WO2022268087A1 - 一种抗高温二氧化硅接枝叔胺纳米封堵剂及水基钻井液 - Google Patents

一种抗高温二氧化硅接枝叔胺纳米封堵剂及水基钻井液 Download PDF

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WO2022268087A1
WO2022268087A1 PCT/CN2022/100217 CN2022100217W WO2022268087A1 WO 2022268087 A1 WO2022268087 A1 WO 2022268087A1 CN 2022100217 W CN2022100217 W CN 2022100217W WO 2022268087 A1 WO2022268087 A1 WO 2022268087A1
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parts
weight
tertiary amine
nano
drilling fluid
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French (fr)
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谢刚
汪若兰
黄进军
白杨
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西南石油大学
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Definitions

  • the invention relates to the technical field of oil and gas field drilling, in particular to a high-temperature resistant silicon dioxide grafted tertiary amine nano-sealing agent and water-based drilling fluid.
  • the particle size of sulfonated asphalt or emulsified asphalt commonly used in drilling fluids is mostly at the micron level, which can effectively seal micro-cracks at the micron level.
  • Surface deposits are easily damaged by drilling fluid erosion and collision of drilling tools, and cannot achieve a good plugging effect. Therefore, effective plugging of nano-pores and fractures that are likely to cause wellbore instability is the focus of maintaining wellbore stability, and it is also a difficult point that needs to be solved urgently in drilling engineering.
  • the present invention provides a high-temperature-resistant silica-grafted tertiary amine nano-sealing agent with a particle size of Nano-scale, can effectively seal nano-scale fractures in shale formations, so as to achieve the purpose of stabilizing the well wall.
  • a new type of nano-blocking water-based drilling fluid suitable for shale formations has been developed to replace oil-based drilling fluids, which can solve problems such as wellbore stability and reservoir pollution.
  • the technical solution of the present invention is: a high temperature resistant silica grafted tertiary amine nano-blocking agent, the plugging agent is prepared by mixing tertiary amine-modified silica and water.
  • the high-temperature resistant silicon dioxide grafted tertiary amine nano-blocking agent uses hydrazine compounds, diallyl compounds, enamine compounds, silicon dioxide (10-20nm), and amino-containing silane coupling agents as raw materials , synthesized by the following steps:
  • the amino group-containing silane coupling agent is one of 3-aminopropyltriethoxysilane (KH550) and 3-aminopropyltrimethoxysilane (KH540).
  • the hydrazine compounds are 2-hydroxybenzoylhydrazide, 3-hydroxybenzohydrazide, 4-hydroxybenzohydrazide, 4-hydroxyphenylacetohydrazide, 2,4-dihydroxybenzohydrazide, 3,4 -Dihydroxyphenylhydrazide, a kind of 3,5-dihydroxybenzohydrazide.
  • the diallyl compound containing ethylenic bonds is one of 1,5-hexadiene, diallylamine and N-methyldiallylamine.
  • the enamine compound is one of N-methyl-N-vinylacetamide, N,N-diethyl-2-acrylamide, N-vinyl-N-methyl-2-acrylamide .
  • Another object of the present invention is to provide a water-based drilling fluid, which is added with the high-temperature resistant silica-grafted tertiary amine nano-sealing agent of the present invention.
  • the composition of the drilling fluid is as follows: the water-based drilling fluid according to claim 5, wherein the drilling fluid comprises the following components: 100 parts by weight of water+2-4 parts by weight of bentonite +0.1-0.3 parts by weight NaOH+0.01-0.03 parts by weight KPAM+0.3-0.8 parts by weight PAC-LV+4-6 parts by weight RSTF+5-6 parts by weight SMP-1+3-5 parts by weight FRH+1-2 Parts by weight of PPL+4-5 parts by weight of FK-10+0.3-0.5 parts by weight of SP-80+1-5 parts by weight of high temperature resistant silica grafted tertiary amine nano-blocking agent+1-1.5 parts by weight of desulfurizer+0.3- 0.5 parts by weight of CaO+5-20 parts by weight of barite.
  • the drilling fluid comprises the following components: 100 parts by weight of water+2-4 parts by weight of bentonite +0.1-0.3 parts by weight NaOH+0.01-0.03 parts by weight KPAM+0.3-0.8 parts by weight PAC-LV+4-6 parts by weight
  • the synthesis method of the present invention is simple, and the compound required for synthesis is cheap and easy to produce.
