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CN103013466B - Solid paraffin lubricant for drilling fluid and preparation method of solid paraffin lubricant - Google Patents

Solid paraffin lubricant for drilling fluid and preparation method of solid paraffin lubricant Download PDF

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CN103013466B
CN103013466B CN201210591634.XA CN201210591634A CN103013466B CN 103013466 B CN103013466 B CN 103013466B CN 201210591634 A CN201210591634 A CN 201210591634A CN 103013466 B CN103013466 B CN 103013466B
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lubricant
oil
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CN103013466A (en
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周风山
王婷婷
熊正强
国文月
王焕娜
向玺
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China University of Geosciences Beijing
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Abstract

The invention relates to a solid paraffin lubricant for drilling fluid and a preparation method of the solid paraffin lubricant. The preparation method comprises the following steps of respectively adding oil phase, sodium hydroxide, a compound emulsifier, a stabilizer and a water phase in a reactor, heating and stirring, so as to obtain a liquid emulsified paraffin lubricant; immersing the prepared liquid paraffin lubricant in a characteristic water soluble high molecular material by using a semi-dry method, drying at low temperature, and crushing, so as to obtain the solid paraffin lubricant for drilling fluid. The lubricant product obtained according to the method provided by the invention has the characteristics of high drilling fluid dispersion speed, small particles and excellent composite lubricating effect. Compared with the traditional emulsion type paraffin lubricant, the solid paraffin lubricant provided by the invention has higher overall performances such as lubricating property, high temperature resistance, filtrate loss reducing property and salt resistance, and is convenient to store and transport, thus packaging and transporting costs are reduced but also the problems of emulsion instability of the traditional paraffin lubricant after being stored for a long time and freezing in winter are solved.

Description

一种钻井液用固体石蜡润滑剂及其制备方法A kind of solid paraffin lubricant for drilling fluid and preparation method thereof

技术领域technical field

本发明涉及一种润滑剂及其制备方法,尤其涉及一种钻井液用固体石蜡润滑剂及其制备方法。The invention relates to a lubricant and a preparation method thereof, in particular to a solid paraffin lubricant for drilling fluid and a preparation method thereof.

背景技术Background technique

钻井过程中的润滑防卡问题是钻井工程,特别是深井、定向井、水平井、多分支井等复杂井钻井中经常遇到的技术难题。钻井液润滑剂作为一种重要的钻井液化学处理剂,其作用是改善钻井液的润滑性能,降低钻具与井壁(或套管)之间的摩擦,降低钻柱旋转扭矩和起下钻阻力,减少卡钻事故的发生。The problem of lubrication and anti-sticking during drilling is a technical problem often encountered in drilling engineering, especially in complex wells such as deep wells, directional wells, horizontal wells, and multi-branch wells. Drilling fluid lubricant is an important chemical treatment agent for drilling fluid. Its function is to improve the lubrication performance of drilling fluid, reduce the friction between the drilling tool and the well wall (or casing), reduce the rotational torque of the drill string and trip out resistance, reducing the occurrence of stuck pipe accidents.

近年来,随着深井、定向井和水平井钻井技术的不断发展和提高,对钻井液润滑剂性能的要求越来越高,使用的润滑剂种类和数量也越来越多。外排废弃钻井液中的润滑剂有些是有毒有害的,还有相当一部分在自然条件下较难降解,由此造成这类物质在环境中长期滞留和积累,对人类和生态环境构成威胁。随着环保意识的增强,人们在开发新型钻井液润滑剂时越来越重视环保性,同时还要求尽可能无荧光或低荧光,对钻井液流变性无影响,进一步提高抗高温抗盐能力。In recent years, with the continuous development and improvement of deep well, directional well and horizontal well drilling technology, the requirements for the performance of drilling fluid lubricants are getting higher and higher, and the types and quantities of lubricants used are also increasing. Some of the lubricants in the discharged waste drilling fluid are toxic and harmful, and a considerable part of them are difficult to degrade under natural conditions, resulting in long-term retention and accumulation of such substances in the environment, posing a threat to humans and the ecological environment. With the increasing awareness of environmental protection, people pay more and more attention to environmental protection when developing new drilling fluid lubricants. At the same time, they also require as little or low fluorescence as possible, which has no effect on the rheology of drilling fluids, and further improves the ability to resist high temperature and salt.

我国原油多数为石蜡基原油,这就为发展石蜡类产品的生产提供了丰富和宝贵的资源。上个世纪50年代,美孚石油公司开始研究开发乳化石蜡,70年代,英国、日本也开始研究和应用乳化石蜡。近些年,国内也开始了大量这方面的研究。Most of my country's crude oil is paraffin-based crude oil, which provides abundant and valuable resources for the development of the production of paraffin products. In the 1950s, Mobil Oil Company began to research and develop emulsified paraffin. In the 1970s, Britain and Japan also began to study and apply emulsified paraffin. In recent years, a lot of researches in this area have been started in China.

钻井液用石蜡润滑剂按照形态可分为液体类和固体类。乳液型石蜡润滑剂的研究相对较多,近些年,关于固体型钻井液润滑剂的研究也有不少,但有关固体粉末状石蜡润滑剂尚没有公开的技术文献和专利。Paraffin lubricants for drilling fluids can be divided into liquid and solid according to their form. There are relatively many studies on emulsion-type paraffin lubricants. In recent years, there are also many studies on solid-type drilling fluid lubricants, but there are no published technical documents and patents on solid powder paraffin lubricants.

专利CN 1306012C、CN 101423752A、CN 1699500A公开了几种制备乳液型石蜡润滑剂的技术方法,但是乳液型产品均存在长时间储存不稳定、冬季容易上冻等问题,使得现场应用受到限制。Patents CN 1306012C, CN 101423752A, and CN 1699500A disclose several technical methods for preparing emulsion-type paraffin lubricants, but emulsion-type products have problems such as long-term storage instability and easy freezing in winter, which limit field application.

