1）王晋槐等利用煤矸石和焦宝石为主要原料，在1410℃恒温烧结2h制备得到69MPa闭合压力下破碎率为7.9%的低密高强陶粒支撑剂；（2）李福洲等利用Al2O3含量79.1wt%的轻烧铝矾土为主要原料，经1510℃烧结制备了69MPa闭合压力下破碎率为4.0%的高强度陶粒支撑剂。
发明内容
本发明的目的是提供一种刚玉–莫来石陶粒支撑剂及其制备方法，可有效地克服现有技术存在的缺点。
本发明是这样实现的，其特征在于所述刚玉–莫来石陶粒支撑剂中的铝矾土的化学组成按照重量比为：Al2O3含量为60~63%，SiO2含量为10~13%，Fe2O3含量为4~6%，TiO2含量为2~3%，烧失量为16~18%；钙长石的化学组成按照重量比为：Al2O3含量为17~19%，SiO2含量为62~65%，CaO含量为15~17%。刚玉–莫来石陶粒支撑剂的制备方法是按如下步骤实施：
（1）将铝矾土和钙长石进行破碎和球磨处理制成粉状，再通过325目标准筛进行筛分，在100~110℃条件下恒温干燥5~6h；
（2）按质量比92~99：1~8称取铝矾土和钙长石进行均匀混料，二者重量之和为100%，然后将铝矾土与钙长石混合粉料置于爱力许强力混合机内造粒制成生料球，造粒过程中添加14~19wt%的水；
（3）将上述生料球放入烘干箱中在30~50℃条件下干燥，并筛选出所需规格的半成品生料球；
（4）将半成品生料球放入烧结炉中进行烧结，烧结温度为1300~1450℃，烧结时间为3~5h，之后随炉冷却至室温，经20/40目标准筛筛分，即得到各项性能指标均满足中华人民共和国石油天然气行业标准SY/T 5108–2014要求的刚玉–莫来石陶粒支撑剂。
本发明的有益效果在于：
1. 利用Al2O3含量为60~63wt%的低品位铝矾土为主要原料制备陶粒支撑剂，从而降低生产成本；
2. 添加钙长石作为烧结助剂，烧结过程中有利于形成玻璃相，可有效降低烧结温度；
3. 制备得到的刚玉–莫来石陶粒支撑剂的破碎率、圆球度、酸溶度、浊度等指标均满足中华人民共和国石油天然气行业标准SY/T5108–2014要求。
具体实施方式：
实施例1：
1. 将铝矾土（Al2O3含量为63wt%，SiO2含量为13wt%，Fe2O3含量为5wt%，TiO2含量为3wt%，烧失量为16wt%）和钙长石（Al2O3含量为18wt%，SiO2含量为65wt%，CaO含量为17wt%）进行破碎和球磨处理制成粉状，再通过325目标准筛进行筛分，在100℃条件下恒温干燥6h；
2. 按质量比98：2称取铝矾土和钙长石进行均匀混料，然后将铝矾土与钙长石混合粉料置于爱力许强力混合机内造粒制成生料球，造粒过程中添加18wt%的水；
3. 将上述生料球放入烘干箱中在40℃条件下干燥，并筛选出所需规格的半成品生料球；
4. 将半成品生料球放入烧结炉中进行烧结，其中烧结温度为1300℃，烧结时间为4.5h，之后随炉冷却至室温，经20/40目标准筛筛分，即得到圆球度≥0.9，浊度为50FTU，酸溶解度<5%，体积密度为1.64g/cm3，视密度为3.10g/cm3，52MPa闭合压力下破碎率为4.2%，69MPa闭合压力下破碎率为6.4%的刚玉–莫来石陶粒支撑剂。
实施例2：
1. 将铝矾土（Al2O3含量为63wt%，SiO2含量为12wt%，Fe2O3含量为4wt%，TiO2含量为3wt%，烧失量为18wt%）和钙长石（Al2O3含量为19wt%，SiO2含量为65wt%，CaO含量为16wt%）进行破碎和球磨处理制成粉状，在110℃条件下恒温干燥5h；
2. 按质量比96：6称取铝矾土和钙长石进行均匀混料，然后将铝矾土与钙长石混合粉料置于爱力许强力混合机内造粒制成生料球，造粒过程中添加17wt%的水；
3. 将上述生料球放入烘干箱中在50℃条件下干燥，并筛选出所需规格的半成品生料球；
