CN109201025A - A kind of regeneration method of petroleum-type spent bleaching clay - Google Patents
A kind of regeneration method of petroleum-type spent bleaching clay Download PDFInfo
- Publication number
- CN109201025A CN109201025A CN201811425201.0A CN201811425201A CN109201025A CN 109201025 A CN109201025 A CN 109201025A CN 201811425201 A CN201811425201 A CN 201811425201A CN 109201025 A CN109201025 A CN 109201025A
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- CN
- China
- Prior art keywords
- bleaching clay
- spent bleaching
- carclazyte
- petroleum
- oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000004061 bleaching Methods 0.000 title claims abstract description 116
- 239000004927 clay Substances 0.000 title claims abstract description 113
- 238000011069 regeneration method Methods 0.000 title claims abstract description 57
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 claims abstract description 150
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims abstract description 77
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 239000002156 adsorbate Substances 0.000 claims abstract description 18
- 238000000638 solvent extraction Methods 0.000 claims abstract description 18
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 230000003213 activating effect Effects 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 93
- 239000002283 diesel fuel Substances 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000010687 lubricating oil Substances 0.000 claims description 14
- 238000011084 recovery Methods 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 39
- 230000008929 regeneration Effects 0.000 abstract description 33
- 239000000463 material Substances 0.000 abstract description 16
- 150000002148 esters Chemical class 0.000 abstract description 8
- 238000001179 sorption measurement Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000007670 refining Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 16
- 241000196324 Embryophyta Species 0.000 description 15
- 230000004913 activation Effects 0.000 description 15
- 238000003756 stirring Methods 0.000 description 15
- 238000001914 filtration Methods 0.000 description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 239000003208 petroleum Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000004064 recycling Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920000570 polyether Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- -1 sulphonic acid ester Chemical class 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- AQEFLFZSWDEAIP-UHFFFAOYSA-N di-tert-butyl ether Chemical compound CC(C)(C)OC(C)(C)C AQEFLFZSWDEAIP-UHFFFAOYSA-N 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
Classifications
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
Abstract
The present invention provides a kind of regeneration method of petroleum-type spent bleaching clay, specifically includes the following steps: step (1): based organic solvent and ether organic solvent are mixed to get double solvent extraction agent；Step (2): petroleum-type spent bleaching clay adsorbate is extracted using extractant made from step (1)；Step (3): it will be separated by the petroleum-type spent bleaching clay of extraction with extractant, obtain wet carclazyte and miscella；Step (4): wet carclazyte is vacuum dried, revolution obtains the atlapulgite that can be utilized again after activating.It is mixed in certain proportion using ester and ether as extractant, is regenerated after being extracted to petroleum-type spent bleaching clay, effect of extracting is good, and obtained the Regeneration Bleaching Clay adsorption capacity is strong, meets requirement standard of the industry to oil refining carclazyte, can utilize again；It recycles obtained carclazyte oil and is also used as pitch auxiliary material, without being handled or being discharged；Preferred sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are bulk raw material, are easy to get.
Description
Technical field
The present invention relates to a kind of regeneration methods of spent bleaching clay, and in particular to a kind of regeneration method of petroleum-type spent bleaching clay.
Background technique
During petroleum refining, generallys use atlapulgite and carry out adsorption bleaching, removal of impurities, active lean type is being adsorbed
While certain impurity, more oil product has also been adsorbed, with the increase of adsorbance, has been reformed into after bleaching earth adsorption saturation
The petroleum-type spent bleaching clay of oil-containing, becomes a kind of brown solid waste.Both the normal production work of oil plant had been affected, even more
Great pollution is caused to ecological environment.
