CN112264048A - WS (WS)2-NiFe2O4Preparation method and application of/GO heavy oil catalytic viscosity reducer - Google Patents
WS (WS)2-NiFe2O4Preparation method and application of/GO heavy oil catalytic viscosity reducer Download PDFInfo
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Abstract
The invention belongs to the field of catalyst synthesis, and particularly relates to WS2‑NiFe2O4Preparation method and application of/GO heavy oil catalysis viscosity reducer. The preparation method comprises the following steps: preparing graphene oxide by a Hummers method, and then mixing the graphene oxide and NiCl2·6H2O、Fe(NO3)3·9H2Mixing O, and preparing NiFe by a hydrothermal method under the assistance of urea2O4GO, then with Na2WO4·2H2The raw materials of O and reduced glutathione are NiFe2O4Surface loading WS of/GO2Preparation of WS from Quantum dots2‑NiFe2O4A GO heavy oil catalysis viscosity reducer. The catalytic viscosity reducer can effectively reduce the viscosity of heavy crude oil and reduce the content of heavy component substances.
Description
Technical Field
The invention belongs to the field of catalyst synthesis, and particularly relates to WS2-NiFe2O4Preparation method and application of/GO heavy oil catalysis viscosity reducer.
Background
With the rapid development of industry, especially the continuous advance of industrialization in third world countries, the exploitation of conventional light oil reserves has been urgently insufficient to cope with the explosively increasing demand for fossil fuels. In the face of such increasingly tense energy situation, the development of novel energy is really a bright future, but the deep utilization of the original fossil fuel is a field with great potential, for example, the united states is transformed from an oil import country to an oil export country through the breakthrough of shale oil extraction technology.
The heavy oil is crude oil with the viscosity of more than 100mPa & s or the API gravity range of 10-20 degrees, and is characterized by large molecular weight, high viscosity, and higher proportion of resin, asphaltene and other heavy components than common crude oil; as a typical unconventional energy source, it occupies 70% of the global oil reserves, and in the future, the utilization of heavy oil will play a crucial role in meeting the global energy supply. However, the fuel must have the requirements of high calorific value, low viscosity, low freezing point, high flash point, low impurity content and low sulfur content.
Therefore, reducing high viscosity is the most important way to recover and utilize heavy oil resources. The method widely used in the exploitation of heavy oil is a physical method relying on heat, microwave/sound wave, magnetic force or thin oil displacement, and the method can improve the mobility and improve the recovery ratio of the heavy oil; but generally has the disadvantages of high energy consumption or incapability of large-scale application. While chemical recovery is the most promising technology for heavy oil utilization, catalytic hydrothermal decomposition is the decomposition of heavy components mediated by injected hot steam with the help of a catalyst, and the viscosity of heavy crude oil is irreversibly reduced by the catalyst, with extremely high efficiency. The existing catalytic viscosity reducer still has the problems of poor thermal stability and low efficiency, and cannot achieve an ideal viscosity reduction effect.
Disclosure of Invention
Aiming at the problems of low catalytic efficiency and poor viscosity reduction effect of the catalytic viscosity reducer in the prior art, the invention provides WS2-NiFe2O4Preparation method and application of/GO heavy oil catalysis viscosity reducer.
In order to achieve the purpose, the invention adopts the following technical scheme:
WS (WS)2-NiFe2O4The preparation method of the/GO heavy oil catalytic viscosity reducer comprises the following steps:
the method comprises the following steps: preparing graphene oxide by using a Hummers method; sequentially adding a certain amount of potassium nitrate and graphite powder into a proper amount of concentrated sulfuric acid under an ice bath condition, stirring for 20-30min, slowly adding a proper amount of potassium permanganate into the solution, placing the solution at a water bath temperature of 35-38 ℃ after the addition is finished, quickly stirring for 2-3h, then slowly dropping a proper amount of deionized water into the mixed solution, and continuously stirring for 15-20min at a system temperature of 90-95 ℃; and then, dropwise adding a proper amount of hydrogen peroxide into the solution at room temperature until the solution is bright yellow, performing suction filtration, washing the solution for multiple times by using dilute hydrochloric acid, performing centrifugal washing by using deionized water until the washing solution is neutral, and then placing the sample in a vacuum oven at 50-60 ℃ for drying to obtain the graphene oxide.
