CN109825331B - Preparation and use method of emulsified crude oil solid demulsifier in microwave field - Google Patents
Preparation and use method of emulsified crude oil solid demulsifier in microwave field Download PDFInfo
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- CN109825331B CN109825331B CN201910182558.9A CN201910182558A CN109825331B CN 109825331 B CN109825331 B CN 109825331B CN 201910182558 A CN201910182558 A CN 201910182558A CN 109825331 B CN109825331 B CN 109825331B
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- 239000010779 crude oil Substances 0.000 title claims abstract description 28
- 239000007787 solid Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 15
- 239000012798 spherical particle Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 230000005855 radiation Effects 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 5
- SHKUUQIDMUMQQK-UHFFFAOYSA-N 2-[4-(oxiran-2-ylmethoxy)butoxymethyl]oxirane Chemical compound C1OC1COCCCCOCC1CO1 SHKUUQIDMUMQQK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 4
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 4
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims abstract description 4
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 4
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 4
- 229960004853 betadex Drugs 0.000 claims abstract description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 229940057995 liquid paraffin Drugs 0.000 claims abstract description 4
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims abstract description 4
- 239000008108 microcrystalline cellulose Substances 0.000 claims abstract description 4
- 229940016286 microcrystalline cellulose Drugs 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims 1
- 239000013043 chemical agent Substances 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract 2
- PTHCMJGKKRQCBF-UHFFFAOYSA-N Cellulose, microcrystalline Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC)C(CO)O1 PTHCMJGKKRQCBF-UHFFFAOYSA-N 0.000 abstract 1
- 229940105329 carboxymethylcellulose Drugs 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 208000005156 Dehydration Diseases 0.000 description 5
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 239000000839 emulsion Substances 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011033 desalting Methods 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 235000010980 cellulose Nutrition 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000002332 oil field water Substances 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- -1 salt ions Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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Abstract
The invention relates to a preparation and use method of a crude oil solid demulsifier in a microwave field, which is technically characterized in that beta-cyclodextrin, carboxymethyl cellulose, microcrystalline cellulose, graphene and 1, 4-butanediol diglycidyl ether are sequentially dissolved in a sodium hydroxide solution under stirring, the mixture is continuously stirred for a certain time, liquid paraffin is poured, the mixture is stirred at 30 ℃ to react for 24 hours, and then washing and drying are carried out to obtain supermolecule graphene doped solid demulsifier spherical particles with different particle sizes. The preparation method of the demulsifier is simple and easy to implement, crude oil demulsification is realized through a fixed bed under microwave field radiation, and the demulsifier has the characteristics of cleanness, environmental protection and no introduction of new chemical agents in the treatment process.
Description
Technical Field
The invention relates to a preparation and application method of a solid demulsifier for demulsification of crude oil by microwave radiation in oil field enterprises.
Technical Field
After half a century of crude oil exploitation in China, most oil fields are enhanced by water injection, chemical agent injection and other strengthening means to improve the recovery efficiency. Although the chemical agent obviously improves the recovery efficiency of crude oil, the emulsification behavior of the crude oil tends to be more stable due to the complexity of chemical components and emulsion structures, the difficulty of ground demulsification and dehydration operation is increased, and the treatment cost is also increased year by year.
Because the water in the crude oil contains salt ions such as sodium, calcium, magnesium and the like, the most common method for oil field ground engineering is to add a demulsifier under the condition of an electric field to demulsify. Electric field demulsification is also called electric desalting because electric field demulsification mainly achieves the aim of destroying the stability of the aqueous crude oil emulsion through desalting.
Crude oil demulsification technology adopting microwave or ultrasonic auxiliary chemical agent [ Xiarixin, palace. sand-containing emulsified crude oil demulsification method, ZL200710158560. X; a high-efficiency crude oil dehydration treatment system and a dehydration treatment method, such as sangyuyuan, ZL200610046997.X, have better effect, but have the problems that a chemical demulsifier used in the prior art is liquid, is dissolved in an oil phase or a water phase, the former causes difficulty in subsequent processing of a refinery, and the latter increases the burden of an oil field water treatment process.
