CN107880866A - 一种稠油原位催化改质金属纳米晶降粘剂及其制备方法 - Google Patents
一种稠油原位催化改质金属纳米晶降粘剂及其制备方法 Download PDFInfo
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Abstract
本发明属于稠油开采、集输和加工领域,特别涉及一种稠油原位催化改质金属纳米晶降粘剂及其制备方法。本发明所要解决的技术问题是提供一种尺寸均一、形貌良好的稠油降粘用油溶性金属纳米晶降粘剂及其制备方法。该降粘剂制备方法为:采用无机或有机溶液作为还原剂在一定温度和无氧条件下,将金属有机盐还原为金属纳米胶体溶液,并将所得溶液用乙醇洗涤、离心分离即得金属纳米晶降粘剂。本发明提供的金属纳米晶降粘剂制备方法简单可控,晶粒尺寸均一,并能均匀分散于稠油中。将其用于渤海稠油原位催化改质反应,降粘效果明显,特别是低粘度范围内降粘效果显著。
Description
技术领域
本发明涉及稠油开采、集输和加工领域,特别涉及一种稠油原位催化改质金属纳米晶降粘剂及其制备方法。
背景技术
近年来常规易开采原油储量不断减少,已难以满足全球日益增长的能源需求,有效开发稠油和超稠油资源已变得十分重要。稠油是石油资源的重要组成部分,全球现存的石油储备70%左右都是很难开采的稠油,因此具有比常规石油资源高数倍的资源潜力。稠油由于具有粘度大、流动性差、凝点高等特性,使得常规开采方法的采收率都极低。提高稠油采收率的关键是降低稠油粘度、提高稠油流动性。目前稠油开采技术的发展趋势是借鉴稠油炼化和改质的思路,尝试使稠油在地下实现原位催化改质,将稠油中的大分子部分裂解为小分子,不可逆地降低稠油粘度,从而达到易于开采的目的。该项技术的关键是采用高催化选择性、良好分散性和高密度活性中心的降粘剂,因此研发新型高效的稠油降粘剂具有重要的战略意义。
鉴于常规的过渡金属络合物类型的降粘剂存在降粘效果不佳等缺点,本发明采用液相还原法制备一种金属纳米晶降粘剂,该降粘剂对稠油的降粘改质效果非常显著。
发明内容
本发明所要解决的技术问题是提供一种稠油原位催化改质金属纳米晶降粘剂的制备方法,该降粘剂的活性组分为金属纳米颗粒,采用无机或有机溶液作为还原剂,将金属有机盐还原为金属纳米颗粒并以该形式存在于降粘剂中。本发明提供的金属纳米晶降粘剂制备方法简单可控,颗粒尺寸均一,将其用于稠油原位催化改质反应,降粘效果明显。
本发明的技术方案:
本发明提供了一种稠油原位催化改质金属纳米晶降粘剂,将金属有机盐还原为金属纳米颗粒作为活性组分制备而成。
本发明提供的上述用于稠油原位催化改质的金属纳米晶降粘剂的制备方法,即在一定温度和无氧条件下,采用液相还原法将金属有机盐还原为金属纳米胶体溶液,然后经乙醇洗涤3次,离心后获得尺寸均一的油溶性金属纳米晶降粘剂。具体步骤如下:
1)将0.1-0.2g金属有机盐、7.66mL有机胺和有机酸混合加入到50mL三颈烧瓶中,磁力搅拌充分溶解,并升温至60-180℃,完全去除体系中的水分及氧气,然后将0.10-0.15g还原剂加入到上述溶液中,待还原反应充分后,降温至30℃,获得金属纳米晶胶体溶液。
2)向步骤(1)所得胶体溶液加入30mL乙醇溶液,洗涤并离心(10000r/min,10min),获得金属纳米晶降粘剂。
本发明具有以下有益效果:
本发明金属纳米晶降粘剂的制备过程中,采用无机或有机溶液作为还原剂,制备方法简单可控,所制备的金属纳米晶降粘剂油溶性良好,金属纳米晶表面的有机配体能够有效阻止金属纳米颗粒的团聚,易分散在有机溶剂中;制备的金属纳米晶降粘剂稳定性好,在稠油原位改质反应中降粘效果明显。
