CN113603136A - Method for removing vanadium from titanium tetrachloride by using waste lubricating oil - Google Patents
Method for removing vanadium from titanium tetrachloride by using waste lubricating oil Download PDFInfo
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 74
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000002699 waste material Substances 0.000 title claims abstract description 62
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title claims abstract description 60
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000003921 oil Substances 0.000 claims abstract description 62
- 239000012535 impurity Substances 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000003463 adsorbent Substances 0.000 claims abstract description 10
- VZVLQKOGWNLVAC-UHFFFAOYSA-J tetrachlorotitanium vanadium Chemical compound [V].Cl[Ti](Cl)(Cl)Cl VZVLQKOGWNLVAC-UHFFFAOYSA-J 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000004927 clay Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000008346 aqueous phase Substances 0.000 claims 2
- 239000012071 phase Substances 0.000 claims 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 19
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 17
- 238000007670 refining Methods 0.000 abstract description 9
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 8
- 239000002480 mineral oil Substances 0.000 abstract description 8
- 235000010446 mineral oil Nutrition 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- 239000004408 titanium dioxide Substances 0.000 abstract description 8
- 238000005660 chlorination reaction Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 241000544032 Limnobium Species 0.000 abstract description 2
- 238000012824 chemical production Methods 0.000 abstract description 2
- 235000019198 oils Nutrition 0.000 description 55
- 235000010215 titanium dioxide Nutrition 0.000 description 10
- 239000002893 slag Substances 0.000 description 9
- 239000010936 titanium Substances 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 239000002802 bituminous coal Substances 0.000 description 4
- 239000003599 detergent Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 239000002199 base oil Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 230000016615 flocculation Effects 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910003074 TiCl4 Inorganic materials 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000003137 locomotive effect Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 150000004671 saturated fatty acids Chemical class 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- 239000005662 Paraffin oil Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012208 gear oil Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- QLOKAVKWGPPUCM-UHFFFAOYSA-N oxovanadium;dihydrochloride Chemical compound Cl.Cl.[V]=O QLOKAVKWGPPUCM-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
- C01G23/024—Purification of tetrachloride
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0016—Working-up used lubricants to recover useful products ; Cleaning with the use of chemical agents
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0058—Working-up used lubricants to recover useful products ; Cleaning by filtration and centrifugation processes; apparatus therefor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a method for removing vanadium from titanium tetrachloride by using waste lubricating oil, belongs to the technical field of chemical production, and aims to solve the problems that in the prior art, vanadium removing reagents are high in cost and a large amount of waste lubricating oil is difficult to treat in a titanium sponge plant and a titanium dioxide production plant by a chlorination process. The method comprises the steps of uniformly mixing the waste lubricating oil and the adsorbent, preheating to 80-110 ℃, removing impurities in the mixture, introducing the oil after impurity removal as a vanadium removal agent into a titanium tetrachloride vanadium removal reaction kettle, enabling the temperature of the vanadium removal reaction kettle to be 140 ℃, enabling titanium tetrachloride steam to enter a rectifying tower, detecting that the content of vanadium in distilled titanium tetrachloride is less than 1ppm, meeting production requirements, and using the 'regenerated' lubricating oil as a mineral oil vanadium removal agent for refining vanadium removal, changing waste into valuable, saving production cost and reducing environmental pollution.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a method for removing vanadium from titanium tetrachloride by using waste lubricating oil.
