CN104560122B - A kind of forming oil column oil reclaiming method - Google Patents
A kind of forming oil column oil reclaiming method Download PDFInfo
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- CN104560122B CN104560122B CN201310520724.4A CN201310520724A CN104560122B CN 104560122 B CN104560122 B CN 104560122B CN 201310520724 A CN201310520724 A CN 201310520724A CN 104560122 B CN104560122 B CN 104560122B
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- 238000000034 method Methods 0.000 title claims abstract description 59
- 239000002699 waste material Substances 0.000 claims abstract description 87
- 239000003463 adsorbent Substances 0.000 claims abstract description 56
- 238000000465 moulding Methods 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000003921 oil Substances 0.000 claims description 300
- 238000010438 heat treatment Methods 0.000 claims description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000009418 renovation Methods 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002808 molecular sieve Substances 0.000 claims description 5
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 5
- 239000008157 edible vegetable oil Substances 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 27
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 14
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 abstract description 14
- 238000011069 regeneration method Methods 0.000 abstract description 14
- 230000008929 regeneration Effects 0.000 abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 12
- 229910021529 ammonia Inorganic materials 0.000 abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 description 17
- 230000000694 effects Effects 0.000 description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 13
- 239000004411 aluminium Substances 0.000 description 10
- 239000011148 porous material Substances 0.000 description 10
- 238000010792 warming Methods 0.000 description 10
- 239000008187 granular material Substances 0.000 description 9
- 239000002199 base oil Substances 0.000 description 8
- 239000003344 environmental pollutant Substances 0.000 description 8
- 231100000719 pollutant Toxicity 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- -1 aluminum ions Chemical class 0.000 description 5
- 239000008279 sol Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 4
- 238000007493 shaping process Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000003384 small molecules Chemical class 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 239000004312 hexamethylene tetramine Substances 0.000 description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000010913 used oil Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
-
- B01J35/51—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0072—Preparation of particles, e.g. dispersion of droplets in an oil bath
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
- C10G31/06—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for by heating, cooling, or pressure treatment
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Wood Science & Technology (AREA)
- Dispersion Chemistry (AREA)
- Materials Engineering (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of forming oil column oil reclaiming method, wherein, the method includes any one in following manner: mode one: forming oil column waste oil is contacted by (1) with adsorbent；(2) mixture obtained after step (1) being contacted heats under vacuum conditions, filters, obtains reclaimed oil；Mode two: forming oil column waste oil is heated by (a) under vacuum conditions；B forming oil column waste oil that () obtains after step (a) being heated contacts with adsorbent, filters, obtains reclaimed oil.The forming oil column oil reclaiming method provided by the present invention, aluminium ion in forming oil column waste oil, water and gas (mainly ammonia and formaldehyde) etc. are removed, make the forming oil column oil surface tension that gives up be reduced to after regeneration work as with fresh molding oil phase, and the color of reclaimed oil also makes moderate progress.Make can continue on for the forming oil column of catalyst through the forming oil column waste oil of regeneration.
Description
Technical field
The present invention relates to a kind of forming oil column oil reclaiming method.
Background technology
Oil-drop method is a kind of method of shaping of catalyst, is the important step in catalyst preparation process.The method
Utilizing the characteristic of colloidal sol generation gelation, make colloidal sol drip in oil medium, form globule by means of capillary effect, globule coagulates
Gel forms bead, thus prepares evengranular catalyst spheroid.The method is applicable to the material with gelatination property.
To use oil in the method indispensably, its Main Function is beneficially molding.But these oil are employing a period of time
After become waste oil, it is impossible to reoffering good molding effect, the catalyst spheroid regularity of molding is deteriorated.Waste oil is also for enterprise simultaneously
Industry and environment bring the pressure of pollution, it is therefore desirable to process these forming oil column waste oil.
At present useless oil treatment process is a lot, such as separation by precipitation, Filtration and pressure partition method etc., but these methods master
It is directed to the used oil that refinery's waste oil of poor quality and automobile (or steamer etc.) use.As CN102191123A discloses one
Waste oil regeneration production process, is included under pressure 0.1-0.4MPa and by magnetic filter, waste oil is filtered to remove metal impurities；
Then under pressure 0.1-0.4MPa, the large granular impurity in waste oil is removed by basket filter；Blood pressure lowering dehydration again, molecule steam
Evaporate purification and filter polishing.But, this process technique is unsuitable for forming oil column and gives up oil handling.