Traditional treatment method is landfill or incineration method, but after spent bleaching clay is filled, organic impurities therein i.e. other have
Evil substance still can be to farmland, river, and underground water etc. causes serious pollution, and spent bleaching clay removes only therein after burning
Organic matter, and there is still a need for carry out landfill disposal for the spent bleaching clay after burning.There are also enterprises using thermokalite water washing point
Substance from spent bleaching clay absorption, but need to consume a large amount of water and the energy, and generating fluid carclazyte is in emulsifying, is difficult to carry out
Subsequent processing, process water cyclic utilization rate is not high, secondly, environment can be produced by discharging a large amount of greenhouse gases and toxic carclazyte tail water
Remote adverse effect is grown, and thermokalite water washing hair does not separate all spent bleaching clays and is applicable in.
The method in this year, organic solvent extraction regenerates petroleum-type spent bleaching clay, and organic solvent used is mainly 6
Number solvent finish, n-hexane, petroleum ether, methanol etc., extract unclean, and the rate of recovery of carclazyte oil is relatively low.
Summary of the invention
The purpose of the present invention is to provide a kind of regeneration methods of petroleum-type spent bleaching clay, are combined as extracting using ester ether
Agent carries out extraction regeneration to spent bleaching clay, and effect of extracting is good, and carclazyte oil recovery rate is high, and obtained the Regeneration Bleaching Clay adsorption capacity is strong.
Technical scheme is as follows:
A kind of regeneration method of petroleum-type spent bleaching clay, specifically includes the following steps:
Step (1): based organic solvent and ether organic solvent are mixed to get double solvent extraction agent；
Step (2): petroleum-type spent bleaching clay adsorbate is extracted using extractant made from step (1)；
Step (3): it will be separated by the petroleum-type spent bleaching clay of extraction with extractant, obtain wet carclazyte and miscella；
Step (4): wet carclazyte is vacuum dried, revolution obtains the atlapulgite that can be utilized again after activating.
The regeneration method for petroleum-type spent bleaching clay, wherein in step (1), the based organic solvent is vinegar
The secondary butyl ester of acid, the ether organic solvent are methyl tertiary butyl ether(MTBE).
The regeneration method for petroleum-type spent bleaching clay, wherein in step (1), the sec-Butyl Acetate and methyl
The volume ratio of tertbutyl ether is 1:4-4:1.
The regeneration method for petroleum-type spent bleaching clay, wherein in step (2), the petroleum-type spent bleaching clay is profit
The volume ratio of lubricating oil spent bleaching clay, step (1) sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) is 1:1-4:1.
The regeneration method for petroleum-type spent bleaching clay, wherein in step (2), the petroleum-type spent bleaching clay is bavin
The volume ratio of oily spent bleaching clay, step (1) sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) is 1:1-1:4.
The regeneration method for petroleum-type spent bleaching clay, wherein in step (2), the temperature for extracting extraction is 30-60
℃。
The regeneration method for petroleum-type spent bleaching clay, wherein in step (2), the dosage of the extractant is useless
1-4 times of carclazyte.
The regeneration method for petroleum-type spent bleaching clay, wherein in step (3), the miscella is steamed by decompression
It evaporates recycling and obtains extractant and carclazyte oil.
The regeneration method for petroleum-type spent bleaching clay, which is characterized in that in step (3), the miscella passes through
Following steps recycling extractant and carclazyte oil: A, distilling mixed liquor under conditions of 60-80 DEG C, collects the first fraction and obtains first
Base tertbutyl ether；B, after methyl tertiary butyl ether(MTBE) has steamed, the temperature of mixed liquor is improved, makes it in 110-120 DEG C of temperature range
Continue to distill, collects the second fraction and obtain sec-Butyl Acetate；C, after band sec-Butyl Acetate has steamed, stop heating, it is after cooling remaining
Liquid is carclazyte oil.