  • the shale plugging agent provided by the present invention has stable performance and strong adaptability. In addition to high temperature resistance and excellent plugging performance, it also has good suppression performance, and the suppression performance is significantly improved compared with similar products. It can meet the drilling requirements of various complex well conditions.
  • the particle size of the shale plugging agent provided by the present invention is 58-280nm, which can block the nano-pores and cracks in the shale formation, is not easy to agglomerate, can maintain good dispersion, and has excellent plugging rate performance.
  • Fig. 1 is the particle size distribution diagram of high temperature resistant silica grafted tertiary amine nano-blocking agent in embodiment one;
  • Fig. 2 is the particle size distribution diagram of high temperature resistant silicon dioxide grafted tertiary amine nano-blocking agent in embodiment two;
  • Fig. 3 is the particle size distribution diagram of high temperature resistant silica grafted tertiary amine nano-blocking agent in embodiment three;
  • Fig. 4 is a particle size distribution diagram of the high temperature resistant silica grafted tertiary amine nano-sealing agent in Example 4.
  • the BI-200SM laser scattering instrument produced by Brookhaven Instruments in the United States was used to test the particle size of the anti-high temperature silica grafted tertiary amine nano-blocking agent.
  • the high temperature resistant silica grafted tertiary amine prepared in the four examples The particle size test results of the nano-blocking agent are shown in Figure 1, Figure 2, Figure 3 and Figure 4, respectively.
  • the high-temperature resistant silicon dioxide grafted tertiary amine nano-blocking agent of the invention has a particle size range of 58-280 nm and can be used for nano-blocking.
  • the present invention is mainly described in the application mode of the anti-high temperature silica grafted tertiary amine nano-blocking agent with the following specific formula. Based on 100 parts by weight of fresh water, the present embodiment illustrates the formula of water-based drilling fluid by the following method.
  • water-based drilling fluid is as follows: 100 parts by weight of water+3 parts by weight of bentonite+0.2 parts by weight of NaOH+0.02 parts by weight of KPAM +0.4 parts by weight PAC-LV+5 parts by weight RSTF+5 parts by weight SMP-1+5 parts by weight FRH+1 parts by weight PPL+4 parts by weight FK-10+0.4 parts by weight SP-80+1.2 parts by weight desulfurizer +0.4 parts by weight of CaO+10 parts by weight of barite.
  • drilling fluid 1 Five kinds of drilling fluids with different additions of amine nano-blocking agent are named as drilling fluid 1, drilling fluid 2, drilling fluid 3, drilling fluid 4 and drilling fluid 5, and drilling fluid 1 does not contain high temperature resistant silica graft Tertiary amine nano-blocking agent, as a blank experimental group.
  • AV apparent viscosity
  • PV plastic viscosity
  • YP dynamic shear force
  • API normal temperature medium pressure filtration loss
  • HTHP High temperature and high pressure filtration loss, the unit is mL.
  • the high-temperature and high-pressure filtration loss is the smallest, indicating that the high-temperature-resistant silica grafted tertiary amine nano-blocking agent has good rheological properties and water loss wall-building properties, and can effectively reduce the high-temperature and high-pressure filtration loss of drilling fluid, even in high-temperature environments. It can also provide better plugging performance, effectively prevent the filtrate from entering the formation, and improve the stability of the wellbore wall.
  • the GGS-71 high temperature and high pressure filter uses the GGS-71 high temperature and high pressure filter to prepare a mud cake with a certain size, thickness, and permeability, and use it as a simulated formation for a microfracture formation.
  • the grafted tertiary amine nano plugging agent is subjected to high temperature and high pressure fluid loss experiments to simulate the high temperature and high pressure water loss of the plugging agent in the formation, and the water loss is used to calculate the permeability of the plugging agent to evaluate the plugging agent in the drilling fluid system.
  • the plugging effect is judged by its high-temperature and high-pressure fluid loss.
  • the high-temperature resistant silica-grafted tertiary amine nano-blocking agent has excellent plugging performance
  • the high-temperature-resistant silica-grafted tertiary amine nano-blocking agent has been subjected to high-temperature and high-pressure water loss experiments of mud cakes.
  • the calculated average water loss and mud cake permeability are much smaller than the data obtained by clear water in the mud cake, and with the increase of the amount of anti-high temperature silica grafted tertiary amine nano-sealing agent
  • the blocking agent of the present invention can block nanopores.
