CN102091440B - Dewatering material for removing water dissolved in oil and preparation method thereof - Google Patents
Dewatering material for removing water dissolved in oil and preparation method thereof Download PDFInfo
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- CN102091440B CN102091440B CN201010587138A CN201010587138A CN102091440B CN 102091440 B CN102091440 B CN 102091440B CN 201010587138 A CN201010587138 A CN 201010587138A CN 201010587138 A CN201010587138 A CN 201010587138A CN 102091440 B CN102091440 B CN 102091440B
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- montmorillonite
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- needle coke
- ball milling
- magnesium powder
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Abstract
本发明公开一种除去油中溶解水的脱水材料及其制备方法，该脱水材料选取蒙脱石、活性炭、针状焦、镁粉为制备原料，所述原料的用量(质量百分含量)为：5％～15％的蒙脱石、4％～9％的活性炭、4％～9％的针状焦、余量的镁粉；上述脱水材料的制备方法主要包括：先将蒙脱石原矿进行提纯、钠化、250℃～350℃脱水、研磨，得到蒙脱石，再将蒙脱石与活性炭、针状焦在乙醇中混合球磨，然后经300℃～400℃氩气中热处理，再与镁粉在氢气中进行混合球磨。本发明的脱水材料具有不与油中有机化合物反应、能深度脱除油中溶解水、原料成本低、无毒、使用方便等优点。The invention discloses a dehydration material for removing dissolved water in oil and a preparation method thereof. The dehydration material selects montmorillonite, activated carbon, needle coke, and magnesium powder as raw materials for preparation, and the amount (mass percentage) of the raw materials is: : 5% to 15% of montmorillonite, 4% to 9% of activated carbon, 4% to 9% of needle coke, and the rest of the magnesium powder; the preparation method of the above-mentioned dehydration material mainly includes: Purify, sodiumize, dehydrate and grind at 250°C to 350°C to obtain montmorillonite, then mix and ball-mill the montmorillonite with activated carbon and needle coke in ethanol, then heat-treat in argon at 300°C to 400°C, and then Mix and ball mill with magnesium powder in hydrogen. The dehydrating material of the invention has the advantages of not reacting with organic compounds in oil, capable of deeply removing dissolved water in oil, low raw material cost, non-toxic, convenient to use and the like.
Description
Technical field
The invention belongs to oil plant and purify upgrading technical field, particularly a kind of dehydrating material of removing dissolved water in fuel, and the preparation method of this dehydrating material.
Background technology
Water in the oil mainly contains three kinds of existences: free state, suspended state, dissolved state.Free water is meant the water that just can separate with method of tilting; Water in suspension is meant with the fine droplet mechanical mixture and is dispersed in the water in the oil; Dissolving water is meant owing to organic matter is dissolved in the water in the oil to the dissolution of water.Free water and water in suspension are easy to remove with methods such as sedimentation, coarse separation, filtrations, but dissolving water is not easy to remove.
Aviation Fuel (aviation gasoline, aviation kerosine) for the fuel oil for vehicles (gasoline, diesel oil) that uses in severe cold area and season, use under the low temperature of high-altitude; Dissolving water in the oil can produce ice crystal; Ice crystal is separated out from oil; Accumulate in the petroleum pipeline in the fuel system with oil filter on, hinder oil normally to pass through, influence engine operation; Moreover the separating out of ice crystal can be impelled the brilliant generation of wax, and making some original non crystallized hydrocarbon is nucleus with the ice crystal, and it is brilliant to grow into bigger wax.In addition, the existence of dissolving water may make microorganism (like bacterium) grow, and causes the biochemistry corrosion of oil plant container; And the microorganism that is produced and corrupt body be distributed in the oil, measures to form suspension when big, can stop up oil filter.
