RU2188851C1 - Method of refining spent lube oils - Google Patents

Abstract

FIELD: lubrication materials. SUBSTANCE: refining is effected with adsorbent suspended in spent oils, after which oil is filtered. Adsorbent is represented by peat modified with 50-100% orthophosphoric acid. Refining is conducted at ambient temperature for 30-60 min. EFFECT: increased degree of refining and speeded up refining process without heating. 1 tbl, 27 ex

Description

 The invention relates to a technology for the recovery of the hydrocarbon base of used industrial oils by adsorption refining.

 Industrial oils are used as cutting fluids in the processing of metals. Metalworking industries, due to the lack of technology for cleaning oil residues, burn or dump them into dumps. Therefore, the need for refining used (waste) oils is determined by large losses of energy-consuming and expensive mineral hydrocarbon raw materials and related environmental problems.

Known methods for refining residues from used industrial oils are based on the following methods: extraction (Patents: 2094450, 2100425, 2153527 RU, C 10 G 17/06, C 10 M 175/02; Application 2743570 FR C 10 M 175/02; Application 2735785 US , C 10 M 175/02; Application 19739659 Germany, C 10 M 175/00; Application 2334034 GB, C 10 M 175/00), adsorption on silica gel at 120-125 ^o C and stirring for 3-4 hours (Application 96101385 RU, С 10 М 175/02), on the ground after hydroprocessing of raw materials (Pat. 2099397 RU, С 10 М 175/00), on clay with simultaneous electrohydrocyclone (Pat. 2106398 RU, С 10 М 175/02), on clay together with a dechlorination catalyst the odoids contained in the oily residues (Application 2757873 US, C 10 M 175/00), attapulgite / smectite activated by alcohols (C ₁ -C ₆ ) and esters (C ₂ -C ₆ ) until a sludge-like mass is formed (US Pat. 5908500 US , С 09 С 1/02), on diatomite and kaolin with sand (Application 1104697 JP, С 10 М 177/00; Pat. 2153526 RU, С 10 М 175/02) and on white clay enriched with oxides of silicon, aluminum, iron and magnesium (Pat. 2058380 RU, C 10 M 175/02).

 There are also known methods of purification of used oils using bactericidal treatment (Pat. 2105045 RU, C 10 M 175/04; Pat. 2100290 RU, C 02 F 3/00; Application 96119614/04 RU, C 10 M 175/04).

In some cases, oil residues and fractions are partially (incompletely) refined by hydrotreatment at elevated temperature and pressure in the presence of a catalyst containing nickel, molybdenum, and aluminum oxides (Application 97113431 RU, C 10 G 67/04), by the action of electric fields of 35-50 kV / cm at 50-75 ^o C (Pat. 2101335 RU, C 10 M 175/02), sparging with compressed air heated to 110-140 ^o C (Pat. 2075506 RU, C 10 M 175/04), sedimentation of metal particles from heated oil to 110-130 ^o With (Pat. 96964 Finland, With 10 M 175/00).

 Removal of aromatic sulfur and nitrogen compounds from oils is carried out on a sulfidized catalyst containing nickel, cobalt, iron, tungsten, molybdenum, chromium and zinc (US Pat. 5676822 US, C 10 G 45/46).

In the method of purification of spent mineral oil (Pat. 2112018 RU, C 10 M 175/02), the raw material is treated by heating to 70-100 ^o C in the presence of 3-15 wt.% Waste biomass production of antibiotics.

 In order to isolate and purify oils from waste water-oil emulsions, they are pre-treated with demulsifiers and a large amount of water (Application 2743570 FR, С 10 М 175/02, Pat. 5874008 US, В 01 D 17/04), light hydrocarbons (10-50 rev %) and water (US Pat. 5882506 US, C 10 G 33/04), ammonium salts, fatty alcohols and amines, and centrifuged (Applications 4317046, 4317047 Germany, C 10 M 175/04), as well as thermal decomposition of water-oil emulsion in a special device (Application 19736281 DE, 01 D 17/035).