Background
The lubricating oil is a liquid or semisolid lubricating agent which is used on various mechanical equipment to reduce friction and protect mechanical workpieces, and mainly plays roles of lubrication, cooling, cleaning, buffering, rust prevention, corrosion prevention and the like, the lubricating oil is generally composed of base oil and additives, the base oil is a main component of the lubricating oil, the base oil is divided into three categories of mineral oil, synthetic oil and vegetable oil, and the mineral oil is most widely applied (more than about 95%). Titanium sponge plants and titanium dioxide plants have a large number of vacuum pumps, fans and motors, generate a large amount of waste oil every month, are complex in oil-wasting components, contain heavy metals and harmful substances such as arsenic, chromium and lead, and can cause potential threats to the environment and human health due to improper treatment. On the other hand, the undenatured mineral oil content in the waste oil is very high (more than 70 percent), metal elements and deteriorated parts in the waste oil can be effectively removed through a corresponding impurity removal process to realize regeneration, but the quality of the regenerated mineral oil is lower than that of crude oil, and the regenerated mineral oil cannot be directly reused as lubricating oil due to the lack of corresponding additives. In order to avoid the harm to the environment and human health caused by improper disposal of the waste lubricating oil, the development of new application approaches thereof has become a necessary trend
Titanium tetrachloride is an important intermediate for producing titanium dioxide and titanium sponge, the impurity content in titanium tetrachloride has serious influence on the quality of titanium dioxide and titanium sponge, and the influence of related compounds of vanadium on the whiteness of titanium dioxide and the hardness of titanium sponge is particularly obvious. If vanadium is not removed, titanium tetrachloride with high vanadium content is adopted to produce titanium white, so that the titanium white is colored, and the performance of the titanium white is affected; if titanium tetrachloride with high vanadium content is used for producing titanium sponge, the hardness of the titanium sponge is obviously increased, and the mechanical property of the product is seriously influenced.
Vanadium in crude titanium mainly adopts VOCl3The product has a boiling point of 127 ℃ close to that of titanium tetrachloride (136 ℃), and the two have small separation coefficients and cannot be separated by ordinary distillation or rectification. The process for removing vanadium from crude titanium tetrachloride generally adopts a chemical method, namely, a chemical reagent is added into the crude titanium tetrachloride to ensure that VOCl3 impurities are selectively reduced or selectively precipitated to generate insoluble vanadium compounds which are separated from TiCl4, and generally, organic matters are added to obtain better vanadium removal effect.
Application No. 201510749816.9 discloses an organic vanadium removal reagent in which saturated fatty acids are mixed with unsaturated fatty acids.
The' 201410398848.4 patent discloses a mixed organic vanadium removal solution made of paraffin oil, saturated fatty acid, p-phenylenediamine, 2, 4-trimethyl-1, 2-dihydroquine polymer.
The vanadium removing reagent can effectively remove the vanadium impurity of TiCl4, but the vanadium removing reagent has high cost.
In consideration of the refining vanadium removal process of titanium tetrachloride, the 'regenerated' lubricating oil can be used as a mineral oil vanadium removal reagent for refining vanadium removal, so that the production cost is saved, and the problem of difficult treatment of waste lubricating oil is solved.
Disclosure of Invention
Aiming at the problems of high cost of vanadium removal reagent and difficulty in treatment of a large amount of waste lubricating oil in a titanium sponge factory and a titanium dioxide factory by a chlorination process in the prior art, the invention provides a method for removing vanadium from titanium tetrachloride by using the waste lubricating oil, which combines the refining process of a workshop and takes 'regenerated' lubricating oil as a mineral oil vanadium removal reagent for refining vanadium removal, thereby changing waste into valuable, saving production cost and reducing environmental pollution.
The technical scheme adopted by the invention is as follows:
a method for removing vanadium from titanium tetrachloride by using waste lubricating oil comprises the following steps:
uniformly mixing the waste lubricating oil and the adsorbent, preheating to 80-110 ℃, removing impurities in the mixture, introducing the oil after impurity removal as a vanadium removal agent into a titanium tetrachloride vanadium removal reaction kettle, wherein the temperature of the vanadium removal reaction kettle is 140 ℃, titanium tetrachloride steam enters a rectifying tower, and detecting that the content of vanadium in the distilled titanium tetrachloride is less than 1ppm, so that the production requirement is met.
Wherein, one mode of edulcoration is: adding distilled water into the mixture for washing, standing for 2-5h after washing to form an oil phase and a water phase, and separating the oil phase and the water phase. The distilled detergent water is added, so that metals can be dissolved in the distilled detergent water, meanwhile, the water layer is positioned below, and the flocculated impurities can fall into the water phase through an interface under the action of gravity; the layered lubricating oil contains a small part of trace water after being washed, the trace water is added into the crude titanium and then reacts with aluminum trichloride in the crude titanium to generate precipitate, and meanwhile, the effect of removing aluminum is achieved, and the corrosion of the aluminum trichloride to equipment is reduced.
And the water phase is discharged into a factory sewage treatment system through a pipeline for treatment.
