CN103396781B - 含有螯合剂的酸性水溶液及其用途 - Google Patents

含有螯合剂的酸性水溶液及其用途 Download PDF

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CN103396781B
CN103396781B CN201310230862.9A CN201310230862A CN103396781B CN 103396781 B CN103396781 B CN 103396781B CN 201310230862 A CN201310230862 A CN 201310230862A CN 103396781 B CN103396781 B CN 103396781B
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C·A·德沃尔夫
J·N·勒佩奇
J·H·贝姆拉尔
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Abstract

本发明涉及一种含有螯合剂和酸的酸性水溶液，其中螯合剂是谷氨酸N,N-二乙酸（GLDA）或其盐，和其中GLDA或其盐的量是至少10重量%，基于水溶液的重量计；还涉及酸性水溶液用做油田化学品的用途，以及在脱垢工艺中、在使用高浓度含水酸的工艺例如清洁工艺或镀覆工艺中的用途。

Description

含有螯合剂的酸性水溶液及其用途
本申请是中国专利申请200880124468.4的分案申请，该中国专利申请的申请日为2008年10月10日，发明名称是“含有螯合剂的酸性水溶液及其用途”。
发明领域
本发明涉及含有螯合剂和酸的酸性水溶液及其用途。
现有技术背景
含有螯合剂的酸性水溶液及其在油井刺激中的应用是公知的，例如参见SPE63242，W.W.Frenier等,“UseofHighlyAcid-SolubleChelatingAgentsinWellStimulationServices”,2000SPEAnnualTechnicalConference,DallasTX,2000年10月1-4日，其中公开了刺激酸，其可以用于油田化学处理中以防止当酸作用于被处理的岩层时固体的沉淀，并防止和除去结垢。所公开的酸性水溶液含有例如乙二胺四乙酸（EDTA），羟基乙基乙二胺三乙酸（HEDTA）或次氮基三乙酸（NTA）以及盐酸。据说EDTA在盐酸中具有较低的溶解度，但是NTA和HEDTA更易于溶解，并更好地控制铁的沉淀。
US2007/281868公开了用于处理地下岩层的酸性处理流体。这些流体可以含有任选的螯合剂，例如EDTA或GLDA。但是，此文献没有提供关于螯合剂在流体中的加入量的内容，也没有提到几种螯合剂在酸性流体中的不同溶解度。
但是，在现有技术中需要含有螯合剂和（其它）酸的酸性水溶液，其具有更高的螯合剂含量和酸性更强的pH，其中螯合剂在储存和运输过程中保持溶解态。
发明内容
惊奇地发现，谷氨酸N,N-二乙酸（GLDA）和其盐在这些含水酸的整个可得浓度范围内中的溶解度高于其它螯合剂例如NTA和HEDTA，并且另外它们保持溶解于具有更强酸性pH的水溶液中。
本发明提供了含有螯合剂和酸的酸性水溶液，其中螯合剂是谷氨酸N,N-二乙酸或其盐，和其中GLDA或其盐的量是至少10重量%，基于水溶液的重量计。
发现与其它螯合剂相比，谷氨酸N,N-二乙酸（GLDA）作为一种可生物降解的螯合剂，能高度溶解于宽范围的含水酸中，例如盐酸水溶液、甲酸水溶液和乙酸水溶液。
新溶液可以用于例如酸化中，这是目前用于确保提高油源产量的方法，其中在更小的通道中在油层中进行酸消化以保证更好的油流动。目前，采油公司使用NTA在盐酸水溶液中的溶液。螯合剂具有双重功能；其能络合在岩层中释放出来的铁，并防止由于使用酸而溶解的钙（再次）沉淀。
在作为油田化学品的应用中，本发明的酸性水溶液能防止铁沉淀物，并除去结垢。结垢一般是钙盐、钡盐或锶盐，例如碳酸钙或硫酸钡。本发明的酸性水溶液特别适用于除去碳酸钙结垢。另外，酸性水溶液用做在油井中的碳酸盐岩层的溶解剂。
因此，本发明还涉及上述含有GLDA和其它酸的溶液作为油田化学品的用途。
在本申请中，油田化学品表示用于油田工业中的化学品，例如在通过酸化、压裂和脱垢的完成和刺激中。
另外，本发明还涉及上述酸性水溶液在工艺例如清洁工艺或镀覆工艺中的用途，其中使用高度浓缩的含水酸，例如工业清洁、电镀和无电镀覆。
本发明还涉及上述酸性水溶液在除油田工业之外的其它工业中的脱垢工艺中的用途。
应当注意的是，JP2006/183079在实施例4中公开了用于镀铋的无电浴，其含有N,N-二羧基甲基L-谷氨酸和乙烷磺酸，以及相应量的含铋组分。在此实施例4中，N,N-二羧基甲基L-谷氨酸的量是3重量%，对于在此文献中的其它实施例中的几种溶液，其中螯合剂不是GLDA，螯合剂在酸性水溶液中的量总是低于10重量%。
另外应当注意的是，JP2006/117980也涉及镀铋，在实施例17中公开了制备含有10.1g/L的GLDA的酸性水溶液，其对应于含有约1重量%GLDA的酸性水溶液。另外，此文献没有公开任何含有多于10重量%螯合剂的酸性水溶液，也没有提供关于螯合剂在酸性水溶液中的溶解度的任何内容。
最后，JP2004/315412公开了一种过氧化氢组合物，其含有（A）过氧化氢、（B）尤其谷氨酸二乙酸盐、（C）水和（D）选自磷酸、柠檬酸和羟基乙烷二膦酸中的化合物。在实施例中，化合物（B）的用量是仅仅0.1重量%。
应当理解的是，另外含有铋或任何其它金属的酸性溶液不适用于油田刺激或清洁工艺中，并且铋是在镀覆工艺中最不优选的金属。另外，本领域技术人员将不会使用含有过氧化氢的组合物作为油田化学或镀覆中的化学品。
