CN104136381B - 用于游离氧的还原和水的保存的液体制剂 - Google Patents
用于游离氧的还原和水的保存的液体制剂 Download PDFInfo
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- CN104136381B CN104136381B CN201380011214.2A CN201380011214A CN104136381B CN 104136381 B CN104136381 B CN 104136381B CN 201380011214 A CN201380011214 A CN 201380011214A CN 104136381 B CN104136381 B CN 104136381B
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Abstract
本发明涉及一种制剂,所述制剂包含a)至少一种N‑缩甲醛和b)至少一种二烷基羟胺。该制剂优选配制成浓缩物。本发明进一步涉及制剂(特别是浓缩物的形式)在游离氧的还原和水的保存中的用途,以及相应的有添加剂水。N‑缩甲醛与二烷基羟胺的混合物不仅显著相容,而且相当地改进二烷基羟胺作为除氧剂的活性。
Description
本发明涉及用于游离氧的还原和水的保存的液体制剂。该制剂优选配制成浓缩物。本发明进一步涉及制剂(特别是浓缩物的形式)在游离氧的还原和水的保存中的用途,以及相应的有添加剂水。
在天然气和油田开发及其开采中,除化学腐蚀外,微生物腐蚀起到不可低估的作用。另外,微生物的过度生长是个问题。形成粘质物的细菌可阻塞管道。其它微生物可引起腐蚀(硫酸产生)。硫酸盐还原有机体产生干涉硫化氢。另外,可形成非常难以再次除去的生物膜。可侵染整个油田。因此,微生物可导致巨大的经济损害。为抑制微生物腐蚀,使用杀生物剂,例如季铵化合物(quats)、戊二醛(GDA)、丙烯醛、异噻唑啉酮、四(羟甲基)硫酸(THPS)以及二溴次氮基丙酰胺(DBNPA)。
在化学腐蚀中,溶于水中的氧主要起重要作用。取决于温度和盐含量,至多约10ppm O2溶于水中。在8ppm的氧含量下,腐蚀速率已比无氧水高25倍。
因此,在管道和压力容器的安装和修补中,通常用水测试系统中对较高压力的抗性(其称为水压试验)。当这进行时,通常取出现场可得到的水,在钻井平台的情况下盐水,在其它管道中还有来自河和湖的水。该水通常具有特定微生物数和至多约10ppm的溶解氧含量。
迫入油田中的水(称为注射水)(以便然后将水和原油的混合物输送至表面上)引起其它问题。该水通常为淡水和在输送并与原油分离以后强制回到油田中的水的混合物。该水混合物还包含微生物和溶解氧。
还必须充分地保护气和油开采中用于稳定钻孔和管道直至常规开采开始的流体(称为完井液)、在中断至操作期间用于相同目的的流体(称为修井液)以及用于电力传输的水基水力流体以防腐蚀和微生物侵染。
在管道中除去溶解氧以及保存水的必要性是油和气开采工业中长期已知的。这些应用中最常用的除氧剂为亚硫酸钠、亚硫酸氢铵和二氧化硫。由于致癌性能,仅罕见地使用高反应性腈。受限程度地使用在较高的温度下是非常活性的化合物,例如碳酰肼(1,3-二氨基脲)、氢醌、异抗坏血酸盐、二乙基羟胺(DEHA)以及甲乙酮肟(丁肟)。
然而,上述杀生物剂中的许多与水压试验中所用的除氧剂不相容。因此,厂商建议除氧剂不与其它化学品一起使用,因为活性可能完全损失。