The quantity of dissolved water in fuel depends on the chemical composition and the temperature of oil, and the ability of different hydrocarbons compound dissolving water is from being followed successively by to weak by force: aromatic hydrocarbons＞alkene＞cycloalkane＞alkane; For same type of hydrocarbon, molecular weight is more little, viscosity is more little, and the ability of dissolving water is strong more; Temperature is high more, and the ability of dissolving water is strong more.Aromatic hydrocarbons can dissolve more water, and therefore, the arene content in oil refining process in the control oil helps reducing the dissolving water in the oil.
In order to prevent the living ice crystal of soluble aquatic in the oil, method has three kinds: one is to use antifreeze additives such as glycol monoethyl ether, two glycol monoethyl ethers.The 2nd, remove water with frozen filtration, when carrying out freezing and filtering, with the fuel oil that is stored in underground or the semi underground tank, in the ground tanks that the capacity that is pumped into is less, temperature is lower, freezing through more than 24 hours separated out ice crystal, refilters and removes ice crystal.The 3rd, remove water with drier, the drier that can be used for dry organic liquid has: 1. MgSO
4, CaCl
2, Na
2SO
4In the drier that can form hydrate with water, 2. silica gel, molecular sieve etc. can carry out the drier of physical absorption, 3. P to water
2O
5, CaO, Na etc. can with the drier of water generation chemical reaction.Because of functional groups such as the carboxyl of compound in the oil, carbonyl, hydroxyl, amino, two keys can with above-mentioned drier generation chemical reaction; Cause chemical element even the subparticle of drier to get into oil and oil is polluted; And drying effect is poor, the drier consumption is big, is difficult to industrial applications.
The above-mentioned subject matter of the method existence of dissolved water in fuel generation ice crystal that prevents is; Used poisonous, the poor stability of glycol methyl ether class antifreeze additive; With frozen filtration remove that complex equipments, the investment of water is big, during operating cost, used dehydrate agent to oil pollution is arranged, drying effect is poor, the drier consumption is big.
Summary of the invention
In order to solve the problems of the technologies described above, the present invention provides a kind of dehydrating material of removing dissolved water in fuel, the dissolving water in this dehydrating material ability deep removal oil; The present invention provides a kind of preparation method of this dehydrating material simultaneously.
Its technical solution is:
A kind of dehydrating material of removing dissolved water in fuel is by following feedstock production: montmorillonite, active carbon, needle coke and magnesium powder; Each proportioning raw materials is in mass percent, and montmorillonite is 5%～15%, and active carbon is 4%～9%, and needle coke is 4%～9%, and the magnesium powder is a surplus.
Above-mentioned montmorillonite is that the montmorillonite raw ore obtains after purification, sodium, dehydration, grinding successively.
In the treatment step of above-mentioned montmorillonite raw ore, the temperature of control dehydration is 250 ℃～350 ℃.
A kind of preparation method who removes the dehydrating material of dissolved water in fuel may further comprise the steps:
A mixes pack ball grinder with montmorillonite, active carbon with needle coke by selected amount, in ball grinder, adds ethanol then, places the ball mill ball milling, the powder behind the ball milling is heat-treated in argon gas again;
The powder of b after with step a heat treatment mixes the ball grinder of packing into a selected amount of magnesium powder, in ball grinder, charges into hydrogen then, places the ball mill ball milling to make finished product again.
Among the above-mentioned steps a, the granularity of montmorillonite, active carbon and needle coke all＜74 μ m, the ball milling time is 1～3 hour, heat treatment temperature is 300 ℃～400 ℃; Among the above-mentioned steps b, the granularity of magnesium powder＜74 μ m, the ball milling time is 1～3 hour.
Useful technique effect of the present invention is:
The dehydrating material that the present invention makes have not with oil in advantages such as organic compound reaction, dissolving water (being removed to dissolved water in fuel content＜20 μ g/g), cost of material in can deep removal oil are low, nontoxic, easy to use.
The specific embodiment
At first the mechanism of action to dehydrating material of the present invention describes, and then the narration embodiments of the invention.
