CN104479730A - Compound metal oxide decoloring agent for waste mineral oil and decoloring method thereof - Google Patents

Compound metal oxide decoloring agent for waste mineral oil and decoloring method thereof Download PDF

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Publication number
CN104479730A
CN104479730A CN201410688294.1A CN201410688294A CN104479730A CN 104479730 A CN104479730 A CN 104479730A CN 201410688294 A CN201410688294 A CN 201410688294A CN 104479730 A CN104479730 A CN 104479730A
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oil
waste
mineral oil
decoloring
waste mineral
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CN201410688294.1A
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Chinese (zh)
Inventor
陆永生
张在屋
杨兴兴
钱光人
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Priority to CN201410688294.1A priority Critical patent/CN104479730A/en
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    • 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
    • C10G29/00—Refining of hydrocarbon oils, in the absence of hydrogen, with other chemicals
    • C10G29/16—Metal oxides
    • 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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • 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
    • C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
    • C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
    • C10G53/10—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one acid-treatment step
    • 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
    • C10M175/0008—Working-up used lubricants to recover useful products ; Cleaning with the use of adsorbentia
    • 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
    • C10M175/02—Working-up used lubricants to recover useful products ; Cleaning mineral-oil based

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention relates to a compound metal oxide decoloring agent for waste mineral oil and a decoloring method thereof. The decoloring agent belongs to the scope of solid alkalis and solid adsorbents and is a metal compound oxide which is obtained by calcining hydrotalcite as a precursor at high temperature. The compound metal oxide is applied to the waste mineral oil decoloring process by the following steps: filtering the waste mineral oil to remove solid impurities by virtue of a conventional method; adding 5-15% by mass of acid; fully stirring at 40-80 DEG C and filtering; and then, adding 3-15% of the compound metal oxide decoloring agent to decolor, wherein the chroma of the treated oil product can be reduced to below color number 0.9 of GB/T6540-1986. Quality indexes of the treated waste oil reach the standard request of basic oil. The compound metal oxide applied to the waste mineral oil decoloring process has the advantages that the decoloring agent not only can provide alkalinity, but also has an adsorption effect, so that the conventional waste oil decoloring process is simplified; the decoloring agent is low in oil absorption and high in repeating utilization factor, meets the request of sustainable development and has a good characteristic of environmental friendliness.