Beneficial effects of the present invention:
It is mixed in certain proportion using ester and ether as extractant, is regenerated after being extracted to petroleum-type spent bleaching clay, extraction effect
Fruit is good, and obtained the Regeneration Bleaching Clay adsorption capacity is strong, meets requirement standard of the industry to oil refining carclazyte, can utilize again；It returns
It receives obtained carclazyte oil and is also used as pitch auxiliary material, without being handled or being discharged；Preferred sec-Butyl Acetate and methyl- tert
Butyl ether is bulk raw material, is easy to get；The boiling point of ester and ether used and the boiling point difference of carclazyte oil are larger, after extraction, lead to
It crosses distillation and is easy to recycling design.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Embodiments of the present invention are described below in detail, the example of the embodiment is shown in the accompanying drawings, wherein from beginning
Same or similar element or element with the same or similar functions are indicated to same or similar label eventually.Below by ginseng
The embodiment for examining attached drawing description is exemplary, and for explaining only the invention, and is not considered as limiting the invention.
Embodiment 1
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 1:4
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during refined diesel oil is weighed, addition configures
Extractant 500ml, at 30 DEG C, stirring after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 153g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 46.3g, can be with
As pitch auxiliary material, the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate recycled can be re-used for configuration mixed extractant.This
5 groups of experiments are arranged in parallel in embodiment, and the above results are the average value (similarly hereinafter) of 3 groups of experimental results.
Embodiment 2
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 1:4
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during bright stock is weighed, configuration is added
Good extractant 500ml, at 30 DEG C, stirring is after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 157g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 41.7g, can be with
As pitch auxiliary material, the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate recycled can be re-used for configuration mixed extractant.
Embodiment 3
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 1:3
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during refined diesel oil is weighed, addition configures
Extractant 500ml, at 40 DEG C, stirring after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 147g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 51.42g, can
Configuration mixed extractant can be re-used for using the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate that as pitch auxiliary material, recycle.
Embodiment 4
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 1:3
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during bright stock is weighed, configuration is added
Good extractant 500ml, at 40 DEG C, stirring is after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 157g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 41.78g, can
Configuration mixed extractant can be re-used for using the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate that as pitch auxiliary material, recycle.
Embodiment 5
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 1:2
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during refined diesel oil is weighed, addition configures
Extractant 500ml, at 50 DEG C, stirring after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 148g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 52.3g, can be with
As pitch auxiliary material, the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate recycled can be re-used for configuration mixed extractant.
Embodiment 6
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 1:2
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during bright stock is weighed, configuration is added
Good extractant 500ml, at 50 DEG C, stirring is after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 157g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 41.8g, can be with
As pitch auxiliary material, the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate recycled can be re-used for configuration mixed extractant.
Embodiment 7
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 1:1
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during refined diesel oil is weighed, addition configures
Extractant 500ml, at 60 DEG C, stirring after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 150g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 48.54g, can
Configuration mixed extractant can be re-used for using the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate that as pitch auxiliary material, recycle.
Embodiment 8
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 1:1
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during bright stock is weighed, configuration is added
Good extractant 500ml, at 60 DEG C, stirring is after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 148g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 51.3g, can be with
As pitch auxiliary material, the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate recycled can be re-used for configuration mixed extractant.
Embodiment 9
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 2:1
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during refined diesel oil is weighed, addition configures
Extractant 500ml, at 60 DEG C, stirring after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 158g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 40.5g, can be with
As pitch auxiliary material, the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate recycled can be re-used for configuration mixed extractant.
Embodiment 10
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 2:1
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during bright stock is weighed, configuration is added
Good extractant 500ml, at 60 DEG C, stirring is after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 145g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 53.52g, can
Configuration mixed extractant can be re-used for using the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate that as pitch auxiliary material, recycle.
Embodiment 11
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 3:1
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during refined diesel oil is weighed, addition configures
Extractant 500ml, at 50 DEG C, stirring after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 159g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 39.84g, can
Configuration hybrid extraction can be re-used for using the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate that obtain as pitch auxiliary material, extraction recycling
Agent.
Embodiment 12
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 3:1
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during bright stock is weighed, configuration is added
Good extractant 500ml, at 50 DEG C, stirring is after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 147g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 51.72g, can
Configuration mixed extractant can be re-used for using the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate that as pitch auxiliary material, recycle.
