CN104877706A - Demulsification method of oil-in-water type crude oil emulsion - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 31
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- 238000003756 stirring Methods 0.000 claims description 2
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Abstract
本发明公开了一种水包油型原油乳状液的破乳方法。该方法采用氧化石墨烯作为破乳剂，在常温下对水包油型原油乳状液进行脱水处理。水包油乳状液的脱油率大于96%，能够用于石油工业中高含水量的油水乳状液的脱水处理。The invention discloses a demulsification method for oil-in-water type crude oil emulsion. In the method, graphene oxide is used as a demulsifier, and the oil-in-water type crude oil emulsion is dehydrated at normal temperature. The deoiling rate of the oil-in-water emulsion is greater than 96%, which can be used for the dehydration treatment of the oil-water emulsion with high water content in the petroleum industry.
Description
技术领域 technical field
本发明属于原油开采特别是三次采油中采出液的处理技术，具体涉及一种常温下快速破坏原油中水包油型乳状液的破乳方法。 The invention belongs to the treatment technology of produced fluid in crude oil exploitation, especially in tertiary oil recovery, and in particular relates to a demulsification method for rapidly destroying oil-in-water emulsion in crude oil at normal temperature.
背景技术 Background technique
在原油的生产加工的过程中都面临这一个重要环节，即油水乳状液的脱水处理，又称为破乳。原油开采的过程中，油水乳状液经过喷油嘴和集输管道的机械混合后，极易形成稳定的乳状液。原油乳状液会大大增加储运负担和降低输油管线的寿命。另外，在原油炼制的过程中，由于水中含有大量无机盐，常常会导致催化剂的中毒和蒸馏设备的严重腐蚀。因此，原油进入炼制之前必须进行破乳脱水处理。 In the process of crude oil production and processing, we all face this important link, that is, the dehydration treatment of oil-water emulsion, also known as demulsification. In the process of crude oil extraction, the oil-water emulsion is easily formed into a stable emulsion after being mechanically mixed by the injector and the gathering pipeline. Crude oil emulsion will greatly increase the storage and transportation burden and reduce the life of oil pipelines. In addition, in the process of refining crude oil, because the water contains a large amount of inorganic salts, it often leads to catalyst poisoning and severe corrosion of distillation equipment. Therefore, demulsification and dehydration must be carried out before crude oil enters refining.
油水乳状液之所以能够稳定存在，主要是因为原油中沥青质、胶质和有机酸等极性物质在油水界面形成了牢固的交叉网络结构的保护膜。保护膜的存在，使液滴之间无法进行聚集分层，因此破坏油水乳状液稳定性的关键在于破坏油水界面保护膜。 The reason why oil-water emulsion can exist stably is mainly because polar substances such as asphaltene, colloid and organic acid in crude oil form a strong cross-network structure protective film at the oil-water interface. The existence of the protective film makes it impossible for the droplets to aggregate and stratify. Therefore, the key to destroying the stability of the oil-water emulsion is to destroy the protective film at the oil-water interface.
在油气田开发的过程中，一次采油和二次采油采出液主要为油包水型乳状液，采用电—化学联合破乳的方式即能实现油水分离。目前，我国各大油田相继进入高含水开发阶段。三次采油技术被广泛使用，油田采出液多为水包油型乳状液或者复杂的复合型乳状液。这种采出液含有大量的水而导致常规方法的失效。具体来说，这种乳状液进入电脱水器中易破坏电场，造成跳闸，连续生产难以顺利进行。因此，急需研发出高效快速处理水包油型乳状液的破乳方法。 In the process of oil and gas field development, the primary oil recovery and secondary oil recovery fluids are mainly water-in-oil emulsions, and the oil-water separation can be realized by means of combined electrochemical-chemical demulsification. At present, major oil fields in my country have successively entered the stage of high water cut development. The tertiary oil recovery technology is widely used, and the oilfield produced fluids are mostly oil-in-water emulsions or complex composite emulsions. This production fluid contains a large amount of water, which leads to the failure of conventional methods. Specifically, if this emulsion enters the electric dehydrator, it is easy to destroy the electric field, causing tripping, and continuous production is difficult to proceed smoothly. Therefore, there is an urgent need to develop an efficient and rapid demulsification method for oil-in-water emulsions.
