CN105087124A - Preparation method of biodegradable caster oil-based lubricant oil - Google Patents

Abstract

The invention discloses a preparation method of biodegradable caster oil-based lubricant oil and belongs to the field of preparation by virtue of biotechnology. The preparation method of the biodegradable caster oil-based lubricant oil comprises the following steps: adding alkali for cracking caster oil, so as to obtain sebacic acid; then preparing a self-made phosphotungstic/silica catalyst, and esterifying in presence of the catalyst, so as to obtain flavescent di-iso-octyl sebacate; mixing the flavescent di-iso-octyl sebacate with caster oil in a mass ratio of 3:2, and adding a right amount of thickening agent for regulating viscosity; and then concentrating and dehydrating, and adsorbing with activated carbon, so as to finally obtain the biodegradable caster oil-based lubricant oil. Examples prove that the preparation method of the biodegradable caster oil-based lubricant oil has the advantages that no harm is caused to the surrounding environment in an operation process, the duration of usage is prolonged by more than 5 months after use compared with common lubricant oil, damages caused by machine fraction are reduced, and the service life of a machine is prolonged.

Description

A kind of preparation method of biodegradable castor oil-base lubricating oil

Technical field

The invention discloses a kind of preparation method of biodegradable castor oil-base lubricating oil, belong to biotechnology preparation field.

Background technology

Lubricating oil is used in reduce friction in all kinds automobile, mechanical means, protection machinery and the liquid of workpiece or semi-solid lubricants, mainly play lubrication, cooling, antirust, clean, seal and the effect such as buffering.

In recent years, China's industry develop rapidly, processing industry is also advanced fast, lubricating oil is one of important petroleum chemicals, so that various mechanical means is also growing to the demand of lube product, also more and more higher to the performance requriements of lubricating oil, in order to meet the situation of mechanical means harshness to the requirement of lubricating oil use properties, the content of manufacturer's additive in lubricating oil finished product also becomes more and more, traditional is that lubricating oil oily based on mineral oil flows into environment, each heavy metal species and harmful substance contents in lubricating oil are increased, can not degrade voluntarily, and the larger harm to environment structure, therefore some countries have made laws and forbid using the nonconforming lubricating oil of biodegradability in environmentally sensitive area in the world.Meanwhile, petroleum resources reduce just gradually, in order to alleviate Pressure on Energy and protection of the environment, Study and Development novel, biodegradable lubricating oil proxy mineral oil has great society and economic implications.

Because in waste lubricating oil, additive level significantly rises, generally adopt the rear sulfuric acid of first distillation now, the old technique such as clay-filtered, can not produce the rerefined oil basestocks of high-quality, and this technique in process of production, due to the existence of a large amount of additive, equipment coking can be produced during distillation, acid, alkali, time clay-filtered, sulfuric acid, carclazyte consumption significantly rises, cause carbonic acid gas, sulphur slag, a large amount of discharges of spent bleaching clay, severe contamination environment, but also there is a lot of defect in the quality of institute's product, and it is low to there is product recovery rate, tooling cost is high, loss is large, complex process, potential safety hazard is many, the problems such as investment is high.

Summary of the invention

The technical problem that the present invention mainly solves: for current conventional lubrication oil be based on mineral oil oil flow into environment, self can not degrade voluntarily, and the existence containing a large amount of additive, not only pollute environment, improve tooling cost, and quality product existing defects, potential safety hazard is many, in addition, petroleum resources reduce gradually, Pressure on Energy is made to can not get slowing down drawback, provide a kind of preparation method of biodegradable castor oil-base lubricating oil, the method is by obtaining SA to the cracking of Viscotrol C plus-minus, make phosphorus tungsten/silicon dioxide catalyzer afterwards by oneself, under the effect of catalyzer, esterification obtains flaxen diisooctyl sebacate, by its with Viscotrol C in mass ratio for 3:2 carries out mixing and add appropriate thickening material and regulate its viscosity, again through thickening, a kind of biodegradable castor oil-base lubricating oil is finally obtained after charcoal absorption.This lubricating oil is not only by extracting in plant, can degrade voluntarily, reduce production cost, for environment without any pollution, and improves quality product, alleviates Pressure on Energy.