结果，在一个实施方案中，本发明的酸性水溶液不含相当大量的铋；优选，它们基本不含这种金属。在优选实施方案中，根据这些溶液的预期用途，它们也基本不含过氧化氢。
如果本发明的溶液用于镀覆工艺，在一个优选实施方案中，它们含有含铝、镍或铜的组分。
发现本发明的酸性水溶液具有比现有技术的含螯合剂的酸性水溶液更好的铁结合能力。同样，本发明的水溶液可以具有酸性更强的pH，因为GLDA即使在酸性非常强的pH和高浓度下也能保持溶解。组合的低pH和高螯合剂含量将得到组合的更高铁结合能力和油层的消化，以及改进的防垢和除垢效果。
在一个优选实施方案中，本发明的酸性水溶液具有低于7的pH，优选低于3，最优选低于1。在一个实施方案中，pH高于-5，优选高于-3，更优选高于-1，最优选高于0。
在本发明酸性水溶液中的酸可以是能以较高浓度溶解于水溶液中的酸，是本领域技术人员熟知的。在一个实施方案中，酸选自盐酸、氢溴酸、氢氟酸、氢碘酸、硫酸、硝酸、磷酸、甲酸、乙酸、柠檬酸、乳酸、苹果酸、酒石酸、马来酸、硼酸、硫化氢或两种或多种这些酸的混合物。在本发明中也可以使用这些酸的前体，例如二氟化铵，它是氢氟酸前体。优选，酸不是太昂贵的酸，例如乙烷磺酸。在另一个更优选的实施方案中，酸选自盐酸、氢溴酸、氢氟酸、硫酸、硝酸、磷酸、甲酸、乙酸或两种或多种这些酸的混合物。
酸在酸性水溶液中的存在量是至少5重量%，优选至少10重量%，甚至更优选至少15重量%，最优选至少20重量%。也应当理解的是，每种酸具有在水中的不同最大溶解度；例如，氢氟酸是以在水中48重量%的浓度商购的。但是，优选，酸浓度低于40重量%，因为这种水溶液能以合理价格商购，并证明是足够有效的。
GLDA在酸性水溶液中的存在量是至少10重量%和至多60重量%，基于水溶液的重量计，优选20-60重量%，甚至更优选30-60重量%，最优选40-60重量%。
本发明的水溶液可以另外含有在其它申请中单独要求保护的合适的添加剂，例如表面活性剂、助洗剂、润湿剂、乳化剂、漂白剂。
附图说明
图1显示螯合剂乙二胺四乙酸（EDTA）、二亚乙基三胺五乙酸(DTPA)、次氮基三乙酸(NTA)、羟基乙基乙二胺三乙酸(HEDTA)、乙醇二甘氨酸(EDG)、甲基甘氨酸二乙酸(MGDA)和谷氨酸二乙酸(GLDA)在含水乙酸、甲酸和盐酸中的最大溶解度。
图2显示上述螯合剂在含水硫酸、磷酸和硝酸中的最大溶解度。
实施例
酸性水溶液是基于15%乙酸、28%乙酸（都从来自Fluka的乙酸制备）、15%甲酸、28%甲酸（都从来自Fluka的甲酸制备）、15%盐酸和28%盐酸（都从来自Fluka的37%盐酸制备）、15%硫酸和28%硫酸（都从来自Fluka的96%硫酸制备）、15%磷酸和28%磷酸（都从来自Fluka的85%H3PO4制备）、15%硝酸和28%硝酸（都从来自Fluka的65%HNO3制备）。
向上述酸性水溶液加入几种螯合剂，直至达到最大溶解度。这通过将螯合剂加入酸性水溶液直到获得饱和溶液（目测）并随后搅拌3天进行，然后使存在的任何固体材料沉降。在溶液中存在的固体材料应当是由于材料从未溶解或材料在溶液的3天搅拌期间固化。
透明液体层中的螯合剂的量是通过用金属阳离子滴定（对于EDG是Cu，对于所有其它螯合剂是Fe）检测的，但是在溶液直接透明的情况下不是如此，其中螯合剂的溶解量小于约0.5重量%。
所用的螯合剂是以下酸：
-乙二胺四乙酸（EDTA），DissolvineZ，来自AkzoNobel;
-二亚乙基三胺五乙酸(DTPA),DissolvineDZ，来自AkzoNobel;
-次氮基三乙酸(NTA),DissolvineAZ，来自AkzoNobel;
-羟基乙基乙二胺三乙酸(HEDTA)，来自Aldrich;
-乙醇二甘氨酸(EDG),DissolvineEDG，来自AkzoNobel，用盐酸处理并在结晶后分离;
-甲基甘氨酸二乙酸(MGDA)，TrilonM，来自BASF，用盐酸处理并在结晶后分离；和
-谷氨酸二乙酸(GLDA)，DissolvineGL-38，来自AkzoNobel，用离子交换酸性树脂处理并干燥。
最大溶解度如下图1和2所示。可见，螯合剂GLDA在所有浓缩酸性水溶液中的溶解度显然好于任何其它实验螯合剂，但是一些螯合剂较好地溶解于15%盐酸和硫酸中。
螯合剂的最大溶解度是在主要部分实验中使用Fe-TSV方法检测的（工业中公知的一种方法，其中将Fe（III）离子加入公知量的螯合物溶液中，其中滴定的终点是由过量铁离子不会被螯合物捕捉来指示的）。EDG的溶解度是通过使用Cu-TSV方法检测的（在此方法中，Cu离子代替Fe离子加入）。在乙酸水溶液的透明液体层中的EDG量的检测不能通过用铜滴定来检测，因为乙酸的缓冲能力将阻碍这种滴定。为了能检测在乙酸水溶液中的EDG量，将少量EDG加入所述溶液中。在添加1%EDG后，溶液保持透明，添加2%的EDG导致浑浊的混合物，其中显然一些EDG以固化形式存在。所以，结论是EDG在乙酸中的溶解度是约1.5重量%。当检测螯合剂在磷酸中的溶解度时遵循相同的程序，因为这些溶液也难以滴定；再次，将螯合剂逐步（1重量%/每步）添加到酸中直到螯合剂不再能溶解。
MGDA的溶解度仅仅在有限数目的含水酸中检测。MGDA表现出首先合理地溶解于15%盐酸水溶液中，但是相当大量的螯合剂在加入后3天时在酸性溶液中固化。DTPA和15%硝酸的水溶液也出现同样的现象，其中也有大量的螯合剂在3天后固化。
GLDA实际上比实验中更容易溶解，但是增加的粘度表示向溶液加入更多的GLDA会使得进一步搅拌变得过于复杂。
HEDTA和EDG在硝酸中的溶解度不能作为这些螯合剂与硝酸的组合来检测，这导致有害的分解，因为硝酸是潜在的氧化介质。