  • the preparation method of the silica-grafted tertiary amine nano-blocking agent of the present invention is stable and reliable, the price of the synthetic product is low, and the polymer plugging agent made has plugging properties, rheological properties, water solubility, dispersibility, The adsorption is good, which is greatly improved compared with similar products, and the effect of stabilizing the well wall is excellent.
  • the plugging agent only needs a small amount to achieve excellent plugging effect, and is an effective way to solve the problems of wellbore stability and drilling fluid loss.

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  • Engineering & Computer Science (AREA)
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Abstract

一种抗高温二氧化硅接枝叔胺纳米封堵剂及水基钻井液，属于油气田钻井技术领域，所述抗高温二氧化硅接枝叔胺纳米封堵剂以含羟基的肼类化合物、二烯丙基类化合物、烯胺类化合物、含氨基的硅烷偶联剂为原料，通过改性二氧化硅，用分步合成法合成。本发明提供的抗高温二氧化硅接枝叔胺制成的封堵剂，其粒径在58-280nm之间，封堵性能相比于同类封堵剂性能有显著提升，除了其封堵性能之外，其外部的多个叔胺支链还具有很强的吸附性能和抑制性能，该封堵剂抗高温，可应用于深井、超深井中。该封堵剂还具有，原料易得，价格便宜，其等优点，所提供的合成方法稳定可靠，简单快捷，适用于工业化生产。

Description

一种抗高温二氧化硅接枝叔胺纳米封堵剂及水基钻井液 技术领域
本发明涉及油气田钻井技术领域，具体涉及一种抗高温二氧化硅接枝叔胺纳米封堵剂及水基钻井液。
背景技术
目前在国内和国外钻井中，经常存在井壁不稳定问题，国内外数百口井的统计说明，所钻页岩地层占所钻总地层的70％，而90％以上的井塌发生在页岩地层。页岩具有特殊的孔缝结构，属超低孔、低渗类型，多为纳米级孔喉。针对页岩气的成藏特征，水平井钻井已成为页岩气开发的主要钻井方式。不管使用水基钻井液体系或者油基钻井液体系钻页岩地层都会出现井壁垮塌的现象，其根本原因是“水力劈裂作用”，钻井液或滤液进入裂缝，使裂缝张开，同时大大降低缝面间摩擦力，使坍塌压力大幅度上升。若不能有效封堵住裂缝阻断泥浆液相进入裂缝，则不能防塌。
钻井液中常用的磺化沥青或乳化沥青的粒径大多在微米级别，能对微米级别的微裂缝进行有效封堵，但对于尺寸一般在纳米-微米之间的裂缝，其粒子只能在裂缝表面沉积，极易被钻井液冲刷，钻具的碰撞等作用破坏，起不到良好的封堵效果。因此对易造成井壁失稳的纳米孔缝进行有效的封堵是保持井壁稳定的重点，也是钻井工程中急需解决的难点。
发明内容
针对目前常规封堵剂无法有效封堵泥页岩中的纳米裂缝而导致的井壁失稳问题，本发明提供了一种抗高温二氧化硅接枝叔胺纳米封堵剂，其粒径为纳米级，能够有效对泥页岩地层中的纳米级裂缝进行封堵，从而达到稳定井壁的目的。且研制了一种能适用于页岩地层的新型纳米封堵水基钻井液替代油基钻井液能够解决井壁稳定、储层污染等问题。
