CN102091440A - 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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- CN102091440A CN102091440A CN 201010587138 CN201010587138A CN102091440A CN 102091440 A CN102091440 A CN 102091440A CN 201010587138 CN201010587138 CN 201010587138 CN 201010587138 A CN201010587138 A CN 201010587138A CN 102091440 A CN102091440 A CN 102091440A
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- montmorillonite
- oil
- ball milling
- active carbon
- needle coke
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Abstract
The invention discloses a dewatering material for removing water dissolved in oil and a preparation method thereof. The dewatering material comprises the following raw materials in percentage by mass: 5 to 15 percent of montmorillonite, 4 to 9 percent of active carbon, 4 to 9 percent of needle coke and the balance of magnesium powder. The dewatering material preparation method mainly comprises the following steps of: purifying the montmorillonite raw ore, performing sodium treatment on the purified product, dewatering the obtained material at the temperature of 250 to 350 DEG C, and grinding to obtain the montmorillonite; mixing and ball milling the montmorillonite, the active carbon and the needle coke in ethanol; performing thermal treatment on the mixed material at the temperature of 300 to 400 DEG C in argon gas; and blending and ball milling the obtained product with magnesium powder in hydrogen gas. The dewatering material in the invention has the advantages of avoiding reacting with organic compounds in oil, deeply removing water dissolved in the oil, along with low raw material cost, no toxicity, convenience for 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 water in the oil; Dissolving water is meant owing to organic matter is dissolved in 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.
For the fuel oil for vehicles (gasoline, diesel oil) that uses in severe cold area and season, the Aviation Fuel (aviation gasoline, aviation kerosine) that under the low temperature of high-altitude, uses, 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 and on the oil filter, hinder oil normally to pass through, influence engine operation; Moreover, ice crystal separate out the generation that can impel the wax crystalline substance, making some original non crystallized hydrocarbon is nucleus with the ice crystal, grows into bigger wax crystalline substance.In addition, the existence of dissolving water may make microorganism (as 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 class 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 the chemical element of drier even subparticle to enter 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 equipment complexity, 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 invention provides a kind of dehydrating material of removing dissolved water in fuel, the dissolving water in this dehydrating material energy 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 raw material proportioning 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, adds ethanol then in ball grinder, 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, charges into hydrogen then in ball grinder, 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, length 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, it be the compound that a millimeter level, internal void prosperity, nanostructured are enriched that powder forms lumpiness.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, thus can be except that 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, grind, and be the hydrochloric acid removal CaCO of 0.2mol/L then with concentration
3, be 10% H again with concentration
2O
2Boil and removed organic impurities in 1 hour; Be Na in the NaOH solution of 0.4mol/L with concentration 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 described 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 that records in the gasoline of dehydration back with WS-8 type micro-water analyzer 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 raw material proportioning 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: described 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, adds ethanol then in ball grinder, 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, charges into hydrogen then in ball grinder, places the ball mill ball milling to make finished product again.
5. a kind of preparation method who removes the dehydrating material of dissolved water in fuel according to claim 4, it is characterized in that: among the described 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 described 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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|---|---|---|---|
| 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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| CN102091440A true CN102091440A (en) | 2011-06-15 |
| CN102091440B CN102091440B (en) | 2012-09-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103283979A (en) * | 2013-06-17 | 2013-09-11 | 内蒙古润隆化工有限责任公司 | Preparation method of montmorillonite powder with large specific surface for feeds and papermaking |
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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 |
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| 《硅酸盐通报》 20100831 李国平等 蒙脱石对蛋白质吸附行为的研究 834-837及851 1-5 第29卷, 第4期 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103283979A (en) * | 2013-06-17 | 2013-09-11 | 内蒙古润隆化工有限责任公司 | Preparation method of montmorillonite powder with large specific surface for feeds and papermaking |
| CN103283979B (en) * | 2013-06-17 | 2014-07-02 | 内蒙古润隆化工有限责任公司 | Preparation method of montmorillonite powder with large specific surface for feeds and papermaking |
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| CN102091440B (en) | 2012-09-26 |
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