Step two: at room temperature, adding a certain amount of NiCl2·6H2O and Fe (NO)3)3·9H2Adding O into a proper amount of deionized water, performing ultrasonic treatment for 5-8min, adding a certain amount of urea into the solution, simply stirring, adding the graphene oxide prepared in the step one, performing ultrasonic treatment for 20-30min at room temperature, transferring the mixed solution into a reaction kettle, reacting for 12-15h at 190 ℃ at 180 ℃, cooling to room temperature, centrifuging, repeatedly washing for 6-8 times by using deionized water, and then placing the sample in a vacuum drying box at 70-80 ℃ for 10-12h to obtain NiFe2O4a/GO material.
Step three: mixing Na2WO4·2H2Adding O into a proper amount of deionized water, stirring for 6-8min, and adjusting the pH value of the mixed solution to about 6 by using dilute hydrochloric acid; the NiFe prepared in the second step2O4Adding GO into deionized water, stirring in water bath at 45-50 deg.C for 15-20min, and sequentially adding reduced glutathione and Na2WO4Continuously stirring the solution for 8-10min, placing the mixed solution in a reaction kettle, preserving the temperature at 190-200 ℃ for 9-11h, cooling to room temperature, performing suction filtration, and washing with deionized water to obtain WS2-NiFe2O4A GO heavy oil catalysis viscosity reducer.
In the first step, the addition amount of graphite powder is 2-3g, the mass ratio of potassium nitrate to graphite powder is 1:1.8-1:2, the mass ratio of graphite powder to potassium permanganate is 1:3.2-1:3.5, and the volume ratio of deionized water to concentrated sulfuric acid is 1.1:1-1.3: 1.
NiCl in the second step2·6H2The mass ratio of O to graphene oxide is 0.63:1-0.71:1, and NiCl2·6H2O and Fe (NO)3)3·9H2The molar ratio of O is 1:2, NiCl2·6H2The mass ratio of the O to the urea is 1:1.2-1: 1.4.
Na in the third step2WO4·2H2O and NiFe2O4The mass ratio of the/GO is 0.45:1-0.57:1, Na2WO4·2H2The mass ratio of the O to the reduced glutathione is 1:13-1: 15.
Preferably, in the first step, the concentration of the graphite powder in the concentrated sulfuric acid is 0.03g/ml, the dropping speeds of the deionized water and the hydrogen peroxide are both 3ml/min, and the concentration of the dilute hydrochloric acid is 4 mol/L.
Preferably, NiCl is adopted in the second step2·6H2The concentration of O in deionized water was 15 mg/ml.
Preferably, Na in step three2WO4·2H2The concentration of O in deionized water is 0.01g/ml, the concentration of dilute hydrochloric acid is 0.1M, Na2WO4The dropping rate of the solution was 5 ml/min.
The invention also provides another technical scheme, wherein the heavy oil catalysis viscosity reducer prepared by the method comprises NiFe2O4The load on the graphene oxide is 62-70 wt%, WS2Quantum dot in NiFe2O4The loading on/GO is between 34 and 43 wt%.
Another aspect of the present invention provides the above WS2-NiFe2O4The application of the/GO heavy oil catalytic viscosity reducer in the degradation of heavy crude oil comprises the following steps: after heavy oil, catalyst which accounts for 1-1.3 wt% of the weight of the heavy oil and reservoir water which accounts for 10-15 wt% of the weight of the heavy oil are mixed, the concentration of the crude oil can be effectively reduced after a period of high-temperature reaction.