为实现上述目的，本发明的技术方案为：一种抗高温二氧化硅接枝叔胺纳米封堵剂，所述封堵剂由叔胺类改性二氧化硅与水混合配制而成。所述抗高温二氧化硅接枝叔胺纳米封堵剂以肼类化合物、二烯丙基类化合物、烯胺类化合物、二氧化硅(10-20nm)、含氨基的硅烷偶联剂为原料，采用如下步骤合成：
S1、在70mL甲苯溶液中加入0.25-0.29mol纳米二氧化硅，升温至50-60℃后搅拌至溶解并通入氮气20-30min，升温至80-90℃边搅拌边加入一定量硅烷偶联剂，使二氧化硅和含氨基的硅烷偶联剂反应5h。减压蒸馏2h得到粗产品，用甲苯洗涤、过滤，除去未反应的单体，真空干燥2h，得到纳米二氧化硅的改性产物。
S2、将上一步制得的纳米二氧化硅的改性产物用90-110mL四氢呋喃溶解，加入0.24-0.29mol二烯丙基类化合物，在50-60℃的条件下搅拌并反应24h，减压蒸馏得到粗产品， 真空干燥2h，取一定量干燥后的粗产品加入到90-110mL四氢呋喃中，快速搅拌至溶解，通入氮气20-30min，保持搅拌和通入氮气，快速将0.48-0.53mol含羟基的肼类化合物加入混合体系，升温至30-40℃，反应8-12h后，减压蒸馏得到仲胺类化聚合物。
S3、将上一步制得的仲胺类聚合物用90-110mL四氢呋喃溶解，加入0.24-0.28mol烯胺类化合物，在60-68℃的条件下搅拌并反应36h，减压蒸馏得到粗产品，将粗产品真空干燥2h，得到含羟基的叔胺型聚合物，将烘干的样品研磨，然后密封保存。
所述的含氨基的硅烷偶联剂为3-氨基丙基三乙氧基硅烷(KH550)，3-氨丙基三甲氧基硅烷(KH540)中的一种。
所述的肼类化合物为2-羟基苯甲酰肼，3-羟基苯酰肼，4-羟基苯甲酰肼，4-羟基苯乙酰肼，2,4-二羟基苯酰肼，3,4-二羟基苯酰肼，3,5-二羟基苯酰肼中的一种。
所述含烯键的二烯丙基类化合物为1,5-已二烯，二烯丙基胺，N-甲基二烯丙基胺中的一种。
所述烯胺类化合物为N-甲基-N-乙烯基乙酰胺，N,N-二乙基-2-丙烯酰胺,N-乙烯基-N-甲基-2-丙烯酰胺中的一种。
本发明的另一种目的是提供一种水基钻井液，所述钻井液添加有本发明所述的一种抗高温二氧化硅接枝叔胺纳米封堵剂。
以重量份计，所述钻井液的组成如下：根据权利要求5所述的水基钻井液，其特征在于，所述钻井液包括以下组分：100重量份的水+2-4重量份膨润土+0.1-0.3重量份NaOH+0.01-0.03重量份KPAM+0.3-0.8重量份PAC-LV+4-6重量份RSTF+5-6重量份SMP-1+3-5重量份FRH+1-2重量份PPL+4-5重量份FK-10+0.3-0.5重量份SP-80+1-5抗高温二氧化硅接枝叔胺纳米封堵剂+1-1.5重量份除硫剂+0.3-0.5重量份CaO+5-20重量份重晶石。
本发明有益效果如下：
1、本发明的合成方法简单，合成所需化合物价格低廉，易于生产。
2、本发明提供的页岩封堵剂性能稳定，适应性强，除了具有抗高温和优异的封堵性能之外还具有很好的抑制性能，且抑制性能相比于同类产品有明显提升，能满足各种复杂井况的钻井要求。
3、本发明提供的页岩封堵剂粒径为58-280nm，可以对页岩地层中的纳米孔缝进行封堵，且不易团聚，可以保持良好的分散性，封堵率性能优异。
附图说明
图1为实施例一中抗高温二氧化硅接枝叔胺纳米封堵剂的粒径分布图；
图2为实施例二中抗高温二氧化硅接枝叔胺纳米封堵剂的粒径分布图；
图3为实施例三中抗高温二氧化硅接枝叔胺纳米封堵剂的粒径分布图；
图4为实施例四中抗高温二氧化硅接枝叔胺纳米封堵剂的粒径分布图。
具体实施方式
