CN112480945A - Rice hull charcoal, demulsifier, preparation method and application thereof - Google Patents
Rice hull charcoal, demulsifier, preparation method and application thereof Download PDFInfo
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- CN112480945A CN112480945A CN202011191683.5A CN202011191683A CN112480945A CN 112480945 A CN112480945 A CN 112480945A CN 202011191683 A CN202011191683 A CN 202011191683A CN 112480945 A CN112480945 A CN 112480945A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/04—Dewatering or demulsification of hydrocarbon oils with chemical means
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to rice husk charcoal, a demulsifier, a preparation method and application thereof. The preparation method comprises the step of heating and carbonizing the rice hulls at the temperature of 400-600 ℃ under the anoxic condition to obtain the rice hull carbon. The invention also comprises a demulsifier, wherein the demulsifier comprises the rice husk charcoal. The rice husk charcoal has good demulsification effect, and the dehydration rate can reach 93.10 percent when water-in-oil demulsification treatment is carried out. The invention also comprises the application of the demulsifier in demulsification of water-in-oil emulsion.
Description
Technical Field
The invention relates to the field of oil field chemicals, in particular to rice husk charcoal, a demulsifier, and a preparation method and application thereof.
Background
Crude oil is typically a stable emulsion containing large amounts of water and inorganic salts, which requires removal of the water by breaking. Chemical demulsification is the most commonly used method for dehydrating crude oil.
Wang et al nano Si02Dispersing into a polyether demulsifier TA1031, and forming the nano demulsifier by adopting an in-situ preparation method. When nano SiO2When the proportion of the modified emulsion and TA1031 is 1:10, the demulsification efficiency is improved by about 20 percent, and the settling time is shortened. Nikkhah et al reported a method of treating a tumor with nano-sized Ti0 under ultrasonic conditions2A commercial demulsifier modified with particles,the demulsification rate is more than 90 percent, and the settling time is also shortened. Liu et al report a magnetic graphene oxide (M-GO) demulsifier which can be reused for 6-7 times and has demulsification efficiency of 99.98%. Xu et al prepared a series of functionalized Fluorinated Graphene (FG) and hydrazine hydrate modified graphene (HFG), and have excellent demulsification performance in acidic, alkaline and oily wastewater with different NaCl concentrations. Wang et al prepared a series of reduced graphene oxides (rGO) that settled for 30 minutes at room temperature to recover 99.97% oil from an oil-in-water emulsion.
Chinese patent CN109705896A discloses a preparation method of a composite demulsifier, which comprises AR type demulsifier, SP type demulsifier and AE type demulsifier, and the demulsifier prepared by the demulsifier composition can effectively demulsify the ternary complex flooding produced fluid containing high-content alkali, surfactant and polymer. Chinese patent CN107474873B discloses a super heavy oil demulsifier, which aims at super heavy oil in Liaohe oil field light oil extraction plant and has the characteristics of high demulsification efficiency, good stability, clean water and clean oil after demulsification, clear and smooth oil-water interface and the like. Chinese patent CN109054888A discloses a carbon nano tube/nano SiO2The composite nano demulsifier can be used for quickly demulsifying stable crude oil emulsion. The demulsifier mainly has the problems of complex preparation process, higher raw material cost, potential toxic action of medicaments and the like.
Therefore, the search for a novel demulsifier with wide source, low cost and excellent performance still faces a great challenge.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to obtain rice husk charcoal with good demulsification effect by using rice husks as raw materials.
In order to solve the technical problems, the invention provides rice husk charcoal, a demulsifier, and a preparation method and application thereof.
A preparation method of rice husk charcoal comprises the following steps: under the anoxic condition, the rice hulls are heated and carbonized at the temperature of 400-600 ℃ to obtain the rice hull carbon.
Further, the method also comprises the step of crushing the carbonized rice husk carbon.