Pollution condition in forming oil column waste oil is diverse with the pollution condition of refinery's waste oil and used oil, because of
This, need a kind of method that can regenerate forming oil column waste oil, enables the forming oil column waste oil through regeneration to be used further to oil column
Molding.
Summary of the invention
Present invention aim to address the problem that forming oil column waste oil can not carry out forming oil column again, it is provided that a kind of new oil
Post molding oil reclaiming method.
The present inventor finds under study for action, and through use after a while, molding oil darkens, molding effect
It is deteriorated.Tracing it to its cause, molding oil is contaminated, and causes molding oil surface tension to become big, causes carrying out effect during shaping of catalyst
It is deteriorated.The major pollutants polluted are metallic aluminium ion, water and gas (mainly ammonia and formaldehyde), and they come from
Catalyst colloidal sol and the gelation process of colloidal sol.Therefore, effectively remove above-mentioned pollutant, improve used forming oil column waste oil
Surface tension, forming oil column waste oil can be regenerated so that it is can continue to for shaping of catalyst, it is thus achieved that there is preferable spheroid
The catalyst of regularity.
To achieve these goals, the present invention provides a kind of forming oil column oil reclaiming method, and wherein, the method includes
In following manner any one: mode one: forming oil column waste oil is contacted by (1) with adsorbent；After (2) step (1) being contacted
To mixture heat under vacuum conditions, filter, obtain reclaimed oil；Mode two: (a) by forming oil column waste oil at vacuum state
Lower heating；B forming oil column waste oil that () obtains after step (a) being heated contacts with adsorbent, filters, obtains reclaimed oil.
The forming oil column oil reclaiming method provided by the present invention, by the aluminium ion in forming oil column waste oil, water and
Gas (mainly ammonia and formaldehyde) etc. remove, and make the forming oil column oil surface tension that gives up be reduced to after regeneration become with fresh
Type oil phase is worked as, and the color of reclaimed oil also makes moderate progress.Make the forming oil column waste oil through regeneration can continue on for urging
The forming oil column of agent.Such as, aluminium composition in the forming oil column waste oil after the method regeneration of embodiment 3 is used to be reduced to 62
μ g/g, surface tension is reduced to 27.21mN/m, and the color of reclaimed oil S3 reverts to yellow, and it carries out catalyst oil column again
Molding can obtain the catalyst granules with preferable spheroid regularity.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and constitutes the part of description, with following tool
Body embodiment is used for explaining the present invention together, but is not intended that limitation of the present invention.In the accompanying drawings:
Fig. 1 is that the outer of spherical regularity using fresh molding oil to carry out the catalyst granules that forming oil column obtains is taken into consideration
Sheet；
Fig. 2 is to use forming oil column waste oil to carry out forming oil column to obtain the outer of spherical regularity of catalyst granules and take into consideration
Sheet；
Fig. 3 is that the reclaimed oil S3 using regeneration methods of the invention to obtain carries out the catalyst granules that forming oil column obtains
The outward appearance photo of spherical regularity.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is described in detail.It should be appreciated that described herein specifically
Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
The present invention provides a kind of forming oil column oil reclaiming method, and wherein, it is any that the method includes in following manner
A kind of: mode one: forming oil column waste oil is contacted by (1) with adsorbent；(2) mixture obtained after step (1) being contacted is very
Heat under dummy status, filter, obtain reclaimed oil；Mode two: forming oil column waste oil is heated by (a) under vacuum conditions；B () will step
Suddenly the forming oil column waste oil obtained after (a) heating contacts with adsorbent, filters, obtains reclaimed oil.