下面将结合本发明实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本实施例中，若无特殊说明，所述的份数均为重量份数。
一、抗高温二氧化硅接枝叔胺纳米封堵剂的合成：
实施例1：
(1)二氧化硅的改性
在70mL甲苯溶液中加入0.25mol纳米二氧化硅，升温至60℃后搅拌至溶解并通入氮气30min，升温至90℃边搅拌边加入一定量3-氨基丙基三乙氧基硅烷(KH550)，使二氧化硅和3-氨基丙基三乙氧基硅烷(KH550)反应5h。减压蒸馏2h得到粗产品，用甲苯洗涤、过滤，除去未反应的单体，真空干燥2h，得到纳米二氧化硅的改性产物。
(2)仲胺类聚合物的合成
将上一步制得的纳米二氧化硅的改性产物用110mL四氢呋喃溶解，加入0.24mol 1,5-已二烯，在60℃的条件下搅拌并反应24h，减压蒸馏得到粗产品，真空干燥2h，取一定量干燥后的粗产品加入到110mL四氢呋喃中，快速搅拌至溶解，通入氮气30min，保持搅拌和通入氮气，快速将0.48mol 2-羟基苯甲酰肼加入混合体系，升温至40℃，反应12h后，减压蒸馏得到仲胺类化聚合物。
(3)叔胺类聚合物的合成
将上一步制得的仲胺类聚合物用110mL四氢呋喃溶解，加入0.24mol N-甲基-N-乙烯基乙酰胺，在68℃的条件下搅拌并反应36h，减压蒸馏得到粗产品，将粗产品真空干燥2h，得到含羟基的叔胺型聚合物，将烘干的样品研磨，然后密封保存。
实施例2：
(1)二氧化硅的改性
在70mL甲苯溶液入0.25mol纳米二氧化硅，升温至60℃后搅拌至溶解并通入氮气30min，升温至90℃边搅拌边加入一定量3-氨基丙基三乙氧基硅烷(KH540)，使二氧化硅和3-氨基丙基三乙氧基硅烷(KH540)反应5h。减压蒸馏2h得到粗产品，用甲苯洗涤、过滤，除去未反应的单体，真空干燥2h，得到纳米二氧化硅的改性产物。
(2)仲胺类聚合物的合成
将上一步制得的纳米二氧化硅的改性产物用110mL四氢呋喃溶解，加入0.24mol二烯丙基胺，在60℃的条件下搅拌并反应24h，减压蒸馏得到粗产品，真空干燥2h，取一定量干燥后的粗产品加入到110mL四氢呋喃中，快速搅拌至溶解，通入氮气30min，保持搅拌和通入氮气，快速将0.48mol 3-羟基苯酸肼加入混合体系，升温至40℃，反应12h后，减压蒸馏得到仲胺类化聚合物。
(3)叔胺类聚合物的合成
将上一步制得的仲胺类聚合物用110mL四氢呋喃溶解，加入0.24mol N,N-二乙基-2-丙烯酰胺，在68℃的条件下搅拌并反应36h，减压蒸馏得到粗产品，将粗产品真空干燥2h，得到含羟基的叔胺型聚合物，将烘干的样品研磨，然后密封保存。
实施例3：
(1)二氧化硅的改性
在70mL甲苯溶液中加入0.25mol纳米二氧化硅，升温至60℃后搅拌至溶解并通入氮气30min，升温至90℃边搅拌边加入一定量3-氨基丙基三乙氧基硅烷(KH550)，使二氧化硅和3-氨基丙基三乙氧基硅烷(KH550)反应5h。减压蒸馏2h得到粗产品，用甲苯洗涤、过滤，除去未反应的单体，真空干燥2h，得到纳米二氧化硅的改性产物。
将上一步制得的纳米二氧化硅的改性产物用110mL四氢呋喃溶解，加入0.24mol N-甲基二烯丙基胺，在60℃的条件下搅拌并反应24h，减压蒸馏得到粗产品，真空干燥2h，取一定量干燥后的粗产品加入到110mL四氢呋喃中，快速搅拌至溶解，通入氮气30min，保持搅拌和通入氮气，快速将0.48mol 4-羟基苯甲酰肼加入混合体系，升温至40℃，反应12h后，减压蒸馏得到仲胺类化聚合物。
(3)叔胺类聚合物的合成
将上一步制得的仲胺类聚合物用110mL四氢呋喃溶解，加入0.24mol N-乙烯基-N-甲基-2-丙烯酰胺，在68℃的条件下搅拌并反应36h，减压蒸馏得到粗产品，将粗产品真空干燥2h，得到含羟基的叔胺型聚合物，将烘干的样品研磨，然后密封保存。
实施例4：
(1)二氧化硅的改性
