CN101724428A - Method for modifying oil and method for preparing magnetite pulverulent body - Google Patents
Method for modifying oil and method for preparing magnetite pulverulent body Download PDFInfo
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- CN101724428A CN101724428A CN200810166692A CN200810166692A CN101724428A CN 101724428 A CN101724428 A CN 101724428A CN 200810166692 A CN200810166692 A CN 200810166692A CN 200810166692 A CN200810166692 A CN 200810166692A CN 101724428 A CN101724428 A CN 101724428A
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- magnetite
- oil
- pulverulent body
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Abstract
In the invention, modified raw crude oil or waste oil of the magnetite pulverulent body act as raw materials and modified oil featuring higher heat value, lower viscosity and density can be obtained.The invention also provides a method for recovering magnetite pulverulent body from iron-rich wastes and the recovered magnetite pulverulent body can be further applied to modify raw crude oil or waste oil.
Description
Technical field
The invention relates to a kind of method of modifying oil, especially in regard to the recovery of the magnetite of its application with utilize again.
Background technology
To give birth to this class oil product upgrading of matter crude oil and waste oil product (comprising: waste lubricating oil, useless turbine wet goods) is the method for oil used in fuel, and main imitative refining preparation technology from the refining of petroleum industry mainly is divided into catalyzer hydrogenation and is cracking catalyst.The former needs to carry out hydrogenation under 5～20MPa at 300～500 ℃, and the rate of recovery is different with preparation process condition according to catalyzer, is about 30～70wt.%.The latter is under normal pressure, and 350～500 ℃ of operations down are by catalyst pores
Alkane derivative after the control gasification obtains liquid fuel, and its rate of recovery is about 25wt.%.Above-mentioned preparation technology is former to be used for petrochemical industry refining industry, in the crude oil of ton, is applied to quantity low livings pledge cracked oil and waste oil product when handling, and it is also not obvious for commercial profit, only can highlight its waste and utilize, and with the substitute energy generation, but its cost is higher.
Above-mentioned catalyzer hydrogenation often is used for the commercialization catalyzer of hydrogenating desulfurization such as Co-Mo, Ni-Mo as catalyzer with present petrochemical plant, is that solvent carries out the catalyzer hydrogenation with four naphthalene hydrogen.Right this type of catalyzer generally is used for the hydrogenating desulfurization preparation technology of petrochemical plant, and the sulphur content of general petrochemical industry crude oil is lower than 2wt.%.The problem of giving birth to matter crude oil is that oxygen level is too high, be about 35～40wt.%, directly use the Hydrobon catalyst of petrochemical plant, though can reach living matter crude oil upgrading effect, but its operational condition belongs to high pressure preparation technology, operational doubt is arranged, and the scholar who carries out this type of research wishes that the refining of matter crude oil or the waste oil product of next life not can combine with existing petrochemical plant, therefore in the selection of catalyzer, temperature of reaction, reaction pressure all with reference to the hydrogenating desulfurization preparation technology of petrochemical plant.But remove the non-government bright law compulsion execution of deciding, the petrochemical plant in the running is reluctant to accept living matter crude oil and waste oil product more and is charging for taking the rear end quality product into account at present.Therefore still need develop at present oil product refining catalyzer and the preparation technology who is applicable to this type of charging, reduce preparation technology's temperature, working pressure, catalyzer cost, and improve the Oil Recovery rate.
Summary of the invention
The object of the present invention is to provide a kind of method of modifying oil and the preparation method of magnetite pulverulent body.
The method of modifying oil provided by the invention comprises oil product and magnetite pulverulent body are placed cracker; The heating pyrolyze device makes the oil product boiling form steam; And condensation and collect steam, promptly get modifying oil.
The present invention also provides a kind of preparation method of magnetite pulverulent body, comprises that getting rich iron waste material is dissolved in acid solution after-filtration acid solution; With in the alkali lye and acid solution forming neutralizer, and neutralizer contains magnetite pulverulent body; And with filtration method separation neutralizer and magnetite pulverulent body.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the magnetite pulverulent body that reclaimed of the embodiment of the invention 1.
