CN111393614B - 一种树脂水下固化剂及其制备方法 - Google Patents

一种树脂水下固化剂及其制备方法 Download PDF

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CN111393614B
CN111393614B CN202010443504.6A CN202010443504A CN111393614B CN 111393614 B CN111393614 B CN 111393614B CN 202010443504 A CN202010443504 A CN 202010443504A CN 111393614 B CN111393614 B CN 111393614B
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王润亭
史胜龙
房堃
温庆志
张东晓
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Qingdao Dadi Institute Of New Energy Technologies
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Abstract

本发明属于油气藏开发的技术领域，具体的涉及一种树脂水下固化剂及其制备方法。该种树脂水下固化剂由胺类固化剂、酸酐类固化剂和促进剂复合而成。该水下固化剂不仅可以使得树脂在水下高速固化，而且所形成的固化材料具有优异的耐压强度和极好的耐温性能。

Description

一种树脂水下固化剂及其制备方法
技术领域
本发明属于油气藏开发的技术领域，具体的涉及一种树脂水下固化剂及其制备方法。
背景技术
在油气藏开发过程中，通过水力压裂技术进行造缝，为了防止裂缝在高闭合压力下重新闭合，需向裂缝中充填支撑材料。常规压裂技术中，通常是通过高黏度压裂液携带支撑剂注入，但是由于压裂液黏度太大，会导致液体在管线、井筒中以及地层裂缝中流动的摩阻增大，增加泵注难度；同时加砂压裂工艺复杂，高填砂伴随的高排量、高泵压对井口、施工设备以及施工管柱要求高，加砂过程中如果控制不当还会造成砂堵，潜在较大的工程施工风险和人员安全风险。为了解决这一问题，现采用注入液态树脂(比如环氧树脂)的方式，在液态树脂到达裂缝之后固化从而形成支撑材料，但是由于地下环境中水的存在，严重降低了液态树脂的固化效率。
近些年树脂水下固化剂在混凝土结构修补，水下胶粘剂等方面有着不错的应用。目前市场上的树脂水下固化剂主要为酮亚胺类固化剂或曼尼希固化剂，其中酮亚胺类固化剂是酮亚胺遇水反应生成释放胺活性基团，由胺活性基团与树脂进行交联固化，这种固化机制反应时间较慢，所需温度较高，固化时间较长；曼尼希固化剂的结构中有很多疏水性及活性高的基团，使其能在低温、潮湿等环境中表现出优异的固化性能。然而水下环境与低温、潮湿环境不同，很多固化剂在低温、潮湿环境中表现出优异的固化性能，但水下固化性能较差。因此探究和研发能在水下固化树脂的固化剂，对于大坝、水利设施和人防工程等建筑物的粘接、修补以及油气藏开发等方面有着非常重要的意义。
发明内容
本发明的目的在于针对传统水下固化剂固化效率低；固化后材料力学性能降低等问题而提供一种树脂水下固化剂，该水下固化剂不仅可以使得树脂在水下高速固化，而且所形成的固化材料具有优异的耐压强度和极好的耐温性能。
本发明的技术方案为：一种树脂水下固化剂，由胺类固化剂、酸酐类固化剂和促进剂复合而成。
按照重量百分比所述胺类固化剂：酸酐类固化剂：促进剂为50％～80％：15％～45％：0.5％～5％。
该树脂水下固化剂与所需固化的树脂之间质量比为1:1～25。
该树脂水下固化剂适用的树脂为环氧树脂、酚醛树脂和聚酯树脂中的一种。
所述胺类固化剂为三亚乙基四胺、三乙烯四胺、三亚乙基三胺、间苯二胺、乙二胺和二氨基二苯基甲烷中至少一种。
所述酸酐类固化剂为邻苯二甲酸酐、顺丁烯二酸酐、六氢苯二甲酸酐和戊二酸酐中至少一种。
所述促进剂为咪唑类促进剂、三乙胺和乙酰丙酮金属盐中至少一种。
所述树脂水下固化剂的制备方法，包括以下步骤：将胺类固化剂、酸酐类固化剂与促进剂按配比加入反应釜中，在30～80℃下以100～500r/min的搅拌速率搅拌30～90min。
所述水下固化剂的理化指标如下：25℃条件下粘度值为80～1650mPa﹒s；常温下为液态，密度为1.0～2.0g/mL。
所述树脂水下固化剂作为金属粘接剂的应用。
本发明的有益效果为：本发明所述树脂水下固化剂由胺类固化剂、酸酐类固化剂和促进剂复合而成，其固化效率极高。以环氧树脂为例进行测试，将环氧树脂与该水下固化剂按照比例混合均匀，在40～80℃水环境下水浴加热，可在30min内将环氧树脂完全固化。使用所述水下固化剂形成的固化材料具有优异的耐压强度和极好的耐温性能；同时该水下固化剂在水下应用后与金属具有极强的粘接性能，亦可作为金属粘接剂。
附图说明
图1为实施例1中环氧树脂与水下固化剂混合后的示意图。
图2为实施例1中环氧树脂混合液水环境固化示意图。
图3为实施例1中环氧树脂混合液抽真空示意图。
图4为实施例1中环氧树脂压缩样条示意图。
图5为对比例1所述的环氧树脂水下固化剂水下固化效果图。
图6为对比例2所述的环氧树脂水下固化剂水下固化效果图。