According to the present invention, take adsorbent removing and the method heated under vacuum conditions that forming oil column waste oil is entered
Row regeneration, it is possible to the pollutant such as effective aluminium ion, water and gas (predominantly ammonia and methane) removed in forming oil column waste oil,
So that forming oil column waste oil regeneration.In the present invention, forming oil column waste oil is connect by forming oil column oil reclaiming method with adsorbent
The not particularly requirement of the order of the step that the step touched and forming oil column waste oil heat under vacuum conditions, can be mode
One, it is also possible to for mode two.Under preferable case, forming oil column oil reclaiming method is mode one.The regeneration of employing mode one
The reclaimed oil that method obtains has lower metallic aluminium ion concentration and the closer surface tension of green oil and color, again enters
During row forming oil column, shaping of catalyst effect is more preferable.
According to the present invention, use adsorbent can remove the metallic aluminium ion in forming oil column waste oil, part water, ammonia with
And the pollutant such as formaldehyde.Under preferable case, described adsorbent is 1:10-30 with the weight ratio of described forming oil column waste oil；More excellent
Choosing, described adsorbent is 1:15-20 with the weight ratio of described forming oil column waste oil.Carry out regenerating in above-mentioned weight ratio
To forming oil column waste oil can again carry out forming oil column, it is thus achieved that the molding effect of catalyst granules more preferable.
According to the present invention, described adsorbent can be the various adsorbents being capable of objects of the present invention, i.e. permissible
Absorption removes the aluminum ions various adsorbents of metal in forming oil column waste oil, under preferable case, described adsorbent be silicon oxide,
At least one in activated alumina, activated carbon and molecular sieve；It is further preferred that described adsorbent is activated alumina and/or activity
Charcoal.
According to the present invention, described adsorbent is the porous material with loose structure, and this loose structure can use this area
Known physico-chemical parameter specific surface area and pore volume describe, and concrete numerical value is measured by N2 adsorption BET.The present invention can make
With having the adsorbent of various pore structure, the specific surface area of the most described adsorbent is 197-1091m2/ g, pore volume is 0.29-
0.94mL/g。
In the present invention, described adsorbent can have certain shape, the most described adsorbent to be silicon oxide, activated alumina
Or during molecular sieve, can be the particle diameter granular substance that is more than 3mm, can be bar shaped, cylindricality or spherical；If described adsorbent is for living
During property charcoal, adsorbent can be lamellar.Described adsorbent can be commercially available, and such as silicon oxide can be available from Qingdao Haiyang
The ocean board of factory, activated alumina can be purchased from Chalco Shandong branch company, and molecular sieve can be purchased from middle Effect of Catalysis In Petrochemistry agent
Branch company, activated carbon can be purchased from Li Yang Zhuxi, Jiangsu Tan Ye company limited.
In the method that the present invention provides, adsorbent is used directly for contacting with forming oil column waste oil.In order to make preferably
Ensure the adsorption effect of adsorbent, under preferable case, before adsorbent is contacted with forming oil column waste oil, adsorbent is carried out pre-
Process, remove the small-molecule substances such as the water adsorbed in described adsorbent and gas.Under preferable case, adsorbent is carried out by invention
The method of pretreatment can use the technology removing the small-molecule substances such as the water adsorbed in adsorbent and gas that this area is conventional
Means, such as, can be dried 10-24 hour at 100-140 DEG C, then be evacuated to 0.01-0.1MPa in terms of gauge pressure, to remove
Remove the water in duct and micro-molecular gas.
According to the present invention, in described renovation process, in mode one, forming oil column waste oil contacts with adsorbent and mode two
Described in after heating the forming oil column waste oil that obtains contact with adsorbent, it is possible to achieve the pollution in removal forming oil column waste oil
Thing.Under preferable case, the condition of described contact includes, in terms of gauge pressure, the pressure of described contact is 0.01-0.1MPa, described in connect
The temperature touched is 20-40 DEG C；It is further preferred that in terms of gauge pressure, the pressure of described contact is 0.08-0.09MPa.The time of described contact
As long as guaranteeing fully to be removed by the metallic aluminium ion in forming oil column waste oil, counterbalance effect and cost, it is preferable that described
The time of contact is 20-50 minute.In the condition and range of above-mentioned contact, it is possible to achieve preferably in removing forming oil column waste oil
Pollutant.In the present invention, under preferable case, described contact is under agitation carried out.
