CN102746881B - Crude oil demetallization method - Google Patents
Crude oil demetallization method Download PDFInfo
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Abstract
The invention discloses a crude oil demetallization method to solve a bad demetallization effect problem existing in present crude oil demetallization methods. The crude oil demetallization method of the invention comprises the following steps: 1, heating the crude oil, adding a demetallization agent, water and a de-emulsifier to the crude oil, and fully mixing to obtain a mixed solution; 2, allowing the mixed solution obtained in step 1 to undergo a microwave reaction in a microwave reactor; and 3, carrying out oil-water separation on the mixed solution subjected to the microwave reaction in step 2 in an electric desalting and dewatering device to obtain demetallized crude oil. The method is especially suitable for removing organic acid salts of Ca, Fe and Mg, and porphyrin compounds of Ni and V in the crude oil.
Description
Technical field
The present invention relates to a kind of method that removes metal from crude oil in refining of petroleum industry.
Background technology
In crude oil, contain a small amount of metal, exist with various forms.The more metallic element of content has calcium, iron, magnesium, nickel, vanadium etc.Wherein, most calcium, iron, magnesium exist with the form such as organic acid salt, phenates, and nickel, vanadium exist mainly with the form of porphyrin compound.Metallic element in crude oil can produce some negative impacts in Crude Oil Processing, for example, in equipment and pipeline, deposit, cause corrosion, makes catalyst activity reduction, poisoning and deactivation, etc.Along with the in poor quality year by year of crude oil, in crude oil, the harm of metallic element and the technology that removes more and more come into one's own.In crude oil, in the removal methods of metal, having one is chemical stripping method; In crude oil, add certain metal remover and oil soluble metal compound (organic acid salt and porphyrin compound) to react, generate water-soluble metal salt, or generation is not only insoluble in water but also be insoluble in oily metallic salt, then by electric desalting process, it is separated from crude oil.
Chinese patent CN1693424A discloses a kind of process for demetalizating of hydrocarbon ils, taking methyl ethyl diketone as metal remover, hydrocarbon ils is fully mixed and is contacted with methyl ethyl diketone, water, emulsion splitter, removes the metal in hydrocarbon ils by oily water separation.The method is not high to the decreasing ratio of Calcium in Crude Oil, iron, magnesium, and nickel, vanadium are not had to removal effect.CN101085932A discloses a kind of compound demetalizate agent for hydrocarbon ils, comprises following component: (a) metal remover of 0.2～10 of calcium weight times in hydrocarbon ils, and described metal remover is alkyl benzene sulphonate (ABS); (b) assistant agent of 0.2～10 of calcium weight times in hydrocarbon ils, described assistant agent is the one or more combination thing of levulinic acid, oxyacetic acid, lactic acid, disodium EDTA, ethylenediamine tetraacetic acid (EDTA), gluconic acid, tartrate or citric acid; (c) emulsion splitter of 2～100ppm of hydrocarbon ils weight.This invention also discloses the method that uses above-mentioned compound demetalizate agent to remove metal from hydrocarbon ils, and described method is poor to the removal effect of iron, magnesium and nickel, vanadium in crude oil.CN101381620A discloses a kind of process for demetalizating of oil product, comprises the steps: 1) oil product taking is preheated to 50～70 DEG C, make oil product be flow state; 2) in oil product, add metal remover and water, after fully mixing, carry out the ul-trasonic irradiation of 10～18 minutes; 3) by after the mixed solution of ultrasonication leaves standstill 1 hour at 60～90 DEG C of temperature, carry out oily water separation.The method adds metal remover to carry out demetalization reaction in oil product, and take ul-trasonic irradiation to strengthen demetalization reaction, make metalloporphyrin and non-porphyrin oil-soluble compounds in oil product be converted into hydrophilic compounds, then carry out oily water separation, the metal in oil product is removed; The problem existing is not high to the decreasing ratio of nickel, vanadium in oil product.