另外,大量杀生物剂如戊二醛、丙烯醛、异噻唑啉酮、DBNPA等不能配制成稳定的、可储存的碱性浓缩物,因为杀生物剂在碱性环境中是不稳定的。
因此,首先必须使水不含碱性pH范围内的溶解氧,然后保存。用于除去溶解氧的操作和随后消除微生物的这一分离是耗时且昂贵的,且分离脱气水不总是毫无问题的。另外,由于必须首先除去溶解氧且除氧剂过量使用,所用杀生物剂的量必须使得过量除氧剂可完全反应并存在仍充分活性量的杀生物剂。
N-缩甲醛和二乙基羟胺的使用由其它申请中已知。
WO 2011/000794 A1和WO 2010/142790 A1涉及用吸附到载体材料上的1-氮杂环丙烷化合物稳定化的涂料。作为其它任选组分,描述了甲醛释放化合物如双唑烷和羟胺如二乙基羟胺。
WO 2004/050733 A2公开了苯酚树脂。描述的固化剂为唑烷和羟胺。
GB 2 354 771 A公开了清净剂中的杀菌组合。在活性杀菌化合物的广泛列表(BPD列表)中,尤其列出了二乙基羟胺和3,3'-亚甲基双-5-甲基唑烷。
US 2011/0180759 A1描述了用于降低包含生物乙醇的钢运输和储存容器中的应力腐蚀裂化的方法和组合物。该组合物包含除氧剂和成膜添加剂的组合。除氧剂的一个实例为二乙基羟胺。成膜添加剂的一个实例为二异丙醇胺。
WO 2004/029119 A1描述了将酚醛树脂固化的方法。合适的添加剂为甲醛缓释化合物如唑烷。合适的任选聚合抑制剂为例如N-丙基羟胺和二乙基羟胺。
EP 0 902 017 A1描述了可聚合单体的酯交换方法。适于酯交换的一种醇为羟乙基唑烷。聚合抑制剂的一个实例为二乙基羟胺。
本发明的目的是提供用于将水(特别是用于水压试验和作为注射水的水)中的游离氧还原和保存该水的制剂。
该试剂甚至作为浓缩物应是稳定且容易计量加入的。
现在惊讶地发现这些目的和其它目的通过液体制剂实现,所述液体制剂包含:
a)至少一种N-缩甲醛,和
b)至少一种式RR'NOH的二烷基羟胺,其中R和R'独立地选自线性、支化和环状C1-C10烷基。
液体制剂用于同时游离氧的还原和水的保存,特别是盐水的保存。此外,对于恒定杀生物活性,除氧剂的活性显著提高而不在使用以前进一步添加。
本发明尤其基于这一事实:发现将N-缩甲醛与二烷基羟胺混合不仅显著相容,而且二烷基羟胺的活性通过甲醛释放剂相当地改进。二烷基羟胺的活性也通过pH升高而显著提高。该协同活性不仅在自来水中,而且在氯化钠在自来水中的3%溶液中是明显的。
发明详述
a)N-缩甲醛
本发明制剂包含至少一种N-缩甲醛。这些杀微生物活性成分的优点公开在尤其是DE 103 40 830 A1和DE 10 2009 033 161 A1中。特别合适的N-缩甲醛为具有摩尔甲醛过量的甲醛和胺(优选链烷醇胺)的反应产物。优选低水甲醛缓释化合物,其在水中以碱性方式反应。
N-缩甲醛的实例为摩尔比3:2的低聚甲醛和异丙醇胺的缩合物,摩尔比3:2的仲甲醛和异丙醇胺以及脲的缩合物,和摩尔比3:2的仲甲醛和异丙醇胺以及脲和乙二醇的缩合物。
根据本发明优选使用的N-缩甲醛为N,N’-亚甲基双(5-甲基唑烷)、α,α',α″-三甲基-1,3,5-三嗪-1,3,5-(2H,4H,6H)三乙醇、4,4-二甲基唑烷、二羟甲基脲、5-乙基-3,7-二氧杂-1-氮杂二环[3.3.0]辛烷、2-(羟基甲基氨基)乙醇、亚甲基双四氢-1,3-双嗪、N-羟甲基氯乙酰胺、双(羟甲基)-5,5-二甲基乙内酰脲、二偶氮烷基脲、羟甲基甘氨酸钠、3,4,4-三甲基唑烷、2,2',2″-(六氢-1,3,5-三嗪-1,3,5-三基)三乙醇和四氢-1,3,4,6-四(羟甲基)咪唑[4,5-d]咪唑-2,5-(1H,3H)二酮。