According to the present invention, in described renovation process, described in mode one, mixture heats and mode under vacuum conditions
In two, forming oil column waste oil heats under vacuum conditions, can remove the water in mixture or forming oil column waste oil and gas is (main
Ammonia to be and formaldehyde) etc. small-molecule substance.Under preferable case, the condition heated under vacuum conditions includes, in terms of gauge pressure, and institute
The pressure stating vacuum is 0.01-0.10MPa, and the temperature of described heating is 130-180 DEG C；It is further preferred that in terms of gauge pressure, described vacuum
Pressure be 0.08-0.09MPa, the temperature of described heating is 150-160 DEG C.As long as the time of described heating guarantees fully
By the water in forming oil column waste oil and gas removal, counterbalance effect and cost, it is preferable that the time of described heating is that 3-5 is little
Time.In the present invention, under preferable case, described heating is under agitation carried out.
According to the present invention, described forming oil column waste oil be molding oil during the forming oil column of catalyst through being used for multiple times
After the oil that obtains.The molding oil that can use in forming oil column can select according to the character of the catalyst colloidal sol in forming oil column
Select.Under preferable case, at least in oily based on forming the molding oil of described forming oil column waste oil, pumping fluid and edible oil
Kind, can be such as SN500 base oil.
According to the present invention, molding oil gradually contains aluminium ion etc. during the forming oil column of catalyst after being used for multiple times
Pollutant, molding oil properties changes.When the most aluminum ions content of pollutant increases, molding oil properties is deteriorated, then carries out
During catalyst forming oil column, the spherical regularity of the catalyst granules obtained is deteriorated, and the catalyst quality of preparation declines.With described
On the basis of the gross weight of forming oil column waste oil, in described forming oil column waste oil, during aluminum ions content >=305 μ g/g, character is deteriorated,
Need regeneration；In described forming oil column waste oil, aluminum ions content can be 305-1000 μ g/g.
According to the present invention, after containing the pollutant such as aluminium ion in described forming oil column waste oil, oil properties changes, such as surface
Tension force increases, and causes forming oil column effect to be deteriorated.Under preferable case, described forming oil column waste oil surface tension at 40 DEG C >=
30mN/m；Described forming oil column waste oil surface tension at 40 DEG C can be 30-40mN/m.
Hereinafter will be described the present invention by embodiment.In following example, in forming oil column waste oil aluminum from
Sub-content surpasses oil plant spectroanalysis instrument by Spectro Si group of the U.S. and records according to ASTM D6595 standard-required；Surface tension
Shanghai Hengping Instrument & Meter Plant BYX-2 model instrument is used to record according to GB6541-86 standard-required；Specific surface area and pore volume
N2 adsorption BET is used to measure.
Embodiment 1
The present embodiment is for illustrating the forming oil column oil reclaiming method that the present invention provides.
By 10.0g activated alumina (particle diameter 3mm, spherical.Purchased from Chalco Shandong branch company.Specific surface area is
197m2/ g, pore volume is 0.62mL/g) be dried 24 hours at 100 DEG C, it is subsequently adding in Dewar bottle, is evacuated to 0.01MPa.
(1) adsorbent.By 150g forming oil column waste oil (forming oil column waste oil μ g/g Han aluminium ion 756,40 DEG C of surfaces
Tension force is 30.47mN/m.Forming oil column oil is SN500 base oil, fresh described forming oil column 40 DEG C of surface tension of oil
For 27.20mN/m) add in Dewar bottle and contact with adsorbent stirring.Contact pressure is 0.01MPa, and Contact Temperature is 25 DEG C, connects
The tactile time is 30 minutes.
(2) heating in vacuum.Adsorbent forming oil column waste oil will be completed add in there-necked flask together with adsorbent
Stirring.It is evacuated to 0.08MPa, and is warming up to 150 DEG C of heating 4 hours.Filter out adsorbent and obtain reclaimed oil S1.
The aluminium composition of the reclaimed oil S1 that mensuration obtains and the surface tension of 40 DEG C, and observe color.The results are shown in Table 1.
Embodiment 2
The present embodiment is for illustrating the forming oil column oil reclaiming method that the present invention provides.