例如CN 101157850,采用动植物油脂制备液体润滑剂,再将液体与油溶性树脂、石墨混合得到钻井液用抗高温润滑剂,其润滑性较好;专利US 5826669通过在钻井液中加入充足的富有弹性的石墨颗粒,设计了一种有效减小起下钻阻力和旋转扭矩的润滑剂,但石墨作为润滑油吸附载体对于环保要求较高的海洋钻井很难达到要求,且几乎没有降滤失性能。For example CN 101157850 adopts animal and vegetable fats and oils to prepare liquid lubricants, and then liquid is mixed with oil-soluble resin and graphite to obtain high-temperature resistant lubricants for drilling fluids, which have better lubricity; Elastic graphite particles, designed a lubricant that can effectively reduce tripping resistance and rotational torque, but graphite as a lubricating oil adsorption carrier is difficult to meet the requirements of marine drilling with high environmental protection requirements, and has almost no fluid loss control performance .

专利CN 1861736A公布了一种利用钠基膨润土负载表面活性剂制备钻井液用固体润滑剂的方法,但其在使用时需加入柴油进行现场复配,使用起来不方便,且柴油荧光性很强,对录井产生干扰。另外,专利CN 1183231C利用熔融石蜡与表面活性共混后降温冷却成型,发明了一种的固体自乳化石蜡,虽然解决了产品的储运问题,但是石蜡固体需要在热水中溶解乳化,而且不具有一剂多效的作用。Patent CN 1861736A discloses a method for preparing a solid lubricant for drilling fluid by using sodium-based bentonite-loaded surfactant, but it needs to add diesel oil for on-site compounding when it is used, which is inconvenient to use, and the fluorescence of diesel oil is very strong. Interference with mud logging. In addition, the patent CN 1183231C uses molten paraffin and surface active blending to cool and form a solid self-emulsifying paraffin. Although it solves the problem of product storage and transportation, the paraffin solid needs to be dissolved and emulsified in hot water. It has a multi-effect effect in one dose.

因此,开发一种适合低温条件下使用、具有一剂多效作用的低荧光无毒固体润滑剂产品对于油田钻井具有重要意义。Therefore, it is of great significance for oil field drilling to develop a low-fluorescence non-toxic solid lubricant product suitable for use under low temperature conditions and having multiple effects in one dose.

发明内容Contents of the invention

针对现有研究的不足,本发明要解决的问题是提供一种钻井液用固体石蜡润滑剂以及其制备方法,利用本发明方法得到的固体润滑剂具有在钻井液中分散性好,综合润滑性能好,粘附系数和摩阻系数降低率高的特点,同时具有较好的抗高温抗盐降滤失性。此外,本发明制备方法简单,工艺易于实现,所制备的固体润滑剂状态为自由流动粉末固体,运输便捷,低温使用性能不受影响。In view of the deficiencies in existing research, the problem to be solved by the present invention is to provide a solid paraffin lubricant for drilling fluid and its preparation method. The solid lubricant obtained by the method of the present invention has good dispersibility in drilling fluid and comprehensive lubricating performance. Good, high adhesion coefficient and friction coefficient reduction rate, and good resistance to high temperature, salt and fluid loss. In addition, the preparation method of the present invention is simple, the process is easy to realize, the state of the prepared solid lubricant is a free-flowing powder solid, the transportation is convenient, and the low-temperature performance is not affected.

因此,根据本发明第一方面,提供一种钻井液用固体石蜡润滑剂的制备方法,其包括以下步骤:Therefore, according to the first aspect of the present invention, a kind of preparation method of paraffin wax lubricant for drilling fluid is provided, it may further comprise the steps:

(1)称取如下重量配比组分:油相20-50份,氢氧化钠0.5-2份,复合乳化剂1-10份,稳定剂0.1-1份、水相37-78.4份;(1) Weigh the following components by weight: 20-50 parts of oil phase, 0.5-2 parts of sodium hydroxide, 1-10 parts of compound emulsifier, 0.1-1 part of stabilizer, and 37-78.4 parts of water phase;

(2)将上述油相、氢氧化钠、复合乳化剂、稳定剂及水相按所述组分比例混合加入反应器中,70-100℃、100-2000转/分条件下,搅拌15-60min,制得液体润滑剂;(2) Mix the above-mentioned oil phase, sodium hydroxide, compound emulsifier, stabilizer and water phase into the reactor according to the stated component ratio, and stir for 15- 60min, obtained liquid lubricant;

(3)称取如下重量配比组分:特性高分子材料50-80份,步骤(2)中获得的液体润滑剂20-50份;(3) Weigh the following components by weight: 50-80 parts of characteristic polymer material, 20-50 parts of liquid lubricant obtained in step (2);

(4)将上述液体润滑剂与特性高分子按所述组分比例侵浸反应;(4) Immersing and reacting the above-mentioned liquid lubricant and the characteristic polymer according to the ratio of the components;

(5)经60-100℃低温烘干、粉碎工艺,得到钻井液用固体润滑剂;(5) After low-temperature drying and crushing at 60-100°C, solid lubricants for drilling fluids are obtained;

其中:in:

所述油相为矿物油和蜡质物;The oily phase is mineral oil and waxy matter;

所述复合乳化剂为多元醇脂类非离子表面活性剂;The composite emulsifier is a polyol lipid nonionic surfactant;

所述稳定剂为无机纳米粒子;The stabilizer is an inorganic nanoparticle;

所述特性高分子材料为具有降滤失作用的水溶性高分子材料。The characteristic polymer material is a water-soluble polymer material with fluid loss reducing function.

上述钻井液用固体石蜡润滑剂的制备方法中,所述矿物油是液体石蜡、7#白油、10#白油、15#白油、26#白油或46#白油;进一步优选46#白油。In the preparation method of solid paraffin lubricant for above-mentioned drilling fluid, described mineral oil is liquid paraffin, 7# white oil, 10# white oil, 15# white oil, 26# white oil or 46# white oil; More preferably 46# white oil.

所述蜡质物为石蜡、蜡膏、植物蜡、蜡模回收蜡、油井清蜡作业回收蜡;进一步优选蜡膏,因为蜡膏更易乳化,制备得到的乳液均一稳定。The waxy substance is paraffin wax, wax paste, vegetable wax, wax mold recovery wax, oil well wax removal operation recovery wax; wax paste is further preferred, because wax paste is easier to emulsify, and the prepared emulsion is uniform and stable.