Further, the rice hulls are heated and carbonized at the temperature of 400-600 ℃ for 30-50 minutes to obtain the rice hull carbon.
Further, crushing the rice husk carbon by a crusher; the rotating speed of the pulverizer is 25000rpm, and the fineness of the pulverizer is 50-300 meshes.
Further, sieving the crushed rice husk carbon to obtain the rice husk carbon with 50-300 meshes.
The invention also comprises the rice husk carbon prepared by the preparation method.
The invention also comprises a demulsifier, wherein the demulsifier comprises the rice husk charcoal.
In addition, the invention also provides an application of the demulsifier in demulsification of water-in-oil emulsion.
Further, the above application comprises dispersing the demulsifier into an ethanol solvent to obtain a suspension, and then mixing the suspension with the water-in-oil emulsion.
Further, the suspension is mixed with the water-in-oil emulsion and treated at 70-80 ℃ for 60-120 min.
Compared with the prior art, the invention has the advantages that: under the condition of oxygen deficiency, rice hulls are heated and carbonized at the temperature of 400-600 ℃, the obtained rice hull carbon has a hydrophobic carbon substrate, the surface of the rice hull carbon is rich in a large number of hydrophilic hydroxyl groups and hydrophilic silicon dioxide, the surface of the rice hull carbon has certain hydrophilicity due to the large number of hydroxyl groups and the silicon oxide, an amphiphilic structure similar to a surfactant is formed with the hydrophobic carbon substrate, the rice hull carbon can quickly reach an oil-water interface and penetrate through an interface membrane, and further surface active substances in the interface membrane are damaged or replaced, the demulsification process is promoted, the rice hull carbon carries out demulsification treatment on water-in-oil, and the dehydration rate can reach 93.10%.
Drawings
The features and advantages of the present invention will be more clearly understood by reference to the accompanying drawings, which are illustrative and not to be construed as limiting the invention in any way, and in which:
FIG. 1 is an infrared spectrum of rice husk charcoal prepared in example 1.
Detailed Description
The specific embodiment provides a preparation method of rice husk charcoal, which comprises the following steps: under the condition of oxygen deficiency, the rice hulls are placed in an iron container and heated and carbonized at the temperature of 400-600 ℃ for 30-50 minutes to obtain rice hull carbon, then the rice hull carbon is crushed by a crusher and sieved by a screen mesh to obtain the rice hull carbon with the particle size of 50-300 meshes. Further, the rotating speed of the pulverizer is 20000-25000rpm, and the fineness of the pulverizer is 50-300 meshes; the rice hull is preferably added in an amount of 1/3-2/3 of the volume of the iron container. Preferably 2/3 for the iron container volume.
The specific embodiment also comprises the rice husk carbon prepared by the preparation method.
The specific embodiment also comprises a demulsifier, which comprises the rice husk charcoal.
In addition, the embodiment also provides the application of the demulsifier in demulsification of the water-in-oil emulsion, which comprises the steps of dispersing the demulsifier into an ethanol solvent to obtain a suspension, mixing the suspension with the water-in-oil emulsion, and treating at 70-80 ℃ for 60-120 min.
The following detailed description of the preferred embodiment of the present invention is provided to illustrate the principles of the present invention and not to limit the scope of the invention.
In the following examples or comparative examples, the rotating speed of the crusher was 25000rpm, the fineness was 50 to 300 mesh, and the amount of rice husk added was 2/3 of the volume of the iron container.
Example 1
This example provides a rice husk char, which is obtained by the following steps:
putting the rice hull into an iron container, covering the upper part of the iron container, allowing a small amount of air to enter (under an anoxic condition), heating the iron container at 600 ℃ for 30 minutes, and observing white dense smoke in the heating process to obtain the rice hull carbon.
Pulverizing the rice husk carbon in a pulverizer, and sieving with a screen to obtain 50-300 mesh powdered rice husk carbon.