By 10.0g activated carbon (lamellar.Purchased from Li Yang Zhuxi, Jiangsu Tan Ye company limited.Specific surface area is 1091m2/ g, hole
Volume is 0.54mL/g) it is dried 10 hours at 140 DEG C, it is subsequently adding in Dewar bottle, is evacuated to 0.05MPa.
(1) adsorbent.By 200g forming oil column waste oil (forming oil column waste oil μ g/g Han aluminium ion 756,40 DEG C of surfaces
Tension force is 30.47mN/m.Forming oil column oil is SN500 base oil, fresh described forming oil column 40 DEG C of surface tension of oil
For 27.20mN/m) add in Dewar bottle and contact with adsorbent stirring.Contact pressure is 0.05MPa, and Contact Temperature is 20 DEG C, connects
The tactile time is 50 minutes.
(2) heating in vacuum.Adsorbent forming oil column waste oil will be completed add in there-necked flask together with adsorbent
Stirring.It is evacuated to 0.085MPa, and is warming up to 155 DEG C of heating 5 hours.Filter out adsorbent and obtain reclaimed oil S2.
The aluminium composition of the reclaimed oil S2 that mensuration obtains and the surface tension of 40 DEG C, and observe color.The results are shown in Table 1.
Embodiment 3
The present embodiment is for illustrating the forming oil column oil reclaiming method that the present invention provides.
By 10.0g activated alumina (particle diameter 3mm, spherical.Purchased from Chalco Shandong branch company.Specific surface area is
197m2/ g, pore volume is 0.62mL/g) be dried 16 hours at 120 DEG C, it is subsequently adding in Dewar bottle, is evacuated to 0.09MPa.
(1) adsorbent.By 180g forming oil column waste oil (forming oil column waste oil μ g/g Han aluminium ion 756,40 DEG C of surfaces
Tension force is 30.47mN/m.Forming oil column oil is SN500 base oil, fresh described forming oil column 40 DEG C of surface tension of oil
For 27.20mN/m) add in Dewar bottle and contact with adsorbent stirring.Contact pressure is 0.09MPa, and Contact Temperature is 40 DEG C, connects
The tactile time is 20 minutes.
(2) heating in vacuum.Adsorbent forming oil column waste oil will be completed add in there-necked flask together with adsorbent
Stirring.It is evacuated to 0.09MPa, and is warming up to 160 DEG C of heating 3 hours.Filter out adsorbent and obtain reclaimed oil S3.
The aluminium composition of the reclaimed oil S3 that mensuration obtains and the surface tension of 40 DEG C, and observe color.The results are shown in Table 1.
Embodiment 4
The present embodiment is for illustrating the forming oil column oil reclaiming method that the present invention provides.
According to the method for embodiment 3, forming oil column waste oil is regenerated, except for the difference that, with " 10.0g silicon oxide (particle diameter
3mm is spherical.Purchased from Haiyang Chemical Plant, Qingdao.Specific surface area is 374m2/ g, pore volume is 0.94mL/g) " " 10.0g's replacement lives
Property aluminium oxide ".Obtain reclaimed oil S4.The aluminium composition of the reclaimed oil S4 that mensuration obtains and the surface tension of 40 DEG C, and observe
Color.Result is as shown in table 1.
Embodiment 5
The present embodiment is for illustrating the forming oil column oil reclaiming method that the present invention provides.
According to the method for embodiment 3, forming oil column waste oil is regenerated, except for the difference that, with " the 5A molecular sieve of 10.0g
(particle diameter 3mm, spherical.Purchased from middle Effect of Catalysis In Petrochemistry agent branch company.Specific surface area is 625m2/ g, pore volume is 0.29mL/g) " substitute
" 10.0g activated alumina ".Obtain reclaimed oil S5.Measure the aluminium composition of reclaimed oil S5 obtained and the surface of 40 DEG C is opened
Power, and observe color.Result is as shown in table 1.
Embodiment 6
The present embodiment is for illustrating the forming oil column oil reclaiming method that the present invention provides.