所述多元醇脂类非离子表面活性剂优选Sp an和Tween系列表面活性剂;进一步优选Sp an20、Sp an40、Sp an 60或Span80以及Tween20、Tween40、Tween60或Tween80;最优选Span80和Tween80。The preferred Span and Tween series surfactants of described polyol lipid nonionic surfactant; Further preferably Span20, Span40, Span60 or Span80 and Tween20, Tween40, Tween60 or Tween80; Most preferably Span80 and Tween80.

所述脂肪酸烷醇酰胺类助乳化剂优选脂肪酸与三乙醇胺直接反应产物。The fatty acid alkanolamide co-emulsifier is preferably a direct reaction product of fatty acid and triethanolamine.

所述无机纳米粒子稳定剂优选白炭黑、超细碳酸钙、膨润土凝胶、凹凸棒土凝胶或其任意比例的混合物;进一步优选白炭黑和凹凸棒土凝胶。The inorganic nanoparticle stabilizer is preferably white carbon black, superfine calcium carbonate, bentonite gel, attapulgite gel or a mixture thereof in any proportion; more preferably white carbon black and attapulgite gel.

上述钻井液用固体石蜡润滑剂的制备方法中,在步骤(2)中,所述组分优选以80-100℃、200-500转/分条件搅拌20-40min。In the above preparation method of solid paraffin lubricant for drilling fluid, in step (2), the components are preferably stirred at 80-100° C. and 200-500 rpm for 20-40 minutes.

所述具有降滤失作用的特性水溶性高分子材料优选硅油接枝淀粉(SiM)、纤维素接枝淀粉(PPS)、聚丙烯腈铵盐(NH4PAN)、聚(丙烯腈-丙烯酰胺)铵盐(双聚铵盐)(HMP-21)、褐煤树脂(SPNH)、磺化褐煤(SMC)或其任意比例的混合物;进一步优选PPS,因为PPS为纤维状结构,使得水包油型石蜡乳液粒子能够侵入其中,经半干法工艺、烘干粉碎得到润滑性能较好的固体润滑剂。The characteristic water-soluble polymer material with fluid loss reducing effect is preferably silicone oil grafted starch (SiM), cellulose grafted starch (PPS), polyacrylonitrile ammonium salt (NH 4 PAN ), poly(acrylonitrile-acrylamide ) ammonium salt (double polyammonium salt) (HMP-21), lignite resin (SPNH), sulfonated lignite (SMC) or a mixture thereof in any proportion; PPS is further preferred, because PPS has a fibrous structure, making oil-in-water type The paraffin emulsion particles can penetrate into it, and the solid lubricant with better lubricating performance can be obtained through semi-dry process, drying and pulverization.

上述钻井液用固体石蜡润滑剂的制备方法中,步骤(5)所述组分优选以70-90℃条件烘干。In the above preparation method of solid paraffin lubricant for drilling fluid, the components in step (5) are preferably dried at 70-90°C.

根据本发明第二方面,提供一种根据上述方法制得的钻井液用固体石蜡润滑剂,其特征在于,所述固体润滑剂包含以下重量配比的组分:特性高分子材料50-80份,优选55-75份,液体润滑剂20-50份,优选25-45份;其中:According to the second aspect of the present invention, there is provided a solid paraffin lubricant for drilling fluid prepared according to the above method, wherein the solid lubricant comprises the following components by weight: 50-80 parts of characteristic polymer material , preferably 55-75 parts, 20-50 parts of liquid lubricant, preferably 25-45 parts; wherein:

所述液体润滑剂包含以下重量配比的组分:油相30-50份,氢氧化钠0.5-2份,复合乳化剂2-6份,稳定剂0.1-1份,水相41-67.4份,基于100重量份液体润滑剂;The liquid lubricant comprises the following components by weight: 30-50 parts of oil phase, 0.5-2 parts of sodium hydroxide, 2-6 parts of composite emulsifier, 0.1-1 part of stabilizer, and 41-67.4 parts of water phase , based on 100 parts by weight of liquid lubricant;

其中:in:

所述油相为矿物油和蜡质物;The oily phase is mineral oil and waxy matter;

所述复合乳化剂为多元醇脂类非离子表面活性剂;The composite emulsifier is a polyol lipid nonionic surfactant;

所述稳定剂为无机纳米粒子;The stabilizer is an inorganic nanoparticle;

所述特性高分子材料为具有降滤失作用的水溶性高分子材料。The characteristic polymer material is a water-soluble polymer material with fluid loss reducing function.

根据本发明优选的实施方式,所述钻井液用固体石蜡润滑剂中,特性高分子材料为60-70重量份,液体润滑剂为30-40重量份。According to a preferred embodiment of the present invention, in the solid paraffin lubricant for drilling fluid, the characteristic polymer material is 60-70 parts by weight, and the liquid lubricant is 30-40 parts by weight.

根据本发明优选的实施方式,所述钻井液用固体石蜡润滑剂中,所述液体润滑剂包含以下重量配比的组分:油相40-45份,氢氧化钠0.8-1份,复合乳化剂3-5份,稳定剂0.5-0.8份,水相48.2-55.7份,基于100重量份液体润滑剂。According to a preferred embodiment of the present invention, in the solid paraffin lubricant for drilling fluid, the liquid lubricant contains the following components in weight ratio: 40-45 parts of oil phase, 0.8-1 part of sodium hydroxide, compound emulsification 3-5 parts of agent, 0.5-0.8 parts of stabilizer, 48.2-55.7 parts of water phase, based on 100 parts by weight of liquid lubricant.

根据本发明优选的实施方式,所述钻井液用固体石蜡润滑剂中,所述矿物油优选46#白油;和/或所述蜡质物优选蜡膏;所述多元醇脂类非离子表面活性剂优选Sp an80和Twe en80;和/或所述无机纳米粒子稳定剂优选白炭黑和凹凸棒土凝胶;和/或所述具有降滤失作用的特性水溶性高分子材料优选PP S。According to a preferred embodiment of the present invention, in the solid paraffin lubricant for drilling fluid, the preferred 46# white oil of the mineral oil; and/or the preferred wax paste of the waxy substance; the non-ionic surface of the polyol lipid The preferred Span80 and Twe en80 active agent; And/or the preferred white carbon black and attapulgite gel of the inorganic nano particle stabilizer; And/or the preferred PPS with the characteristic water-soluble macromolecular material of fluid loss reducing effect .