Embodiment
The invention provides a kind of method of modifying oil.At first, oil product and magnetite pulverulent body are placed cracker.Oil product make a living matter crude oil or waste oil as the lubricating oil, wheel machine oil or the tower that reclaim at the bottom of oil.Generally speaking, give birth to the chemical constitution complexity of matter crude oil and waste oil product, the oxygen level height, calorific value low (being about between the 3000kcal/kg to 4000kcal/kg), and viscosity too high (＞40cps), be difficult to direct application.Magnetite pulverulent body mainly consist of Fe
3O
4, can be the magnetite pulverulent body of commercial goods or recovery.The weight ratio of magnetite pulverulent body and oil product if the weight ratio of magnetite pulverulent body very little, then can cause lytic effect not good between 5: 100 to 30: 100, must improve cracking temperature again, caused energy consume.If the weight ratio of magnetite pulverulent body is too many, then can cause the magnetite pulverulent body waste.
Then the heating pyrolyze device makes the high carbon number oil product of high viscosity cracking boiling form steam, and condensation is afterwards also collected steam and promptly got low-viscosity low carbon number modifying oil.The Heating temperature of cracker is approximately between 200 ℃ to 450 ℃.Above-mentioned heating preparation technology's pressure can carry out under normal pressure, also can pressurize or underpressure distillation, and its pressure is between between the 0.5atm to 5atm.The advantage of atmospheric cracking is simply to implement this cleavage step, does not need extra increasing/pressure regulating equipment.Decompression cracked advantage can reduce the thermal source loss for reducing cracking temperature, and it is higher to reclaim the oil product carbon number.Pressurization or atmospheric cracking can utilize higher temperature to quicken the oil product cracking, reduce the average carbon number of modifying oil.No matter but which kind of pressure the present invention adopts, all, can significantly improve operational safety much smaller than required 3MPa to the 10MPa pressure of known hydrocracking.
In cracking process, the oil product steam of low carbon number can be condensed in the collector through prolong, and the oil product steam of high carbon number can be got back in the former cracker because of gravity factor, could be condensed in the collector through prolong with the steam attitude up to the oil product that is cracked into low carbon number.After upgrading finished, the average carbon number of the modifying oil of collection was less than 15, and calorific value is greater than 9, and 000kcal/kg, viscosity are less than 10cps, and density is less than 0.90g/cm
3Compare with giving birth to matter crude oil or waste oil, significantly increase calorific value, reduce viscosity and density.By outward appearance, viscid and opaque living matter crude oil or waste oil can form transparent low-viscosity oil product behind upgrading.The weight ratio of above-mentioned modifying oil and the oil product of upgrading not was greater than 75: 100.In other words, when the oil product of upgrading was not the waste oil product, the rate of recovery of modifying oil was greater than 75%.
After above-mentioned cracking finished, the cracker bottom can stay solid-state dregs (scum), and its major ingredient is the rich iron waste material that is full of magnetite.Because the present invention has magnetic in the solid-state dregs of cracker bottom, modes such as available magnetic force absorption are taken out above-mentioned solid-state dregs.Compare with known method for modifying, the present invention is not like the residual many full-bodied greasy filth of meeting on traditional cracking wall.Known technology will cause secondary pollution in order to remove the greasy filth on the wall.In addition, above-mentioned solid-state dregs can further reclaim, and reply once more to be magnetite pulverulent body.
The present invention further provides the formation method of magnetite pulverulent body.At first, get rich iron waste material and be dissolved in acid solution.The source of rich iron waste material is trade waste, mining wastes, spent pickle liquor or factory's tankage (left-over material).Method with above-mentioned modifying oil is an example, and rich iron waste material is solid dregs residual after the cracking.In an embodiment of the present invention, the iron content ratio of rich iron waste material is greater than 25wt%, and its form can be elemental iron, ferric oxide such as FeO, Fe
3O
4, Fe
2O
3, or the alloy of ferric oxide and other metal such as MFe
2O
4(M is other divalent metal).Be understandable that,, can directly add acid solution adjustment pH value when rich iron waste material is liquid during as spent pickle liquor.But when Ruo Dangfu iron waste material is solid-state, can be earlier with physics mode as press, squeeze, mode such as mill makes size of waste less than 1mm, makes its accelerate dissolution in acid solution.The acid solution kind can be common strong acid, example hydrochloric acid, sulfuric acid, nitric acid or above-mentioned mixing.For the iron that makes various kenels in the rich iron waste material is completed into divalence or ferric ion, the pH value of acid solution is approximately between 0-2.