The montmorillonite raw ore is a kind of silicate clay mineral with layer structure, flaky crystal; Tetrahedral si-o film folder one deck that is connected by two-layer altogether top aluminium (magnesium) oxygen (hydrogen-oxygen) octahedral sheet of connecting of rib altogether constitutes 2: 1 types and contains crystallization water structure; Its geometrical body is a nanoscale; The about 1nm of lamellar spacing, long and wide about 100～1000nm, the about 1～1.5nm of interlamellar spacing.The montmorillonite raw ore removes the concurrent first portion interlayer of intermediary water through purification, sodium, 250 ℃～350 ℃ successively and subsides, obtains montmorillonite after grinding pre-treatment step.Montmorillonite is done under the grinding aid of intercalator and active carbon and needle coke at ethanol; Synusia is peeled off; And be dispersant and carrier and high degree of dispersion with active carbon and needle coke, again after 300 ℃～400 ℃ heat treatment, form stronger combining between montmorillonite and active carbon, the needle coke; During again with the magnesium mixing and ball milling; The magnesium high degree of dispersion is on montmorillonite synusia and active carbon and needle coke, and because the cold conditions weldability of magnesium, powder forms the compound that lumpiness be the millimeter level, internal void is flourishing, nanostructured is enriched.The montmorillonite of high temperature dehydration and high degree of dispersion has strong absorptive.In addition, the magnesium of nanoscale high degree of dispersion has very high reactivity, can react with water at normal temperatures.Dehydrating material is put into oil, the dissolving water generation chemical reaction in magnesium and the oil, reaction equation is Mg+H
2O=Mg (OH)
2+ H
2, the Mg of generation (OH)
2With montmorillonite and active carbon and more firm the combining of needle coke formation in the dehydrating material, the H of generation
2Overflow, thereby can remove the dissolving water in deoiling.
Embodiment 1
Choose montmorillonite raw ore (originating in the Laixi City, Shandong Province), it is mixed with water slurry, standing sedimentation is 20 minutes again, extracts about 10 centimetres of upper strata with siphonage, in 100 ± 10 ℃ of drying in oven, grinds, and uses concentration to remove CaCO as the hydrochloric acid of 0.2mol/L then
3, using concentration again is 10% H
2O
2Boil and removed organic impurities in 1 hour; Use concentration to be the Na in the NaOH solution of 0.4mol/L again
+Ca between the exchange montmorillonite layer
2+, then in 100 ± 10 ℃ of drying in oven; Processed 0.5 hour in 300 ℃ of Muffle furnaces again; Be ground to granularity＜74 μ m (Tyler screen 200 orders sieve) again, obtain montmorillonite; Take by weighing four kinds of raw materials more respectively, its proportioning is respectively in mass percent: 10% montmorillonite (the montmorillonite raw ore obtains after above-mentioned pre-treatment step), 5% activated carbon, 5% needle coke, 80% magnesium powder; More than four kinds of raw materials granularity all＜74 μ m, certainly, also can choose the bigger active carbon of granularity, needle coke, magnesium then through pulverized 200 order Tyler screens obtain granularity all＜raw material of 74 μ m; Again montmorillonite, active carbon (apricot shell charcoal), three kinds of raw materials of needle coke (granularity＜74 μ m) are mixed the 250mL vacuum ball grinder (abrading-ball is 45: 1 with the quality of material ratio) of packing into; Add 50mL ethanol, place ND7-2 type planetary ball mill ball milling then 2 hours (the ball mill speed of mainshaft is 270r/min); Again with the heat treatment 1 hour in the argon gas in 350 ℃ of Muffle furnaces of the powder behind the ball milling; After the cooling, mix the ball grinder of packing into magnesium powder (granularity＜74 μ m) again, feed the air in the hydrogen exchange ball grinder; Place the ball mill ball milling again 2 hours, and made said dehydrating material.With pack into the fixed bed reaction pipe (bed diameter 10mm, high 100mm) of continued operation of dehydrating material; At normal temperatures No. 97 gasoline (water content is 1mg/g) that are dissolved with water are carried out processed; Liquid air speed is 0.5LHSV/h, and the moisture of using WS-8 type micro-water analyzer to record in the gasoline of dehydration back is 10.3 μ g/g.