本发明所述方法制得的钻井液用固体石蜡润滑剂外观为浅褐色固体粉末,无异味,润滑剂分散于钻井液中为纳微米尺寸颗粒。The appearance of the solid paraffin lubricant for drilling fluid prepared by the method of the invention is a light brown solid powder without peculiar smell, and the lubricant is dispersed in the drilling fluid as particles of nanometer size.

本发明的钻井液用固体石蜡润滑剂,粘附系数降低率和摩阻系数降低率均可控制在55%-90%,综合润滑性能较好。The solid paraffin lubricant for drilling fluid of the present invention can control both the adhesion coefficient reduction rate and the friction coefficient reduction rate at 55%-90%, and the comprehensive lubricating performance is good.

本发明与现有技术相比的有益效果在于:The beneficial effect of the present invention compared with prior art is:

(1)原料之一的蜡膏更易乳化,制备得到的乳液均一稳定;特性水溶性高分子材料之一的PPS为纤维状结构,使得水包油型石蜡乳液粒子能够浸入其中,经半干法工艺、烘干粉碎得到润滑性能较好的固体润滑剂。(1) Wax paste, one of the raw materials, is easier to emulsify, and the prepared emulsion is uniform and stable; PPS, one of the characteristic water-soluble polymer materials, has a fibrous structure, so that the oil-in-water paraffin emulsion particles can be immersed in it. process, drying and crushing to obtain a solid lubricant with better lubricating properties.

(2)具有优良的综合润滑性能,能有效降低钻井液基浆的粘附系数及摩阻系数,起到润滑钻具和井壁的作用。(2) It has excellent comprehensive lubrication performance, can effectively reduce the adhesion coefficient and friction coefficient of drilling fluid base slurry, and play a role in lubricating drilling tools and well walls.

(3)能在井壁内形成油膜保护层,阻止钻井液及其滤液进入地层,封堵地层裂隙,防止井壁坍塌,具有很好的保护储油层的性能。(3) It can form an oil film protection layer in the borehole wall, prevent drilling fluid and its filtrate from entering the formation, seal formation fissures, prevent the borehole wall from collapsing, and have a good performance in protecting the oil reservoir.

(4)具有很好的抗高温性、抗盐性,易分散、低荧光、低毒性,满足环境保护的要求。(4) It has good high temperature resistance, salt resistance, easy dispersion, low fluorescence, low toxicity, and meets the requirements of environmental protection.

(5)具有较好的高温高压降滤失性能,4%盐水基浆、120℃、3.5MPa压差的高温高压下降滤失率达到50%以上。(5) It has good high-temperature and high-pressure fluid loss reduction performance, and the high-temperature and high-pressure fluid loss reduction rate of 4% brine-based slurry, 120°C, and 3.5MPa pressure difference reaches more than 50%.

(6)低温条件使用不受影响,有效防止传统液体石蜡润滑剂因长时间储存而分层凝固和冬季易上冻,具有运输和储存方便,节约包装和运输成本的特点。(6) The use under low temperature conditions will not be affected, effectively preventing the traditional liquid paraffin lubricant from layering and solidifying due to long-term storage and easy to freeze in winter. It has the characteristics of convenient transportation and storage, and saves packaging and transportation costs.

附图说明Description of drawings

图1:固体石蜡润滑剂不同加量对基浆粘附系数降低率和摩阻系数降低率的影响程度;Figure 1: The degree of influence of different additions of solid paraffin lubricant on the reduction rate of adhesion coefficient and friction coefficient of base slurry;

图2:特性高分子材料与固体石蜡润滑剂的扫描电镜照片对比:(a)特性高分子;(b)本发明固体石蜡润滑剂;Figure 2: Comparison of scanning electron microscope photos between characteristic polymer materials and solid paraffin lubricants: (a) characteristic polymers; (b) solid paraffin lubricants of the present invention;

图3:固体石蜡润滑剂激光粒度分布图。Figure 3: Laser particle size distribution map of paraffin wax lubricant.

具体实施方式Detailed ways

以下通过实施例来进一步解释或说明本发明内容。但所提供的实施例不应被理解为对本发明保护范围构成限制。The content of the present invention is further explained or illustrated by the following examples. However, the provided examples should not be construed as limiting the protection scope of the present invention.

性能评价performance evaluation

本发明涉及的润滑剂的粘附系数降低率、摩阻系数降低率、高温高压降滤失性测量实验如下:The adhesion coefficient reduction rate, friction coefficient reduction rate, and high temperature and high pressure fluid loss reduction measurement experiment of the lubricant involved in the present invention are as follows:

1、粘附系数降低率测量:1. Measurement of adhesion coefficient reduction rate:

在500mL蒸馏水中加入26g钙质钠化膨润土,在高速搅拌器上以10000转/分的转速高速搅拌20min,然后室温密闭陈化16h,即得到含土量为5.2%的淡水基浆。测量时将已经陈化16h的5.2%淡水基浆按一定的配比加入润滑剂,高速搅拌20min,测量采用NF-1型粘附系数测定仪。将配置好的泥浆倒入盛液杯中,加3.5MPa的压力30min,然后测定此时的滤失量,并加3.5MPa的压力于粘附盘,压5min后扭矩仪测量扭矩,然后进行计算,计算公式如下:Add 26g of calcareous sodium bentonite to 500mL of distilled water, stir on a high-speed stirrer at a speed of 10,000 rpm for 20 minutes, and then age in airtight conditions at room temperature for 16 hours to obtain a freshwater base slurry with a soil content of 5.2%. During the measurement, the 5.2% freshwater base slurry that has been aged for 16 hours is added with a lubricant according to a certain ratio, and stirred at a high speed for 20 minutes. The measurement adopts the NF-1 type adhesion coefficient tester. Pour the configured mud into the liquid cup, apply a pressure of 3.5MPa for 30 minutes, then measure the fluid loss at this time, and apply a pressure of 3.5MPa to the adhesion plate, and measure the torque with a torque meter after 5 minutes of pressure, and then calculate ,Calculated as follows:

f=M×0.845×10-2 f=M×0.845×10 -2

式中:f为粘附系数M为扭矩(Nm)Where: f is the adhesion coefficient M is the torque (Nm)

粘附系数降低率的计算:Calculation of adhesion coefficient reduction rate:

△Kf=(f1-f2)/f1×100%△K f = (f 1 - f 2 )/f 1 × 100%

式中:f1为基浆本身的粘附系数,f2为加入一定含量润滑剂后泥浆的粘附系数。In the formula: f 1 is the adhesion coefficient of the base slurry itself, and f 2 is the adhesion coefficient of the mud after adding a certain amount of lubricant.