特别优选作为甲醛缓释化合物的是3,3'-亚甲基双(5-甲基唑烷)、2,2',2″-(六氢-1,3,5-三嗪-1,3,5-三基)-三乙醇、α,α',α″-三甲基-1,3,5-三嗪-1,3,5-(2H,4H,6H)三乙醇、四氢-1,3,4,6-四(羟甲基)咪唑[4,5-d]咪唑-2,5-(1H,3H)二酮、二羟甲基脲以及产品OF(亚甲基双(5-甲基唑烷)+脲)和OK(亚甲基双(5-甲基唑烷)+脲+乙二醇)。
非常特别优选作为甲醛缓释化合物的是3,3'-亚甲基双(5-甲基唑烷)。
b)二烷基羟胺
本发明制剂包含至少一种式RR'NOH的二烷基羟胺,其中R和R'相互独立地选自线性、支化和环状C1-C10烷基。R和R'的实例相互独立地为甲基、乙基、丙基、丁基、戊基、己基、辛基和癸基。特别优选作为组分b)的是二乙基羟胺(DEHA)。
在根据本发明优选的组合物中,组分a)与组分b)的重量比通常为30:1-1:5,优选25:1-1:1,特别是20:1-3:1,例如9:1。
c)抗氧化剂
本发明制剂进一步优选包含c)至少一种抗氧化剂。优选的抗氧化剂在室温下是液体或者充分可溶于甲醛缓释化合物中。抗氧化剂的实例选自位阻酚、胺、维生素E及其衍生物,和没食子酸的烷基酯,优选3-叔丁基-4-羟基茴香醚(BHA)、2,6-二-叔丁基-对-甲酚(BHT)、2,6-二-叔丁基苯酚、没食子酸月桂酯和维生素E。
特别地,优选2,6-二-叔丁基苯酚和BHT作为抗氧化剂。
d)碱化剂
另外,本发明制剂优选包含d)至少一种碱化剂,所述碱化剂具有在即用稀释(有添加剂水)中,保持足够的碱性pH的效果,这对除氧剂的短时间活性而言是特别有利的。碱化剂的实例为胺或链烷醇胺,例如异丙醇胺、丙醇胺、单乙醇胺、二乙醇胺、三乙醇胺、氨基甲基丙醇和氨基丁醇。
所提到的碱化剂提高除氧剂的活性,并且应当能够提高即用浓度下有添加剂水的pH。合适的碱化剂为在组分a)和b)的本发明混合物中是稳定的且容易溶于水中的所有物质。
可选碱化剂为无机化合物,例如碱金属氢氧化物或碱金属盐,例如KOH、NaOH、碳酸钠、钾或钠水玻璃、胺或链烷醇胺如乙醇胺、异丙醇胺、脂肪胺、中链胺或链烷醇胺如二异丙醇胺、羟胺和氢氧化铵。优选的碱化剂为乙醇胺、异丙醇胺、NaOH、KOH、水玻璃、羟胺和氢氧化铵。
另外,优选的制剂进一步包含e)稳定剂、活化剂、腐蚀抑制剂、积垢抑制剂、络合剂、杀真菌剂、杀藻剂、消泡剂、冷稳定剂、溶剂和助促进剂中的至少一种。
可与本发明制剂组合的其它功能添加剂的实例为:
-稳定剂,例如脲,二醇如乙二醇、丙二醇;
-催化剂,例如氧化还原催化剂如Cu、Co、Mn、Ni和Fe的盐,氢醌(特别是在低使用温度下,催化剂的使用可能是有利的);
-溶剂,例如醇、二醇、二醇醚、烃、燃料和
-已知的可选除氧剂,例如丙醇二酸或者丙醇二酸衍生物或盐,亚硫酸盐、肼、二羟基丙酮、碳酰肼、氢醌、异抗坏血酸盐、甲乙酮肟以及没食子酸盐。
另外,也可存在其它抗微生物活性成分。可存在于本发明组合物中的其它抗微生物活性成分的实例为醛如GDA、甲醛缓释化合物如乙二醇双半缩甲醛(ethylene glycolbishemiformal)、THPS、有机卤化合物如DBNPA、季铵盐如苯扎氯铵、胺如Lonzabac 12、苯酚、异噻唑酮如MI、CMI、OIT、DCOIT、BIT、n-Bu-BIT和Bunte盐。
本发明制剂可与其它杀生物活性成分、官能添加剂和辅助剂组合,如例如WO2009/060057 A2、DE 10 2006 035013 A1或DE 103 40 830 A1中所公开的。
