CN110702477B - 一种无机/有机化合物复合胶结人造岩心的制备方法 - Google Patents
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Abstract
本发明属于采油技术领域，具体涉及一种无机/有机化合物复合胶结人造岩心的制备方法，包括以下步骤：1、有机填料制备：将重量份数为100份的合成树脂、12份的固化剂、0.5份的固化促进剂、1份的流平剂和0.5份的消泡剂放入高速搅拌破碎机中充分混合；2、无机原料制备：将无机氧化物与功能剂放入对流式搅拌器中充分混合；3、原料预混合；4、原料覆膜和破碎；5、高压成型和脱模；6、控温固化；7、切割成型：根据设计的形状，采用线切割机床对固化后的材料进行切割。制备过程中岩心微观结构及性能可调性较强；制备获得的岩心物性重复性强；制备的人造岩心可用于岩土工程和石油工程等领域的相关多孔介质实验研究。
Description
技术领域：
本发明属于采油技术领域，具体涉及一种无机/有机化合物复合胶结人造岩心的制备方法。
背景技术：
岩石是油气资源、地层水、地热等流体资源的渗流空间，是室内实验中认识相关机理（油气运移、地下水污染、地热开采）的重要介质。近年来，国内人造岩心主要有：石英砂或玻璃球充填、磷酸盐烧结和石英砂环氧树脂胶结等岩石模型。与前两种岩石模型相比，石英砂环氧树脂胶结岩石模型在孔隙尺寸和结构与天然岩石相近，且制作工艺简单。因而，在国内石油科学研究中被广泛应用。但该制作工艺中，所用的环氧树脂是为液体状，模型中的孔喉往往被环氧树脂占据，与天然岩石“点-面接触胶结”的孔喉结构存在明显差别，当渗透率越低时，孔喉结构的差距越明显。此外，由于常规胶结方法所用环氧树脂具有一定粘度，在与石英砂混合过程中，由于加入量有限，难以保证均匀分布于石英砂表面，如此也会带来岩心本身的局部强非均质性，同时混砂过程也费时费力。为此，建立一套简单高效、经济环保的人造岩心制作新工艺，多孔介质相关渗流机理研究具有重要意义。
发明内容：
本发明的目的是提供一种无机/有机化合物复合胶结人造岩心的制备方法，制作工艺简单、可操作性强，经济高效；制备过程中岩心微观结构及性能可调性较强；制备获得的岩心物性重复性强；制备的人造岩心可用于岩土工程和石油工程等领域的相关多孔介质实验研究。
本发明采用的技术方案为：一种无机/有机化合物复合胶结人造岩心的制备方法，其特征在于：所述方法包括以下步骤：
步骤一、有机填料制备：将重量份数为90-110份的合成树脂、10-25份的固化剂、0.3-2份的固化促进剂、0.4-1.5份的流平剂和0.2-0.6份的消泡剂放入高速搅拌破碎机中充分混合；
步骤二、无机原料制备：将无机氧化物与功能剂放入对流式搅拌器中充分混合，其中无机组分与有机组分重量比为（3:1）-（20:1），无机化合物与功能剂重量比为(500：1)-(1000：1)；
步骤三、原料预混合:将有机填料和部分无机原料放入分散式搅拌器中充分混合；
步骤四、原料覆膜和破碎:将混合好后的原料缓慢加入塑料挤出机，设置温度，调节螺杆转速，挤出得到细条状混合料并冷却晾干，再将细条状混合料倒入磨粉机，设置筛网目数，得到表面覆有有机填料的无机原料颗粒；
步骤五、高压成型和脱模：在压制模具内壁涂抹脱模剂后，将覆膜后的无机原料颗粒与未覆膜的无机原料放入分散式搅拌器中充分混合，混合过程中加入覆膜、未覆膜无机材料总质量的2%-5%无机溶剂来保证成型，物料混合后放入压制模型的压槽中，设定成型压力，设定成型压力为8MPa-40MPa，单向加压并保持压力0-1小时后脱模；
步骤六、控温固化：将压制成型的复合材料放入可调温烘箱，设置加热固化程序，固化人造岩心，加热固化结束后，取出岩心冷却至室温后，储存待使用；
步骤七、切割成型：根据设计的形状，采用线切割机床对固化后的材料进行切割。
进一步地，所述合成树脂为高纯线性环氧树脂，固化剂为类酚醛树脂，固化促进剂为2-甲基咪唑，流平剂为丙烯酸酯、消泡剂为常规环氧消泡剂。
进一步地，所述无机氧化物为氧化硅、氧化钙或黏土中的一种或多种混合物；所述功能剂为润湿性调控剂或增韧剂；所述无机液体为含0.1%-0.5%NaCl浓度的蒸馏水。
进一步地，所述加热固化时间为0-48小时，温度为0-190℃。
进一步地，多孔材料有机部分为合成树脂、固化剂、固化促进剂、流平剂和消泡剂。多孔材料无机部分包括但不局限于氧化硅、氧化钙和黏土中的一种或多种混合物；多孔材料无机部分均为固体材料、其类型以及有机部分不同组分间配比可根据实际用途选择性调控。