The invention aims to: based on microwave responsiveness, the solid demulsifier can convert electromagnetic wave energy into heat energy under microwave radiation and can effectively provide demulsification performance, and particularly provides a preparation and use method of the solid demulsifier for emulsifying crude oil in a microwave field.
Disclosure of Invention
In order to achieve the purpose, the invention adopts the following technical scheme:
accurately measuring 20mL of NaOH solution with the concentration of 1mol/L, pouring the NaOH solution into a 500mL beaker, placing the beaker on a magnetic stirrer to start stirring at the rotating speed of 300-2000 rpm, sequentially adding 3.00-5.00 g of beta-cyclodextrin, 0.70-0.85 g of carboxymethyl cellulose, 0.45-0.65 g of microcrystalline cellulose and 0.03-0.07 g of graphene, after 15min, adding 6g of 1, 4-butanediol diglycidyl ether, continuing stirring for 15min, pouring 200mL of liquid paraffin, stirring at 30 ℃, washing the product for 3-5 times by using a mixed solution of deionized water and acetone with the volume ratio of 2:1 after 24h, washing for 2-3 times by using deionized water, and drying for 24h at 40 ℃ to finally obtain the supermolecule graphene doped solid demulsifier spherical particles with different particle sizes.
3.5g of spherical particles of the supermolecule graphene doped solid demulsifier are taken, filled according to the attached drawing 1 and supported and fixed by a glass wire mesh, a microwave radiation button is opened, emulsified crude oil is added from the upper end, and the oil and water in the crude oil can be well separated from a collector flowing out of a microwave reactor.
Compared with the prior art, the invention has the beneficial effects that: the graphene has a high dielectric constant, and can be uniformly dispersed in the supramolecular cyclodextrin cellulose spheres by the method, so that the graphene is beneficial to receiving microwave energy. When the emulsified crude oil containing water contacts with the microspheres, the microwave and the crude oil emulsion react on the surfaces of the microspheres, and the stability of the crude oil emulsion is destroyed.
Drawings
Fig. 1 shows a spherical particle structure of a supramolecular graphene doped solid demulsifier.
Reference numbers in the figures:
1 emulsifying crude oil; 2, a fixed bed; 3, a microwave generator; 4 solid emulsion breaker particles; 5, de-emulsifying the crude oil; 6 Water
Detailed Description
The invention is further illustrated by the following examples.
Example 1
Accurately measuring 20mL of NaOH solution with the concentration of 1mol/L, pouring the NaOH solution into a 500mL beaker, placing the beaker on a magnetic stirrer, starting stirring at the rotating speed of 1000rpm, sequentially adding 4.00g of beta-cyclodextrin, 0.75g of carboxymethyl cellulose, 0.50g of microcrystalline cellulose and 0.05g of graphene, adding 6g of 1, 4-butanediol diglycidyl ether after 15min, continuing stirring for 15min, pouring 200mL of liquid paraffin, stirring at 30 ℃, washing the product for 3-5 times by using a mixed solution of deionized water and acetone with the volume ratio of 2:1 after 24h, washing the product for 2-3 times by using deionized water, drying the product for 24h at 40 ℃, and finally obtaining 7.23g of spherical demulsifier particles doped with supramolecular graphene with the average diameter of 3 mm.
Comparative example 1
The rotation speed described in example 1 was changed to 1800rpm, and other conditions were not changed, and the result showed that 7.15g of spherical particles of supramolecular graphene-doped solid demulsifier were obtained, but the average diameter was changed to 2.12 mm.
Comparative example 2
The graphene addition described in example 1 was increased to 0.08g, and other conditions were unchanged, and the results showed that 7.21g of supramolecular graphene-doped solid demulsifier spherical particles were obtained.