Has the advantages that: the catalytic viscosity reducer prepared by the invention has good magnetism, and the catalyst is more convenient to recycle. On one hand, the decomposition of heavy components can be promoted through the interaction of pi-pi bonds between the graphene and aromatic hydrocarbon structures in heavy oil by taking the graphene as a substrate; and nano-sized WS2And NiFe2O4The load on the matrix can prevent agglomeration in the hydrothermal decomposition process, and the utilization efficiency of the catalytic component is improved; promotes the removal of S-containing components and prevents carbon deposition to improve the pot life of the catalyst. WS in the present invention2The catalyst is quantum dot in size, and the catalyst can play a role in sensitization when loaded on the catalyst, so that the cracking capability of the catalyst on C-S bonds is improved.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The method comprises the following steps: sequentially adding 1.11g of potassium nitrate and 2g of graphite powder into 66.6ml of concentrated sulfuric acid under an ice bath condition, stirring for 20min, slowly adding 7g of potassium permanganate into the solution, placing the solution into a water bath temperature of 35 ℃ after the addition is finished, quickly stirring for 2h, then slowly dropping 86.6ml of deionized water into the mixed solution, and controlling the system temperature to be 95 ℃ and continuously stirring for 15 min; and then, dropwise adding a proper amount of hydrogen peroxide into the solution at room temperature until the solution is bright yellow, performing suction filtration, washing the solution for multiple times by using dilute hydrochloric acid, then centrifugally washing the solution by using deionized water until the washing solution is neutral, and then placing the sample in a vacuum oven at 60 ℃ for drying to obtain the graphene oxide.
Step two: 1.15g of NiCl are added at room temperature2·6H2O and 3.91g Fe (NO)3)3·9H2Putting O into 76.7ml deionized water, performing ultrasonic treatment for 5min, adding 1.61g of urea into the solution, simply stirring, adding 1.62g of graphene oxide prepared in the step one, performing ultrasonic treatment at room temperature for 20min, transferring the mixed solution into a reaction kettle, reacting at 180 ℃ for 15h, cooling to room temperature, centrifuging, repeatedly washing with deionized water for 8 times, and then putting the sample into a vacuum drying oven at 70 ℃ for 12h to obtain NiFe2O4a/GO material.
Step three: 0.86g of Na2WO4·2H2Adding O into 86ml deionized water, stirring for 8min, and adjusting the pH value of the mixed solution to about 6 by using dilute hydrochloric acid; 1.5g of NiFe obtained in step two2O4/GO into deionized waterStirring in 48 deg.C water bath for 15min, adding reduced glutathione 12.9g and Na sequentially2WO4Stirring the solution for 10min, placing the mixed solution in a reaction kettle, keeping the temperature at 200 ℃ for 10h, cooling to room temperature, performing suction filtration, and washing with deionized water to obtain WS2-NiFe2O4A GO heavy oil catalysis viscosity reducer.
Mixing 1g of catalytic viscosity reducer, 100g of crude oil with viscosity of 87000mPa & s and 15g of oil layer water, and reacting at 250 ℃ for 15 h; after the reaction is finished, the viscosity is measured to be 1794 mPas, and the viscosity reduction rate is 97.9%; the colloid content is reduced by 11.8 percent, and the asphaltene content is reduced by 1.6 percent.
Example 2
The method comprises the following steps: sequentially adding 1.5g of potassium nitrate and 3g of graphite powder into 99.9ml of concentrated sulfuric acid under an ice bath condition, stirring for 30min, slowly adding 9.6g of potassium permanganate into the solution, placing the solution at the water bath temperature of 36 ℃ after the addition is finished, quickly stirring for 2h, then slowly dropping 109.9ml of deionized water into the mixed solution, and controlling the system temperature to be 91 ℃ and continuously stirring for 20 min; and then, dropwise adding a proper amount of hydrogen peroxide into the solution at room temperature until the solution is bright yellow, performing suction filtration, washing the solution for multiple times by using dilute hydrochloric acid, then centrifugally washing the solution by using deionized water until the washing solution is neutral, and then placing the sample in a vacuum oven at 53 ℃ for drying to obtain the graphene oxide.
