CN107709662A - 在用于一次采油的流体中使用的纳米原纤化纤维素 - Google Patents

在用于一次采油的流体中使用的纳米原纤化纤维素 Download PDF

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CN107709662A
CN107709662A CN201680030593.3A CN201680030593A CN107709662A CN 107709662 A CN107709662 A CN 107709662A CN 201680030593 A CN201680030593 A CN 201680030593A CN 107709662 A CN107709662 A CN 107709662A
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M.阿-巴古里
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Abstract

本发明涉及用于钻井液、压裂液、隔离液等的纳米原纤化纤维素(NFC)。所述流体包含具有大于100的长径比的NFC作为增粘剂，并且其中所述纳米原纤维具有5与100纳米之间的直径和大于1μm的长度。

Description

在用于一次采油的流体中使用的纳米原纤化纤维素
技术领域
本发明涉及纳米原纤化纤维素(NFC)作为钻井液、压裂液、隔离液等中的粘度调节剂的用途。
背景技术
大分子(聚合物材料)，特别是水溶性大分子属于用于从地下地层提取烃的最常用的化学品。无论提取是一次提取还是三次提取，聚合物被用于各种功能。例如，在油气井钻探中，聚合物被用作粘度调节剂、分散剂或用于过滤控制目的。在通过酸处理或水力压裂使井增产的情况下，聚合物也被用作粘度调节剂以及用作过滤控制添加剂。
在采油中使用的聚合物是生物基材料或化石基材料。一般地，在<150℃的低温至中温下使用生物聚合物。合成聚合物由于其高热稳定性而在更宽的温度范围内使用。
纳米原纤化纤维素(NFC)是由可再生资源产生的一类新材料，并且它具有作为用于油田应用的有用添加剂的潜能。非常关注使用可再生资源来替代来自石化工业的化学品，以减少碳足迹。在WO 2014148917中公开了NFC或微原纤化纤维素(MFC)作为用于诸如压裂液、钻井液、隔离液和EOR液的油田流体的增粘剂的用途。用NFC增粘的流体显示优异的剪切稀化性质，并且这归因于纳米原纤维>100的高长径比。原纤维的长径比是原纤维的长度除以直径(长度/直径)。另外，与诸如黄原胶和瓜尔胶、纤维素以及淀粉衍生物等的天然聚合物相比，NFC更加热稳定。此外，取决于其表面电荷，与市售可得的生物聚合物或合成聚合物相比，NFC具有高耐盐性。
可通过各种方法由任何含纤维素或含木质纤维素的原材料来生产NFC，并且其特性可被定制。对NFC的大多数研究集中于使用漂白浆粕作为原料来制备NFC。然而，使用木质纤维素生物质代替提纯浆粕作为原料来生产纳米原纤化木质纤维素(NFLC)是经济有利的。木质纤维素生物质的来源很多，诸如木材、禾秆、农业废弃物诸如甘蔗渣和甜菜浆等。这仅可在最终应用耐受在最终产物中存在木质素的情况下适用。
植物细胞壁主要由木质纤维素生物质组成，所述木质纤维素生物质由纤维素、半纤维素和木质素组成。这三种主要组分的比率和它们的结构复杂性根据植物的类型而显著变化。一般地，纤维素是植物细胞壁中的最大组分并且其在干物质重量的35-50%范围内，半纤维素在15-30%范围内且木质素在10-30%范围内。作为用于油田应用的其它大分子，在使用后去除NFLC是合意的。幸运的是，存在借助酶促降解或氧化降解的两种可能的解决方案来去除或降解NFLC。大量研究了木质纤维素生物质的酶促降解，因为它是由生物质产生生物燃料中的主要步骤。通过优化酶效率、找到对目标生物质的最佳酶组合、对生物质进行预处理使其可易于被酶接近以及找到最优降解条件，最近的发展实现了酶促降解总成本的显著降低。