Summary of the invention
The object of this invention is to provide a kind of process for demetalizating of crude oil, to solve the bad problem of the existing metal removal effect of existing crude oil process for demetalizating.
For addressing the above problem, the technical solution used in the present invention is: a kind of process for demetalizating of crude oil, is made up of following steps:
A. by heating crude oil, in crude oil, add metal remover, water and emulsion splitter afterwards, fully mix, obtain mixed solution;
B. mixed solution steps A being obtained in microwave reactor by microwave action;
C. the mixed solution after microwave action step B being obtained carries out oily water separation in electrical desalting and dewatering device, obtains demetalization crude oil.
Adopt the present invention, there is following beneficial effect: principal character of the present invention be the mixed solution that obtains after crude oil is mixed with metal remover, water and emulsion splitter in microwave reactor by microwave action; Utilize the interior heat characteristic of microwave to mixed solution and the effect of the electromagnetic field that changes of the high frequency that produces, the level of response of strengthening metal remover and oil soluble metal compound, makes the metal existing with organic acid salt and porphyrin compound form in crude oil be converted into water-soluble and hydrophilic compound.Afterwards, by conventional oily water separation mode, the metal in crude oil is removed.
The present invention is specially adapted to remove the calcium, iron, the magnesium that in crude oil, exist with organic acid salt form, and the nickel, the vanadium that exist with porphyrin compound form, and these several metals are all had to good removal effect.Test shows, adopts the present invention program, and the decreasing ratio of calcium is more than 90%, and the decreasing ratio of iron, magnesium is more than 85%, and the decreasing ratio of nickel, vanadium is more than 80%.In addition, the present invention also have that technique is simple, easy and simple to handle, metal remover consumption is few, investment and the lower feature of running cost.
Below in conjunction with embodiment and embodiment, the present invention is further detailed explanation.Embodiment and embodiment do not limit the scope of protection of present invention.
Embodiment
The process for demetalizating of crude oil of the present invention, is made up of following steps:
A. by heating crude oil, in crude oil, add metal remover, water and emulsion splitter afterwards, fully mix, obtain mixed solution.This step is basic identical with existing crude oil process for demetalizating.
B. mixed solution steps A being obtained in microwave reactor by microwave action.
C. the mixed solution after microwave action step B being obtained carries out oily water separation in electrical desalting and dewatering device; Metal in crude oil is removed, and obtains demetalization crude oil.This step is basic identical with existing crude oil process for demetalizating.
In steps A, be generally by heating crude oil to 50～120 DEG C.Be generally one or both in hydrochloric acid, phosphoric acid, formic acid, acetic acid, oxalic acid, citric acid, trimethyl phosphite 99 and triethyl phosphate to the metal remover adding in crude oil, add-on is generally every gram of crude oil and adds 50～2000 μ g (μ g represents microgram; While adding two kinds of metal removers, add-on refers to total add-on).Described metal remover is all existing, can buy from the market; It uses kind and consumption, can based on crude in kind, the content of metal determine.In steps A, be generally that pH value is 6～9 fresh water or purifies waste water to the water adding in crude oil; Add-on is generally 2%～10% of former weight of oil.In steps A, can be existing various emulsion splitter to the emulsion splitter adding in crude oil; It uses kind and consumption, and the character of based on crude is determined (comprising water content).Can choice for use single emulsion splitter or use composite demulsifying agent, such as BP2040, FC961, FC9301, ST14 or ERI1160 etc.; These emulsion splitters can be buied from the market.Emulsion splitter is generally selected one; The add-on of emulsion splitter is generally every gram of crude oil and adds 5～100 μ g.
In step B, be generally mixed solution that steps A is obtained in microwave reactor by microwave action 1～10 minute.Mixeding liquid temperature after microwave action is generally 70～140 DEG C.In microwave action process, can be uniformly mixed liquid with agitator, also can not stir.The frequency of microwave reactor is generally 2450MHz, and power is generally 100～1000W (watt).Described microwave reactor is existing, can buy from the market.