According to the method for embodiment 3, forming oil column waste oil is regenerated, except for the difference that, with " being warming up in step (2)
130 DEG C " replacement " is warming up to 160 DEG C ".Obtain reclaimed oil S6.The aluminium composition of the reclaimed oil S6 that mensuration obtains and the table of 40 DEG C
Surface tension, and observe color.Result is as shown in table 1.
Embodiment 7
The present embodiment is for illustrating the forming oil column oil reclaiming method that the present invention provides.
According to the method for embodiment 3, forming oil column waste oil is regenerated, except for the difference that, with " being warming up in step (2)
180 DEG C " replacement " is warming up to 160 DEG C ".Obtain reclaimed oil S7.The aluminium composition of the reclaimed oil S7 that mensuration obtains and the table of 40 DEG C
Surface tension, and observe color.Result is as shown in table 1.
Embodiment 8
The present embodiment is for illustrating the forming oil column oil reclaiming method that the present invention provides.
By 10.0g activated alumina (particle diameter 3mm, spherical.Purchased from Chalco Shandong branch company.Specific surface area is
197m2/ g, pore volume is 0.62mL/g) be dried 16 hours at 120 DEG C, it is subsequently adding in Dewar bottle, is evacuated to 0.09MPa.
(a) heating in vacuum.By 180g forming oil column waste oil, (forming oil column waste oil μ g/g Han aluminium ion 756,40 DEG C of surfaces are opened
Power is 30.47mN/m.Forming oil column oil is SN500 base oil, and fresh described forming oil column 40 DEG C of surface tension of oil are
27.20mN/m) add stirring in there-necked flask.It is evacuated to 0.09MPa, and is warming up to 160 DEG C of heating 3 hours；
(b) adsorbent.With absorption in the forming oil column waste oil addition Dewar bottle that will obtain after step (a) heating in vacuum
Agent stirring contact.Contact pressure is 0.09MPa, and Contact Temperature is 40 DEG C, and time of contact is 20 minutes.Filter out adsorbent to obtain
Reclaimed oil S8.
The reclaimed oil S8 obtained is measured aluminium composition and the surface tension of 40 DEG C, and observes color.The results are shown in Table 1.
Embodiment 9
The present embodiment is for illustrating the forming oil column oil reclaiming method that the present invention provides.
According to the method for embodiment 3, forming oil column waste oil is regenerated, except for the difference that, with " being warming up in step (2)
120 DEG C " replacement " is warming up to 160 DEG C ".Obtain reclaimed oil S9.The aluminium composition of the reclaimed oil S9 that mensuration obtains and the table of 40 DEG C
Surface tension, and observe color.Result is as shown in table 1.
Test case
Reclaimed oil S1-S9 embodiment 1-9 obtained carries out forming oil column.The Step By Condition of forming oil column is: by height
The Alumina gel with Tyndall phenomenon that pure metallic aluminum (aluminum content is more than 99.6 weight %) is prepared as with hydrochloric acid, with six methines
The aqueous solution (Alumina gel and weight ratio 4:1 of hexamethylenetetramine, hexamethylenetetramine concentration of aqueous solution is 38 weight %) of tetramine
Mixing, by the deep fat post of water dropper instillation 90 DEG C, (oil column height is 1 meter to the mixture obtained, and in oil column, oil is respectively adopted regeneration
Oil S1-S9) in, respectively obtain catalyst granules.
The molding effect of gained catalyst granules is as shown in table 2.
Fig. 1-3 is followed successively by and uses fresh molding oil (fresh molding oil is SN500 base oil), forming oil column waste oil
(described forming oil column waste oil be fresh SN500 base oil is carried out repeatedly molding after the waste oil that obtains, wherein, aluminium ion contains
Amount is 756 μ g/g, and 40 DEG C of surface tension are 30.47mN/m, and color is bronzing) and reclaimed oil S3 carry out catalyst forming oil column
The photo of the spherical regularity outward appearance of the catalyst granules obtained.