Then filter acid solution to remove insolubles.In an embodiment of the present invention, silica sand is added as slag former for the steelworks dust-collector in the source of rich iron waste material, add coke as reductive agent, the solid phase slag of gained after hot carbon reduction method reclaims ZnO, its ultimate analysis is as follows: Fe＞35wt%, Si＞20wt%, Ca＞10wt%, Mn＞3wt% and trace (＜2wt%) Al, K, Mg, Zn, Cu, Pb, Cl.Be understandable that, when utilizing acid fluid dissolves, still have a large amount of insolubless such as silicon-dioxide from the solid phase slag of Steel Plant.The purpose of filtering acid solution is to remove those insolubless, and insoluble silicon-dioxide is also recyclable as slag former.
Then with in the alkali lye and above-mentioned acid solution to form neutralizer, this moment, iron ion will form Fe
3O
4For avoiding strong neutralization reaction, alkali lye is preferably weak base such as the ammoniacal liquor (NH of pH value between 8-10
4OH), L-Ala (C
3H
5O
2NH
2), methylamine (CH
3NH
2) or above-mentioned combination.
Separate neutralizer and magnetite pulverulent body with filtration method at last, through measuring as can be known Fe by the magnetite pulverulent body of rich iron waste recovery
3O
4Content is greater than 85wt%, and specific surface area is greater than 10m
2/ g, saturated magnetism intensity are greater than 15emu/g, and specific heat is less than 0.4cal/g. ℃.
The present invention utilizes magnetite pulverulent body to have following some benefit as the modifying oil catalyzer.Though magnetite is nonmetal, have speciality such as metal specific heat is low, heat conduction efficiency is good, tool magnetic, and this is as the oxidation phase, can be because of the temperature in modifying oil and the removal process, atmosphere or sour environment corrosion.Magnetite pulverulent body is added in full-bodied primary oil product or the waste oil product, can make the waste oil product thermally equivalent of contact, significantly improve the phenomenon of waste oil product heating bumping.In addition, the magnetite pulverulent body after the use can reclaim once more, can save the expense of modifying catalyst.Part by weight gained recovery oil product of different nature by adjusting magnetite pulverulent body and oil product can be made for base oil or oil fuel respectively.
For making the clearer feature of the present invention of those skilled in the art, the spy is schematically illustrated in following embodiment.
Every data owner that the present invention measures oil product and modifying oil will adopt U.S. material to measure the standard (American Society for Testing and Materials is called for short ASTM) of association.The analytical procedure that measures viscosity is ASTM D445, the analytical procedure that measures calorific value is ASTM D240, the analytical procedure that measures flashing point is ASTM D93, measure moisture content analytical procedure be ASTM D1744, the analytical procedure that measures density is ASTM D5057～90, the analytical procedure that measures ash is ASTMD482, and the analytical procedure of measurement sulfur is ASTM D4294.Use Micromeritics ASAP2010 to measure Fe
3O
4Specific surface area.With the model is the X-x-ray diffraction instrument of Model PW1700 by Philips, measures its compound crystalline phase.Use model to measure its saturated magnetism intensity as MPMS7 superconductive quantum interference quantity of magnetism instrument (SQUID, Superconducting QUantum Interference Device).To measure the physical properties measurement system of module with specific heat, model is DSC Q2000, measures powder specific heat.
Embodiment 1 (in rich iron waste material, taking out magnetite pulverulent body)
The rich iron waste material of getting 100g is dissolved in 1N, the hydrochloric acid of 20mL.The source of rich iron waste material is certain steelworks, learns that after ultimate analysis the elementary composition of this richness iron waste material is: Fe＞35wt%, Si＞20wt%, Ca＞10wt%, Mn＞3wt% and trace (＜2wt%) Al, K, Mg, Zn, Cu, Pb, Cl.Hydrochloric acid is available from Scharlau Chemie S.A., European, and concentration is 1N.
After filtering above-mentioned acid solution, with 1N, the neutralization of the ammoniacal liquor of 55mL.Ammoniacal liquor is available from Showa, Japan, and concentration is 28%.Can be observed neutralizer bottom deposit one deck black flour this moment.
After filtering above-mentioned neutralizer, the oven dry of the black flour of filter cake dewatered promptly gets the magnetite pulverulent body of 50g, and its XRD analysis such as Fig. 1 can confirm that its main compound composition is Fe
3O
4The Fe of magnetite pulverulent body
3O
4Content is 90wt%, and specific surface area is 13m
2/ g, saturated magnetism intensity are 18emu/g, and specific heat is 0.35cal/g. ℃.