In step C, the strength of electric field of electrical desalting and dewatering device is generally 200～2000V/cm (volt/cm); Electric field can be alternating-electric field (50Hz) or DC electric field.The service temperature of oily water separation is generally 70～140 DEG C, and the operating time is generally 10～60 minutes.Described electrical desalting and dewatering device can be the level that arranges commonly used or the electrical desalting and dewatering device of vertical electrode plate.
Preferred version of the present invention is as follows:
In steps A, by heating crude oil to 60～80 DEG C.Be one or both in acetic acid, citric acid and trimethyl phosphite 99 to the metal remover adding in crude oil, add-on is that every gram of crude oil adds 500～1200 μ g.Being former weight of oil to the amount of the water adding in crude oil 5%～10%, is that every gram of crude oil adds 10～40 μ g to the amount of the emulsion splitter adding in crude oil.
In step B, the mixed solution that steps A is obtained in microwave reactor by microwave action 2～6 minutes.Mixeding liquid temperature after microwave action is 90～120 DEG C, and the power of microwave reactor is 300～800W.
In step C, the strength of electric field of electrical desalting and dewatering device is 600～1000V/cm.The service temperature of oily water separation is 90～120 DEG C, and the operating time is 20～40 minutes.
Mixeding liquid temperature after step B microwave action, generally than steps A by heating crude oil to temperature exceed 20～40 DEG C.The service temperature of step C oily water separation generally equals the mixeding liquid temperature after step B microwave action.The unaccounted temperature of the present invention is normal temperature (25 DEG C).
Embodiment
Carry out 4 groups of tests (embodiment 1～embodiment 4) by the present invention program in laboratory, also correspondingly carried out 4 groups of simultaneous tests (comparative example 1～comparative example 4).In embodiment 1～embodiment 4 and comparative example 1～comparative example 4, all use beaker heating in crude oil, and in beaker, the crude oil of heating is mixed with metal remover, water and emulsion splitter.Electrical desalting and dewatering device is YS-3 type electric desalting tester, and electric field is 50Hz alternating-electric field.The model of inductively coupled plasma emission spectrometer is DV5300.In embodiment 1～embodiment 4, all use WF-4000C type microwave reactor (volume is 1000 milliliters); It is provided with temperature sensor and stirring system (stirring system does not use), and power can regulate, and carries microwave reaction kettle.In embodiment 1～embodiment 4 and comparative example 1～comparative example 4, the metal remover using is commercially available chemical pure metal remover, and emulsion splitter is commercially available emulsion splitter; The method of calculation of metal removal rate are all identical.
Embodiment 1
Get 500g (gram) North SinKiang heating crude oil to 60 DEG C, in crude oil, add metal remover, water and emulsion splitter afterwards, fully mix, obtain mixed solution.The density of described crude oil is 891.2kg/m
3(kilograms per cubic meter), calcium contents is 144.8 μ g/g (micrograms/gram), and iron level is 38.4 μ g/g, and nickel content is 14.3 μ g/g, and Mg content is 8.5 μ g/g.Metal remover is the mixture (mass ratio of acetic acid and trimethyl phosphite 99 is 10: 1) of acetic acid and trimethyl phosphite 99, and add-on is that every gram of crude oil adds 1200 μ g.Water is that pH value is 7 fresh water, and add-on is former weight of oil 10%.Emulsion splitter is BP2040 type emulsion splitter, and add-on is that every gram of crude oil adds 10 μ g.
Above-mentioned mixed solution is poured in microwave reaction kettle, and be placed in microwave reactor.Mixture is by microwave action 5 minutes in microwave reactor, and the mixeding liquid temperature after microwave action is 90 DEG C.The frequency of microwave reactor is 2450MHz, and power is 300W.