As can be seen from FIG. 1, the rice husk carbon is rich in hydroxyl groups, and absorption peaks of Si-O-Si, Si-O-C and Si-O can be found.
TABLE 1 elemental distribution of rice husk char prepared in example 1
From Table 1, it can be seen that the rice husk carbon contains 30.48% of carbon and 27.67% of silicon.
Example 2
This example provides a rice husk char, which is obtained by the following steps:
putting the rice hull into an iron container, covering the upper part of the iron container, allowing a small amount of air to enter (under an anoxic condition), heating the iron container at 600 ℃ for 40 minutes, and observing white dense smoke in the heating process to obtain the rice hull carbon.
Pulverizing the rice husk carbon in a pulverizer, and sieving with a screen to obtain 50-300 mesh powdered rice husk carbon.
Example 3
This example provides a rice husk char, which is obtained by the following steps:
putting the rice hull into an iron container, covering the upper part of the iron container, allowing a small amount of air to enter (under an anoxic condition), heating the iron container at 400 ℃ for 50 minutes, and observing white dense smoke in the heating process to obtain the rice hull carbon.
Pulverizing the rice husk carbon in a pulverizer, and sieving with a screen to obtain 50-300 mesh powdered rice husk carbon.
Example 4
This example provides a rice husk char, which is obtained by the following steps:
putting the rice hull into an iron container, covering the upper part of the iron container, allowing a small amount of air to enter (under an anoxic condition), heating the iron container at 550 ℃ for 30 minutes, and observing white dense smoke in the heating process to obtain the rice hull carbon.
Pulverizing the rice husk carbon in a pulverizer, and sieving with a screen to obtain 50-300 mesh powdered rice husk carbon.
Comparative example 1
This comparative example provides a rice husk char, obtained by the steps of:
putting the rice hull into an iron container, covering and sealing the upper part of the iron container (under an oxygen-free condition), and heating the iron container at 600 ℃ for 30 minutes to obtain the rice hull carbon.
Pulverizing the rice husk carbon in a pulverizer, and sieving with a screen to obtain 50-300 mesh powdered rice husk carbon.
Comparative example 2
This comparative example provides a rice husk char, obtained by the steps of:
putting the rice hull into an iron container, covering the upper part of the iron container, allowing a small amount of air to enter (under an anoxic condition), heating the iron container at 800 ℃ for 30 minutes, and observing white dense smoke in the heating process to obtain the rice hull carbon.
Pulverizing the rice husk carbon in a pulverizer, and sieving with a screen to obtain 50-300 mesh powdered rice husk carbon.
Application example 1
Suspensions of different concentrations were prepared based on the rice husk charcoal prepared in example 1 and comparative example 1 for characterizing the demulsification performance of the rice husk charcoal of different concentrations in water-in-oil emulsions.
150 parts by weight of crude oil is added into 350 parts by weight of deionized water and stirred and mixed, heated to 60 ℃, and then stirred for 20 minutes at the rotating speed of 11000r/min, and the process is repeated three times until stable water-in-oil emulsion is obtained.
Adding different weight parts of the rice husk carbon prepared in the example 1 into absolute ethyl alcohol to prepare rice husk carbon suspensions with the mass fractions of 1%, 0.8%, 0.6%, 0.4%, 0.2% and 0%, namely experimental groups 1-6; and adding the rice husk carbon prepared in the comparative examples 1 and 2 into absolute ethyl alcohol to prepare a rice husk carbon suspension with the mass fraction of 1%.
1 part by volume of the rice hull charcoal suspension with different mass fractions is added into 20 parts by volume of water-in-oil emulsion, then the mixture is fully shaken and mixed evenly, and then the mixture is transferred into a 70 ℃ water bath kettle to stand for 120min, and the dehydration rate is measured, and the result is shown in table 2.