Preferably, another way of removing the impurities is: filtering the mixture by using an oil filter to remove impurities, doping the filtered impurities into bituminous coal, and using the bituminous coal as boiler fuel, wherein the recovery rate of the oil is about 85-95 percent
The used waste lubricating oil is used in the method for removing vanadium from titanium tetrachloride, the waste lubricating oil is vacuum pump waste oil or gear waste oil, and further the vacuum pump waste oil and the gear waste oil are waste lubricating oil which is replaced between a vacuum pump, a fan and an electric locomotive in a titanium sponge factory and a titanium dioxide factory.
Preferably, the adsorbent is clay or concentrated sulfuric acid with the mass fraction of 98%, and the clay or the concentrated sulfuric acid can effectively adsorb or flocculate impurities in the oil.
Preferably, the ratio of the adsorbent to the used lubricating oil is 1 to 5%.
Preferably, the lubricating oil after impurity removal is collected in an oil storage tank, the oil storage tank is connected with a titanium tetrachloride vanadium removal reaction kettle through a pipeline, the pipeline is provided with a regulating valve and a flowmeter, the oil addition can be regulated according to the flow of titanium tetrachloride, and the proportioning coefficient of the waste lubricating oil after impurity removal and the titanium tetrachloride is 0.5-1.5 thousandth.
Preferably, the waste lubricating oil is vacuum pump waste oil or gear waste oil.
Wherein, the vanadium slag obtained after vanadium removal can be enriched and discharged, and can be used as a vanadium extraction raw material and also can be returned to a chlorination furnace quench tower for use.
The invention has the beneficial effects that: the method for removing vanadium from titanium tetrachloride by using waste lubricating oil provided by the invention is characterized in that the waste lubricating oil is subjected to flocculation precipitation and filtration and then is used as regenerated lubricating oil for refining and removing vanadium from titanium tetrachloride, so that a new utilization way is provided for the waste lubricating oil, waste is turned into wealth, the cost for refining and removing vanadium from titanium tetrachloride is saved, and environmental pollution is reduced.
Drawings
The invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is a schematic flow diagram of a process for removing vanadium from titanium tetrachloride using a spent lubricating oil.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all the embodiments. The components of embodiments of the present application, generally described and illustrated in the figures herein, may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present application, presented in the accompanying drawings, is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present application without making any creative effort, shall fall within the protection scope of the present application.
In the description of the embodiments of the present application, it should be noted that the terms "first", "second", "third", and the like are used for distinguishing the description, and are not to be construed as indicating or implying relative importance.
The present invention will be described in detail with reference to fig. 1.
The waste lubricating oil from workshop replacement contains mechanical impurities and colloid formed after oil deterioration, and the existence of the impurities affects the kinematic viscosity of the oil on one hand, so that the oil is not easy to add into a reaction kettle, and the pipeline can be blocked to affect production. Meanwhile, impurities in the waste oil can be introduced into the refined titanium tetrachloride, so that the contents of metal impurities and carbon in the refined titanium tetrachloride exceed the standard, and the waste oil needs to be treated before use.
A method for removing vanadium from titanium tetrachloride by using waste lubricating oil comprises the following steps:
uniformly mixing the waste lubricating oil and the adsorbent, preheating to 80-110 ℃, removing impurities in the mixture, introducing the oil after impurity removal as a vanadium removal agent into a titanium tetrachloride vanadium removal reaction kettle, wherein the temperature of the vanadium removal reaction kettle is 140 ℃, titanium tetrachloride steam enters a rectifying tower, and detecting that the content of vanadium in the distilled titanium tetrachloride is less than 1ppm, so that the production requirement is met.
The mechanism of oil vanadium removal is as follows: after the oil after impurity removal is added into titanium tetrachloride, the oil is gradually cracked into high-activity nascent carbon particles under the catalysis of Lewis acids such as aluminum trichloride, niobium pentoxide and the like dissolved in the titanium tetrachloride at a certain temperature (110-3Adsorbing and reducing VOCl3Separating out from titanium tetrachloride to achieve the vanadium removal effect, and the reaction equation is as follows:
VOCl3+C＝VOCl2↓+CO↑
the top of the reaction kettle is connected with a rectifying tower, the bottom of the rectifying tower is provided with a return pipe, rising titanium tetrachloride steam is in countercurrent contact with refluxing titanium tetrachloride liquid on a tower plate, mass transfer and heat transfer are carried out for rectification, the bottom of the kettle is provided with a slag discharge port, solid residues after reaction are periodically discharged through the slag discharge port, the discharged residues are transferred to the next vanadium extraction process to be used as raw materials, and the whole process is finished.