Mixed solution after above-mentioned microwave action is carried out in electrical desalting and dewatering device to oily water separation, obtain demetalization crude oil.The strength of electric field of electrical desalting and dewatering device is 800V/cm; The service temperature of oily water separation is 90 DEG C, and the operating time is 40 minutes.
The metal content of the demetalization crude oil obtaining after to oily water separation with inductively coupled plasma emission spectrometer is measured, and calculates by the formula of the metal removal rate=content (μ g/g) of certain metal before [before crude oil demetalization after content (μ the g/g)-crude oil demetalization of certain metal the content (μ g/g) of certain metal] ÷ crude oil demetalization × 100%.Result is: in embodiment 1, the decreasing ratio of calcium is 96.8%, and the decreasing ratio of iron is 89.6%, and the decreasing ratio of nickel is 85.8%, and the decreasing ratio of magnesium is 89.5%.
Comparative example 1
Press embodiment 1.Difference is that comparative example 1 is not used microwave reactor; The mixed solution that crude oil obtains after mixing with metal remover, water and emulsion splitter not in microwave reactor by microwave action, in electrical desalting and dewatering device, carry out oily water separation but directly send into be heated to 90 DEG C in beaker after.Comparative example 1 remaining all material, operation steps and condition, the equipment using are all identical with embodiment 1.
In comparative example 1, the decreasing ratio of calcium is 58.2%, and the decreasing ratio of iron is 50.6%, and the decreasing ratio of nickel is 24.8%, and the decreasing ratio of magnesium is 40.6%.
Embodiment 2
Get 500g Tahe high-sulfur crude oil and be heated to 80 DEG C, in crude oil, add metal remover, water and emulsion splitter afterwards, fully mix, obtain mixed solution.The density of described crude oil is 927.3kg/m
3, sulphur content is 2.25w% (w% represents weight percentage), and iron level is 8.1 μ g/g, and nickel content is 17.2 μ g/g, and content of vanadium is 139.4 μ g/g.Metal remover is trimethyl phosphite 99, and add-on is that every gram of crude oil adds 800 μ g.Water is that pH value is 7 fresh water, and add-on is former weight of oil 8%.Emulsion splitter is ERI1160 type emulsion splitter, and add-on is that every gram of crude oil adds 25 μ g.
Above-mentioned mixed solution is poured in microwave reaction kettle, and be placed in microwave reactor.Mixture is by microwave action 8 minutes in microwave reactor, and the mixeding liquid temperature after microwave action is 120 DEG C.The frequency of microwave reactor is 2450MHz, and power is 450W.
Mixed solution after above-mentioned microwave action is carried out in electrical desalting and dewatering device to oily water separation, obtain demetalization crude oil.The strength of electric field of electrical desalting and dewatering device is 1000V/cm; The service temperature of oily water separation is 120 DEG C, and the operating time is 30 minutes.
The metal content of the demetalization crude oil obtaining after to oily water separation with inductively coupled plasma emission spectrometer is measured, and calculates metal removal rate.Result is: in embodiment 2, the decreasing ratio of iron is 90.8%, and the decreasing ratio of nickel is 86.9%, and the decreasing ratio of vanadium is 92.5%.
Comparative example 2
Press embodiment 2.Difference is that comparative example 2 is not used microwave reactor; The mixed solution that crude oil obtains after mixing with metal remover, water and emulsion splitter not in microwave reactor by microwave action, in electrical desalting and dewatering device, carry out oily water separation but directly send into be heated to 120 DEG C in beaker after.Comparative example 2 remaining all material, operation steps and condition, the equipment using are all identical with embodiment 2.
In comparative example 2, the decreasing ratio of iron is 38.4%, and the decreasing ratio of nickel is 26.8%, and the decreasing ratio of vanadium is 40.8%.