 Along with the development of chemical parameters (methods), devices (devices) are created and improved for the implementation of methods for the regeneration of used oils and coolants (US Pat. 5676840 US, B 01 D 35/06; Pat. 2142980 RU, C 10 M 175/02; Pat. 2123512 RU and Yugoslavia, C 10 G 25/00; Application 4405109 Germany, C 10 G 15/08; Application 9615380 France, C 10 M 175/00).

 The main structural elements of devices (installations) for the implementation of oil cleaning methods are: adsorbers, extractors, coarse filters, degassers, ultrafilters, irradiators with infrared and ultraviolet light, magnetic and electric fields, dehydrators, hydrogenators.

 The most effective oil refining technologies are based on extraction and adsorption methods.

 However, these methods have advantages and disadvantages. Therefore, one of them can either complement the other, or compensate for the shortcomings of the other in the technology of refining oils. Thus, for example, a liquid extractant is more difficult to disperse to dust particles in the volume of oil used than a finely divided solid adsorbent. Extraction and adsorption technologies for the purification of oils differ among themselves and in the duration of phase separation due to the different stability of the emulsion and suspension.

According to the technical nature of the proposed method of refining used oils, the closest method is the regeneration of used oil (Pat. 2058380 RU, C 10 M 175/02) using an adsorbent based on white palygorskite clay. Enriched with oxides of silicon and aluminum, white clay in an amount of 2-6 wt.% Suspended in the used oil at 80-90 ^o C for 2 hours and filtered through a filter press.

The disadvantage of clay as an adsorbent for the purification of used oils is the fact that the activity of the adsorbent depends on the content and ratio of metal oxides in clay. For example, dark (gray) clays exhibit a very low ability to clean oils. Even white clay, enriched with oxides of silicon and aluminum, refines the oil to a degree of 70-80% only at 80-90 ^o C for 2 hours

 The objective of the invention is to increase the activity and versatility of the method of refining used oils without heating.

The technical result is achieved by the fact that the natural material, peat is modified with phosphoric acid. Processing peat is 50-100% H ₃ PO ₄ followed by filtration and drying. The particle size of peat is from 50 to 1000 microns.

 Refining of used industrial oils of the type I-12, I-20, I-30, I-40 is carried out by suspending from 0.5 to 4.5 wt.% Adsorbent in oil at room temperature for 30-60 minutes and centrifuged. The degree of oil refining in this case is from 96.6 to 99.6%. Suspension of the adsorbent in oil residues is provided either by mechanical mixing of the phases, or by bubbling of compressed air in a mixture of oil and adsorbent.

 The invention uses peat from the Tomsk field. The degree of oil refining is determined using a KFK-3 photometer.

 Example. Methods of modification of peat and refining of used oils (IM).

 Natural peat is pre-dried, crushed and moistened with 50-100% phosphoric acid. A peat sample is kept in acid for an interval of time from 30 minutes to 3 days without heating. After that, the peat sample is filtered off and dried. A certain sample of modified peat (adsorbent) is suspended in a certain amount of used oils, provided that the adsorbent in the MI contains from 0.5 to 4.5 wt.%. The resulting suspension is stirred using a swinging or rolling electromechanical device for 30-90 minutes The purified (refined) hydrocarbon feed is separated from the adsorbent by centrifugation or natural sedimentation of the suspended adsorbent.

 The table shows experimental examples of the modification of peat and refining of MI, carried out by this method.

 As can be seen from examples 1-27, the modification of peat with phosphoric acid increases the degree of purification of oil residues by 10-14% and accelerates the refining process by 3-5 times without the use of heating in comparison with the prototype (Pat. 2058380 RU) under the same conditions for refining used oils .

Claims (1)

 A method of refining used oils, including suspending the adsorbent in used oils, followed by filtration, characterized in that peat modified with 50-100% phosphoric acid is used as an adsorbent, the process is carried out at a natural temperature for 30-60 minutes.

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