TABLE 2 demulsification results of the rice hull charcoals manufactured in the experimental groups 1-6, the comparative example 1 and the comparative example 2
As can be seen from Table 2, the rice husk charcoal provided by the invention has good demulsification performance, the rice husk charcoal with the concentration of 500mg/L is settled at 70 ℃ for 120min, the demulsification efficiency on water-in-oil emulsion is 92.65%, and the demulsification rate on water-in-oil emulsion of the rice husk charcoal prepared in the comparative example 1 is only 21.72%, because the rice husk charcoal prepared in the comparative example 1 is completely carbonized under the anaerobic condition, and the completely carbonized rice husk charcoal almost completely decomposes oxygen-containing groups, so that the rice husk charcoal only has super-hydrophobic performance, no hydrophilicity and poor demulsification effect. In addition, the demulsification effect of the rice hull charcoal prepared in the comparative example 2 is poor, because part of the rice hulls can be burnt into ash due to overhigh temperature, and the rice hulls can be completely carbonized, so that the rice hull charcoal is in a hydrophobic state and is not easy to induce the demulsification process.
Application example 2
Based on the rice husk carbon prepared in example 1, experimental groups 8 to 11 for characterizing the demulsification performance of the rice husk carbon at different temperatures were sequentially established.
150 parts by weight of crude oil (from the Changqing oil field) was added to 350 parts by weight of deionized water, stirred and mixed, heated to 60 ℃ and then stirred at 11000r/min for 20 minutes, and this process was repeated three times until a stable water-in-oil emulsion was obtained.
The rice husk charcoal prepared in example 1 was added to 20 parts by weight of absolute ethanol to prepare a rice husk charcoal suspension having a mass fraction of 1%.
Adding 1 volume part of the rice hull carbon suspension into 20 volume parts of water-in-oil emulsion, fully oscillating and uniformly mixing, transferring to a water bath kettle with different set temperatures, namely experiment groups 8-12, standing for 120min, and measuring the dehydration rate, wherein the results are shown in Table 3.
TABLE 3 results of demulsification of experimental groups 8-12
| Temperature/. degree.C | Percentage of dehydration% | |
| Experimental group 8 | 80 | 93.10 |
| Experimental group 9 | 70 | 92.65 |
| Experimental group 10 | 60 | 74.096 |
| Experimental group 11 | 50 | 34.04 |
| Experimental group 12 | 40 | 15.05 |
As can be seen from Table 3, the optimal demulsification temperature of the rice husk char provided by the present invention is 80 ℃.
In conclusion, the rice hull charcoal provided by the invention can be suitable for demulsification of water-in-oil emulsion, and has the characteristics of simple preparation method, wide raw material source, no pollution, easy degradation, excellent demulsification performance and the like.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (10)
1. A preparation method of rice husk charcoal is characterized by comprising the following steps: under the anoxic condition, the rice hulls are heated and carbonized at the temperature of 400-600 ℃ to obtain the rice hull carbon.
2. The method according to claim 1, further comprising pulverizing the carbonized rice husk carbon.
3. The method as claimed in claim 1, wherein the rice husk is carbonized by heating at 400-600 ℃ for 30-50 minutes to obtain the rice husk carbon.
4. The production method according to claim 2, wherein the rice husk char is pulverized by a pulverizer; the rotating speed of the pulverizer is 25000rpm, and the fineness of the pulverizer is 50-300 meshes.
5. The method according to claim 2, wherein the crushed rice husk carbon is sieved to obtain 50 to 300 mesh rice husk carbon.
6. Rice husk charcoal produced by the production method according to any one of claims 1 to 5.
7. A demulsifier comprising the rice husk char according to claim 6.
8. Use of the demulsifier of claim 7 in demulsification of water-in-oil emulsions.
9. The use according to claim 8, comprising: dispersing the demulsifier into an ethanol solvent to obtain a suspension, and then mixing the suspension with the water-in-oil emulsion.
10. Use according to claim 9, wherein the suspension is mixed with the water-in-oil emulsion and treated at 70-80 ℃ for 60-120 min.
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