Embodiment 3
Get 500g Peng Lai 19-3 high-acid crude oil and be heated to 70 DEG C, in crude oil, add metal remover, water and emulsion splitter afterwards, fully mix, obtain mixed solution.The density of described crude oil is 927.6kg/m
3, acid number is 3.24mgKOH/g (milligram KOH/ gram).Calcium contents is 32.6 μ g/g, and nickel content is 31.3 μ g/g.Metal remover is the mixture (mass ratio of citric acid and trimethyl phosphite 99 is 6: 1) of citric acid and trimethyl phosphite 99, and add-on is that every gram of crude oil adds 500 μ g.Water is that pH value is 7 fresh water, and add-on is former weight of oil 5%.Emulsion splitter is FC961 type emulsion splitter, and add-on is that every gram of crude oil adds 30 μ g.
Above-mentioned mixed solution is poured in microwave reaction kettle, and be placed in microwave reactor.Mixture is by microwave action 2 minutes in microwave reactor, and the mixeding liquid temperature after microwave action is 110 DEG C.The frequency of microwave reactor is 2450MHz, and power is 800W.
Mixed solution after above-mentioned microwave action is carried out in electrical desalting and dewatering device to oily water separation, obtain demetalization crude oil.The strength of electric field of electrical desalting and dewatering device is 600V/cm; The service temperature of oily water separation is 110 DEG C, and the operating time is 20 minutes.
The metal content of the demetalization crude oil obtaining after to oily water separation with inductively coupled plasma emission spectrometer is measured, and calculates metal removal rate.Result is: in embodiment 3, the decreasing ratio of calcium is 91.2%, and the decreasing ratio of nickel is 83.8%.
Comparative example 3
Press embodiment 3.Difference is that comparative example 3 is not used microwave reactor; The mixed solution that crude oil obtains after mixing with metal remover, water and emulsion splitter not in microwave reactor by microwave action, in electrical desalting and dewatering device, carry out oily water separation but directly send into be heated to 110 DEG C in beaker after.Comparative example 3 remaining all material, operation steps and condition, the equipment using are all identical with embodiment 3.
In comparative example 3, the decreasing ratio of calcium is 50.2%, and the decreasing ratio of nickel is 31.6%.
Embodiment 4
Get 500g triumph commingled crude and be heated to 80 DEG C, in crude oil, add metal remover, water and emulsion splitter afterwards, fully mix, obtain mixed solution.The density of described crude oil is 913.0kg/m
3, calcium contents is 41.9 μ g/g, nickel content is 18.6 μ g/g.Metal remover is the mixture (mass ratio of acetic acid and trimethyl phosphite 99 is 5: 1) of acetic acid and trimethyl phosphite 99, and add-on is that every gram of crude oil adds 600 μ g.Water is that pH value is 7 fresh water, and add-on is former weight of oil 10%.Emulsion splitter is ST14 type emulsion splitter, and add-on is that every gram of crude oil adds 40 μ g.
Above-mentioned mixed solution is poured in microwave reaction kettle, and be placed in microwave reactor.Mixture is by microwave action 6 minutes in microwave reactor, and the mixeding liquid temperature after microwave action is 120 DEG C.The frequency of microwave reactor is 2450MHz, and power is 400W.
Mixed solution after above-mentioned microwave action is carried out in electrical desalting and dewatering device to oily water separation, obtain demetalization crude oil.The strength of electric field of electrical desalting and dewatering device is 1000V/cm; The service temperature of oily water separation is 120 DEG C, and the operating time is 20 minutes.
The metal content of the demetalization crude oil obtaining after to oily water separation with inductively coupled plasma emission spectrometer is measured, and calculates metal removal rate.Result is: in embodiment 4, the decreasing ratio of calcium is 94.8%, and the decreasing ratio of nickel is 84.5%.
Comparative example 4
Press embodiment 4.Difference is that comparative example 4 is not used microwave reactor; The mixed solution that crude oil obtains after mixing with metal remover, water and emulsion splitter not in microwave reactor by microwave action, in electrical desalting and dewatering device, carry out oily water separation but directly send into be heated to 120 DEG C in beaker after.Comparative example 4 remaining all material, operation steps and condition, the equipment using are all identical with embodiment 4.