在70mL甲苯溶液中加入0.25mol纳米二氧化硅，升温至60℃后搅拌至溶解并通入氮气30min，升温至90℃边搅拌边加入一定量3-氨基丙基三乙氧基硅烷(KH540)，使二氧化硅和3-氨基丙基三乙氧基硅烷(KH540)反应5h。减压蒸馏2h得到粗产品，用甲苯洗涤、过滤，除去未反应的单体，真空干燥2h，得到纳米二氧化硅的改性产物。
将上一步制得的纳米二氧化硅的改性产物用110mL四氢呋喃溶解，加入0.240.29mol N-甲基二烯丙基胺，在60℃的条件下搅拌并反应24h，减压蒸馏得到粗产品，真空干燥2h，取一定量干燥后的粗产品加入到110mL四氢呋喃中，快速搅拌至溶解，通入氮气30min，保持搅拌和通入氮气，快速将0.48mol 3,5-二羟基苯酰肼加入混合体系，升温至40℃，反应12h后，减压蒸馏得到仲胺类化聚合物。
(3)叔胺类聚合物的合成
将上一步制得的仲胺类聚合物用110mL四氢呋喃溶解，加入0.24mol N-甲基-N-乙烯基乙酰胺，在68℃的条件下搅拌并反应36h，减压蒸馏得到粗产品，将粗产品真空干燥2h，得到含羟基的叔胺型聚合物，将烘干的样品研磨，然后密封保存。
为了进一步说明本发明环保型封堵剂的效果，对实施例1、实施例2、实施例3和实施例4中的封堵剂进行性能测试。
二、性能测试
1、抗高温二氧化硅接枝叔胺纳米封堵剂粒径测试
利用美国布鲁克海文仪器公司生产的BI-200SM型激光散射仪对抗高温二氧化硅接枝叔胺纳米封堵剂进行粒径测试，四个实施例中制备的抗高温二氧化硅接枝叔胺纳米封堵剂粒径测试结果分别如图1、图2、图3和图4所示。本发明一种抗高温二氧化硅接枝叔胺纳米封堵剂的粒径范围在58-280nm之间，可用于纳米封堵。
2.钻井液流变性能和失水造壁性能测试
本发明主要以以下具体配方对抗高温二氧化硅接枝叔胺纳米封堵剂的应用方式进行说明。以100重量份淡水为基准，本实施例通过以下方法对水基钻井液配方进行说明，具体水基钻井液配方如下∶100重量份水+3重量份膨润土+0.2重量份NaOH+0.02重量份KPAM+0.4重量份PAC-LV+5重量份RSTF+5重量份SMP-1+5重量份FRH+1重量份PPL+4重量份FK-10+0.4重量份SP-80+1.2重量份除硫剂+0.4重量份CaO+10重量份重晶石。
具体配制过程如下∶
(1)、预水化膨润土浆
在100质量份温度为70℃的自来水中加入3质量份的膨润土，在室温下搅拌均匀后加入0.2重量份的NaOH，充分搅拌30min后，密封静置水化24h。
(2)、钻井液的配制
分别取400mL预水化土膨润土浆4份，再依次加入0.02重量份KPAM，0.4重量份PAC-LV，5重量份RSTF，5重量份SMP-1，5重量份FRH，1重量份PPL，4重量份FK-10，0.4重量份SP-80，1.2重量份除硫剂，0.4重量份CaO，10-20重量份重晶石调节密度至1.81g/cm 3。每加 入一种物质，需搅拌10～15min。
搅拌均匀后，分别向4份膨润土浆中加入0、4g、8g、12g、16g上述方式制备的抗高温二氧化硅接枝叔胺纳米封堵剂，制得含抗高温二氧化硅接枝叔胺纳米封堵剂添加量不同的五种钻井液，分别命名为钻井液1、钻井液2、钻井液3、钻井液4和钻井液5，其中钻井液1不含抗高温二氧化硅接枝叔胺纳米封堵剂，作为空白实验组。
依据中华人民共和国国家标准GB/T 16783.1-2014《石油天然气工业钻井液现场测试第1部分∶水基钻井液》，分别对步骤配制好的钻井液进行老化前后钻井液流变性和失水造壁性进行测试，结果记录在表1中。
表1钻井液流变性能及滤失性能记录表
Figure PCTCN2022100217-appb-000001
注∶AV—表观黏度，单位为mPa·s；PV—塑性黏度，单位为mPa·s；YP—动切力，单位为Pa；API—常温中压滤失量，单位为mL；HTHP—高温高压滤失量，单位为mL。