Step two: 1.53g of NiCl are added at room temperature2·6H2O and 5.2g Fe (NO)3)3·9H2Putting O into 102ml of deionized water, performing ultrasonic treatment for 6min, adding 1.84g of urea into the solution, simply stirring, adding 2.43g of graphene oxide prepared in the step one, performing ultrasonic treatment for 30min at room temperature, transferring the mixed solution into a reaction kettle, reacting for 13h at 190 ℃, cooling to room temperature, centrifuging, repeatedly washing for 6 times by using deionized water, and then putting the sample into a vacuum drying oven at 80 ℃ for 11h to obtain NiFe2O4a/GO material.
Step three: 0.9g of Na2WO4·2H2Adding O into 90ml of deionized water, stirring for 6min, and adjusting the pH value of the mixed solution to about 6 by using dilute hydrochloric acid; 1.99g of NiFe prepared in the second step2O4/GO plusAdding into deionized water, stirring in 50 deg.C water bath for 20min, adding reduced glutathione and Na 11.7g sequentially2WO4Stirring the solution for 8min, placing the mixed solution in a reaction kettle, keeping the temperature at 190 ℃ for 11h, cooling to room temperature, performing suction filtration, and washing with deionized water to obtain WS2-NiFe2O4A GO heavy oil catalysis viscosity reducer.
Mixing 1.3g of catalytic viscosity reducer, 100g of crude oil with the viscosity of 87000mPa & s and 10g of oil layer water, and reacting at 250 ℃ for 18 h; after the reaction is finished, the viscosity is measured to be 1752mPa & s, and the viscosity reduction rate is 98.0 percent; the colloid content is reduced by 10.9 percent, and the asphaltene content is reduced by 1.5 percent.
Example 3
The method comprises the following steps: sequentially adding 1.3g of potassium nitrate and 2.34g of graphite powder into 77.9ml of concentrated sulfuric acid under an ice bath condition, stirring for 25min, slowly adding 8.02g of potassium permanganate into the solution, after the addition is finished, placing the solution in a water bath temperature of 37 ℃, quickly stirring for 3h, then slowly dropping 93.5ml of deionized water into the mixed solution, and controlling the system temperature to be 92 ℃ and continuously stirring for 18 min; and then, dropwise adding a proper amount of hydrogen peroxide into the solution at room temperature until the solution is bright yellow, performing suction filtration, washing the solution for multiple times by using dilute hydrochloric acid, then centrifugally washing the solution by using deionized water until the washing solution is neutral, and then placing the sample in a vacuum oven at 56 ℃ for drying to obtain the graphene oxide.
Step two: 1.23g of NiCl was added at room temperature2·6H2O and 4.19g Fe (NO)3)3·9H2Putting O into 82.6ml deionized water, performing ultrasonic treatment for 7min, adding 1.54g of urea into the solution, simply stirring, adding 1.9g of graphene oxide prepared in the step one, performing ultrasonic treatment for 25min at room temperature, transferring the mixed solution into a reaction kettle, reacting for 12h at 183 ℃, cooling to room temperature, centrifuging, repeatedly washing for 7 times by using deionized water, and then putting the sample into a vacuum drying oven at 76 ℃ for 10h to obtain NiFe2O4a/GO material.
Step three: 0.83g of Na2WO4·2H2Adding O into 83ml of deionized water, stirring for 7min, and adjusting the pH value of the mixed solution to about 6 by using dilute hydrochloric acid; 1.6g of NiFe obtained in step two2O4Adding GO into deionized water, stirring at 45 deg.C for 18min, and sequentially adding 11.4g reduced glutathione and Na2WO4Stirring for 9min, placing the mixed solution in a reaction kettle, keeping the temperature at 195 deg.C for 9h, cooling to room temperature, vacuum filtering, and washing with deionized water to obtain WS2-NiFe2O4A GO heavy oil catalysis viscosity reducer.