Description

A kind of complex metal oxides discoloring agent for waste mineral oil and decoloring method thereof
Technical field
The present invention relates to a kind of complex metal oxides discoloring agent for waste mineral oil, particularly discoloring agent is to waste mineral oil decolouring regeneration, belongs to discoloring agent field and energy regeneration field.
Background technology
Waste mineral oil; especially the waste lubrication oil reclaimed from industrial park, hydraulic efficiency oil or used oil mixing waste oil; due to waste oil complicated component, recycling difficulty is large and environmental hazard serious, obtains very large concern from the sustainable use energy and environment protection aspect to waste oil regeneration utilization.It is carclazyte that traditional process waste lubrication oil commonly uses sorbent material.Usually the atlapulgite using oil to weigh 5% ~ 15 % in decolorization carries out adsorption bleaching, if the spent bleaching clay process after decolouring not in time, can cause secondary pollution.Because carclazyte has stronger oil absorption, be up to 30%.Relative to traditional bleaching earth adsorption agent, it is high that the composite oxide of metal that the present invention relates to has repeating utilization factor, and oil absorbency is low, the high and eco-friendly feature of economic worth.
At present, most method conventional to waste oil decolouring divides two large classes: one is that soda acid is washed and added sorbent material and decolour, and another kind is organic solvent extraction.Comparatively inorganic process efficiency is high in organic solvent aftertreatment, effective, but it is unclean to there is removal of solvents in oil product, to shortcomings such as environmental hazard are large.Now more research all focuses on inorganic treatment process.And atlapulgite selected by conventional sorbent material, this has larger specific surface area and stronger adsorptive power due to carclazyte, rarely has report for composite oxide of metal decolouring.
" refining of petroleum and chemical industry " November the 31st in 2000, volume o. 11th Wang Yan attained, Li Ruili " the clay-filtered discussion to lube base oil decolorization and denitrogenation " points out that the adsorptive power of carclazyte to different substances is different, be followed successively by: colloid, bituminous matter > aromatic hydrocarbons > naphthenic hydrocarbon > alkane, and the number of rings of aromatic hydrocarbons and naphthenic hydrocarbon is more, more easily adsorbed.In patent CN102504933A, waste oil regeneration is by the step of pre-treatment, short-path distillation and hydrogenation hydrogen manufacturing, obtains good decolorizing effect, but cost is corresponding higher.Patent CN1962837A lubricant oil regeneration is by making it reach standards for recycling adding of additive in ordinary method.Use molecular distillation in patent CN102161930A, after deodorization, add carclazyte decolouring again.Patent CN102295979A had first carried out the high temperature dehydration process of more than 120 DEG C before pickling, alkali cleaning add sorbent material.
In sum, mostly adopt clay-filtered at present to the desolventing technology of waste mineral oil, though obtain good decolorizing effect, carclazyte itself has larger adsorptive power to oils, thus causes secondary pollution, limits its use range.So now propose a kind of complex metal oxides discoloring agent for waste mineral oil and decoloring method thereof, decoloration process is simply effective, can replace traditional activated carclazyte.
Summary of the invention
The object of this invention is to provide a kind of complex metal oxides discoloring agent for waste mineral oil and decoloring method thereof, decoloration process operating process can be simplified, effectively replace conventional lightening agents, cost-saving and environmental protection sustainable use.
A kind of complex metal oxides discoloring agent for waste mineral oil, it is characterized in that there is following chemical composition and formula: for the complex metal oxides discoloring agent of waste mineral oil, be mol ratio and the magnesium salts of two kinds of raw materials: aluminium salt=2:1, described magnesium salts is MgCl 27H 2o or Mg(NO 3) 26H 2o, described aluminium salt is AlCl 36H 2o; Or the mol ratio of its two kinds of raw materials and calcium salt: aluminium salt=2:1, described calcium salt is CaCl 2or Ca(NO 3) 24H 2o, described aluminium salt is AlCl 36H 2o or Al(NO 3) 39H 2o.
A kind of preparation method of the complex metal oxides discoloring agent for waste mineral oil, it is characterized in that there is following process and step: by divalence calcium salt or magnesium salts and the trivalent aluminium salt solution mol ratio wiring solution-forming according to 2 ~ 4:1, slowly add the sodium hydroxide solution with 0.1 ~ 0.5mol, still aging 5 ~ 8h after stirring at normal temperature 2 ~ 5h, then obtains solid chemical compound by dry at solution filtration washing and 105 DEG C.Solid chemical compound is calcined 1 ~ 5h at 500 ~ 800 DEG C, and namely grinding fragmentation obtains complex metal oxides discoloring agent.For a using method for the complex metal oxides discoloring agent of waste mineral oil, its treating processes is as follows: by waste oil solids removed by filtration foreign material, and the acid adding 5% ~ 15% of waste oil quality fully stirs rear filtration at 40 ~ 80 DEG C; Then add 3% ~ 15% complex metal oxides discoloring agent of supernatant oil quality after filtering to decolour, decolouring 10 ~ 50min waste oil colourity can be down in GB/T6540-1986 look number less than 0.9.
The composite oxide of metal that the present invention relates to is applied to waste mineral oil decoloration process, have and simplify traditional waste oil decoloration process, and oil absorbency is low, repeating utilization factor is high, meets Sustainable development requirement, has good environmentally friendly characteristic.
Embodiment
The composite oxide of metal preparation method that the present invention relates to, the effect being applied to waste mineral oil decoloration process, given by the following examples and further illustrating.