Embodiment 13
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 4:1
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during refined diesel oil is weighed, addition configures
Extractant 500ml, at 40 DEG C, stirring after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 159g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 40.12g, can
Configuration mixed extractant can be re-used for using the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate that as pitch auxiliary material, recycle.
Embodiment 14
The process flow chart of the present embodiment is as shown in Figure 1, sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) are mixed with the ratio of 4:1
After even, double solvent extraction agent is obtained；Spent bleaching clay of 200g oil plant during bright stock is weighed, configuration is added
Good extractant 500ml, at 40 DEG C, stirring is after twenty minutes；Wet spent bleaching clay and miscella is obtained by filtration；Wet carclazyte is dry through vacuum
Regeneration activity carclazyte 151g is obtained after dry, revolution activation, the miscella recycles extractant and carclazyte oil by following steps: A,
Mixed liquor is distilled under conditions of 60-80 DEG C, the first fraction is collected and obtains methyl tertiary butyl ether(MTBE)；B, it is steamed to methyl tertiary butyl ether(MTBE)
After complete, the temperature of mixed liquor is improved, it is made to continue to distill in 110-120 DEG C of temperature range, the second fraction is collected and obtains acetic acid
Secondary butyl ester；C, after band sec-Butyl Acetate has steamed, stop heating, extraction raffinate after cooling is a kind of oil of brown, and main component is
Adsorbate of carclazyte during turpentole, we term it carclazyte oil.Weighed, obtained carclazyte oil is 47.46g, can
Configuration mixed extractant can be re-used for using the methyl tertiary butyl ether(MTBE) and sec-Butyl Acetate that as pitch auxiliary material, recycle.
The performance detection and data of regeneration activity carclazyte are analyzed:
The resulting regeneration activity carclazyte of the various embodiments described above is collected, detects regeneration activity carclazyte referring to HG/T 2569-94
Performance, and count the rate of recovery of carclazyte oil in the various embodiments described above, the results are shown in Table 1.
Each embodiment table of comparisons of table 1
| Group | Spent bleaching clay type | Ester/ether (V/V) | Carclazyte oil recovery rate (%) | The activity degree of regeneration activity carclazyte | The percent of decolourization of regeneration activity carclazyte | The free acid of regeneration activity carclazyte |
| Embodiment 1 | Diesel oil spent bleaching clay | 1:4 | 23.15 | 224 | 88% | 0.13% |
| Embodiment 2 | Lubricating oil spent bleaching clay | 1:4 | 20.85 | 209 | 83% | 0.16% |
| Embodiment 3 | Diesel oil spent bleaching clay | 1:3 | 25.71 | 226 | 91% | 0.11% |
| Embodiment 4 | Lubricating oil spent bleaching clay | 1:3 | 20.89 | 217 | 85% | 0.16% |
| Embodiment 5 | Diesel oil spent bleaching clay | 1:2 | 26.8 | 234 | 94% | 0.10% |
| Embodiment 6 | Lubricating oil spent bleaching clay | 1:2 | 20.9 | 212 | 90% | 0.17% |
| Embodiment 7 | Diesel oil spent bleaching clay | 1:1 | 24.27 | 228 | 91% | 0.10% |
| Embodiment 8 | Lubricating oil spent bleaching clay | 1:1 | 25.65 | 228 | 93% | 0.10% |
| Embodiment 9 | Diesel oil spent bleaching clay | 2:1 | 20.25 | 203 | 89% | 0.18% |
| Embodiment 10 | Lubricating oil spent bleaching clay | 2:1 | 26.76 | 235 | 93% | 0.10% |
| Embodiment 11 | Diesel oil spent bleaching clay | 3:1 | 19.92 | 208 | 86% | 0.20% |
| Embodiment 12 | Lubricating oil spent bleaching clay | 3:1 | 25.86 | 230 | 90% | 0.11% |
| Embodiment 13 | Diesel oil spent bleaching clay | 4:1 | 20.06 | 211 | 85% | 0.15% |
| Embodiment 14 | Lubricating oil spent bleaching clay | 4:1 | 23.73 | 224 | 88% | 0.13% |
As seen from the above table, it is extracted with the different types of petroleum of comparison with spent bleaching clay using different ester ether, resulting carclazyte
The rate of recovery of oil is different, i.e., different to the extraction completeness of spent bleaching clay adsorbate.Ether polyester is rare to be conducive to diesel oil spent bleaching clay