发明内容 Contents of the invention
本发明的目的是提供一种对原油开采特别是三次采油中采出液具有良好破乳效果的破乳方法。 The object of the present invention is to provide a demulsification method which has a good demulsification effect on the produced fluid in crude oil exploitation, especially in tertiary oil recovery.
一种水包油型原油乳状液的破乳方法，其特征在于该方法采用氧化石墨烯作为破乳剂，在常温下对水包油型原油乳状液进行脱水处理。 A method for demulsifying an oil-in-water crude oil emulsion is characterized in that the method uses graphene oxide as a demulsifier to dehydrate the oil-in-water crude oil emulsion at normal temperature.
本发明采用少量的氧化石墨烯即可强烈地破坏油水界面的保护膜，从而使油水乳状液的稳定性下降，经充分震荡，油滴之间通过碰撞而迅速聚集，与水快速分离，并悬浮于水面，从而实现了油水分离的目的。 The invention uses a small amount of graphene oxide to strongly destroy the protective film of the oil-water interface, thereby reducing the stability of the oil-water emulsion. After sufficient vibration, the oil droplets quickly gather through collisions, quickly separate from water, and suspend On the water surface, so as to achieve the purpose of oil-water separation.
一种水包油型原油乳状液的破乳方法，其特征在于该方法包括以下步骤： A kind of demulsification method of oil-in-water type crude oil emulsion, it is characterized in that the method comprises the following steps:
A、将氧化石墨配制成悬浮液，并充分超声分散，获得氧化石墨烯破乳剂； A. Prepare graphite oxide into a suspension and fully ultrasonically disperse it to obtain a graphene oxide demulsifier;
B、将氧化石墨烯分散液加入到水包油型原油乳状液中，加入量为1mg/L~200mg/L，搅拌均匀，静置后进行油水分离。 B. Add the graphene oxide dispersion into the oil-in-water crude oil emulsion, the addition amount is 1mg/L~200mg/L, stir evenly, and separate the oil and water after standing.
本发明所述的1公斤氧化石墨烯破乳剂能够处理水包油型原油乳状液15-30吨。 1 kg of graphene oxide demulsifier described in the present invention can treat 15-30 tons of oil-in-water type crude oil emulsion.
本发明所述的水包油型原油乳状液中的含水量为80-99.5%。 The water content in the oil-in-water type crude oil emulsion of the present invention is 80-99.5%.
我们具体的破乳实验参照中华人民共和国石油天然气行业标准SY/T 5797-93《水包油乳状液破乳剂使用性能评定方法（瓶试法）》进行测试。参考中华人民共和国石油天然气标准SY/T5329-2012《碎屑岩油注水水质推荐指标及分析方法》定量测定出脱出水的含油量。 Our specific demulsification experiments are tested according to the People's Republic of China Petroleum and Natural Gas Industry Standard SY/T 5797-93 "Evaluation Method for Performance of Oil-in-Water Emulsion Demulsifiers (Bottle Test Method)". Refer to the Petroleum and Natural Gas Standard of the People's Republic of China SY/T5329-2012 "Recommended Indicators and Analysis Methods for Water Quality of Clastic Rock Oil Injection Water" to quantitatively measure the oil content of the extracted water.