2、摩阻系数降低率测量:2. Measurement of friction coefficient reduction rate:

在500mL蒸馏水中加入26g钙质钠化膨润土,在高速搅拌器上以10000转/分的转速高速搅拌20min,然后室温密闭陈化16h,即得到含土量为5.2%的淡水基浆。采用E—P极压润滑仪进行测定基浆、蒸馏水及基浆加润滑剂后的摩阻系数,将已陈化的5.2%淡水基浆按一定的配比加入润滑剂,采用GJ-2S型高速搅拌机高速搅拌5min,将液体倒入润滑仪样品杯中,测试条件为60r/min,测试压力为1.5MPa,测试时间为5min,5min后读数。校正因子=34/蒸馏水读数,摩阻系数f=0.01×读数×校正因子。Add 26g of calcareous sodium bentonite to 500mL of distilled water, stir on a high-speed stirrer at a speed of 10,000 rpm for 20 minutes, and then age in airtight conditions at room temperature for 16 hours to obtain a freshwater base slurry with a soil content of 5.2%. Use the E-P extreme pressure lubrication instrument to measure the friction coefficient of the base slurry, distilled water and base slurry with lubricant, add the lubricant to the aged 5.2% fresh water base slurry according to a certain ratio, and use the GJ-2S type Stir at high speed with a high-speed mixer for 5 minutes, pour the liquid into the sample cup of the lubrication meter, the test conditions are 60r/min, the test pressure is 1.5MPa, the test time is 5 minutes, and the reading is taken after 5 minutes. Correction factor=34/distilled water reading, friction coefficient f=0.01×reading×correction factor.

△f=(f1-f2)/f1×100%△f=(f 1 -f 2 )/f 1 ×100%

式中:f1为基浆本身的摩阻系数,f2为加入一定含量润滑剂后泥浆的摩阻系数。In the formula: f 1 is the friction coefficient of the base slurry itself, and f 2 is the friction coefficient of the mud after adding a certain amount of lubricant.

3、高温高压滤失量:3. High temperature and high pressure filtration loss:

(1)淡水基浆:在400mL去离子水中加入24g钙质钠化膨润土,在高速搅拌器上以10000转/分的转速高速搅拌20min,然后室温密闭陈化16h,即得到6.0%的淡水基浆。测量时将已经陈化16h的基浆按一定的配比加入润滑剂,高速搅拌20min,测量采用GGS 42-2型高温高压滤失仪。将配置好的泥浆倒入压滤器中,加压3.5Mp a、升温至120℃,打开上下部阀杆的同时计时,记录30min的滤液滤失量。(1) Freshwater base slurry: add 24g of calcium sodium bentonite to 400mL of deionized water, stir on a high-speed stirrer at a speed of 10,000 rpm for 20 minutes, and then age in a closed room at room temperature for 16 hours to obtain 6.0% freshwater base slurry. pulp. When measuring, the base slurry that has been aged for 16 hours is added with lubricant according to a certain ratio, and stirred at high speed for 20 minutes. The measurement uses GGS 42-2 high temperature and high pressure filter loss instrument. Pour the configured mud into the filter press, pressurize to 3.5Mpa, raise the temperature to 120°C, open the upper and lower valve stems while timing, and record the filtrate loss for 30 minutes.

高温高压降失水率=(V1-V2)/V1×100%Water loss rate under high temperature and high pressure = (V 1 -V 2 )/V 1 × 100%

式中:V1为基浆本身的滤液的滤失量,V2为加入一定含量润滑剂后滤液的滤失量。In the formula: V 1 is the fluid loss of the filtrate of the base pulp itself, and V 2 is the fluid loss of the filtrate after adding a certain amount of lubricant.

(2)盐水基浆:在400mL去离子水中加入16gNa Cl,10000转/分高速搅拌20min,再加入24g钙质钠化膨润土,在高速搅拌器上以10000转/分的转速高速搅拌20min,然后室温密闭陈化16h,即得到含土量为6.0%的盐水基浆。测量时将已经陈化16h的基浆按一定的配比加入润滑剂,高速搅拌20min,测量采用GGS42-2型高温高压滤失仪。将配置好的泥浆倒入压滤器中,加压3.5Mpa、升温至120℃,打开上下部阀杆的同时计时,记录30min的滤液滤失量。(2) Salt water-based slurry: add 16g Na Cl to 400mL deionized water, stir at 10000 rpm for 20min at high speed, then add 24g of calcium sodium bentonite, stir at 10000rpm on a high-speed stirrer for 20min, then Airtightly aged at room temperature for 16 hours to obtain a brine-based slurry with a soil content of 6.0%. When measuring, the base slurry that has been aged for 16 hours is added with lubricant according to a certain ratio, and stirred at a high speed for 20 minutes. The measurement adopts GGS42-2 high temperature and high pressure filter loss meter. Pour the prepared mud into the filter press, pressurize to 3.5Mpa, raise the temperature to 120°C, open the upper and lower valve stems while timing, and record the filtrate loss for 30 minutes.

高温高压降失水率=(V1-V2)/V1×100%Water loss rate under high temperature and high pressure = (V 1 -V 2 )/V 1 × 100%

式中:V1为基浆本身的滤液的滤失量,V2为加入一定含量润滑剂后滤液的滤失量。In the formula: V 1 is the fluid loss of the filtrate of the base pulp itself, and V 2 is the fluid loss of the filtrate after adding a certain amount of lubricant.