图7为对比例3所述的环氧树脂水下固化剂水下固化效果图。
图8为对比例4所述的环氧树脂水下固化剂水下固化效果图。
具体实施方式
下面通过实施例对本发明进行详细的说明。
实施例1
所述树脂水下固化剂由三亚乙基四胺、顺丁烯二酸酐和三乙胺复合而成；按重量百分比三亚乙基四胺：顺丁烯二酸酐：三乙胺为70％：28％：2％。
该水下固化剂应用于环氧树脂，在该体系中环氧树脂胶液粘度值在1800mPa﹒s，水下固化剂25℃粘度值为500mPa﹒s。将该环氧树脂水下固化剂与环氧树脂按质量比20:100在30℃条件下以300r/min的搅拌速率搅拌30min混合均匀，30℃真空抽气泡，置于60℃水环境，30分钟即可完全固化。所形成的固化材料抗压强度可达70MPa，耐温可达180℃。
由图1可以看出，该水下固化剂与环氧树脂的相容性，配伍性优异，混合过程无需升温，混合后无杂质。
由图2可见，将环氧树脂与水下固化剂的混合液注入模具中，一起置入水环境加热，整个过程无混合液散入水中，无有效物质逸散，证明体系在水中可以稳定存在。
由图3可见，加入水下固化剂的树脂易于抽真空，从侧面证明树脂体系易加工，粘度低；过程中无分层等现象，证明体系的配伍性能优异。
由图4可见，树脂样条颜色透明均一，说明在水中加热受热均匀，树脂固化性能优异。
实施例2
所述树脂水下固化剂由间苯二胺、六氢苯二甲酸酐和三乙胺复合而成；按重量百分比间苯二胺：六氢苯二甲酸酐：三乙胺为75％:20％：5％。
该水下固化剂应用于聚氨酯树脂，在该体系中聚氨酯树脂胶液粘度值在2000mPa﹒s，水下固化剂25℃粘度值为1500mPa﹒s。将该聚氨酯树脂水下固化剂与聚氨酯树脂按质量比30:100在30℃条件下以200r/min的搅拌速率搅拌50min混合均匀，30℃真空抽气泡，置于50℃水环境，30分钟即可完全固化。所形成的固化材料抗压强度可达70MPa，耐温可达220℃。
实施例3
所述树脂水下固化剂由二氨基二苯基甲烷、戊二酸酐和三乙胺复合而成；按重量百分比二氨基二苯基甲烷：戊二酸酐：三乙胺为60％：35％：5％。
该水下固化剂应用于酚醛树脂，在该体系中酚醛树脂胶液粘度值在9000～12000mPa﹒s，水下固化剂25℃粘度值为1500mPa﹒s。将该酚醛树脂水下固化剂与酚醛树脂按质量比10:100在30℃条件下以400r/min的搅拌速率搅拌60min混合均匀，30℃真空抽气泡，置于40℃水环境，30分钟即可完全固化。所形成的固化材料抗压强度可达56MPa，耐温可达180℃。
对比例1
所述树脂水下固化剂由三亚乙基四胺和三乙胺复合而成；按重量百分比三亚乙基四胺：三乙胺为70％：30％。
该水下固化剂应用于环氧树脂，在该体系中环氧树脂胶液粘度值在1800mPa﹒s，水下固化剂25℃粘度值为100mPa﹒s。将该环氧树脂水下固化剂与环氧树脂按质量比20:100在30℃条件下以300r/min的搅拌速率搅拌30min混合均匀，30℃真空抽气泡，置于60℃水环境，24小时未能完全固化，请见图5。
对比例2
所述树脂水下固化剂由顺丁烯二酸酐和三乙胺复合而成；按重量百分比顺丁烯二酸酐：三乙胺为80％：20％。
该水下固化剂应用于环氧树脂，在该体系中环氧树脂胶液粘度值在1800mPa﹒s，水下固化剂25℃粘度值为1500mPa﹒s。将该环氧树脂水下固化剂与环氧树脂按质量比20:100在30℃条件下以300r/min的搅拌速率搅拌30min混合均匀，30℃真空抽气泡，置于60℃水环境，6小时方能完全固化。所形成的固化材料抗压强度为52MPa，耐温为180℃。
对比例3
所述树脂水下固化剂由间苯二胺，顺丁烯二酸酐，2-甲基咪唑复合而成；按重量百分比间苯二胺：顺丁烯二酸酐：2-甲基咪唑为70％：28％：2％。
该水下固化剂应用于环氧树脂，在该体系中环氧树脂胶液粘度值在1800mPa﹒s，水下固化剂25℃粘度值为2000mPa﹒s。将该环氧树脂水下固化剂与环氧树脂按质量比20:100在30℃条件下以300r/min的搅拌速率搅拌30min混合均匀，30℃真空抽气泡，置于60℃水环境，20小时完全固化。所形成的固化材料抗压强度可达60MPa，耐温可达180℃。
对比例4
所述树脂水下固化剂由三亚乙基四胺、顺丁烯二酸酐和三乙胺复合而成；按重量百分比三亚乙基四胺：顺丁烯二酸酐：三乙胺为30％：68％：2％。
该水下固化剂应用于环氧树脂，在该体系中环氧树脂胶液粘度值在1800mPa﹒s，水下固化剂25℃粘度值为1500mPa﹒s。将该环氧树脂水下固化剂与环氧树脂按质量比20:100在30℃条件下以300r/min的搅拌速率搅拌30min混合均匀，30℃真空抽气泡，置于60℃水环境，1小时可完全固化。所形成的固化材料抗压强度可达70MPa，耐温可达180℃。
结论分析
1、通过实施例1-3之间对比可知：本发明所述树脂水下固化剂在水下具有极高的固化效率且固化产物具有极高的耐高温性能。
2、通过对比例1与实施例1的对比可知：胺类固化剂在水中固化效率受到极大的抑制甚至失效，仅依靠胺类固化剂和促进剂无法在水下实现完全固化。
3、通过对比例2与实施例1的对比可知：仅依靠酸酐类固化剂与促进剂，虽然可以固化，但固化时间延长，固化产物力学性能下降。
4、通过对比例3可知：更换固化剂成份，固化效率受到极大的抑制，抗压强度下降。
5、通过对比例4可知：更换固化剂配方比例，固化时间受到影响，其他性能不变。