Mixing 1.2g of catalytic viscosity reducer, 100g of crude oil with the viscosity of 87000mPa & s and 13g of oil layer water, and reacting at 250 ℃ for 16 h; after the reaction is finished, the viscosity is measured to be 1812 mPas, and the viscosity reduction rate is 97.9%; the colloid content is reduced by 11.2 percent, and the asphaltene content is reduced by 1.3 percent.
Example 4
The method comprises the following steps: sequentially adding 1.41g of potassium nitrate and 2.67g of graphite powder into 88.9ml of concentrated sulfuric acid under an ice bath condition, stirring for 23min, slowly adding 8.64g of potassium permanganate into the solution, after the addition is finished, placing the solution in a water bath temperature of 38 ℃, quickly stirring for 3h, then slowly dropping 97.5ml of deionized water into the mixed solution, and controlling the system temperature to be 90 ℃ and continuously stirring for 16 min; and then, dropwise adding a proper amount of hydrogen peroxide into the solution at room temperature until the solution is bright yellow, performing suction filtration, washing the solution for multiple times by using dilute hydrochloric acid, then centrifugally washing the solution by using deionized water until the washing solution is neutral, and then placing the sample in a vacuum oven at 50 ℃ for drying to obtain the graphene oxide.
Step two: 1.42g of NiCl were added at room temperature2·6H2O and 4.85g Fe (NO)3)3·9H2Putting O into 95.2ml deionized water, performing ultrasonic treatment for 8min, adding 1.74g of urea into the solution, simply stirring, adding 2.16g of graphene oxide prepared in the step one, performing ultrasonic treatment at room temperature for 23min, transferring the mixed solution into a reaction kettle, reacting at 187 ℃ for 14h, cooling to room temperature, centrifuging, repeatedly washing with deionized water for 6.5 times, and then putting the sample into a vacuum drying oven at 72 ℃ for 10.5h to obtain NiFe2O4a/GO material.
Step three: 1.06g of Na2WO4·2H2Adding O into 106ml of deionized water, stirring for 7.5min, and adjusting the pH value of the mixed solution to about 6 by using dilute hydrochloric acid; will 186g of NiFe obtained in step two2O4Adding GO into deionized water, stirring in water bath at 47 deg.C for 16min, and sequentially adding 13.78g reduced glutathione and Na2WO4Stirring the solution for 8.5min, placing the mixed solution in a reaction kettle, keeping the temperature at 192 ℃ for 9h, cooling to room temperature, performing suction filtration, and washing with deionized water to obtain WS2-NiFe2O4A GO heavy oil catalysis viscosity reducer.
Mixing 1.1g of catalytic viscosity reducer, 100g of crude oil with viscosity of 87000mPa & s and 14g of oil layer water, and reacting at 250 ℃ for 16 h; after the reaction is finished, the viscosity is measured to be 1804mPa & s, and the viscosity reduction rate is 97.9%; the colloid content is reduced by 11.5%, and the asphaltene content is reduced by 1.4%.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention.
Claims (7)
1. WS (WS)2-NiFe2O4The preparation method of the/GO heavy oil catalytic viscosity reducer is characterized by comprising the following steps:
the method comprises the following steps: sequentially adding potassium nitrate and graphite powder into concentrated sulfuric acid under an ice bath condition, stirring for 20-30min, slowly adding potassium permanganate into the solution, placing the solution at a water bath temperature of 35-38 ℃ after the addition is finished, quickly stirring for 2-3h, then slowly dropping deionized water into the mixed solution, and continuously stirring for 15-20min at a system temperature of 90-95 ℃; then dripping hydrogen peroxide into the solution at room temperature until the solution is bright yellow, then carrying out suction filtration, washing the solution for multiple times by using dilute hydrochloric acid, then centrifugally washing the solution by using deionized water until the washing solution is neutral, and then placing the sample in a vacuum oven at 50-60 ℃ for drying to obtain graphene oxide;
step two: at room temperature, adding NiCl2·6H2O and Fe (NO)3)3·9H2Adding O into deionized water, ultrasonic treating for 5-8min, and adding into the solutionAdding the oxidized graphene prepared in the step one after simple stirring of urea, performing ultrasonic treatment at room temperature for 20-30min, transferring the mixed solution into a reaction kettle, reacting at 180-190 ℃ for 12-15h, cooling to room temperature, centrifuging, repeatedly washing with deionized water for 6-8 times, and then placing the sample in a vacuum drying oven at 70-80 ℃ for 10-12h to obtain NiFe2O4a/GO material;
step three: mixing Na2WO4·2H2Adding O into deionized water, stirring for 6-8min, and adjusting the pH value of the mixed solution to about 6 with dilute hydrochloric acid; the NiFe prepared in the second step2O4Adding GO into deionized water, stirring in water bath at 45-50 deg.C for 15-20min, and sequentially adding reduced glutathione and Na2WO4Continuously stirring the solution for 8-10min, placing the mixed solution in a reaction kettle, preserving the temperature at 190-200 ℃ for 9-11h, cooling to room temperature, performing suction filtration, and washing with deionized water to obtain WS2-NiFe2O4A GO heavy oil catalysis viscosity reducer.