Extraction regeneration, ether lack that ester is more, and the extraction for being conducive to lubricating oil spent bleaching clay regenerates.Wherein, when spent bleaching clay is that diesel oil is white with giving up
When native, it is best that sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) with the ratio of 1:2 are mixed to prepare extractant effect；When spent bleaching clay is lubrication
When oil uses spent bleaching clay, it is best that sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) with the ratio of 2:1 are mixed to prepare extractant effect.This may
Be because are as follows: diesel oil is with the substances such as a large amount of colloid, alkane, polycyclic aromatic hydrocarbon, polyethers have been adsorbed in spent bleaching clay, there are also sub-fractions
Asphalitine, polyesters, sulphonic acid ester etc., and methyl tertiary butyl ether(MTBE) to asphalitine, alkane, polycyclic aromatic hydrocarbon and polyethers have it is extraordinary
Dissolubility, therefore, effect is best when the ratio of sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) is 1:2；And lubricating oil is inhaled with spent bleaching clay
Attached a large amount of asphalitine, polyester, sulphonic acid ester and small part colloid, alkane, polyethers etc., and sec-Butyl Acetate is to asphalitine, poly-
The dissolubility of the components such as ester, sulphonic acid ester is good, and therefore, effect is best when the ratio of the secondary butyl ester of acid and methyl tertiary butyl ether(MTBE) is 2:1.
In addition, the embodiment that carclazyte oil recovery rate is high, obtains the Regeneration Bleaching Clay activity degree, percent of decolourization and content of fatty acid etc.
Aspect performs better than, and it is more preferable to the effect of the abstraction impurity removal of petroleum-type spent bleaching clay also to further illustrate these embodiments.
Comparative example:
In order to further verify technical effect of the invention, organic solvent common in the art compounding preparation is utilized separately below
Extractant, and the operation such as extracted by identical method, filter, dry, distilling, turning round regeneration, as a comparison case.Its
In, as shown in table 2, the performance of obtained carclazyte oil recovery rate and regeneration activity carclazyte is such as the component and proportion of the solvent of comparative example
Shown in table 3.
The component and proportion of solvent in each comparative example of table 2
| Group | Spent bleaching clay type | Solvent A | Solvent B | Solvent A/solvent B (v/v) |
| Comparative example 1 | Diesel oil spent bleaching clay | Methanol | Petroleum ether | 2:1 |
| Comparative example 2 | Lubricating oil spent bleaching clay | Methanol | Petroleum ether | 2:1 |
| Comparative example 3 | Diesel oil spent bleaching clay | Ethyl alcohol | No. 6 solvent naphthas | 1:2 |
| Comparative example 4 | Lubricating oil spent bleaching clay | Ethyl alcohol | No. 6 solvent naphthas | 1:2 |
| Comparative example 5 | Diesel oil spent bleaching clay | N-hexane | Petroleum ether | 1:1 |
| Comparative example 6 | Lubricating oil spent bleaching clay | N-hexane | Petroleum ether | 1:1 |
The carclazyte oil recovery rate of each comparative example of table 3 and the performance of gained regeneration activity carclazyte
| Group | Carclazyte oil recovery rate (%) | The activity degree of regeneration activity carclazyte | The percent of decolourization of regeneration activity carclazyte | The free acid of regeneration activity carclazyte |
| Comparative example 1 | 17.23 | 189 | 72% | 0.41 |
| Comparative example 2 | 12.2 | 154 | 60% | 0.68 |
| Comparative example 3 | 13.82 | 159 | 60% | 0.60 |
| Comparative example 4 | 17.57 | 190 | 74% | 0.42 |
| Comparative example 5 | 15.36 | 167 | 67% | 0.52 |
| Comparative example 6 | 16.84 | 173 | 69% | 0.43 |
By table 2 and 3 it is found that compared with prior art, being mixed using sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) according to suitable ratio
Cooperation is extractant, and effect of extracting is good, and obtained the Regeneration Bleaching Clay adsorption capacity is strong；And raw materials used sec-Butyl Acetate and methyl- tert
Butyl ether is bulk raw material, is easy to get.And it can be easy to separate extractant with carclazyte oil by distillation.