附图说明
图1是本发明的工艺流程图。
图2是反应温度分别为90℃、110℃、150℃和180℃时制备的镍纳米晶降粘剂的直观图像。由图可知,通过液相还原法制备的镍纳米晶降粘剂在有机溶剂中均匀分散,稳定性好。
图3是反应温度分别为90℃、110℃、150℃和180℃时制备的镍纳米晶降粘剂的透射电镜图像。由图可知,通过液相还原法制备的镍纳米晶降粘剂分布均匀,颗粒尺寸均一。
具体实施方式
以下结合具体实施例,以镍纳米晶降粘剂为例进行详细说明。
实施例1:
将0.12g有机镍、7.66mL有机胺和有机酸混合加入到50mL三颈烧瓶中,磁力搅拌充分溶解,得到澄清透明的淡绿色液体。然后升温至90℃,待完全去除体系中的水分及氧气,将0.13g还原剂加入到上述溶液中,待还原反应充分后,降温至30℃,获得黑色的纳米镍胶体溶液。向所得胶体溶液中加入30mL乙醇溶液,洗涤并离心(10000r/min,10min),获得黑色镍纳米晶降粘剂。
实施例2-4:
与实施例1相比制备镍纳米晶降粘剂仅反应温度不同,其他过程与实施例1相同,制得各温度下的成品降粘剂,实施例2至实施例4的反应温度见表1。
表1反应温度表
编号 | 反应温度(℃) |
实施例1 | 90 |
实施例2 | 110 |
实施例3 | 150 |
实施例4 | 180 |
将实施例2制备的镍纳米晶降粘剂用于渤海稠油水热裂解催化降粘性能测试,其降粘效果见表2。
表2稠油降粘效果表
综上所知,本发明降粘剂的制备,采用液相还原反应将金属有机盐还原为金属纳米颗粒,采用无机或有机溶液作为还原剂,制备过程易于控制和实现。将其用于渤海稠油原位催化改质性能测试,不可逆地降低了稠油粘度,改变了稠油流动性,可有效提高稠油采收率并方便常温条件下集输。该方法活性金属用量少,制备成本低,降粘效果明显,特别是低粘度范围内降粘效果显著,可为稠油开采、运输及炼制等领域提供参考和借鉴。
Claims (5)
1.金属纳米晶降粘剂的制备方法,其特征在于:采用无机或有机溶液作为还原剂在一定温度和无氧条件下,将活性组分有机盐还原为金属纳米颗粒。其具体制备主要经过以下步骤:
1)将0.1-0.2g金属有机盐、7.66mL有机胺和有机酸混合加入到50mL三颈烧瓶中,磁力搅拌充分溶解,并升温至60-180℃,完全去除体系中的水分及氧气,然后将0.10-0.15g还原剂加入到上述溶液中,待还原反应充分后,降温至30℃,获得金属纳米晶胶体溶液。
2)向步骤1)所得胶体溶液加入30mL乙醇溶液,洗涤并离心(10000r/min,10min),获得金属纳米晶降粘剂。
2.根据权利要求1所述的金属纳米晶降粘剂制备方法,其特征在于:1)中反应温度分别为90℃、110℃、150℃和180℃等系列温度值。
3.根据权利要求1所述的金属纳米晶降粘剂制备方法,其特征是:采用TBAB、硼氢化钠、氢化铝锂等作为还原剂,在惰性气氛下进行反应。
4.根据权利要求3所述的金属纳米晶降粘剂,其特征是:所制备的降粘剂尺寸均一,活性高,稳定性好。
5.根据权利要求1所述的金属纳米晶降粘剂制备方法,制备镍纳米晶降粘剂用于渤海稠油原位催化改质性能测试,其特征是:所制备的降粘剂具有显著的降粘效果。当降粘剂用量10%(按液体与稠油的质量比计),助剂甲苯用量5%(按液体与稠油的质量比计),250℃反应36h后,渤海稠油粘度由3272mPa·s(30℃)降至219mPa·s(30℃),降粘率可达93.3%。
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