如下文所解释,本发明制剂通常配制成液体浓缩物。
液体浓缩物
在配制成液体浓缩物的本发明制剂中,组分a)的含量优选为至少30重量%,更优选至少35重量%,特别是至少40重量%,例如至少45重量%,例如约50重量%。组分b)的含量通常为至少0.25重量%,优选至少1重量%,特别是至少2重量%,例如5重量%。特别优选由组分a)、b)以及任选c)和/或d)组成的液体浓缩物,即另外不包含其它组分。
优选浓缩物包含0.0001-10重量%,更优选0.001-1重量%,特别优选0.002-0.1重量%,例如0.02重量%的抗氧化剂c)。
当存在碱化剂d)时,液体浓缩物包含优选至少20重量%,更优选至少30重量%,特别是至少40重量%,例如至少45重量%组分d),例如约50重量%的组分d)。
本发明浓缩物优选包含至多30重量%水,更优选至多20重量%水,特别优选至多12重量%水,特别是至多5重量%水,例如少于1.0重量%水。
特别优选的液体浓缩物由如下组分组成:
a)约45重量%的3,3'-亚甲基双(5-甲基唑烷),
b)约5重量%的DEHA和
d)约50重量%的碱化剂。
液体浓缩物通过装入组分a)(例如3,3'-亚甲基双(5-甲基唑烷)),然后随着搅拌将组分b)如DEHA溶解而制备。
本发明液体浓缩物以基于活性成分a)和b)以及任选c)和d)而不具有溶剂或稀释剂的总量为100-2000mg/l(ppm),优选200-1000ppm的浓度预防性地使用。
本发明进一步涉及本发明制剂在将水中的游离氧还原同时保存水的用途。水可以为在油气开采中用于稳定钻孔和管道直至常规萃取开始的流体(称为完井液)、在中断至操作期间用于相同目的的流体(称为油修井液)以及用于电力输送的水基水力流体。
本发明制剂(特别是浓缩物)的其它应用是工艺水、含水体系、工业水、海水、盐水、钻井液、热水、注射水、废水(例如工业废水、来自农业、来自原油或天然气开采的废水)、传输和储存流体(例如矿物、煤、燃料)、加热用水、含水和/或碱性洗涤液、循环水、除气并任选填充惰性气体的水和冷凝水的游离氧还原和保存。
组分a)、b)以及任选c)和/或d)—以及当存在时,e)—根据本发明以有效地将游离氧还原并保存水的量用于水中。
组分a)、b)以及任选c)的组合优选通过加入流体浓缩物而用于水中。作为选择,可单独地加入组分a)、b)以及任选c),但该选择方案不是优选的。
另外,本发明涉及包含组分a)和b)(以及任选c)和/或d),和当存在时e))的有添加剂水。
本发明液体制剂(特别是液体浓缩物)在这种情况下提供以下优点:
-具有活性协同提高的多功能活性,
-提供稳定的液体浓缩物,
-用单阶段方法取代2阶段或多阶段方法,
-生物活性、除氧剂活性、防腐蚀、稳定剂功能和碱化剂的组合,
-通过加入N-缩甲醛改进DEHA的除氧剂活性,
-组分非常好的相容性,
-冷稳定的液体,低水,可水溶混,
-良好的热稳定性,
-作为浓缩物和在即用稀释时的良好稳定性,和
-在较高工艺温度、高盐含量和较高压力下的良好稳定性。
本发明的优点特别从下文的实施例中显现。除非另外说明,所有百分数涉及重量。
实施例
用于实施例中的所选择N-缩甲醛的组成。
N-缩甲醛BK
摩尔比3:3的乙醇胺和甲醛(91%)的反应产物。这形成N,N’,N″-三(2-羟乙基)六氢三嗪。反应水和来自甲醛的水保留在产物中。
N-缩甲醛WS:
摩尔比3:3的异丙醇胺和甲醛(91%)的反应产物。这形成N,N',N″-三-(2-羟丙基)六氢三嗪。反应水和来自甲醛的水保留在产物中。