通过选择原材料，或通过调节生产参数，或通过对生产的原纤维进行后处理，可产生具有宽范围的物理化学性质的NFC或NFLC。例如，NFC原纤维的尺寸可变化以适于应用的目的。一般地，在植物中由原纤维束组成的纤维素纤维的直径在20-40μm范围内，具有0.5-4mm范围内的长度。可由纤维素纤维的完全解原纤获得的单根纤维素原纤维具有几纳米(大约3 nm)的直径和1-100μm的长度。取决于解原纤的能量输入和解原纤之前的预处理，纤维的直径可减至纳米数量级(5-500 nm)。另外，可在一定程度上控制原纤维长度以使它适合于所需应用。此外，从文献中熟知的是可采取各种方式将纤维素分子化学改性，以获得所需化学性质。可采取相同方式调整NFC的表面化学性质以满足最终使用需要。通常，在表面上用羟基中和纤维素分子的表面电荷，但羟基可转化成阴离子或阳离子电荷。醚化和酯化属于用以改变纤维素表面性质的最常用的方法。
NFC的性质允许定制其物理化学性质以匹配在油田流体中使用。可调节原纤维形态和原纤维的化学性质两者以适应应用要求。
具有高木质素含量的NFLC的热稳定性是不令人满意的。然而，包含基于干物质计至多20重量%木质素的NFLC具有在钻井液中使用的可接受的热稳定性。
岩芯驱替(core flooding)试验是用于研究流体流动至多孔介质中的常用方法。该试验方法提供关于流体及其组分与代表目标储层的岩芯样本的相互作用的有用信息。使用该技术来评估流体对油/气储层的地层破坏潜能，还在EOR应用的情况下评价聚合物至储层中的穿透性。通常设定诸如温度压力、流体组成、岩芯类型和流速的试验条件来模拟油田和应用条件。
本发明的目的在于提供用作在钻井液、压裂液、隔离液等中使用的添加剂的纳米原纤化纤维素，其中NFC不能够穿透至地层中。对于其中不期望原纤维穿透至地层中的此类应用，诸如用于钻井液、隔离液或水力压裂液的粘度调节剂或降失水添加剂而言，优选使用具有长原纤维长度的NFC。
发明简述
本发明涉及用作钻井液、压裂液、隔离液等中的粘度调节剂的纳米原纤化纤维素(NFC)，其中所述流体包含具有大于100的长径比的NFC，其中纳米原纤维具有5与50纳米之间的直径和大于1μm的平均长度。
根据优选实施方案，NFC的长径比大于500，其中纳米原纤维具有5与30纳米之间的直径和大于5μm的平均长度。
根据另一优选实施方案，纳米原纤化纤维素是纳米原纤化木质纤维素，其包含基于干物质计至多20重量%木质素，并优选基于干物质计至多10重量%木质素。
可如下控制原纤维尺寸：通过增加所使用的解原纤能量和通过在解原纤之前使用预处理步骤以促进解原纤过程而使得直径变得越来越细。最细的原纤维直径仅几纳米。根据WO 2012119229，NFC的表面电荷(羧基)浓度可在每克NFC 0.1至11 mmol范围内，并且可获得小于10至大于1000范围内的长径比。
本发明的进一步描述
在下文实施例中使用的NFC材料是在实验室中如下列文献中所述产生的。
1) TEMPO介导的NFC (TEMPO-NFC)根据Saito等人的出版物(Saito, T.Nishiyama, Y. Putaux, J.L. Vignon M.和Isogai. A. (2006). Biomacromolecules, 7(6): 1687-1691)产生。TEMPO是2,2,6,6-四甲基哌啶-1-氧自由基。一般地，TEMPO-NFC具有小于15 nm的直径和大于100的长径比。电荷密度通常在0.2-5 mmol/g范围内。