Embodiment 2 (method for modifying of oil product)
Get waste lubricating oil and the 10g embodiment 1 prepared magnetite pulverulent body of 100g under directly letting out from certain motor supply shop, insert in the cracker by locomotive.The calorific value of waste lubricating oil is 8574cal/kg, and viscosity is 95cps, and density is 0.95g/cm
3, moisture content is 11wt%, ash is 2.8wt%, and sulfur is 2.3wt%.The constant temperature reaction was 1 hour after distiller was heated to 350 ℃, can collect the modifying oil of 82g.The average carbon number of modifying oil is 14.5, and calorific value is 10824kcal/kg, and viscosity is 0.9cps, and density is 0.87g/cm
3, moisture content is 1.2wt%, ash is 1.6wt%, and sulfur is 0.6wt%.
Embodiment 3 (method for modifying of oil product)
Get 100g by mixing the prepared magnetite pulverulent body of living matter crude oil that wooden waste cracking produces and 10g embodiment 1, insert in the cracker.The calorific value of giving birth to matter crude oil is 3050kcal/kg, and viscosity is 40cps, and density is 1.16g/cm
3, moisture content is 32wt%, ash is 3.8wt%, and sulfur is 0.5wt%.。The constant temperature reaction was 1 hour after distiller was heated to 350 ℃, can collect the modifying oil of 52g.The average carbon number of modifying oil is 12.5, and calorific value is 6580kcal/kg, and viscosity is 0.9cps, and density is 1.04g/cm
3, moisture content is 1.8wt%, ash is 2.0wt%, and sulfur is 0.1wt%.
Embodiment 4 (method for modifying of oil product)
Get 100g from reclaiming the prepared magnetite pulverulent body of useless bilge oil that hulk oceangoing ship oil company provides and 10g embodiment 1, insert in the cracker.The calorific value of useless bilge oil is 7893kcal/kg, and viscosity is 450cps, and density is 1.02g/cm
3, moisture content is 13wt%, ash is 4.5wt%, and sulfur is 3.2wt%.The constant temperature reaction was 1 hour after distiller was heated to 350 ℃, can collect the modifying oil of 79g.The average carbon number of modifying oil is 15.2, and calorific value is 10568kcal/kg, and viscosity is 1.2cps, and density is 0.89g/cm
3, moisture content is 1.5wt%, ash is 1.4wt%, and sulfur is 0.8wt%.
Embodiment 5 (in rich iron waste material, taking out magnetite pulverulent body)
Draw the solid dregs that residue in the distiller bottom among the embodiment 4 behind the modifying oil with magnet.The solid dregs of 10g are dissolved in the hydrochloric acid, and hydrochloric acid is available from Scharlau Chemie S.A., European, and concentration is 1N.
With 36g concentration is 28% ammoniacal liquor, is made into the ammonia soln of 500mL, and above-mentioned acid solution neutralizes.Ammoniacal liquor is available from Showa, Japan, and concentration is 28%.Can be observed neutralizer bottom deposit one deck black flour this moment.
After filtering above-mentioned neutralizer, the oven dry of the black flour of filter cake dewatered promptly gets the magnetite pulverulent body of 8.3g.The Fe of magnetite pulverulent body
3O
4Content is 91wt%, and specific surface area is 13.2m
2/ g, saturated magnetism intensity are 17.8emu/g, and specific heat is 0.38cal/g. ℃.
By above-mentioned experiment as can be known, the magnetite powder volume property before its character of the magnetite pulverulent body after the recovery and the use is similar, can be used as next modifying oil and uses.
Though the present invention describes as above with several embodiment; right its is not in order to limit the present invention; those skilled in the art without departing from the spirit and scope of the present invention; when can changing arbitrarily and retouching, so protection scope of the present invention is as the criterion when the content that the claim scope that look application is defined.
Claims (15)
1. the method for a modifying oil comprises:
One oil product and a magnetite pulverulent body are placed a cracker;
Heating this cracker makes this oil product boiling form a steam; And
Condensation is also collected this steam, promptly gets a upgrading oil product.
2. the method for modifying oil as claimed in claim 1, wherein, this oil product comprises living matter crude oil or waste oil.