In the above process steps, one way of removing impurities is: adding distilled water into the mixture for washing, standing for 2-5h after washing to form an oil phase and a water phase, and separating the oil phase and the water phase. Wherein the oil phase is used as a vanadium removing agent and is introduced into a titanium tetrachloride vanadium removing reaction kettle, and the water phase is discharged into a factory sewage treatment system through a pipeline for treatment.
The impurity removal mode has the advantages that: the distilled detergent water is added, so that metals can be dissolved in the distilled detergent water, meanwhile, the water layer is positioned below, and the flocculated impurities can fall into the water phase through an interface under the action of gravity; the layered lubricating oil contains a small part of trace water after being washed, the trace water is added into the crude titanium and then reacts with aluminum trichloride in the crude titanium to generate precipitate, and meanwhile, the effect of removing aluminum is achieved, and the corrosion of the aluminum trichloride to equipment is reduced.
Preferably, another embodiment of the impurity removal is: filtering the mixture by using an oil filter, filtering out impurities, introducing the oil after impurity removal as a vanadium removing agent into a titanium tetrachloride vanadium removing reaction kettle,
the impurity removal mode has the advantages that: the filtered impurities are mixed into bituminous coal and used as boiler fuel, and the recovery rate of oil is about 85-95%.
The used waste lubricating oil is used in the method for removing vanadium from titanium tetrachloride, the waste lubricating oil is vacuum pump waste oil or gear waste oil, and further the vacuum pump waste oil and the gear waste oil are waste lubricating oil which is replaced between a vacuum pump, a fan and an electric locomotive in a titanium sponge factory and a titanium dioxide factory.
Preferably, the adsorbent is clay or concentrated sulfuric acid with the mass fraction of 98%, and the clay or the concentrated sulfuric acid can effectively adsorb or flocculate impurities in the oil. On one hand, the addition of concentrated sulfuric acid is oxidation, which decomposes deteriorated waste oil and reduces acidity; on the other hand, the flocculation effect is used for adsorbing and precipitating impurities in the waste oil and purifying the waste oil.
Preferably, the ratio of the adsorbent to the used lubricating oil is 1 to 5%.
Preferably, the lubricating oil after impurity removal is collected in an oil storage tank, the oil storage tank is connected with a titanium tetrachloride vanadium removal reaction kettle through a pipeline, the pipeline is provided with a regulating valve and a flowmeter, the oil addition can be regulated according to the flow of titanium tetrachloride, and the proportioning coefficient of the waste lubricating oil after impurity removal and the titanium tetrachloride is 0.5-1.5 thousandth.
Wherein, the vanadium slag obtained after vanadium removal can be enriched and discharged, and can be used as a vanadium extraction raw material and also can be returned to a chlorination furnace quench tower for use.
The invention has the beneficial effects that: the method for removing vanadium from titanium tetrachloride by using waste lubricating oil provided by the invention is characterized in that the waste lubricating oil is subjected to flocculation precipitation and filtration and then is used as regenerated lubricating oil for refining and removing vanadium from titanium tetrachloride, so that a new utilization way is provided for the waste lubricating oil, waste is turned into wealth, the cost for refining and removing vanadium from titanium tetrachloride is saved, and environmental pollution is reduced.
The following examples are intended to illustrate specific embodiments of the present invention without limiting the scope of the invention to the examples.