In comparative example 4, the decreasing ratio of calcium is 46.4%, and the decreasing ratio of nickel is 22.0%.
Claims (3)
1. a process for demetalizating for crude oil, is characterized in that: the method is made up of following steps:
A. by heating crude oil to 50～120 DEG C, in crude oil, add metal remover, water and emulsion splitter afterwards, fully mix, obtain mixed solution, metal remover is one or both in hydrochloric acid, phosphoric acid, formic acid, acetic acid, oxalic acid, citric acid, trimethyl phosphite 99 and triethyl phosphate, the add-on of metal remover is that every gram of crude oil adds 50～2000 μ g, and the add-on of emulsion splitter is that every gram of crude oil adds 5～100 μ g;
B. mixed solution steps A being obtained is by microwave action 1～10 minute in microwave reactor, and the mixeding liquid temperature after microwave action is 70～140 DEG C, than steps A by heating crude oil to temperature exceed 20～40 DEG C, the frequency of microwave reactor is 2450MHz;
C. the mixed solution after microwave action step B being obtained carries out oily water separation in electrical desalting and dewatering device, obtains demetalization crude oil.
2. the process for demetalizating of crude oil according to claim 1, is characterized in that:
In step B, the power of described microwave reactor is 100～1000W;
In step C, the strength of electric field of electrical desalting and dewatering device is 200～2000V/cm, and the service temperature of oily water separation is 70～140 DEG C, and the operating time is 10～60 minutes.
3. the process for demetalizating of crude oil according to claim 2, is characterized in that:
In steps A, by heating crude oil to 60～80 DEG C, be one or both in acetic acid, citric acid and trimethyl phosphite 99 to the metal remover adding in crude oil, add-on is that every gram of crude oil adds 500～1200 μ g;
In step B, the mixed solution that steps A is obtained is by microwave action 2～6 minutes in microwave reactor, and the mixeding liquid temperature after microwave action is 90～120 DEG C, and the power of described microwave reactor is 300～800W;
In step C, the strength of electric field of electrical desalting and dewatering device is 600～1000V/cm, and the service temperature of oily water separation is 90～120 DEG C, and the operating time is 20～40 minutes.
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| CN104046380B (en) * | 2013-03-15 | 2016-02-17 | 中石化洛阳工程有限公司 | A kind of crude oil with poor quality pretreatment technology |
| CN103450930B (en) * | 2013-03-26 | 2016-06-29 | 湖南长岭石化科技开发有限公司 | A kind of method of crude oil demetalization dehydration |
| CN104962315A (en) * | 2015-06-17 | 2015-10-07 | 成都高普石油工程技术有限公司 | Method of extracting and recovering heavy metals from petroleum fuel products |
| CN108203592B (en) * | 2016-12-16 | 2020-07-31 | 中国石油化工股份有限公司 | Crude oil desalting and dewatering equipment and application thereof |
| CN109097086B (en) * | 2017-06-20 | 2021-04-06 | 中国石油化工股份有限公司 | Coal tar pretreatment method |
| CN109337712A (en) * | 2018-09-19 | 2019-02-15 | 张家港保税区宝成环保科技有限公司 | A kind of microwave heating method for crude oil demulsification dehydration |
| CN115286733B (en) * | 2022-08-26 | 2023-08-01 | 盘锦三力中科新材料有限公司 | Method for removing metal impurities in polymethacrylic acid resin reaction mixture |
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| AU2006335213C1 (en) * | 2005-12-14 | 2011-01-27 | Global Resource Corporation | Microwave-based recovery of hydrocarbons and fossil fuels |
| CN101085932A (en) * | 2006-06-05 | 2007-12-12 | 广州市精至化工有限公司 | Composite metal remover used for hydrocarbon oil and method for removing metal |
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