本发明水包油型原油乳状液破乳方法中采用氧化石墨烯作为破乳剂。一般情况下，水溶性破乳剂分散液浓度越高，带入乳状液中的水量越少。然而，配制破乳剂分散液浓度时要兼顾氧化石墨烯的分散程度。破乳剂的用量可以根据乳状液中的含油量和脱出水的指标要求确定或通过破乳剂浓度优化实验确定。一般来说，水包油型乳状液中含油量越高，脱出水的含油量越低，所需破乳剂的量越大。必须指出的是，当氧化石墨烯的剂量超过最佳使用范围时，脱出水的清洁度和含油量将受到影响。原因在于氧化石墨烯本身为黄褐色，并且在破乳的过程中吸附了油中的部分化合物。破乳后，过量的氧化石墨烯悬浮在水相中使得水相呈黄色，脱出水的含油量也比最佳剂量范围时略高。油水分层时，静置时间为5分钟~2小时。 Graphene oxide is used as a demulsifier in the oil-in-water crude oil emulsion demulsification method of the present invention. In general, the higher the concentration of the water-soluble demulsifier dispersion, the less water will be brought into the emulsion. However, the degree of dispersion of graphene oxide should be taken into account when preparing the concentration of the demulsifier dispersion. The dosage of the demulsifier can be determined according to the oil content in the emulsion and the index requirements of dewatering or determined through the optimization experiment of the demulsifier concentration. Generally speaking, the higher the oil content in the oil-in-water emulsion, the lower the oil content of the exfoliated water, and the greater the amount of demulsifier required. It must be pointed out that when the dosage of graphene oxide exceeds the optimal range, the cleanliness and oil content of the extracted water will be affected. The reason is that graphene oxide itself is yellowish brown, and some compounds in the oil are adsorbed during the demulsification process. After demulsification, the excess graphene oxide is suspended in the water phase to make the water phase yellow, and the oil content of the extracted water is also slightly higher than that in the optimal dosage range. When the oil and water are separated, the standing time is 5 minutes to 2 hours.
该方法处理水包油型乳状液具有以下优点： The method for processing oil-in-water emulsions has the following advantages:
1、本发明水包油乳状液的脱油率大于96%。上浮的油相含水量低，易于后续处理。脱出水含油量低，脱出水基本达到三级排放标准和回注标准。 1. The deoiling rate of the oil-in-water emulsion of the present invention is greater than 96%. The floating oil phase has low water content and is easy for subsequent treatment. The oil content of the produced water is low, and the produced water basically meets the third-level discharge standard and the reinjection standard.
2、本发明的破乳剂为氧化石墨烯分散液。此破乳剂的性质稳定，无毒无害。原料廉价易得，制备方法简单、成熟。破乳后，破乳剂可以通过简单过滤方法进行回收再利用。 2. The demulsifier of the present invention is a graphene oxide dispersion. This demulsifier is stable in nature, non-toxic and harmless. The raw materials are cheap and easy to obtain, and the preparation method is simple and mature. After demulsification, the demulsifier can be recovered and reused by simple filtration.
3、使用本发明的方法处理原油乳状液，对温度依赖程度低。测试均在常温下进行，且效果良好。对于高于常温的工作条件下，破乳效果更佳。 3. Using the method of the present invention to process crude oil emulsion has low dependence on temperature. The tests were all carried out at room temperature, and the results were good. For working conditions higher than normal temperature, the demulsification effect is better. the
4、采用此方法对水包油型原油乳状液进行脱水处理，脱水效率高、破乳时间短。乳状液在短短几分钟内即可迅速破乳。且静置时间越长，脱出水质越好。 4. Using this method to dehydrate the oil-in-water crude oil emulsion, the dehydration efficiency is high and the demulsification time is short. The emulsion breaks rapidly in just a few minutes. And the longer the standing time, the better the water quality.
5、采用此方法处理水包油型乳状液，普适性强，广泛适用于普通水包油型的原油乳状液和重质原油水包油型乳状液。 5. Using this method to treat oil-in-water emulsions has strong universality and is widely applicable to ordinary oil-in-water crude oil emulsions and heavy crude oil-in-water emulsions.
本发明能够用于石油工业中高含水量的油水乳状液的脱水处理。 The invention can be used for dehydration treatment of oil-water emulsion with high water content in petroleum industry.
具体实施方式 Detailed ways
为了更直观、准确理解本发明所述的方法及此方法的优越性，下面将通过具体的实例予以说明。但是本发明并不局限于下面的实施例。 In order to more intuitively and accurately understand the method of the present invention and its superiority, specific examples will be used below to illustrate. However, the present invention is not limited to the following examples.