Example 1: use of vacuum pump waste oil for removing vanadium from coarse titanium
Adding collected waste vacuum pump oil into a heating kettle, adding clay or concentrated sulfuric acid with the mass ratio of 3%, heating to 100 ℃, reacting for 5 hours, adding a proper amount of distilled water for washing, standing for 5 hours, forming an oil phase and a water phase after layering, separating the oil phase and the water phase, adding the oil phase on the upper layer into titanium tetrachloride according to the flow of the titanium tetrachloride according to the proportion of 1.5 per mill, removing vanadium at the temperature of 140 ℃ in the reaction kettle, introducing titanium tetrachloride steam into a rectifying tower, and periodically discharging vanadium slag at the bottom through a bottom slag discharge port. By detecting that the content of vanadium in the distilled titanium tetrachloride is less than 1ppm, the chroma is as follows: less than 5, meets the production requirements.
Example 2: use of gear waste oil for removing vanadium from coarse titanium
Adding the collected waste gear oil into a heating kettle, adding clay or concentrated sulfuric acid with the mass ratio of 3%, heating to 100 ℃, reacting for 5 hours, filtering the mixture by using an oil filter, adding the filtered oil into an oil storage tank, and mixing the slag into bituminous coal to be used as boiler fuel; adding the oil phase into titanium tetrachloride according to the flow rate of the titanium tetrachloride by 1.5 per mill, wherein the temperature of a vanadium removal reaction kettle is 140 ℃, titanium tetrachloride steam enters a rectifying tower, and bottom vanadium slag is periodically discharged through a bottom slag discharge port. By detecting that the content of vanadium in the distilled titanium tetrachloride is less than 1ppm, the chroma is as follows: less than 5, meets the production requirements.
The above-mentioned embodiments only express the specific embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present application. It should be noted that, for those skilled in the art, without departing from the technical idea of the present application, several changes and modifications can be made, which are all within the protection scope of the present application.
Claims (7)
1. A method for removing vanadium from titanium tetrachloride by using waste lubricating oil is characterized by comprising the following steps:
uniformly mixing the waste lubricating oil and the adsorbent, preheating to 80-110 ℃, removing impurities in the mixture, introducing the oil after impurity removal as a vanadium removal agent into a titanium tetrachloride vanadium removal reaction kettle, wherein the temperature of the vanadium removal reaction kettle is 140 ℃, titanium tetrachloride steam enters a rectifying tower, and detecting that the content of vanadium in the distilled titanium tetrachloride is less than 1ppm, so that the production requirement is met.
2. The method for removing vanadium from titanium tetrachloride according to claim 1, wherein the step of removing the impurities comprises adding distilled water to the mixture for washing, standing for 2-5h after washing to form an oil phase and an aqueous phase, and separating the oil phase and the aqueous phase.
3. The method for removing vanadium from titanium tetrachloride according to claim 1, wherein the step of removing impurities comprises filtering the mixture by using an oil filter to remove impurities.
4. The method for removing vanadium from titanium tetrachloride by using waste lubricating oil as claimed in claim 1, wherein the adsorbent is clay or concentrated sulfuric acid with a mass fraction of 98%.
5. The method of claim 4, wherein the ratio of the adsorbent to the used lubricating oil is 1-5%.
6. The method for removing vanadium from titanium tetrachloride according to claim 1, wherein the mixing ratio of the waste lubricating oil after impurity removal to titanium tetrachloride is 0.5-1.5 ‰.
7. The method for removing vanadium from titanium tetrachloride according to claim 1, wherein the used lubricating oil is vacuum pump waste oil or gear waste oil.
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| CN107010656A (en) * | 2017-04-25 | 2017-08-04 | 攀钢集团研究院有限公司 | It is refined to titanium tetrachloride except the method for vanadium using gutter oil |
| CN113046165A (en) * | 2021-03-31 | 2021-06-29 | 武汉工程大学 | Regeneration treatment method of waste lubricating oil |
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| JPH09286618A (en) * | 1996-04-23 | 1997-11-04 | Ishihara Sangyo Kaisha Ltd | Method for purifying titanium tetrachloride |
| JP2010254486A (en) * | 2009-04-21 | 2010-11-11 | Japan Energy Corp | Compounded oil for purifying titanium tetrachloride |
| CN106824055A (en) * | 2017-01-24 | 2017-06-13 | 江苏理工学院 | A kind of sorbent regeneration process of waste lubricating oil |
| CN107010656A (en) * | 2017-04-25 | 2017-08-04 | 攀钢集团研究院有限公司 | It is refined to titanium tetrachloride except the method for vanadium using gutter oil |
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