实施例1Example 1

润滑剂组分如下:均为重量份(单位:公斤):Lubricant components are as follows: all are parts by weight (unit: kilogram):

白油22.5份,蜡膏22.5份,氢氧化钠1份,非离子型表面活性剂Span 80和Tween804.7份,白炭黑0.3份,蒸馏水49份。22.5 parts of white oil, 22.5 parts of wax paste, 1 part of sodium hydroxide, 4.7 parts of non-ionic surfactant Span 80 and Tween 80, 0.3 part of white carbon black, 49 parts of distilled water.

特性水溶性高分子PPS 35份,取上述制备得到的液体润滑剂65份。35 parts of characteristic water-soluble polymer PPS, get 65 parts of liquid lubricants prepared above.

制备方法:将白油22.5份、蜡膏22.5份、非离子型表面活性剂Span 80和Tween804.7份、白炭黑0.3份、蒸馏水49份在反应器中混合均匀,85℃、300转/分条件持续搅拌20min,得到钻井液用液体润滑剂。取上述制得的润滑剂65份与35份PP S混合,在80℃条件下均匀侵浸,80℃低温烘干粉碎,得到钻井液用固体石蜡润滑剂。Preparation method: Mix 22.5 parts of white oil, 22.5 parts of wax paste, 4.7 parts of non-ionic surfactants Span 80 and Tween80, 0.3 parts of white carbon black, and 49 parts of distilled water in a reactor, 85 ° C, 300 rpm Stir continuously for 20 minutes according to different conditions to obtain a liquid lubricant for drilling fluid. Mix 65 parts of the lubricant prepared above with 35 parts of PPS, uniformly impregnate at 80°C, dry and pulverize at a low temperature of 80°C to obtain solid paraffin lubricant for drilling fluid.

根据上述产品性能评价方法,分别对实施例1的固体石蜡润滑剂产品及两种市售乳液型和固体型润滑剂进行评价,结果如表一所示。According to the above-mentioned product performance evaluation method, the solid paraffin lubricant product of Example 1 and two commercially available emulsion-type and solid-type lubricants were evaluated respectively, and the results are shown in Table 1.

表一实施例产品综合润滑性能对比评价结果(5.2%淡水膨润土基浆)Table 1. Comparative evaluation results of the comprehensive lubricating properties of the products of the embodiment (5.2% fresh water bentonite base slurry)

图1为所制得的固体石蜡润滑剂不同加量对基浆粘附系数降低率和摩阻系数降低率的影响程度曲线图。Fig. 1 is a graph showing the degree of influence of different additions of the prepared solid paraffin lubricant on the reduction rate of the adhesion coefficient and the reduction rate of the friction coefficient of the base slurry.

实施例2Example 2

方法基本如实例1所述,所不同的是:The method is basically as described in Example 1, the difference is:

润滑剂组分如下,均为重量份(单位:公斤):The lubricant components are as follows, all in parts by weight (unit: kilogram):

白油20份,蜡膏20份,氢氧化钠1份,非离子型表面活性剂Span80和Tween 805份,超细碳酸钙0.5份,蒸馏水53.5份。20 parts of white oil, 20 parts of wax paste, 1 part of sodium hydroxide, 805 parts of nonionic surfactant Span80 and Tween, 0.5 part of superfine calcium carbonate, and 53.5 parts of distilled water.

特性高分子PPS 30份,取上述制备得到的液体润滑剂70份。30 parts of characteristic polymer PPS, take 70 parts of liquid lubricant prepared above.

制备方法:将上述组分在反应器中混合均匀,75℃、100转/分条件持续搅拌60min,得到钻井液用液体润滑剂。取上述制得的润滑剂70份与30份PPS在70℃条件下均匀侵浸,100℃低温烘干粉碎,得到钻井液用固体石蜡润滑剂。Preparation method: Mix the above components uniformly in a reactor, and continuously stir for 60 minutes at 75°C and 100 rpm to obtain a liquid lubricant for drilling fluid. Take 70 parts of the above-prepared lubricant and 30 parts of PPS, uniformly soak at 70°C, dry and pulverize at 100°C to obtain solid paraffin lubricant for drilling fluid.

根据上述产品性能评价方法,分别对实施例2的固体石蜡润滑剂产品及两种市售乳液型和固体型润滑剂进行评价,结果如表二所示。According to the above-mentioned product performance evaluation method, the solid paraffin lubricant product of Example 2 and two commercially available emulsion-type and solid-type lubricants were evaluated respectively, and the results are shown in Table 2.

表二实施例产品高温高压降滤失性能对比评价结果(6.0%淡水和盐水(4.0%)基浆)Table 2 Comparative evaluation results of high temperature and high pressure fluid loss reduction performance of the products of the examples (6.0% fresh water and salt water (4.0%) base slurry)

实施例3Example 3

方法基本如实施例1或2所述,所不同的是:Method is substantially as described in embodiment 1 or 2, the difference is:

润滑剂组分如下:均为重量份(单位:公斤):Lubricant components are as follows: all are parts by weight (unit: kilogram):

白油20份,蜡膏25份,氢氧化钠1份,非离子型表面活性剂Span80和Tween805份,凹凸棒土凝胶0.6份,蒸馏水48.4份。20 parts of white oil, 25 parts of wax paste, 1 part of sodium hydroxide, 5 parts of nonionic surfactant Span80 and Tween80, 0.6 part of attapulgite gel, 48.4 parts of distilled water.

特性高分子PPS 35份,取上述制备得到的液体润滑剂65份。35 parts of characteristic polymer PPS, get 65 parts of liquid lubricants prepared above.

制备方法:将上述组分在反应器中混合均匀,90℃、2000转/分条件持续搅拌15min,得到钻井液用液体润滑剂。取上述制得的润滑剂65份与35份PPS在90℃条件下均匀侵浸,70℃低温烘干粉碎,得到钻井液用固体石蜡润滑剂。Preparation method: Mix the above components uniformly in a reactor, and continuously stir for 15 minutes under the conditions of 90°C and 2000 rpm to obtain a liquid lubricant for drilling fluid. Take 65 parts of the above-prepared lubricant and 35 parts of PPS, soak them uniformly at 90°C, dry and pulverize them at a low temperature of 70°C, and obtain a solid paraffin lubricant for drilling fluid.

