CN102660373A - Waste oil regeneration method by phosphor salt flocculation, CO2 stirring and clay refining - Google Patents

Abstract

A waste oil regeneration method by phosphor salt flocculation, CO2 stirring and clay refining relates to waste lubricating oil processing, comprises steps of pretreatment for water and debris separation, first alkali washing, first thermal dehydration, contacted refining, press filtration, secondary alkali washing and secondary thermal dehydration. The step of pretreatment for water and debris separation is characterized in that a Na3Po4 solution (weight concentration being 5%) which accounts for 5 wt% of waste oil is added while oiling, and settlement lasts for 4 hours after stopping heating and agitating; the step of first alkali washing is characterized in that alkali lye is a Na3Po4 solution (concentration being 5%) which accounts for 5 wt% of waste oil; the step of contacted refining is characterized in that heating and agitating are carried out until there is no bubble, and then the solution is heated to 150 DEG C; the step of press filtration is characterized in that the solution is cooled to 120 DEG C before press filtration and then oil is pumped; and the step of secondary alkali washing is characterized in that alkali lye is a Na3Po4 solution (concentration being 5%) which accounts for 2 wt% of waste oil, wherein the gas for agitating at each step is CO2 gas. The invention has the following advantages: during the pretreatment process, Na3Po4 is adopted for oil-water and oil-residue separation, flocculating efficiency is good, effective ingredients of various additives are preserved; and CO2 effectively prevents oxidation of oil and has a good flocculation effect.

Description

A kind of microcosmic salt flocculation CO 2Clay-treated waste oil regeneration method is mixed in gas mixing

Technical field

The present invention relates to waste lubricating oil and handle, particularly a kind of microcosmic salt flocculation CO ₂Clay-treated waste oil regeneration method is mixed in gas mixing.

Background technology

The nitrogenous fertilizer enterprises compressor produces a large amount of high viscosity waste lubricating oils every day, and enterprise generally has the oil treatment station and handles waste lubricating oil, is used further to the lubricated of equipment board after the waste oil regeneration.

Technology of waste oil regenerating generally is divided three classes:

The first kind is for purify again.Comprise sedimentation, centrifugal, filter, flocculation.One or several coupling, simple and easy regeneration, main purpose is the water of sloughing in the waste oil, generally outstanding turbid mechanical impurity and with the mechanical impurity of colloidal state stable dispersion.

Second type for re-refining.Be on the basis that purifies again, to increase chemical refining or refining with adsorbents etc.Just after the waste lubricating oil dehydration is assorted, carries out chemical treatment or physical chemistry and handle, remove the oxidation products or the external contaminant that are dissolved in the waste oil.As: in dehydration after the assorted or flocculation, clay-filtered again or sulfuric acid-clay-filtered, or chemical demetalization, chemical demulsification etc.

The 3rd type for re-refining.The reclaiming process flow process that comprises distillation, as: distillation-carclazyte; Distillation-acid-carclazyte; Distillation-hydrogenation etc.Production meets the regeneration base oil of natural oil base oil specification of quality, modulates various basic, normal, high shelves oil products, and the oil product of producing in quality and the natural oil is close.

And various waste oil have carried out the classification recovery for nitrogenous fertilizer, and the overwhelming majority is useless compressor oil and waste hydraulic oil.The recovered oil that the simple heating sedimentation-the processed method is made is lubricating oil inferior, and range of application is very narrow, is difficult to digestion.Adopt the 3rd type of technology of re-refining to be generally specialty oil refining factory and adopt, be mainly used in the high blended waste oil regeneration of high pollution, its investment is big, complex process, and technical requirements is high, and operation easier is big, can not suit enterprise practical conditions.In fact the nitrogenous fertilizer enterprises waste oil regeneration adopts the first kind to add that the technology of re-refining of second type of technology is just renewable to go out can be reused for the lubricated recovered oil of board.

Higher for dustiness, useless compressor oil that deterioration by oxidation is darker and waste hydraulic oil etc., the typical process using of nitrogenous fertilizer enterprises is at present: washing-Na ₂CO ₃Liquid caustic soda washes-technology of mechanical stirring carclazyte contact treating-filter press.Its flow process is following:

1. pre-treatment divides water assorted: useless compressor oil or waste hydraulic oil after emulsive not taking place or adding the DL-32H type emulsion splitter of 0.04-0.05%; In the uncovered regeneration still of oil pump suction 1#; Feed the steam heating of 1.6MPa toward still internal heating spiral pipe; And stop heating and stir sedimentation impurities removal after 9 hours when the gas bubbler stirs fluid to 80 ℃ as stirring to go into air-blowing with air;

2. an alkali cleaning: the Na that adds waste oil weight ratio 5% ₂CO ₃Solution (concentration is 5%) carries out alkali cleaning, and goes into gas bubbler stirring fluid 10-15 minute with air as stirring with air-blowing, gets rid of the slag of lower floor after sedimentation 3-4 hour.