由表1所示的结果可以看出，与不加抗高温二氧化硅接枝叔胺纳米封堵剂的钻井液相比，当抗高温二氧化硅接枝叔胺纳米封堵剂在钻井液中加量为4-16g质量份时，钻井液性能未受到明显的影响，表明该钻井液封堵剂具有良好的配伍性能。随着抗高温二氧化硅接枝叔胺纳米封堵剂加量的增加，在同一实验条件下钻井液的表观黏度、塑性黏度逐渐增大，对切力的影响较小。在150℃下老化16h后的钻井液，随着抗高温二氧化硅接枝叔胺纳米封堵剂加量的增加，高温高压滤失量均逐渐减小，且在加量为16质量份时高温高压滤失量最小，说明抗高温二氧化硅接枝叔胺纳米封堵剂具有良好的流变性能和失水造壁性能，且能有效降低钻井液高温高压滤失量，即使在高温环境下也能提供较好的封堵性能，有效阻止滤液进入地层，提高井壁稳定性。
3、钻井液封堵性能测试
使用以上钻井液体系，用GGS-71型高温高压滤失仪制备一定大小、厚度、渗透率的泥饼，作为微裂缝地层的模拟地层，通过分别加入1％-5％的抗高温二氧化硅接枝叔胺纳米封堵剂进行高温高压滤失实验，来模拟封堵剂在地层中的高温高压失水量，以失水量来计算封堵剂的渗透率，来评价封堵剂在钻井液体系中的封堵效果，并与常规封堵剂超细碳酸钙作比较， 以其高温高压的滤失量来评判其封堵效果，在其它因素都相同的情况下高温高压滤失量越小，钻井液在地层中的渗透率就越小，钻井液就越难浸入地层，封堵效果就越好。
(1)滤饼制备
①制备土浆，取5000mL温度为70℃的纯净水于容器中，用搅拌仪在1000r/min的转速下边搅拌边加入300g膨润土，随后加入40g无水碳酸钠，在800r/min的转速下搅拌3h，随后取出溶液预水化24h。
②取出6％的土浆5000mL于容器中，依次加入0.02重量份KPAM，0.4重量份PAC-LV，5重量份RSTF，5重量份SMP-1，5重量份FRH，1重量份PPL，4重量份FK-10，0.4重量份SP-80，1.2重量份除硫剂，0.4重量份CaO，在转速为1400r/min的搅拌仪中搅拌3h，随后加入温度为150℃的热滚仪中老化16h。
③将(2)中老化好的钻井液用玻璃棒引流，缓慢倒入高温高压滤失仪中，在温度为150℃，压力为3.5MPa的条件下滤失30min，随后取出高温高压滤失仪中沉淀物质，在温度为50℃的清水中洗出泥饼。
(2)封堵性能的评价
按照上述方法制备滤饼，选取渗透率大致相同的滤饼，将不同加量的抗高温二氧化硅接枝叔胺纳米封堵剂各配制100mL溶液，超声分散10min，转入装有滤饼的高温高压失水仪中，在150℃、3.5MPa的相同条件下依次测试，每5min记录读数，测量30min，取出泥饼，吹风机吹干后根据利用公式计算得到不同加量的抗高温二氧化硅接枝叔胺纳米封堵剂的渗透率，结果见表2。
表2不同二氧化硅接枝叔胺纳米封堵剂加量下的封堵效果评价
Figure PCTCN2022100217-appb-000002
从表2中的数据可以看出抗高温二氧化硅接枝叔胺纳米封堵剂的封堵性能优异，抗高温 二氧化硅接枝叔胺纳米封堵剂经泥饼的高温高压失水实验所计算得出的平均失水量和泥饼渗透率均远小于清水在泥饼中的所得出的数据，并且随着抗高温二氧化硅接枝叔胺纳米封堵剂的加量的增加封堵效果越好，随着抗高温二氧化硅接枝叔胺纳米封堵剂加量的增加最大封堵率可达77.52％。说明本发明封堵剂能够封堵纳米孔缝。
综上所述，本发明二氧化硅接枝叔胺纳米封堵剂的制备方法稳定可靠、合成产品价格低廉、制成的聚合物封堵剂封堵性、流变性、水溶性、分散性、吸附性良好，较同类产品有很大的提升，稳定井壁效果极佳。本封堵剂仅需少量就可以达到优异的封堵效果，是解决井壁稳定和钻井液漏失问题的有效途径。
以上所述，仅是本发明的一个实施例而已，并非对本发明作任何形式上的限制，虽然本发明已以较佳实施例揭露如上，然而并非用以限定本发明，任何熟悉本专业的技术人员，在不脱离本发明技术方案范围内，当可利用上述揭示的技术内容做出些许更动或修饰为等同变化的等效实施例，但凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，均仍属于本发明技术方案的范围内。