图2为特性高分子材料与固体石蜡润滑剂的扫描电镜照片对比:(a)特性高分子;(b)本发明制得的固体石蜡润滑剂。由图可见,石蜡颗粒在特性高分子材料上的附着分布为1~10μm级细小颗粒,便于其起到润滑作用。Figure 2 is a comparison of scanning electron micrographs of characteristic polymer materials and solid paraffin lubricant: (a) characteristic polymer; (b) solid paraffin lubricant prepared by the present invention. It can be seen from the figure that the attachment distribution of paraffin wax particles on the characteristic polymer material is 1-10 μm fine particles, which is convenient for it to play a lubricating role.

图3为本发明制得的固体石蜡润滑剂的激光粒度分布图。由图可见,负载了蜡粒后的特性高分子材料的粒径主要分布在10~100μm级微小颗粒,便于其起到润滑作用。Fig. 3 is the laser particle size distribution diagram of the solid paraffin lubricant prepared by the present invention. It can be seen from the figure that the particle size of the characteristic polymer material loaded with wax particles is mainly distributed in tiny particles of 10-100 μm, which is convenient for it to play a lubricating role.

根据上述的实施例对本发明作了详细描述。需说明的是,以上的实施例仅仅为了举例说明本发明而已。在不偏离本发明的精神和实质的前提下,本领域技术人员可以设计出本发明的多种替换方案和改进方案,其均应被理解为在本发明的保护范围之内。The present invention has been described in detail based on the above-mentioned embodiments. It should be noted that the above embodiments are only for illustrating the present invention. Without departing from the spirit and essence of the present invention, those skilled in the art can design various alternatives and improvements of the present invention, all of which should be understood as falling within the protection scope of the present invention.

Claims (13)