Table 1
Table 2
| Numbering | Molding effect (90 DEG C) |
| Fresh SN500 base oil | Spheroid regularity is fine |
| Forming oil column waste oil | Spheroid regularity is very poor |
| S1 | Spheroid regularity is fine |
| S2 | Spheroid regularity is fine |
| S3 | Spheroid regularity is fine |
| S4 | Spheroid regularity is general |
| S5 | Spheroid regularity is general |
| S6 | Spheroid regularity is general |
| S7 | Spheroid regularity is general |
| S8 | Spheroid regularity is fine |
| S9 | Spheroid regularity is slightly worse |
From the data of table 1 and 2 it can be seen that the forming oil column oil reclaiming method that the present invention provides can subtract effectively
The aluminum ions content of metal in few forming oil column waste oil, remove simultaneously the water in forming oil column waste oil and gas (main ammonia and
Formaldehyde) etc..Give up oil surface tension and fresh molding oil phase of forming oil column after regeneration is worked as, and the color of reclaimed oil also by
Improve and work as with fresh molding oil phase.As it is shown on figure 3, what the forming oil column oil reclaiming method using the present invention to provide obtained
Reclaimed oil, carries out forming oil column, it is thus achieved that the spheroid regularity that had of catalyst, better have with using fresh molding oil
Suitable forming oil column effect.
Claims (7)
1. a forming oil column oil reclaiming method, it is characterised in that the method includes any one in following manner:
Mode one: forming oil column waste oil is contacted by (1) with adsorbent；(2) mixture obtained after step (1) being contacted is in vacuum
Heat under state, filter, obtain reclaimed oil；
Mode two: forming oil column waste oil is heated by (a) under vacuum conditions；B forming oil column that () obtains after step (a) being heated
Waste oil contacts with adsorbent, filters, obtains reclaimed oil；
Described adsorbent is at least one in silicon oxide, activated alumina, activated carbon and molecular sieve；
Described adsorbent is 1:10-30 with the weight ratio of described forming oil column waste oil；
The condition of described contact includes, in terms of gauge pressure, the pressure of described contact is 0.01-0.1MPa；The temperature of described contact is
20-40℃。
Renovation process the most according to claim 1, wherein, described adsorbent with the weight ratio of described forming oil column waste oil is
1:15-20.
Renovation process the most according to claim 1, wherein, described adsorbent is activated alumina and/or activated carbon.
Renovation process the most according to claim 1, wherein, in terms of gauge pressure, the pressure of described contact is 0.08-0.09MPa.
Renovation process the most according to claim 1, wherein, the condition heated under vacuum conditions includes, in terms of gauge pressure, institute
The pressure stating vacuum is 0.01-0.1MPa；The temperature of described heating is 130-180 DEG C.
Renovation process the most according to claim 5, wherein, the condition heated under vacuum conditions includes, in terms of gauge pressure, institute
The pressure stating vacuum is 0.08-0.09MPa；The temperature of described heating is 150-160 DEG C.
7. according to the renovation process described in any one in claim 1-6, wherein, form the molding of described forming oil column waste oil
At least one in oil, pumping fluid and edible oil based on oil.
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| CN101280241A (en) * | 2008-05-22 | 2008-10-08 | 南京工业大学 | Method for purifying waste lubricant oil |
| CN102191123A (en) * | 2011-04-14 | 2011-09-21 | 荆门市爱国润滑油有限公司 | Waste oil regeneration production process |
| CN102304413A (en) * | 2011-08-03 | 2012-01-04 | 江苏雕皇石化科技有限公司 | Method for refining and regenerating high-quality rufous waste lubricating oil |
| CN102952622A (en) * | 2012-03-25 | 2013-03-06 | 重庆三力净化设备有限公司 | pure physical cleaning method for recycling and regenerating waste oil |
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|---|---|---|---|---|
| CN101280241A (en) * | 2008-05-22 | 2008-10-08 | 南京工业大学 | Method for purifying waste lubricant oil |
| CN102191123A (en) * | 2011-04-14 | 2011-09-21 | 荆门市爱国润滑油有限公司 | Waste oil regeneration production process |
| CN102304413A (en) * | 2011-08-03 | 2012-01-04 | 江苏雕皇石化科技有限公司 | Method for refining and regenerating high-quality rufous waste lubricating oil |
| CN102952622A (en) * | 2012-03-25 | 2013-03-06 | 重庆三力净化设备有限公司 | pure physical cleaning method for recycling and regenerating waste oil |
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