2. WS according to claim 12-NiFe2O4The preparation method of the/GO heavy oil catalysis viscosity reducer is characterized in that in the first step, the addition amount of graphite powder is 2-3g, the mass ratio of potassium nitrate to graphite powder is 1:1.8-1:2, the mass ratio of graphite powder to potassium permanganate is 1:3.2-1:3.5, and the volume ratio of deionized water to concentrated sulfuric acid is 1.1:1-1.3: 1.
3. WS according to claim 12-NiFe2O4The preparation method of the/GO heavy oil catalytic viscosity reducer is characterized in that in the first step, the concentration of graphite powder in concentrated sulfuric acid is 0.03g/ml, the dropping speeds of deionized water and hydrogen peroxide are both 3ml/min, and the concentration of dilute hydrochloric acid is 4 mol/L.
4. WS according to claim 12-NiFe2O4The preparation method of the/GO heavy oil catalytic viscosity reducer is characterized in that NiCl is adopted in the second step2·6H2The mass ratio of O to graphene oxide is0.63:1-0.71:1,NiCl2·6H2O and Fe (NO)3)3·9H2The molar ratio of O is 1:2, NiCl2·6H2The mass ratio of the O to the urea is 1:1.2-1: 1.4; NiCl2·6H2The concentration of O in deionized water was 15 mg/ml.
5. WS according to claim 12-NiFe2O4The preparation method of the/GO heavy oil catalytic viscosity reducer is characterized in that Na is added in the third step2WO4·2H2O and NiFe2O4The mass ratio of the/GO is 0.45:1-0.57:1, Na2WO4·2H2The mass ratio of O to reduced glutathione is 1:13-1: 15; na (Na)2WO4·2H2The concentration of O in deionized water is 0.01g/ml, the concentration of dilute hydrochloric acid is 0.1M, Na2WO4The dropping rate of the solution was 5 ml/min.
6. The catalytic viscosity reducer prepared by the preparation method of any one of claims 1-5, wherein NiFe is contained in the viscosity reducer2O4The load on the graphene oxide is 62-70 wt%, WS2Quantum dot in NiFe2O4The loading on/GO is between 34 and 43 wt%.
7. The application of the catalytic viscosity reducer prepared by the preparation method according to any one of claims 1 to 5 is characterized in that the preparation method comprises the following steps: after heavy oil, catalyst which accounts for 1-1.3 wt% of the weight of the heavy oil and reservoir water which accounts for 10-15 wt% of the weight of the heavy oil are mixed, the concentration of the crude oil can be effectively reduced after a period of high-temperature reaction.
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WO2012122026A2 (en) * | 2011-03-09 | 2012-09-13 | Conocophillips Company | In situ catalytic upgrading |
CN108654702A (en) * | 2018-03-29 | 2018-10-16 | 南京大学连云港高新技术研究院 | A kind of catalyst of inferior heavy oil cracking desulfurization visbreaking, preparation method and applications |
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