4. 将半成品生料球放入烧结炉中进行烧结，其中烧结温度为1350℃，烧结时间为4h，之后随炉冷却至室温，经20/40目标准筛筛分，即得到圆球度≥0.9，浊度为53FTU，酸溶解度<5%，体积密度为1.64g/cm3，视密度为3.20g/cm3，52MPa闭合压力下破碎率为3.5%，69MPa闭合压力下破碎率为5.1%的刚玉–莫来石陶粒支撑剂。
实施例3：
1. 将铝矾土（Al2O3含量为62wt%，SiO2含量为12wt%，Fe2O3含量为6wt%，TiO2含量为3wt%，烧失量为17wt%）和钙长石（Al2O3含量为18wt%，SiO2含量为65wt%，CaO含量为17wt%）进行破碎和球磨处理制成粉状，在110℃条件下恒温干燥5h；
2. 按质量比96：4称取铝矾土和钙长石进行均匀混料，然后将铝矾土与钙长石混合粉料置于爱力许强力混合机内造粒制成生料球，造粒过程中添加16wt%的水；
3. 将上述生料球放入烘干箱中在40℃条件下干燥，并筛选出所需规格的半成品生料球；
4. 将半成品生料球放入烧结炉中进行烧结，其中烧结温度为1400℃，烧结时间为3.5h，之后随炉冷却至室温，经20/40目标准筛筛分，即得到圆球度≥0.9，浊度为57FTU，酸溶解度<5%，体积密度为1.76g/cm3，视密度为3.25g/cm3，52MPa闭合压力下破碎率为2.2%，69MPa闭合压力下破碎率为3.3%的刚玉–莫来石陶粒支撑剂。
实施例4：
1. 将铝矾土（Al2O3含量为62wt%，SiO2含量为11wt%，Fe2O3含量为6wt%，TiO2含量为3wt%，烧失量为18wt%）和钙长石（Al2O3含量为19wt%，SiO2含量为65wt%，CaO含量为16wt%）进行破碎和球磨处理制成粉状，在110℃条件下恒温干燥5h；
2. 按质量比98：2称取铝矾土和钙长石进行均匀混料，然后将铝矾土与钙长石混合粉料置于爱力许强力混合机内造粒制成生料球，造粒过程中添加17wt%的水；
3. 将上述生料球放入烘干箱中在30℃条件下干燥，并筛选出所需规格的半成品生料球；
4. 将半成品生料球放入烧结炉中进行烧结，其中烧结温度为1450℃，烧结时间为3h，之后随炉冷却至室温，经20/40目标准筛筛分，即得到圆球度≥0.9，浊度为60FTU，酸溶解度<5%，体积密度为1.83g/cm3，视密度为3.33g/cm3，52MPa闭合压力下破碎率为4.2%，69MPa闭合压力下破碎率为6.3%的刚玉–莫来石陶粒支撑剂。

Claims (2)

1.一种刚玉–莫来石陶粒支撑剂，其特征是刚玉–莫来石陶粒支撑剂中的铝矾土的化学组成按照重量比为：Al2O3含量为60~63%，SiO2含量为10~13%，Fe2O3含量为4~6%，TiO2含量为2~3%，烧失量为16~18%；钙长石的化学组成按照重量比为：Al2O3含量为17~19%，SiO2含量为62~65%，CaO含量为15~17%。
2.如权利要求1所述的一种刚玉–莫来石陶粒支撑剂的制备方法，其特征是按如下步骤实施：
（1）将铝矾土和钙长石进行破碎和球磨处理制成粉状，在100~110℃条件下恒温干燥5~6h；
（2）按质量比92~99：1~8称取铝矾土和钙长石进行均匀混料，二者重量之和为100%，然后将铝矾土与钙长石混合粉料置于爱力许强力混合机内造粒制成生料球，造粒过程中添加14~19wt%的水；
（3）将上述生料球放入烘干箱中在30~50℃条件下干燥，并筛选出所需规格的半成品生料球；
（4）将半成品生料球放入烧结炉中进行烧结，其中烧结温度为1300~1450℃，烧结时间为3~5h，之后随炉冷却至室温，经20/40目标准筛筛分，即得到各项性能指标均满足中华人民共和国石油天然气行业标准SY/T 5108–2014要求的刚玉–莫来石陶粒支撑剂。
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