Claims (6)

1.一种含有螯合剂和酸的酸性水溶液用做油田化学品的用途，其中螯合剂是谷氨酸N,N-二乙酸(GLDA)或其盐，其中GLDA或其盐的量是基于水溶液的重量计的10-60重量％，其中所述酸选自盐酸、氢溴酸、氢氟酸、氢碘酸、硫酸、硝酸、磷酸、甲酸、乙酸、柠檬酸、乳酸、苹果酸、酒石酸、马来酸、硼酸、硫化氢或两种或多种这些酸的混合物，并且其中所述用做油田化学品的用途是在油田工业中在通过酸化、压裂和/或脱垢的完成和刺激中的溶液中的用途。
2.一种含有螯合剂和酸的酸性水溶液在清洁工艺、镀覆工艺或脱垢工艺中的用途，其中螯合剂是谷氨酸N,N-二乙酸(GLDA)或其盐，其中GLDA或其盐的量是基于水溶液的重量计的10-60重量％，其中所述酸选自盐酸、氢溴酸、氢氟酸、氢碘酸、硫酸、硝酸、磷酸、甲酸、乙酸、柠檬酸、乳酸、苹果酸、酒石酸、马来酸、硼酸、硫化氢或两种或多种这些酸的混合物。
3.权利要求1或2的用途，其中所述酸性水溶液具有低于3的pH。
4.一种适合权利要求1-3中任一项所述用途的酸性水溶液，其含有螯合剂、酸和添加剂，其中螯合剂是谷氨酸N,N-二乙酸(GLDA)或其盐，其中GLDA或其盐的量是基于水溶液的重量计的10-60重量％，其中所述酸选自盐酸、氢溴酸、氢氟酸、氢碘酸、硫酸、硝酸、磷酸、甲酸、乙酸、柠檬酸、乳酸、苹果酸、酒石酸、马来酸、硼酸、硫化氢，并且其中所述添加剂选自表面活性剂、助洗剂和漂白剂。
5.权利要求4的酸性水溶液，其中所述酸性水溶液具有低于3的pH。
6.权利要求4的酸性水溶液，其中表面活性剂选自润湿剂和乳化剂。
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US9803134B2 (en) 2017-10-31
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CN101918510A (zh) 2010-12-15
CA2711634A1 (en) 2009-07-16
CA2711634C (en) 2016-09-27
RU2476475C2 (ru) 2013-02-27
JP2011512421A (ja) 2011-04-21
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