N-缩甲醛OX:
摩尔比2:3的异丙醇胺和甲醛(91%)的反应产物。这形成3,3'-亚甲基双(5-甲基唑烷)。将反应水和来自甲醛的水蒸馏掉。
N-缩甲醛OF:
摩尔比2:3的异丙醇胺和甲醛(91%)的反应产物。这形成3,3'-亚甲基双(5-甲基唑烷)。将反应水和来自甲醛的水蒸馏掉。加入脲以将游离甲醛还原(混合物包含约4%脲)。
N-缩甲醛OK:
摩尔比2:3的异丙醇胺和甲醛(91%)的反应产物。这形成3,3'-亚甲基双(5-甲基唑烷)。将反应水和来自甲醛的水蒸馏掉。加入脲和乙二醇以将游离甲醛还原和减少胺气味(混合物包含约4.6%脲和约9.5%乙二醇)。
GDA:
戊二醛(可作为至多50浓度水溶液得到),目前是这些应用中最多使用的杀生物剂的一种。
缩甲醛TK 5:
包含摩尔比1:2的乙二醇和低聚甲醛(91%)的反应产物作为杀生物剂。作为稳定组分,进一步存在脲。反应水和来自低聚甲醛的水保留在产物中。
在下文的实施例中,研究水中的氧还原。
设备名称:来自WTW的具有光学氧传感器FDO 925的Multi 3320 Set B。
程序:
对于实验1-4,每种情况下将新鲜自来水(Norderstedt市政用水)以一定量从水管中取出使得对一系列试验中的每个试验而言水量是相同的。在加入所述物质以后,搅拌混合物直至溶液变得清澈。每种情况下构成~100ml。
将氧传感器浸入该溶液中并搅拌直至指定的氧含量保持恒定(约1-2分钟)。在测量以后,使试样静止并在3小时以后重复测量。
如关于实验1的表所示,自来水包含6.4mg/l氧气。在使试样在室温下静止3小时以后,一些氧气再次溶解,并显示出7.2mg/l O2的含量(A)。
在加入50ppm二乙基羟胺以后,氧含量降至1.5mg/l(在静止3小时以后,0.8mg/l)。C的混合物包含50ppm二乙基羟胺和450ppm N-缩甲醛OX。氧气还原更快地进行且残余氧气小于实验B的。与在自来水中具有500ppm N-缩甲醛OX的实验D对比显示单独的缩甲醛对氧含量不具有影响。
实验E-H的结果显示在包含3%氯化钠的自来水中的相同实验以显示N-缩甲醛与10%二乙基羟胺的混合物也与海水一起作用。实验E-H甚至显示与A-D相比混合物对氧气还原仍更大的影响。
I和J的实验显示出丁酮肟不起作用。测试除氧剂丁肟,因为也可由此配制具有N-缩甲醛OX的稳定混合物。由此的结果是不是所有已知的除氧剂在与N-缩甲醛组合时证明令人惊讶的影响,如根据本发明实现的。
关于实验2的表显示各种甲醛缓释化合物与二乙基羟胺(DEHA)的混合物的氧气还原活性。实验1-10在自来水中进行,实验11-20在包含3%氯化钠的自来水中进行。DEHA的活性显示与N-缩甲醛OX和N-缩甲醛WS组合的最好结果。
实验3显示随着加入碱化剂(异丙醇胺)的氧气还原。此处,N-缩甲醛OX的混合物的活性也稍微比单独或与其它缩甲醛或戊二醛(GDA)一起的二乙基羟胺(DEHA)更好。如在实验5中也可以看出,戊二醛与DEHA的组合不能以稳定的方式配制成与异丙醇胺的浓缩物。
程序:取出一份新鲜市政用水(使其运行短时间)。将具有在自来水中的3%氯化钠和在自来水中的具有300ppm异丙醇胺的3%氯化钠使用冰浴冷却至约4℃。
在+4℃下进行以模拟在较冷水中开采油的真实实验条件的实验4中,也证明了用N-缩甲醛与二乙基羟胺的混合物的良好结果。
实验5显示N-缩甲醛对戊二醛(不具有以及具有异丙醇胺)的良好稳定性。GDA和DEHA的浓度在加入异丙醇胺以后是不稳定的。不用异丙醇胺,甚至在25℃下储存2个月以后,几乎一半的所用戊二醛,以及在40℃下储存2个月以后,2/3的所用戊二醛不再存在。