Embodiment 2
Be that with the difference of embodiment 1 dehydration temperaturre during preliminary treatment of montmorillonite raw ore is 350 ℃; The ratio of four kinds of raw materials when ball milling prepares dehydrating material (quality percentage composition) is: 15% montmorillonite, 9% active carbon, 9% needle coke, 67% magnesium powder; Montmorillonite, active carbon, three kinds of raw material mixing and ball milling times of needle coke are 3 hours, and heat treatment temperature is 400 ℃; Time with magnesium powder mixing and ball milling is 3 hours again; Obtained dehydrating material is used for the oil dehydration, and the moisture that records in the gasoline of dehydration back is 12.1 μ g/g.
Embodiment 3
Be that with the difference of embodiment 1 dehydration temperaturre during preliminary treatment of montmorillonite raw ore is 250 ℃; The ratio of four kinds of raw materials when ball milling prepares dehydrating material (quality percentage composition) is: 5% montmorillonite, 4% active carbon, 4% needle coke, 87% magnesium powder; Montmorillonite, active carbon, three kinds of raw material mixing and ball milling times of needle coke are 1 hour, and heat treatment temperature is 300 ℃; Time with magnesium powder mixing and ball milling is 1 hour again; Obtained dehydrating material is used for the oil dehydration, and the moisture that records in the gasoline of dehydration back is 19.5 μ g/g.
Embodiment 4
Be that with the difference of embodiment 1 ratio of four kinds of raw materials when ball milling prepares dehydrating material (quality percentage composition) is: 15% montmorillonite, 4% active carbon, 9% needle coke, 72% magnesium powder; Obtained dehydrating material is used for the oil dehydration, and the moisture that records in the gasoline of dehydration back is 17.2 μ g/g.
Embodiment 5
Be that with the difference of embodiment 1 ratio of four kinds of raw materials when ball milling prepares dehydrating material (quality percentage composition) is: 15% montmorillonite, 9% active carbon, 4% needle coke, 72% magnesium powder; Obtained dehydrating material is used for the oil dehydration, and the moisture that records in the gasoline of dehydration back is 17.9 μ g/g.
Embodiment 6
Be that with the difference of embodiment 1 ratio of four kinds of raw materials when ball milling prepares dehydrating material (quality percentage composition) is: 5% montmorillonite, 9% active carbon, 4% needle coke, 82% magnesium branch; Obtained dehydrating material is used for the oil dehydration, and the moisture that records in the gasoline of dehydration back is 19.1 μ g/g.
Embodiment 7
Be that with the difference of embodiment 1 ratio of four kinds of raw materials when ball milling prepares dehydrating material (quality percentage composition) is: 5% montmorillonite, 4% active carbon, 9% needle coke, 82% magnesium powder; Obtained dehydrating material is used for the oil dehydration, and the moisture that records in the gasoline of dehydration back is 18.4 μ g/g.
Embodiment 8
Be that with the difference of embodiment 1 dehydration temperaturre during preliminary treatment of montmorillonite raw ore is 250 ℃; Montmorillonite, active carbon, three kinds of raw material mixing and ball milling times of needle coke are 1 hour, and heat treatment temperature is 300 ℃; Time with magnesium powder mixing and ball milling is 3 hours again; Obtained dehydrating material is used for the oil dehydration, and the moisture that records in the gasoline of dehydration back is 13.7 μ g/g.