3. the method for modifying oil as claimed in claim 1, wherein, the preparation method of this magnetite pulverulent body comprises that getting a rich iron waste material is dissolved in this acid solution of acid solution after-filtration; Form a neutralizer with an alkali lye this acid solution that neutralizes, and this neutralizer contains magnetite pulverulent body; And separate this neutralizer and this magnetite pulverulent body with filtration method.
4. the method for modifying oil as claimed in claim 1, wherein, the weight ratio of this magnetite pulverulent body and this oil product is between 5: 100 to 30: 100.
5. the method for modifying oil as claimed in claim 1 wherein, heats in the step of this distiller, and temperature is between 200 ℃ to 450 ℃, and pressure is between between the 0.5atm to 5atm.
6. the method for modifying oil as claimed in claim 1, wherein, the average carbon number of this modifying oil is less than 10, and calorific value is greater than 9, and 000kcal/kg, viscosity are less than 10cps, and the little 0.9g/cm of density
3
7. the method for modifying oil as claimed in claim 1, wherein, the weight ratio of this modifying oil and this oil product was greater than 75: 100.
8. the preparation method of a magnetite pulverulent body comprises:
Get a rich iron waste material and be dissolved in this acid solution of acid solution after-filtration;
Neutralize this acid solution forming a neutralizer with an alkali lye, and this neutralizer contains a magnetite pulverulent body; And
Separate this neutralizer and this magnetite pulverulent body with filtration method.
9. the preparation method of magnetite pulverulent body as claimed in claim 8, wherein, this richness iron waste material is from trade waste, mining wastes, spent pickle liquor or factory's tankage.
10. the preparation method of magnetite pulverulent body as claimed in claim 8, wherein, the iron-holder of this richness iron waste material is greater than 25wt%.
11. the preparation method of magnetite pulverulent body as claimed in claim 8, wherein, the pH value of this acid solution is between 0-2.
12. the preparation method of magnetite pulverulent body as claimed in claim 8, wherein, this acid solution comprises sulfuric acid, nitric acid, hydrochloric acid or above-mentioned combination.
13. the preparation method of magnetite pulverulent body as claimed in claim 8, wherein, the pH value of this alkali lye is between 8-10.
14. the preparation method of magnetite pulverulent body as claimed in claim 8, wherein this alkali lye comprises ammoniacal liquor, L-Ala, methylamine or above-mentioned combination.
15. as the preparation method of claim 8 a described magnetite pulverulent body, the Fe of this magnetite pulverulent body wherein
3O
4Content is greater than 85wt%, and specific surface area is greater than 10m
2/ g, saturated magnetism intensity are greater than 15emu/g, and specific heat is less than 0.4cal/g. ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430791A (en) * | 2011-07-28 | 2012-05-02 | 中色奥博特铜铝业有限公司 | Method for recovering and reutilizing emulsified liquid for surface milling machine |
| CN102465004A (en) * | 2010-11-10 | 2012-05-23 | 财团法人工业技术研究院 | Method for modifying oil product |
| US9228133B2 (en) | 2010-11-05 | 2016-01-05 | Industrial Technology Research Institute | Method for refining oil |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2960459A (en) * | 1958-12-08 | 1960-11-15 | Sun Oil Co | Hydrocracking of hydrocarbon oils with spent cracking catalyst containing ferric oxide |
| CN1077308A (en) * | 1992-04-07 | 1993-10-13 | 东北工学院 | Method with preparing ferromagnetic fluid form waste pickle |
| CN1891787B (en) * | 2005-07-07 | 2011-04-06 | 南昌大学 | Production technology for preparing biodiesel by solid magnetic catalyst |
-
2008
- 2008-10-17 CN CN 200810166692 patent/CN101724428B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9228133B2 (en) | 2010-11-05 | 2016-01-05 | Industrial Technology Research Institute | Method for refining oil |
| CN102465004A (en) * | 2010-11-10 | 2012-05-23 | 财团法人工业技术研究院 | Method for modifying oil product |
| CN102465004B (en) * | 2010-11-10 | 2014-12-24 | 财团法人工业技术研究院 | Method for modifying oil product |
| CN102430791A (en) * | 2011-07-28 | 2012-05-02 | 中色奥博特铜铝业有限公司 | Method for recovering and reutilizing emulsified liquid for surface milling machine |
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| CN101724428B (en) | 2013-03-06 |
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