1.一种钻井液用固体石蜡润滑剂的制备方法,其包括以下步骤:1. a preparation method for drilling fluid solid paraffin lubricant, it may further comprise the steps: (1)称取如下重量配比组分:油相20-50份,氢氧化钠0.5-2份,复合乳化剂1-10份,稳定剂0.1-1份、水相37-78.4份;(1) Weigh the following components by weight: 20-50 parts of oil phase, 0.5-2 parts of sodium hydroxide, 1-10 parts of composite emulsifier, 0.1-1 part of stabilizer, and 37-78.4 parts of water phase; (2)将上述油相、氢氧化钠、复合乳化剂、稳定剂及水相按所述组分比例混合加入反应器中,70-100℃、100-2000转/分条件下,搅拌15-60min,制得液体润滑剂;(2) Mix the above-mentioned oil phase, sodium hydroxide, compound emulsifier, stabilizer and water phase into the reactor according to the stated component ratio, and stir for 15- 60min, obtained liquid lubricant; (3)称取如下重量配比组分:特性高分子材料50-80份,步骤(2)获得的液体润滑剂20-50份;(3) Weigh the following components by weight: 50-80 parts of characteristic polymer material, 20-50 parts of liquid lubricant obtained in step (2); (4)将上述液体润滑剂与特性高分子按所述组分比例侵浸反应;(4) impregnating and reacting the above-mentioned liquid lubricant and the characteristic macromolecule according to the component ratio; (5)经60-100℃低温烘干、粉碎工艺,得到钻井液用固体润滑剂;(5) After low-temperature drying and crushing at 60-100°C, a solid lubricant for drilling fluid is obtained; 其特征在于:It is characterized by: 所述油相为矿物油和蜡质物;The oily phase is mineral oil and waxy matter; 所述复合乳化剂为多元醇酯类非离子表面活性剂;The composite emulsifier is a polyol ester nonionic surfactant; 所述稳定剂为无机纳米粒子,所述无机纳米粒子为白炭黑、超细碳酸钙、膨润土凝胶、凹凸棒土凝胶或其任意比例的混合物;和/或The stabilizer is an inorganic nanoparticle, and the inorganic nanoparticle is white carbon black, ultrafine calcium carbonate, bentonite gel, attapulgite gel or a mixture thereof in any proportion; and/or 所述特性高分子材料为具有降滤失作用的水溶性高分子材料,所述具有降滤失作用的水溶性高分子材料为硅油接枝淀粉、纤维素接枝淀粉、聚丙烯腈铵盐(NH4PAN)、聚(丙烯腈-丙烯酰胺)铵盐、褐煤树脂(SPNH)、磺化褐煤(SMC)或其任意比例的混合物。The characteristic polymer material is a water-soluble polymer material with fluid loss reducing effect, and the water-soluble polymer material with fluid loss reducing effect is silicone oil grafted starch, cellulose grafted starch, polyacrylonitrile ammonium salt ( NH 4 PAN), poly(acrylonitrile-acrylamide) ammonium salt, lignite resin (SPNH), sulfonated lignite (SMC) or a mixture thereof in any proportion. 2.根据权利要求1的制备方法,其特征在于,所述矿物油是液体石蜡、7#白油、10#白油、15#白油、26#白油或46#白油;和/或所述蜡质物为石蜡、蜡膏、植物蜡、蜡模回收蜡、油井清蜡作业回收蜡。2. according to the preparation method of claim 1, it is characterized in that, described mineral oil is liquid paraffin, 7# white oil, 10# white oil, 15# white oil, 26# white oil or 46# white oil; And/or The waxy substance is paraffin wax, wax paste, vegetable wax, wax recovered from wax patterns, and wax recovered from oil well wax removal operations. 3.根据权利要求2的制备方法,其特征在于,所述矿物油为46#白油,所述蜡质物为蜡膏。3. according to the preparation method of claim 2, it is characterized in that, described mineral oil is 46# white oil, and described waxy thing is wax ointment. 4.根据权利要求1或2的制备方法,其特征在于,所述多元醇酯类非离子表面活性剂为Span和Tween系列表面活性剂。4. according to the preparation method of claim 1 or 2, it is characterized in that, described polyol ester nonionic surfactant is Span and Tween series surfactant. 5.根据权利要求4的制备方法,其特征在于,所述多元醇酯类非离子表面活性剂为Span20、Span40、Span60或Span80以及Tween20、Tween40、Tween60或Tween80。5. according to the preparation method of claim 4, it is characterized in that, described polyol ester nonionic surfactant is Span20, Span40, Span60 or Span80 and Tween20, Tween40, Tween60 or Tween80. 6.根据权利要求5的制备方法,其特征在于,所述多元醇酯类非离子表面活性剂为Span80和Tween80。6. according to the preparation method of claim 5, it is characterized in that, described polyol ester nonionic surfactant is Span80 and Tween80. 7.根据权利要求1或2的制备方法,其特征在于,所述无机纳米粒子稳定剂为白炭黑和凹凸棒土凝胶。7. The preparation method according to claim 1 or 2, characterized in that, the inorganic nanoparticle stabilizer is white carbon black and attapulgite gel. 8.根据权利要求1或2的制备方法,其特征在于,所述具有降滤失作用的特性水溶性高分子材料为纤维素接枝淀粉。8. The preparation method according to claim 1 or 2, characterized in that, the characteristic water-soluble polymer material having fluid loss reducing effect is cellulose grafted starch. 9.根据权利要求1或2的制备方法,其特征在于,步骤(2)所述组分以80-100℃、200-500转/分条件搅拌20-40min;和/或步骤(5)所述组分以70-90℃条件烘干。9. The preparation method according to claim 1 or 2, characterized in that, the components described in step (2) are stirred at 80-100°C and 200-500 rpm for 20-40min; and/or the components described in step (5) The above components are dried at 70-90°C. 10.根据权利要求1至9之一的方法制得的钻井液用固体石蜡润滑剂,其特征在于,所述固体润滑剂以100重量份计,组分为:特性高分子材料50-80份,液体润滑剂20-50份;其中:10. The solid paraffin lubricant for drilling fluid prepared by the method according to one of claims 1 to 9, characterized in that, the solid lubricant is based on 100 parts by weight, and the components are: 50-80 parts of characteristic polymer materials , 20-50 parts of liquid lubricant; wherein: 所述液体润滑剂包含以下重量配比的组分:油相30-50份,氢氧化钠0.5-2份,复合乳化剂2-6份,稳定剂0.1-1份,水相41-67.4份,基于100重量份液体润滑剂而言;The liquid lubricant comprises the following components by weight: 30-50 parts of oil phase, 0.5-2 parts of sodium hydroxide, 2-6 parts of composite emulsifier, 0.1-1 part of stabilizer, and 41-67.4 parts of water phase , based on 100 parts by weight of liquid lubricant; 其中:in: 所述油相为矿物油和蜡质物;The oily phase is mineral oil and waxy matter; 所述复合乳化剂为多元醇酯类非离子表面活性剂;The composite emulsifier is a polyol ester nonionic surfactant; 所述稳定剂为无机纳米粒子,所述无机纳米粒子为白炭黑、超细碳酸钙、膨润土凝胶、凹凸棒土凝胶或其任意比例的混合物;The stabilizer is an inorganic nanoparticle, and the inorganic nanoparticle is white carbon black, superfine calcium carbonate, bentonite gel, attapulgite gel or a mixture thereof in any proportion; 所述特性高分子材料为具有降滤失作用的水溶性高分子材料,所述具有降滤失作用的水溶性高分子材料为硅油接枝淀粉、纤维素接枝淀粉、聚丙烯腈铵盐(NH4PAN)、聚(丙烯腈-丙烯酰胺)铵盐、褐煤树脂(SPNH)、磺化褐煤(SMC)或其任意比例的混合物。The characteristic polymer material is a water-soluble polymer material with fluid loss reducing effect, and the water-soluble polymer material with fluid loss reducing effect is silicone oil grafted starch, cellulose grafted starch, polyacrylonitrile ammonium salt ( NH4PAN), poly(acrylonitrile-acrylamide) ammonium salt, lignite resin (SPNH), sulfonated lignite (SMC) or a mixture thereof in any proportion. 11.根据权利要求10的钻井液用固体石蜡润滑剂,其特征在于,所述固体润滑剂以100重量份计,组分为:特性高分子材料为55-75份,液体润滑剂为25-45份。11. The solid paraffin lubricant for drilling fluid according to claim 10, characterized in that, in 100 parts by weight, the solid lubricant comprises: 55-75 parts of characteristic polymer material, and 25-75 parts of liquid lubricant. 45 servings. 12.根据权利要求10或11的钻井液用固体石蜡润滑剂,其特征在于,所述固体润滑剂包含:特性高分子材料60-70重量份,液体润滑剂30-40重量份;和/或12. The solid paraffin lubricant for drilling fluid according to claim 10 or 11, characterized in that, the solid lubricant comprises: 60-70 parts by weight of a characteristic polymer material, 30-40 parts by weight of a liquid lubricant; and/or 所述液体润滑剂包含以下重量配比的组分:油相40-45份,氢氧化钠0.8-1份,复合乳化剂3-5份,稳定剂0.5-0.8份,水相48.2-55.7份,基于100重量份液体润滑剂而言。The liquid lubricant comprises the following components by weight: 40-45 parts of oil phase, 0.8-1 part of sodium hydroxide, 3-5 parts of compound emulsifier, 0.5-0.8 parts of stabilizer, and 48.2-55.7 parts of water phase , Based on 100 parts by weight of liquid lubricant. 13.根据权利要求10或11的钻井液用固体石蜡润滑剂,其特征在于,所述矿物油为46#白油;和/或所述蜡质物为蜡膏;所述多元醇酯类非离子表面活性剂为Span80和Tween80;和/或所述无机纳米粒子稳定剂为白炭黑和凹凸棒土凝胶;和/或所述具有降滤失作用的特性水溶性高分子材料为纤维素接枝淀粉。13. according to the solid paraffin lubricant for drilling fluid of claim 10 or 11, it is characterized in that, described mineral oil is 46# white oil; And/or described waxy thing is wax ointment; Described polyol ester non- The ionic surfactant is Span80 and Tween80; and/or the inorganic nanoparticle stabilizer is white carbon black and attapulgite gel; and/or the characteristic water-soluble polymer material with fluid loss reducing effect is cellulose grafted starch.
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