3. thermal dehydration: go into the gas bubbler with air-blowing and stir fluid as stirring with air, be heated to boiling, until no bubble generation;

4. contact treating: go into the stirring of gas bubbler with air as stirring with air-blowing, add the atlapulgite of waste oil weight ratio 5% when continuing to be heated to 120 ℃, answer while adding and stir this moment; No bubble produces post-heating and is warming up to 120 ℃, is incubated 30 minutes, draws oil sample before the shutdown to the test tube static 3 minutes; Oil colours is transparent, and to be yellowish or greenish orange look person qualified for regeneration, otherwise increase by 2% carclazyte consumption, repeats this step aforesaid operations; Qualified until detecting; Wherein the atlapulgite index request is: percent of decolourization is about more than 95%, and NaAc method activity is not less than 200-220, and free acid is not more than 0.2%; More than 95%, moisture is at 8-11% through 200 orders for granularity;

5. press filtration: fluid is pumped into plate-and-frame filter press carry out press filtration, the edible vegetable oil that comes out drains in the uncovered regeneration still of 2#.

6. secondary alkali cleaning: the Na that slowly adds fluid weight ratio 5% ₂CO ₃Solution (concentration is 5%) carries out alkali cleaning, goes into the stirring of gas bubbler with air as stirring with air-blowing, draws oil sample with pH test paper test pH value., the pH value stops to add alkali and stirring when reaching 7.

7. second-heating dehydration:, produce as stirring with air-blowing to go into gas bubbler stirring fluid and be heated to boiling with air, pump in the basic oil groove of regeneration when being cooled to 50 ℃ with water coolant feeding spiral pipe until no bubble.

An alkali cleaning substitutes to remove the oxidated gum thing in the oil as using sulfuric acid process in the above-mentioned technology; Though it is effective; But this method will be destroyed the still effective various additives in the waste oil; Cause the recovered oil physicochemical property to descend, when the formulation of base oil of producing becomes lubricating oil, increase the consumption of additive inevitably.Simultaneously national environmental protection department has prohibited use sulfuric acid-carclazyte method technology, and its reason is that wherein sulfuric acid decoking method can produce deleterious waste gas and waste residue, and waste residue difficult degradation and disposal.Simple carclazyte contact treating or ADSORPTION IN A FIXED BED are refining, and its device is pressurized high-temperature distillation adsorption treatment, and its investment is big, and the carclazyte consumption is big, and safe class is high, and its production cost is higher.

Summary of the invention

The objective of the invention is to overcome above-mentioned defective, a kind of microcosmic salt flocculation CO is provided ₂Clay-treated waste oil regeneration method is mixed in gas mixing.

Scheme of the present invention is: comprise step 1. pre-treatment divide that water is assorted, 2. 3. thermal dehydration, 4. contact treating of step, 5. press filtration of step, 6. secondary alkali cleaning of step, 7. second-heating dehydration of step of an alkali cleaning, step of step, it is characterized in that:

Step 1. pre-treatment divides water assorted: when waste oil injects with uncovered regeneration still in this step, add the Na of waste oil weight ratio 5% simultaneously ₃Po ₄Solution (weight concentration is 5%) stops that the settling time is 4 hours after the heated and stirred;

Step is an alkali cleaning 2.: employed alkali lye is the Na of waste oil weight ratio 5% in this step ₃Po ₄Solution (concentration is 5%);

Step is contact treating 4.: adding the atlapulgite heated and stirred in this step does not have bubble and produces post-heating and heat up and be increased to 150 ℃;

Step is press filtration 5.: before press filtration, must water coolant be passed into cooling oil to 120 ℃ just pump oil pressure filter rapidly in the spiral pipe well heater in this step;

6. secondary alkali cleaning of step: employed alkali lye is the Na of waste oil weight ratio 2% in this step ₃Po ₄Solution (concentration is 5%);

More than each step to stir usefulness gas be CO ₂Gas.