Application example 1
3.5g of the spherical particles of the supramolecular graphene doped solid demulsifier obtained in the example 1 are filled as shown in the attached drawing 1, are firmly supported by a glass wire mesh, are placed into a microwave generator with the frequency of 2450MHz, a microwave radiation button is started, emulsified crude oil is added from the upper end, and the water content in the crude oil is measured from a collector to be 0.05 percent, and the dehydration rate is 98.18 percent.
Application example 2
3.5g of the spherical particles of the supramolecular graphene doped solid demulsifier obtained in the comparative example 2 are filled as shown in the attached drawing 1, are firmly supported by a glass wire mesh, are placed into a microwave generator with the frequency of 2450MHz, a microwave radiation button is started, emulsified crude oil is added from the upper end, and the water content in the crude oil is measured from a collector to be 0.02 percent, and the dehydration rate is 99.57 percent.
Claims (2)
1. A preparation method of a solid demulsifier for demulsification of crude oil by microwave radiation is characterized by comprising the following steps: accurately measuring 20mL of NaOH solution with the concentration of 1mol/L, pouring the NaOH solution into a 500mL beaker, placing the beaker on a magnetic stirrer to start stirring at the rotating speed of 300-2000 rpm, sequentially adding 3.00-5.00 g of beta-cyclodextrin, 0.70-0.85 g of carboxymethyl cellulose, 0.45-0.65 g of microcrystalline cellulose and 0.03-0.07 g of graphene, after 15min, adding 6g of 1, 4-butanediol diglycidyl ether, continuing stirring for 15min, pouring 200mL of liquid paraffin, stirring at 30 ℃, washing the product for 3-5 times by using a mixed solution of deionized water and acetone with the volume ratio of 2:1 after 24h, washing for 2-3 times by using deionized water, and drying for 24h at 40 ℃ to finally obtain the supermolecule graphene doped solid demulsifier spherical particles with different particle sizes.
2. The use method of the solid demulsifier for crude oil microwave radiation demulsification obtained by the preparation method of claim 1 is characterized in that: spherical particles of the supermolecule graphene-doped solid demulsifier are used as a filling agent and are filled into a fixed bed in a microwave generator, and the microwave and the solid demulsifier are demulsified cooperatively by emulsified crude oil flowing through the fixed bed.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910182558.9A CN109825331B (en) | 2019-03-12 | 2019-03-12 | Preparation and use method of emulsified crude oil solid demulsifier in microwave field |
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| CN201910182558.9A CN109825331B (en) | 2019-03-12 | 2019-03-12 | Preparation and use method of emulsified crude oil solid demulsifier in microwave field |
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| CN109825331B true CN109825331B (en) | 2021-01-12 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20150218461A1 (en) * | 2012-09-12 | 2015-08-06 | The University Of Wyoming Research Corporation D/B/A Western Research Institute | Methods for Changing Stability of Water and Oil Emulsions |
| CN104877706A (en) * | 2014-02-27 | 2015-09-02 | 中国科学院兰州化学物理研究所 | Demulsification method of oil-in-water type crude oil emulsion |
| CN108946955A (en) * | 2018-06-26 | 2018-12-07 | 江苏新亿源环保科技有限公司 | A kind of preparation method of degreaser |
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Effective date of registration: 20240105 Address after: 052371 Tian Gong Ying Xiang Xi Lang Yue Cun, Xinji City, Shijiazhuang City, Hebei Province Patentee after: Xinji Xinshuntong Chemical Co.,Ltd. Address before: 073000 West 200m northbound at the intersection of Dingzhou commercial street and Xingding Road, Baoding City, Hebei Province (No. 1910, 19th floor, building 3, jueshishan community) Patentee before: Hebei Kaitong Information Technology Service Co.,Ltd. Effective date of registration: 20240105 Address after: 073000 West 200m northbound at the intersection of Dingzhou commercial street and Xingding Road, Baoding City, Hebei Province (No. 1910, 19th floor, building 3, jueshishan community) Patentee after: Hebei Kaitong Information Technology Service Co.,Ltd. Address before: 132022 No. 45 Chengde street, Longtan District, Jilin, Jilin Patentee before: JILIN INSTITUTE OF CHEMICAL TECHNOLOGY |
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