2) 酶法辅助的NFC (EN-NFC)根据Henriksson等人的出版物，European polymerjournal (2007), 43: 3434-3441 (An environmentally friendly method for enzyme- assisted preparation of microfibrillated cellulose (MFC) nanofibers(酶辅助制 备微原纤化纤维素(MFC)纳米纤维的环境友好的方法))和M. Pääkkö等人的出版物，Biomacromolecules, 2007, 8 (6), 第1934-1941页, Enzymatic Hydrolysis Combined with Mechanical Shearing and High-Pressure Homogenization for Nanoscale Cellulose Fibrils and Strong Gels(用于纳米尺度的纤维素原纤维和强凝胶的结合机 械剪切和高压均化的酶促水解)产生。ME-NFC具有小于50 nm的直径和大于100的长径比。电荷密度通常低于0.2 mmol/g。
3) 机械产生的MFC (NE-NFC)如由Turbak A等人(1983), “Microfibrillated cellulose: a new cellulose product: properties, uses, and commercial potential(微原纤化纤维素：一种新型纤维素产品：性质、用途和商业潜力)”, J ApplPolym Sci Appl Polym Symp 37:815-827所述产生。ME-MFC还可通过以下方法中的一种来产生：均化、微流化、微研磨和低温压碎。关于这些方法的进一步信息可在Spence等人在Cellulose (2011) 18: 1097-1111中的论文，“A comparative study of energy consumption and physical properties of microfibrillated cellulose produced by different processing methods(通过不同加工方法生产的微原纤化纤维素的能量消耗和 物理性质的对比研究)”中找到。ME-NFC具有小于大约50 nm的直径和大于100的长径比。电荷密度(羧酸根含量)通常低于0.2 mmol/g。
4) 羧甲基化NFC (CM-NFC)根据”The build-up of polyelectrolyte multilayers of microfibrillated cellulose and cationic polyelectrolytes (微原 纤化纤维素和阳离子聚电解质的聚电解质多层的建立)”, Wågberg L, Decher G, NorgenM, Lindström T, Ankerfors M, Axnäs K Langmuir (2008) 24(3), 784-795中阐述的方法产生。CM-NFC具有小于30 nm的直径和大于100的长径比。电荷密度通常在0.5-2.0 mmol/g范围内。
用于测量所产生的NFC的各种性质的设备包括物料平衡(mass balance)、至多12000 rpm的恒速混合器、pH计、Fann 35粘度计、Physica流变仪MCR—Anton Paar(具有Couette几何结构CC27)，和热老化烘箱(在100-1000 psi的压力下至多260℃)以及岩芯驱替系统。
实施例1
岩芯驱替试验
使用不同类型的岩芯(砂岩和石灰岩两者)，在不同条件下诸如各种NFC浓度、各种类型的NFC，在各种温度、流速和不同压力下，对NFC流体实施岩芯驱替试验。
用于岩芯驱替试验的程序如下：
1.将岩芯在250℉下干燥4小时并称重以获得其干重。然后，在真空下用盐水溶液(在去离子水中的5重量%KCl)使岩芯饱和6小时并测量其湿重。使用这些测量结果和盐水溶液的密度(在70℉下密度= 1.03 g/cm3)来计算孔体积(PV)。
2.将岩芯置于岩芯夹持器内。在生产方向上将盐水(5重量%KCl)泵送经过岩芯。如果需要高温，则将温度升高至目标值(250℉)并在试验期间保持恒定。监测并记录跨越岩芯的压降直至其稳定。计算初始渗透率。
3.通过用5重量%KCl盐水将1.0重量% NFC分散体稀释至0.4重量%的NFC浓度来制备处理流体。将400 g NFC溶液混合到600 g KCl盐水(5重量%)中，以制得用作处理流体的0.4重量% NFC。