Claims (6)

1.一种树脂水下固化剂，其特征在于，由胺类固化剂、酸酐类固化剂和促进剂复合而成；按照重量百分比所述胺类固化剂：酸酐类固化剂：促进剂为50%～80%：15%～45%：0.5%～5%；所述胺类固化剂为三亚乙基四胺、间苯二胺和二氨基二苯基甲烷中至少一种；所述酸酐类固化剂为顺丁烯二酸酐、六氢邻苯二甲酸酐和戊二酸酐中至少一种；所述促进剂为三乙胺。
2.根据权利要求1所述树脂水下固化剂，其特征在于，该水下固化剂与所需固化的树脂之间质量比为1:1～25。
3.根据权利要求1所述树脂水下固化剂，其特征在于，该水下固化剂适用的树脂为环氧树脂、酚醛树脂和聚酯树脂中的一种。
4.一种权利要求1所述树脂水下固化剂的制备方法，其特征在于，包括以下步骤：将胺类固化剂、酸酐类固化剂与促进剂按配比加入反应釜中，在30～80℃下以100～500r/min的搅拌速率搅拌30～90min。
5.根据权利要求1所述树脂水下固化剂，其特征在于，该水下固化剂的理化指标如下：25℃条件下粘度值为80～1650mPa﹒s；常温下为液态，密度为1.0～2.0g/mL。
6.一种权利要求1所述树脂水下固化剂作为金属粘接剂的应用。
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