实施例1： Example 1:
用去离子水配制浓度为2mg/mL的氧化石墨悬浮液,超声分散90分钟以上,以获得氧化石墨烯分散液，待用。 Prepare a graphite oxide suspension with a concentration of 2 mg/mL with deionized water, and ultrasonically disperse for more than 90 minutes to obtain a graphene oxide dispersion, which is ready for use.
分别将40g塔里木盆地原油和360g去离子水置于塑料容器中。油水混合液通过高剪切乳化机在28000rpm条件下分散3min，以获得均匀分散的含油量为10%的水包油型原油乳状液。取破乳试剂瓶若干支，并依次编号。在破乳试剂瓶中分别加入等量的乳状液，在室温条件下，静置30min。 40g of Tarim Basin crude oil and 360g of deionized water were respectively placed in plastic containers. The oil-water mixture was dispersed by a high-shear emulsifier at 28,000 rpm for 3 minutes to obtain a uniformly dispersed oil-in-water crude oil emulsion with an oil content of 10%. Take several demulsification reagent bottles and number them sequentially. Add an equal amount of emulsion to the demulsification reagent bottle, and let it stand for 30 minutes at room temperature.
将不同体积的氧化石墨烯分散液加入到破乳试剂瓶中震荡均匀、静置，观察并记录水相、油相及界面状况。 Add different volumes of graphene oxide dispersion into the demulsification reagent bottle, shake evenly, let stand, observe and record the water phase, oil phase and interface conditions.
静置60min后，参照SY/T5329-2012所述的标准分析方法，采用煤油为萃取溶剂测定脱出水中的含油量并计算脱油率。 After standing for 60 minutes, refer to the standard analysis method described in SY/T5329-2012, using kerosene as the extraction solvent to measure the oil content in the extracted water and calculate the deoiling rate.
加入破乳剂的剂量及破乳实验结果详见表1。 The dosage of added demulsifier and the results of demulsification experiment are shown in Table 1.
表1 Table 1
实施例2： Example 2:
用去离子水配制浓度为2mg/mL的氧化石墨悬浮液,超声分散90分钟以上,以获得氧化石墨烯分散液，待用。 Prepare a graphite oxide suspension with a concentration of 2 mg/mL with deionized water, and ultrasonically disperse for more than 90 minutes to obtain a graphene oxide dispersion, which is ready for use.
分别将20g塔里木盆地原油和380g去离子水置于塑料容器中。油水混合液通过高剪切乳化机在28000rpm条件下分散3min，以获得均匀分散的含油量为5%的水包油型原油乳状液。取破乳试剂瓶若干支，并依次编号。在破乳试剂瓶中分别加入等量的乳状液，在室温条件下，静置30min。 20g of Tarim Basin crude oil and 380g of deionized water were placed in plastic containers. The oil-water mixture was dispersed by a high-shear emulsifier at 28,000 rpm for 3 minutes to obtain a uniformly dispersed oil-in-water crude oil emulsion with an oil content of 5%. Take several demulsification reagent bottles and number them sequentially. Add an equal amount of emulsion to the demulsification reagent bottle, and let it stand for 30 minutes at room temperature.
将不同体积的氧化石墨烯分散液加入到破乳试剂瓶中，震荡均匀。静置、观察并记录水相、油相及界面状况。 Add different volumes of graphene oxide dispersions into the demulsification reagent bottle and shake evenly. Stand still, observe and record the condition of water phase, oil phase and interface.
静置60min后，参照SY/T5329-2012所述的标准分析方法，采用煤油为萃取溶剂测定脱出水中的含油量并计算脱油率。 After standing for 60 minutes, refer to the standard analysis method described in SY/T5329-2012, using kerosene as the extraction solvent to measure the oil content in the extracted water and calculate the deoiling rate.
加入破乳剂的剂量及破乳实验结果详见表2。 The dosage of added demulsifier and the results of demulsification experiment are shown in Table 2.