It is understood that the dosage about extractant, theoretically speaking be it is The more the better, it is contemplated that recycling design
When energy consumption, the dosage of extractant is limited to 1-4 times of carclazyte amount by the present invention.It is white after extraction and drying in the present invention
Soil can be activated using Conventional activation methods in the prior art.It, can be using in laboratory during being extracted
Common method stirring or concussion, can also be using existing industrialized extracting machine or extracter etc..The present invention is carried out above
Detailed introduction, for those of ordinary skills, it can be modified or changed according to the above description, and it is all this
A little modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (9)
1. a kind of regeneration method for petroleum-type spent bleaching clay, which is characterized in that specifically includes the following steps:
Step (1): based organic solvent and ether organic solvent are mixed to get double solvent extraction agent；
Step (2): petroleum-type spent bleaching clay adsorbate is extracted using extractant made from step (1)；
Step (3): it will be separated by the petroleum-type spent bleaching clay of extraction with extractant, obtain wet carclazyte and miscella；
Step (4): wet carclazyte is vacuum dried, revolution obtains the atlapulgite that can be utilized again after activating.
2. the regeneration method according to claim 1 for petroleum-type spent bleaching clay, which is characterized in that described in step (1)
Based organic solvent is sec-Butyl Acetate, and the ether organic solvent is methyl tertiary butyl ether(MTBE).
3. the regeneration method according to claim 2 for petroleum-type spent bleaching clay, which is characterized in that described in step (1)
The volume ratio of sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) is 1:4-4:1.
4. the regeneration method according to claim 3 for petroleum-type spent bleaching clay, which is characterized in that described in step (2)
Petroleum-type spent bleaching clay is lubricating oil spent bleaching clay, and the volume ratio of step (1) sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) is 1:
1-4:1。
5. the regeneration method according to claim 3 for petroleum-type spent bleaching clay, which is characterized in that described in step (2)
Petroleum-type spent bleaching clay is diesel oil spent bleaching clay, and the volume ratio of step (1) sec-Butyl Acetate and methyl tertiary butyl ether(MTBE) is 1:1-
1:4。
6. the regeneration method according to claim 1 for petroleum-type spent bleaching clay, which is characterized in that in step (2), extracting
The temperature of extraction is 30-60 DEG C.
7. the regeneration method according to claim 1 for petroleum-type spent bleaching clay, which is characterized in that described in step (2)
The dosage of extractant is 1-4 times of spent bleaching clay.
8. the regeneration method according to claim 1 for petroleum-type spent bleaching clay, which is characterized in that described in step (3)
Miscella obtains extractant and carclazyte oil by distillation recovery.
9. the regeneration method according to claim 8 for petroleum-type spent bleaching clay, which is characterized in that described in step (3)
Miscella recycles extractant and carclazyte oil by following steps: A, distilling mixed liquor under conditions of 60-80 DEG C, collects first
Fraction obtains methyl tertiary butyl ether(MTBE)；B, after methyl tertiary butyl ether(MTBE) has steamed, the temperature of mixed liquor is improved, makes it at 110-120 DEG C
Continue to distill in temperature range, collects the second fraction and obtain sec-Butyl Acetate；C, after band sec-Butyl Acetate has steamed, stop heating,
Extraction raffinate after cooling is carclazyte oil.
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