本发明的有益效果：本发明的目的是提供一种无机/有机化合物复合胶结人造岩心的制备方法，可提前制备无机覆膜原料与无机原料，使用时再混合使用即可，制作工艺简单、可操作性强，经济高效；岩心孔喉结构与天然岩心孔喉结构近似，物性重复性强；与以往液体环氧制备岩心需要使用挥发类有机助剂不同，整个过程以固体原料为主，配合无机水溶液，岩心微观结构及性能可调性较强，材料环保；使用材料制备的人造岩心可用于岩土工程和石油工程等领域的相关多孔介质实验研究。
附图说明：
图1为实施例一中人造岩心的实物图片；
图2为实施例一中人造岩心铸体薄片图；
图3为实施例一中人造岩心内部结构电镜图。
具体实施方式：
实施例一
一种无机/有机化合物复合胶结人造岩心的制备方法，具体步骤如下：
步骤一、有机填料制备：将100份高纯线性环氧树脂、15份类酚醛树脂、0.5份2-甲基咪唑、1.0份丙烯酸酯和0.5份常规环氧消泡剂按照比例放入高速搅拌破碎机中充分混合4min。
步骤二、无机原料制备：将800份氧化硅与199份黏土组成的无机氧化物与1份润湿调控剂放入对流式搅拌器充分混合10min；
步骤三、原料预混合: 将全部有机填料和400份无机原料放入分散式搅拌器中充分混合10min；
步骤四、原料覆膜和破碎: 将混合好后的原料缓慢加入塑料挤出机，设置挤出温度150℃，调节螺杆转速25rad/min，挤出得到细条状混合料并风干冷却，设置好筛网目数180目，随后将细条状混合料倒入磨粉机磨碎，得到表面覆有有机填料的无机原料颗粒；
步骤五、高压成型和脱模：在压制模具内壁涂抹液体脱模剂后，将覆膜后的无机原料颗粒与未覆膜的原料放入分散式搅拌器中充分混合15min，混合过程中加入30份0.1%NaCl含量水溶液，加强成型，放入几何尺寸长×宽×高=15cm×5cm×5cm的可拆卸矩形压槽中，设定成型压力35MPa，单向加压并保持压力30min后脱模；
步骤六、控温固化：将压制成型的岩心块放入可调温烘箱，设置加热固化程序，初始每小时温度上升10℃，待温度达到100℃后每两小时上升10℃，温度达到190℃后保持3小时，加热固化结束后，取出人造岩心块冷却至室温后方可使用；
步骤七、切割成型：采用线切割机床对固化后的岩心块进行切割，得到Φ3.8´15cm的长条圆柱状岩心。
对上述长条圆柱状岩心进行渗透率测试，岩心渗透率为5mD，进行铸体薄片分析和电镜观察可以看出岩心内部孔喉分明，可用作渗流力学实验。
Claims (2)
1.一种无机/有机化合物复合胶结人造岩心的制备方法，其特征在于：所述方法包括以下步骤：
步骤一、有机填料制备：将重量份数为90-110份的合成树脂、10-25份的固化剂、0.3-2份的固化促进剂、0.4-1.5份的流平剂和0.2-0.6份的消泡剂放入高速搅拌破碎机中充分混合；
步骤二、无机原料制备：将无机氧化物与功能剂放入对流式搅拌器中充分混合，其中无机组分与有机组分重量比为（3:1）-（20:1），无机化合物与功能剂重量比为(500：1)-(1000：1)；
步骤三、原料预混合:将有机填料和部分无机原料放入分散式搅拌器中充分混合；
步骤四、原料覆膜和破碎:将混合好后的原料缓慢加入塑料挤出机，设置温度，调节螺杆转速，挤出得到细条状混合料并冷却晾干，再将细条状混合料倒入磨粉机，设置筛网目数，得到表面覆有有机填料的无机原料颗粒；
步骤五、高压成型和脱模：在压制模具内壁涂抹脱模剂后，将覆膜后的无机原料颗粒与未覆膜的无机原料放入分散式搅拌器中充分混合，混合过程中加入覆膜、未覆膜无机材料总质量的2%-5%无机溶剂来保证成型，物料混合后放入压制模型的压槽中，设定成型压力，设定成型压力为8MPa-40MPa，单向加压并保持压力0-1小时后脱模；
步骤六、控温固化：将压制成型的复合材料放入可调温烘箱，设置加热固化程序，固化人造岩心，加热固化结束后，取出岩心冷却至室温后，待使用；
步骤七、切割成型：根据设计的形状，采用线切割机床对固化后的材料进行切割；
所述合成树脂为高纯线性环氧树脂，固化剂为类酚醛树脂，固化促进剂为2-甲基咪唑，流平剂为丙烯酸酯、消泡剂为常规环氧消泡剂；
所述无机氧化物为氧化硅、氧化钙或黏土中的一种或多种混合物；所述功能剂为润湿性调控剂或增韧剂；
所述无机液体为含0.1%-0.5%NaCl浓度的蒸馏水。
2.根据权利要求1所述的一种无机/有机化合物复合胶结人造岩心的制备方法，其特征在于：所述加热固化时间为0-48小时，温度为0-190℃。
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