表2 Table 2
实施例3： Example 3:
用去离子水配制浓度为2mg/mL的氧化石墨悬浮液,超声分散90分钟以上,以获得氧化石墨烯分散液，待用。 Prepare a graphite oxide suspension with a concentration of 2 mg/mL with deionized water, and ultrasonically disperse for more than 90 minutes to obtain a graphene oxide dispersion, which is ready for use.
分别将2g塔里木盆地原油和398g去离子水置于塑料容器中。油水混合液通过高剪切乳化机在28000rpm条件下分散3min，以获得均匀分散的含油量为0.5%的水包油型原油乳状液。取破乳试剂瓶若干支，并依次编号。在破乳试剂瓶中分别加入等量的乳状液，在室温条件下，静置30min。 2g of Tarim Basin crude oil and 398g of deionized water were placed in plastic containers. The oil-water mixture was dispersed by a high-shear emulsifier at 28,000 rpm for 3 minutes to obtain a uniformly dispersed oil-in-water crude oil emulsion with an oil content of 0.5%. Take several demulsification reagent bottles and number them sequentially. Add an equal amount of emulsion to the demulsification reagent bottle, and let it stand for 30 minutes at room temperature.
将不同体积的氧化石墨烯分散液加入到破乳试剂瓶中，震荡均匀。静置、观察并记录水相、油相及界面状况。 Add different volumes of graphene oxide dispersions into the demulsification reagent bottle and shake evenly. Stand still, observe and record the condition of water phase, oil phase and interface.
静置60min后，参照SY/T5329-2012所述的标准分析方法，采用煤油为萃取溶剂测定脱出水中的含油量并计算脱油率。 After standing for 60 minutes, refer to the standard analysis method described in SY/T5329-2012, using kerosene as the extraction solvent to measure the oil content in the extracted water and calculate the deoiling rate.
加入破乳剂的剂量及破乳实验结果详见表3。 The dosage of added demulsifier and the results of demulsification experiment are shown in Table 3.
表3 table 3
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106219669A (en) * | 2016-08-01 | 2016-12-14 | 山东交通学院 | A kind of preparation method of magnetic oxygenated Graphene demulsifier |
| CN106978995A (en) * | 2017-05-03 | 2017-07-25 | 中国石油天然气股份有限公司 | Online metering device and method for compact oil surfactant displacement huff and puff experiment |
| CN109825331A (en) * | 2019-03-12 | 2019-05-31 | 吉林化工学院 | Preparation and use method of emulsified crude oil solid demulsifier in microwave field |
| CN110639240A (en) * | 2019-09-24 | 2020-01-03 | 中国科学院兰州化学物理研究所 | Preparation and application of magnetic inorganic clay-graphene composite demulsification material |
| CN111394080A (en) * | 2019-12-30 | 2020-07-10 | 浙江工业大学 | A kind of heavy oil viscosity reducer and using method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106219669A (en) * | 2016-08-01 | 2016-12-14 | 山东交通学院 | A kind of preparation method of magnetic oxygenated Graphene demulsifier |
| CN106219669B (en) * | 2016-08-01 | 2019-03-29 | 山东交通学院 | A kind of preparation method of magnetic oxygenated graphene demulsifier |
| CN106978995A (en) * | 2017-05-03 | 2017-07-25 | 中国石油天然气股份有限公司 | Online metering device and method for compact oil surfactant displacement huff and puff experiment |
| CN106978995B (en) * | 2017-05-03 | 2019-09-10 | 中国石油天然气股份有限公司 | On-line metering device and method for tight oil surfactant displacement huff and puff experiment |
| CN109825331A (en) * | 2019-03-12 | 2019-05-31 | 吉林化工学院 | Preparation and use method of emulsified crude oil solid demulsifier in microwave field |
| CN110639240A (en) * | 2019-09-24 | 2020-01-03 | 中国科学院兰州化学物理研究所 | Preparation and application of magnetic inorganic clay-graphene composite demulsification material |
| CN111394080A (en) * | 2019-12-30 | 2020-07-10 | 浙江工业大学 | A kind of heavy oil viscosity reducer and using method thereof |
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