Claims (6)

  1. 一种抗高温二氧化硅接枝叔胺纳米封堵剂，其特征在于，所述二氧化硅接枝叔胺纳米封堵剂的原料为肼类化合物、二烯丙基类化合物、烯胺类化合物、二氧化硅(10-20nm)、含氨基的硅烷偶联剂，采用如下步骤合成：
    S1、在70mL甲苯溶液中加入0.25-0.30mol纳米二氧化硅，升温至50-60℃后搅拌至溶解并通入氮气20-30min，升温至80-90℃边搅拌边加入一定量硅烷偶联剂，使二氧化硅和含氨基的硅烷偶联剂反应5h，减压蒸馏2h得到粗产品，用甲苯洗涤、过滤，除去未反应的单体，真空干燥2h，得到纳米二氧化硅的改性产物；
    S2、将上一步制得的纳米二氧化硅的改性产物用90-110mL四氢呋喃溶解，加入0.24-0.29mol二烯丙基类化合物，在50-60℃的条件下搅拌并反应24h，减压蒸馏得到粗产品，真空干燥2h，取一定量干燥后的粗产品加入到90-110mL四氢呋喃中，快速搅拌至溶解，通入氮气20-30min，保持搅拌和通入氮气，快速将0.48-0.53mol含羟基的肼类化合物加入混合体系，升温至30-40℃，反应8-12h后，减压蒸馏得到仲胺类化聚合物；
    S3、将上一步制得的仲胺类聚合物用90-110mL四氢呋喃溶解，加入0.24-0.29mol烯胺类化合物，在60-68℃的条件下搅拌并反应36h，减压蒸馏得到粗产品，将粗产品真空干燥2h，得到含羟基的叔胺型聚合物，将烘干的样品研磨，然后密封保存；
    上述步骤中，所述的肼类化合物为2-羟基苯甲酰肼，3-羟基苯酰肼，4-羟基苯甲酰肼，4-羟基苯乙酰肼，2,4-二羟基苯酰肼，3,4-二羟基苯酰肼，3,5-二羟基苯酰肼中的一种；所述的烯胺类化合物为N-甲基-N-乙烯基乙酰胺，N,N-二乙基-2-丙烯酰胺，N-乙烯基-N-甲基-2-丙烯酰胺中的一种。
  2. 根据权利要求1所述的封堵剂，其特征在于，所述硅烷偶联剂为3-氨基丙基三乙氧基硅烷(KH550)，3-氨丙基三甲氧基硅烷(KH540)中的一种。
  3. 根据权利要求1所述的封堵剂，其特征在于，所述含烯键的二烯丙基类化合物为1,5-已二烯，二烯丙基胺，N-甲基二烯丙基胺中的一种。
  4. 一种水基钻井液，其特征在于，所述钻井液中添加有权利要求1-3任一项所述的一种抗高温二氧化硅接枝叔胺纳米封堵剂。
  5. 根据权利要求4所述的水基钻井液，其特征在于，所述钻井液包括以下组分：水，膨润土，NaOH，聚丙烯酰胺钾盐(KPAM)，聚阴离子纤维素(PAC-LV)，腐植酸丙磺酸酰胺多元共聚物(RSTF)，磺化酚醛树脂(SMP-1)，酰胺基胺(FRH)，防卡降滤失剂(PPL)，防卡润滑剂(FK-10)，乳化剂(SP-80)，抗高温二氧化硅接枝叔胺纳米封堵剂，除硫剂，CaO，重晶石。
  6. 根据权利要求5所述的水基钻井液，其特征在于，以100重量份的水为基准，所述膨润土的加量为2-4重量份，所述NaOH的加量为0.1-0.3重量份，所述KPAM的加量为0.01-0.03重量份，所述PAC-LV的加量为0.3-0.8重量份，所述RSTF的加量为4-6重量份，所述SMP-1的加量为5-6重量份，所述FRH的加量为3-5重量份，所述PPL的加量为1-2重量份，所述FK-10的加量为4-5重量份，所述SP-80的加量为0.3-0.5重量份，所述氧化石墨烯基纳米复合水凝胶封堵剂的加量为1-5重量份，所述除硫剂的加量为1-1.5重量份，所述CaO的加量为0.3-0.5重量份，所述重晶石的加量为5-20重量份。
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