Embodiment 1
Take 50 mmol(11.95g respectively) MgCl 27H 2o and 25 mmol(6.04g) AlCl 36H 2o, is dissolved in 50mL without CO 2mixing salt solution is formulated as in water, taking 160 mmol(6.4g simultaneously) NaOH is dissolved in 100mL tap water and is mixed with mixed ammonium/alkali solutions, under magnetic agitation effect, slowly mixing salt solution is added in NaOH solution, rate of addition is 15mL per minute, sealing normal temperature magnetic agitation 6 hours, leave standstill and generate white precipitate after 4 hours, by mixed solution and precipitation suction filtration after taking-up, with distilled water repetitive scrubbing 2 ~ 3 times, solid sample is dried and is obtained magnesium aluminum-hydrotalcite under 105 DEG C of conditions, is calcined by hydrotalcite and obtain composite oxide of metal in 3 hours at 700 DEG C.It is for subsequent use after grinding is broken.
Waste oil decolours: by 40.00g waste mineral oil conventional filtration, the oarse-grained impurity that elimination may contain; The vitriol oil adding waste oil quality 5% reacts 30min at 60 DEG C, cooling, and elimination lower floor acid sludge obtains top edible vegetable oil; Add 5% through calcining after composite oxide of metal, take out react 20min at constant temperature 60 DEG C after, namely elimination catalyzer obtains transparent shinny waste mineral oil, and measuring waste oil colourity after decolouring through chromascope is look number 0.9 in GB/T6540-1986, can reuse 8 times after catalyst activation.
Embodiment 2
Take 50 mmol(12.80g respectively) Mg (NO 3) 26H 2o and 25 mmol(9.38g) Al (NO 3) 39H 2o, is dissolved in 50mL without CO 2mixing salt solution is formulated as in water, taking 160 mmol(6.4g simultaneously) NaOH is dissolved in 100mL tap water and is mixed with mixed ammonium/alkali solutions, under magnetic agitation effect, slowly mixing salt solution is added in NaOH solution, rate of addition is 15mL per minute, sealing normal temperature magnetic agitation 6 hours, leave standstill and generate white precipitate after 4 hours, by mixed solution and precipitation suction filtration after taking-up, with distilled water repetitive scrubbing 2 ~ 3 times, solid sample is dried and is obtained magnesium aluminum-hydrotalcite under 105 DEG C of conditions, is calcined by hydrotalcite and obtain composite oxide of metal in 3 hours at 700 DEG C.It is for subsequent use after grinding is broken.
Waste oil decolours: by 40.00g waste mineral oil conventional filtration, the oarse-grained impurity that elimination may contain; The vitriol oil adding waste oil quality 5% reacts 30min at 60 DEG C, and cooling elimination lower floor acid sludge obtains top edible vegetable oil; Add 5% through calcining after composite oxide of metal, take out react 20min at constant temperature 60 DEG C after, namely elimination catalyzer obtains transparent shinny waste mineral oil, and measuring waste oil colourity after decolouring through chromascope is look number 0.8 in GB/T6540-1986, can reuse 8 times after catalyst activation.
Embodiment 3
Take 50 mmol(5.55g respectively) CaCl 2with 25 mmol(6.04g) AlCl 36H 2o, is dissolved in 50mL without CO 2mixing salt solution is formulated as in water, taking 160 mmol(6.4g simultaneously) NaOH is dissolved in 100mL tap water and is mixed with mixed ammonium/alkali solutions, under magnetic agitation effect, slowly mixing salt solution is added in NaOH solution, rate of addition is 15mL per minute, sealing normal temperature magnetic agitation 6 hours, leave standstill and generate white precipitate after 4 hours, by mixed solution and precipitation suction filtration after taking-up, with distilled water repetitive scrubbing 2 ~ 3 times, solid sample is dried and is obtained magnesium aluminum-hydrotalcite under 105 DEG C of conditions, is calcined by hydrotalcite and obtain composite oxide of metal in 3 hours at 700 DEG C.It is for subsequent use after grinding is broken.
Waste oil decolours: by 40.00g waste mineral oil conventional filtration, the oarse-grained impurity that elimination may contain; The vitriol oil adding waste oil quality 5% reacts 30min at 60 DEG C, and cooling elimination lower floor acid sludge obtains top edible vegetable oil; Add 5% through calcining after composite oxide of metal, take out react 20min at constant temperature 60 DEG C after, namely elimination catalyzer obtains transparent shinny waste mineral oil, and measuring waste oil colourity after decolouring through chromascope is look number 0.8 in GB/T6540-1986, can reuse 6 times after catalyst activation.
Embodiment 4
Take 50 mmol(11.80g respectively) Ca (NO 3) 24H 2o and 25 mmol(9.38g) Al (NO 3) 39H 2o, is dissolved in 50mL without CO 2mixing salt solution is formulated as in water, taking 160 mmol(6.4g simultaneously) NaOH is dissolved in 100mL tap water and is mixed with mixed ammonium/alkali solutions, under magnetic agitation effect, slowly mixing salt solution is added in NaOH solution, rate of addition is 15mL per minute, sealing normal temperature magnetic agitation 6 hours, leave standstill and generate white precipitate after 4 hours, by mixed solution and precipitation suction filtration after taking-up, with distilled water repetitive scrubbing 2 ~ 3 times, solid sample is dried and is obtained magnesium aluminum-hydrotalcite under 105 DEG C of conditions, is calcined by hydrotalcite and obtain composite oxide of metal in 3 hours at 700 DEG C.It is for subsequent use after grinding is broken.
Waste oil decolours: by 40.00g waste mineral oil conventional filtration, the oarse-grained impurity that elimination may contain; The vitriol oil adding waste oil quality 5% reacts 30min at 60 DEG C, and cooling elimination lower floor acid sludge obtains top edible vegetable oil; Add 5% through calcining after composite oxide of metal, take out react 20min at constant temperature 60 DEG C after, namely elimination catalyzer obtains transparent shinny waste mineral oil, and measuring waste oil colourity after decolouring through chromascope is look number 0.9 in GB/T6540-1986, can reuse 6 times after catalyst activation.