Claims (19)
1.液体配制剂,其包含:
a)至少一种N-缩甲醛,其选自N,N'-亚甲基双(5-甲基唑烷)、α,α',α"-三甲基-1,3,5-三嗪-1,3,5-(2H,4H,6H)三乙醇、4,4-二甲基唑烷、二羟甲基脲、5-乙基-3,7-二氧杂-1-氮杂二环[3.3.0]辛烷、2-(羟基甲基氨基)乙醇、亚甲基双四氢-1,3-双嗪、N-羟甲基氯乙酰胺、双(羟甲基)-5,5-二甲基乙内酰脲、二偶氮烷基脲、羟甲基甘氨酸钠、3,4,4-三甲基唑烷、2,2',2”-(六氢-1,3,5-三嗪-1,3,5-三基)三乙醇和四氢-1,3,4,6-四(羟甲基)咪唑[4,5-d]咪唑-2,5-(1H,3H)二酮,和
b)至少一种式RR'NOH的二烷基羟胺,其中R和R'独立地选自线性、支化和环状C1-C10烷基。
2.根据权利要求1的制剂,其特征在于N-缩甲醛为N,N'-亚甲基双(5-甲基唑烷)。
3.根据权利要求1的制剂,其特征在于二烷基羟胺为二乙基羟胺。
4.根据权利要求1的制剂,其特征在于它还包含c)至少一种抗氧化剂,所述抗氧化剂选自3-叔丁基-4-羟基茴香醚(BHA)、2,6-二-叔丁基-对-甲酚(BHT)、2,6-二-叔丁基苯酚、没食子酸月桂酯和维生素E。
5.根据权利要求2的制剂,其特征在于它还包含c)至少一种抗氧化剂,所述抗氧化剂选自3-叔丁基-4-羟基茴香醚(BHA)、2,6-二-叔丁基-对-甲酚(BHT)、2,6-二-叔丁基苯酚、没食子酸月桂酯和维生素E。
6.根据权利要求1-5中任一项的制剂,其特征在于它还包含d)至少一种碱化剂。
7.根据权利要求1-5中任一项的制剂,其特征在于它还包含e)稳定剂、活化剂、腐蚀抑制剂、积垢抑制剂、络合剂、杀真菌剂、杀藻剂、消泡剂、溶剂和助促进剂中的至少一种。
8.根据权利要求6的制剂,其特征在于它还包含e)稳定剂、活化剂、腐蚀抑制剂、积垢抑制剂、络合剂、杀真菌剂、杀藻剂、消泡剂、溶剂和助促进剂中的至少一种。
9.根据权利要求1-5和8中任一项的制剂,其特征在于组分a)与组分b)的重量比为30:1-1:5。
10.根据权利要求1-5和8中任一项的制剂,其特征在于它作为浓缩物存在,且组分a)的含量为至少30重量%。
11.根据权利要求9的制剂,其特征在于它作为浓缩物存在,且组分a)的含量为至少30重量%。
12.根据权利要求10的制剂,其特征在于碱化剂d)的量为至少20重量%。
13.根据权利要求11的制剂,其特征在于碱化剂d)的量为至少20重量%。
14.根据权利要求1-5、8、11-13中任一项的制剂,其特征在于它作为浓缩物存在且组分b)的含量为至少0.25重量%。
15.根据权利要求10的制剂,其特征在于浓缩物中水的量为至多30重量%。
16.根据权利要求11-13中任一项的制剂,其特征在于浓缩物中水的量为至多30重量%。
17.根据权利要求14的制剂,其特征在于浓缩物中水的量为至多30重量%。
18.根据权利要求1-5、8、11-13、15和17中任一项的制剂,在将水中的游离氧还原和保存水中的用途。
19.根据权利要求14的制剂,在将水中的游离氧还原和保存水中的用途。
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CA2863129A1 (en) | 2013-09-06 |
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