The invention has the advantages that: Na is adopted in pre-treatment ₃PO ₄Carry out profit, dregs of fat separation pre-treatment, its flocculating result is better, has kept various additive effective ingredients in the waste oil.Because CO ₂Gas is rare gas element, effectively prevents the oxygenizement of fluid.And CO ₂Pre-treatment divide water assorted with caustic wash process in good flocculating effect is arranged.

Embodiment

" pre-treatment divides water to mix-Na to the present invention's employing ₃PO ₄Flocculation slagging-off-thermal dehydration-CO ₂Gas mixing carclazyte decolorizing and refining-filter press-Na ₃PO ₄Alkali cleaning-thermal dehydration " technology regenerates to useless compressor oil, waste hydraulic oil and useless refrigerator oil.Be a kind of microcosmic salt flocculation CO ₂Clay-treated technology of waste oil regenerating is mixed in gas mixing.The waste oil regeneration rate reaches more than 95%.

The present invention is fit to the nitrogenous fertilizer enterprises waste oil regeneration and uses.

1, pre-treatment divides water assorted and remove the dregs of fat and all use phosphoric acid salt to make flocculation agent.It is characterized in that: Na is adopted in pre-treatment ₃PO ₄Carry out profit, dregs of fat separation pre-treatment, its flocculating result is better.Though each degree of treatment is not dark, passes through Na ₃Po ₄Can remove 1/2 slag after alkali cleaning, the flocculation, and keep various additive effective ingredients in the waste oil.Add-on is the Na of 5% concentration in the alkali cleaning oil ₃Po ₄Consumption is 5%.

2, adopt CO ₂The gas mixing mode of mixing replaces pneumatic blending, because CO ₂Gas is rare gas element, under higher temperature (150 ℃), can effectively prevent the oxygenizement of fluid, makes it under higher temperature, to obtain better carclazyte decolorizing and refining effect.And CO ₂Gas is very wide in the nitrogenous fertilizer enterprises source.

3, adopt this carclazyte decoloring method it is characterized in that: open type regeneration still adds active bleaching clay when using spiral pipe steam indirect heating to the 150 ℃ left and right sides, and drum send CO simultaneously ₂Gas mixing is mixed and is protected fluid to play the anti-oxidation protection effect.

Table one 60t/a waste oil regeneration equipment list

Device name	Specifications and models	Quantity
			1#, the 2# still of regenerating	φ 1000 * 4.5 * 1450, P=normal pressure, T<=150 ℃, F=2.0m 2	2
Gear oil pump	KCB-83.3，Q=5m 3/h，P=0.6MPa，n=1450r/min	2
			The RPP chamber-type press filter	X10MW20/800-UB, 70－120℃	1

Table two regeneration base oil quality index

?	100 #The regeneration base oil	68 #The regeneration base oil
			The color transparency	In vitro oil colours is transparent is faint yellow	In vitro oil colours is transparent is faint yellow
Viscosity (40 ℃)/(mm 2/s）	90－135	60－74
			Acid number/(mgKOH/g)	≤0.15	≤0.10
Ash content/% (weight)	≤0.16	≤0.10
			Moisture/% (weight)	Do not have	Do not have
Open flash point/℃	205	≥180

Claims (1)

1. microcosmic salt flocculation CO ₂Clay-treated waste oil regeneration method is mixed in gas mixing; Comprise step 1. pre-treatment divide that water is assorted, 2. 3. thermal dehydration, 4. contact treating of step, 5. press filtration of step, 6. secondary alkali cleaning of step, 7. second-heating dehydration of step of an alkali cleaning, step of step, it is characterized in that:

Step 1. pre-treatment divides water assorted: when waste oil injects with uncovered regeneration still in this step, add the Na of waste oil weight ratio 5% simultaneously ₃Po ₄Solution (weight concentration is 5%) stops that the settling time is 4 hours after the heated and stirred;

Step is an alkali cleaning 2.: employed alkali lye is the Na of waste oil weight ratio 5% in this step ₃Po ₄Solution (concentration is 5%);

Step is contact treating 4.: adding the atlapulgite heated and stirred in this step does not have bubble and produces post-heating and heat up and be increased to 150 ℃;

Step is press filtration 5.: before press filtration, must water coolant be passed into cooling oil to 120 ℃ just pump oil pressure filter rapidly in the spiral pipe well heater in this step;

6. secondary alkali cleaning of step: employed alkali lye is the Na of waste oil weight ratio 2% in this step ₃Po ₄Solution (concentration is 5%);

More than each step to stir usefulness gas be CO ₂Gas.