Claims (3)

1., for a complex metal oxides discoloring agent for waste mineral oil, it is characterized in that there is following chemical composition and formula:
Magnesium salts: aluminium salt=2:1(mol ratio), described magnesium salts is MgCl 27H 2o or Mg(NO 3) 26H 2o, described aluminium salt is AlCl 36H 2o; Or, calcium salt: aluminium salt=2:1(mol ratio), described calcium salt is CaCl 2or Ca(NO 3) 24H 2o, described aluminium salt is AlCl 36H 2o or Al(NO 3) 39H 2o.
2. the preparation method for the complex metal oxides discoloring agent of waste mineral oil, it is characterized in that there is following process and step: by divalence calcium salt or magnesium salts and the trivalent aluminium salt solution mol ratio wiring solution-forming according to 2 ~ 4:1, slowly add the sodium hydroxide solution with 0.1 ~ 0.5mol, still aging 5 ~ 8h after stirring at normal temperature 2 ~ 5h, then obtains solid chemical compound by dry at 105 DEG C for solution filtration washing; Solid chemical compound is calcined 1 ~ 5h at 500 ~ 800 DEG C, and namely grinding fragmentation obtains complex metal oxides discoloring agent.
3., for a using method for the complex metal oxides discoloring agent of waste mineral oil, by waste oil solids removed by filtration foreign material, the acid adding 5% ~ 15% of waste oil quality fully stirs rear filtration at 40 ~ 80 DEG C; Then add 3% ~ 15% complex metal oxides discoloring agent of supernatant oil quality after filtering to decolour, decolouring 10 ~ 50min waste oil colourity can be down in GB/T6540-1986 look number less than 0.9.
CN201410688294.1A 2014-11-26 2014-11-26 Compound metal oxide decoloring agent for waste mineral oil and decoloring method thereof Pending CN104479730A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105132012A (en) * 2015-07-09 2015-12-09 上海大学 Iron-containing hydrotalcite-like catalytic decolorant, and method for applying decolorant in waste mineral oil decoloring
CN108913325A (en) * 2018-06-01 2018-11-30 上海大学 The method of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil
CN110373257A (en) * 2019-08-08 2019-10-25 山东彼岸化工产品有限公司 A method of tail seal grease of shield is produced with used oil
CN115873008A (en) * 2023-03-01 2023-03-31 中化学科学技术研究有限公司 Method for purifying isosorbide and purified isosorbide

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102295979A (en) * 2011-07-25 2011-12-28 陕西理工学院 Regenerating process of waste lubricating oil
CN102827681A (en) * 2012-08-01 2012-12-19 上海宝钢废旧油处理有限公司 Waste hydraulic oil regeneration technology

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102295979A (en) * 2011-07-25 2011-12-28 陕西理工学院 Regenerating process of waste lubricating oil
CN102827681A (en) * 2012-08-01 2012-12-19 上海宝钢废旧油处理有限公司 Waste hydraulic oil regeneration technology

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曹琳等: "钙铝类水滑石衍生复合氧化物的SO2储存性能研究", 《环境科学》 *
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105132012A (en) * 2015-07-09 2015-12-09 上海大学 Iron-containing hydrotalcite-like catalytic decolorant, and method for applying decolorant in waste mineral oil decoloring
CN108913325A (en) * 2018-06-01 2018-11-30 上海大学 The method of solvent extraction combination composite metal oxide adsorbent regeneration waste lubricating oil
CN110373257A (en) * 2019-08-08 2019-10-25 山东彼岸化工产品有限公司 A method of tail seal grease of shield is produced with used oil
CN115873008A (en) * 2023-03-01 2023-03-31 中化学科学技术研究有限公司 Method for purifying isosorbide and purified isosorbide

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Application publication date: 20150401