4. 在1100 psi的背压下，在注入方向(与生产方向相反)上泵送包含NFC和/或其它化学品的处理流体。跨越岩芯的压降随着注入纤维流体而增加。当注入2 PV时停止注入。记录跨越岩芯的压降。
5. 然后，使流动方向逆转成生产方向，并将盐水(5重量% KCl)注入到岩芯中直至跨越岩芯的压降稳定。计算在流体处理之后的渗透率恢复值(return permeability)。
实施例1：使用具有不同渗透率的岩芯对ME-NFC进行测试。
在该试验中，使用分别具有20、100和400 mD的渗透率的砂岩岩芯来测试具有100以上的长径比和小于50 nm直径的ME-NFC的岩芯驱替。
表1：使用各种岩芯对ME-NFC进行测试。试验在250℉下进行。
。
上述实施例表明具有大约30 nm直径和大于5微米长度的规则NFC品级对低渗透率和中等渗透率岩芯造成较少损坏或不造成损坏。对于具有<100 mD的初始渗透率的岩芯而言，渗透率恢复值在88%以上。这表明具有大于5微米的长原纤维的NFC原纤维足够大以穿透中等渗透率至低渗透率地层如致密气。观察到原纤维在岩芯表面处从注射方向上被滤出。随着渗透率提高，孔喉变大并且纳米原纤维可侵入岩芯。对于具有400 mD的初始渗透率的岩芯而言情况是这样的，其中渗透率恢复值仅为53%。这表明原纤维穿透岩芯并损害地层。需要诸如酶促破坏剂或化学破坏剂的后处理来从地层除去NFC。
实施例2：使用具有中等渗透率(100 mD)的贝雷(Berea)砂岩岩芯对各种类型的NFC进行测试并与瓜尔胶和粘弹性表面活性剂进行比较。
该实施例比较了作为增粘剂的3种类型的NFC与瓜尔胶、改性瓜尔胶(羟丙基瓜尔胶)和粘弹性表面活性剂的渗透率恢复值。如表2中所示制备处理流体。
表2：处理流体的配方
。
表3：使用具有中等渗透率(100 mD)的贝雷砂岩岩芯对各种类型的NFC进行测试并与瓜尔胶和粘弹性表面活性剂进行比较。试验在250℉下进行。
。
该实施例2显示不论原纤维表面上的电荷密度，在相同浓度下，对于诸如贝雷砂岩的中等渗透率岩芯而言，渗透率恢复值在90%以上。对于NFC材料的渗透率恢复值显著高于对于瓜尔胶和改性羟丙基瓜尔胶的渗透率恢复值。
如果在产生NFC的解原纤步骤之前使用酶促或化学预处理，则应当监测和控制所述预处理以避免使纤维缩短，其可能在以后对油气储层造成破坏。
权利要求书(按照条约第19条的修改)
1.一种包含纳米原纤化纤维素(NFC)作为增粘剂的流体，其中所述流体是钻井液、压裂液或隔离液，其特征在于所述NFC具有大于100的长径比，并且其中所述纳米原纤维具有5与100纳米之间的直径和大于1μm的长度。
2.如权利要求1中所要求保护的流体，其中NFC的所述长径比大于500，并且其中所述纳米原纤维具有5与50纳米之间的直径和大于5μm的长度。
3.如权利要求1或2中所要求保护的流体，其中所述NFC是具有基于干物质计至多20重量%的木质素含量的纳米原纤化木质纤维素。
4.如权利要求3中所要求保护的流体，其中所述NFC是具有基于干物质计至多10重量%的木质素含量的纳米原纤化木质纤维素。

Claims (4)

1.用于钻井液、压裂液、隔离液等的纳米原纤化纤维素(NFC)，其中所述流体包含具有大于100的长径比的NFC作为增粘剂，并且其中所述纳米原纤维具有5与100纳米之间的直径和大于1μm的长度。
2.如权利要求1中所要求保护的纳米原纤化纤维素，其中所述长径比大于500，并且其中所述纳米原纤维具有5与50纳米之间的直径和大于5μm的长度。
3.如权利要求1或2中所要求保护的纳米原纤化纤维素，其中所述NFC是具有基于干物质计至多20重量%的木质素含量的纳米原纤化木质纤维素。
4.如权利要求3中所要求保护的纳米原纤化纤维素，其中所述NFC是具有基于干物质计至多10重量%的木质素含量的纳米原纤化木质纤维素。
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