Embodiment 9
Be that with the difference of embodiment 1 dehydration temperaturre during preliminary treatment of montmorillonite raw ore is 250 ℃; Montmorillonite, active carbon, three kinds of raw material mixing and ball milling times of needle coke are 3 hours, and heat treatment temperature is 400 ℃; Time with magnesium powder mixing and ball milling is 1 hour again; Obtained dehydrating material is used for the oil dehydration, and the moisture that records in the gasoline of dehydration back is 14.1 μ g/g.
Embodiment 10
Be that with the difference of embodiment 1 dehydration temperaturre during preliminary treatment of montmorillonite raw ore is 350 ℃; Montmorillonite, active carbon, three kinds of raw material mixing and ball milling times of needle coke are 3 hours, and heat treatment temperature is 400 ℃; Time with magnesium powder mixing and ball milling is 3 hours again; Obtained dehydrating material is used for the oil dehydration, and the moisture that records in the gasoline of dehydration back is 16.5 μ g/g.
Embodiment 11
Be that with the difference of embodiment 1 dehydration temperaturre during preliminary treatment of montmorillonite raw ore is 350 ℃; Montmorillonite, active carbon, three kinds of raw material mixing and ball milling times of needle coke are 1 hour, and heat treatment temperature is 300 ℃; Time with magnesium powder mixing and ball milling is 3 hours again; Obtained dehydrating material is used for the oil dehydration, and the moisture that records in the gasoline of dehydration back is 15.2 μ g/g.
Claims (5)
1. a dehydrating material of removing dissolved water in fuel is characterized in that by following feedstock production: montmorillonite, active carbon, needle coke and magnesium powder; Each proportioning raw materials is in mass percent, and montmorillonite is 5%～15%, and active carbon is 4%～9%, and needle coke is 4%～9%, and the magnesium powder is a surplus.
2. a kind of dehydrating material of removing dissolved water in fuel according to claim 1 is characterized in that: said montmorillonite is that the montmorillonite raw ore obtains after purification, sodium, dehydration, grinding successively.
3. a kind of dehydrating material of removing dissolved water in fuel according to claim 2 is characterized in that: the temperature of control montmorillonite raw ore dehydration is 250 ℃～350 ℃.
4. described preparation method who removes the dehydrating material of dissolved water in fuel of claim 1 is characterized in that may further comprise the steps:
A mixes pack ball grinder with montmorillonite, active carbon with needle coke by selected amount, in ball grinder, adds ethanol then, places the ball mill ball milling, the powder behind the ball milling is heat-treated in argon gas again;
The powder of b after with step a heat treatment mixes the ball grinder of packing into a selected amount of magnesium powder, in ball grinder, charges into hydrogen then, places the ball mill ball milling to make finished product again.
5. preparation method according to claim 4 is characterized in that: among the said step a, the granularity of montmorillonite, active carbon and needle coke all＜74 μ m, the ball milling time is 1～3 hour, heat treatment temperature is 300 ℃～400 ℃; Among the said step b, the granularity of magnesium powder＜74 μ m, the ball milling time is 1～3 hour.
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| CN201010587138A CN102091440B (en) | 2010-12-14 | 2010-12-14 | Dewatering material for removing water dissolved in oil and preparation method thereof |
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| CN102091440B true CN102091440B (en) | 2012-09-26 |
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| US7537700B2 (en) * | 2002-06-03 | 2009-05-26 | Central Research Institute Of Electric Power Industry | Method for removing water contained in solid using liquid material |
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Patent Citations (3)
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| US7537700B2 (en) * | 2002-06-03 | 2009-05-26 | Central Research Institute Of Electric Power Industry | Method for removing water contained in solid using liquid material |
| CN1762576A (en) * | 2005-09-28 | 2006-04-26 | 许盛英 | Production method of aviation kerosene absorption filter agent |
| CN101153224A (en) * | 2007-08-21 | 2008-04-02 | 明光市国阳矿业有限公司 | Assistant absorption agent for removing foreign matter from petroleum product and method of producing the same |
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