In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:

(1) get 100 ~ 400g paraffin oil and put into pyrolyzer, be heated to 80 ~ 100 DEG C, slowly add the sodium hydroxide solution that 60 ~ 100mL mass concentration is 50% while stirring, dehydration technology process is carried out after being decompressed to 1000 ~ 2000Pa, again pyrolyzer temperature is increased to 240 ~ 360 DEG C, slow dropping 100 ~ 150g Viscotrol C, control rate of addition make to dropwise in its 60 ~ 90min, then at 240 ~ 360 DEG C cracking 5 ~ 8h;

(2) split product is put into 2L beaker, add 500 ~ 600mL hot water and regulate pH to 5 ~ 6 with the hydrochloric acid soln that mass concentration is 30%, after paraffin oil and water stratification, be separated and remove paraffin oil reservoir, continue to regulate water layer pH to 2 ~ 3, be warming up to 100 ~ 105 DEG C afterwards, reclaim through fractionation and obtain SA;

(3) 5 ~ 10mL tetraethoxy is got and 10 ~ 20mL phospho-wolframic acid is dissolved in 100 ~ 200mL ethanol, be placed on magnetic stirrer, warming-in-water to 30 ~ 40 DEG C, move into reflux after stirring 15 ~ 30min with the rotating speed of 100 ~ 200r/min, backflow 1 ~ 2h, ageing 24 ~ 30h after taking out, put into vacuum drying oven afterwards, at 80 ~ 90 DEG C, dry 20 ~ 25min, then puts into retort furnace, 5 ~ 6h is calcined, obtained phosphorus tungsten/silicon dioxide catalyzer at 400 ~ 500 DEG C;

(4) in the four-hole boiling flask that thermometer, water-and-oil separator and reflux condensing tube are housed, add the above-mentioned system of 100 ~ 200mL the above-mentioned obtained phosphorus tungsten/silicon dioxide catalyzer of SA, the isooctyl alcohol of 10 ~ 20mL, the toluene of 30 ~ 50mL and 2 ~ 5g, refuxing esterification 3 ~ 5h at 60 ~ 70 DEG C;

(5) mixed solution after above-mentioned esterification is filtered removal catalyzer, with moving into single port flask after deionized water wash, put into oil bath pan, be warming up to 190 ~ 200 DEG C, reduce pressure pressure of the inside of a bottle 1000 ~ 2000Pa, water, toluene and isooctyl alcohol are removed in distillation, and the weak yellow liquid obtained is diisooctyl sebacate;

(6) by Viscotrol C and diisooctyl sebacate in mass ratio for 2:3 carries out oil based on after mixing, thickening material made by the polyacrylamide adding base oil total mass 1 ~ 3% wherein, add again the calcium mahogany sulfonate of base oil total mass 5 ~ 13%, the aminothio ester of 10 ~ 15%, the boronation polyisobutene succinimide of 25 ~ 35% and 3 ~ 16% alkyl diphenylamine be in harmonious proportion, 40 ~ 60min is stirred at 30 ~ 50 DEG C, mixing speed is 100 ~ 200r/min, obtains lubricating oil head product;

(7) above-mentioned lubricating oil head product is put into thickening machine, be decompressed to 1000 ~ 2000Pa, remove the moisture in lubricating oil, then make it from top to bottom by activated carbon column, absorption impurity wherein, finally obtains a kind of biodegradable castor oil-base lubricating oil.

Application method of the present invention is: added by the lubricating oil obtained by the present invention during factory operates machines, lubricating oil 8 ~ 15mL is added with drip irrigation in every platform machine wheel shaft, after using, for periphery crowd and environment without any harm, 5 ~ 8 months are extended than the Use Limitation of plain oil, and decrease the infringement of machine friction generation, extend machine service life.

The invention has the beneficial effects as follows:

(1) by extracting in plant, not only slow down Pressure on Energy, and can degrade voluntarily;

(2) reduce production cost, decrease potential safety hazard, the quality product obtained out is significantly improved;

(3) the base oil acid number regenerated is low, and look is number little, and anti-oxidative stability is good, and all technical meets the specification of quality of lubricant base.

Embodiment

First get 100 ~ 400g paraffin oil and put into pyrolyzer, be heated to 80 ~ 100 DEG C, slowly add the sodium hydroxide solution that 60 ~ 100mL mass concentration is 50% while stirring, dehydration technology process is carried out after being decompressed to 1000 ~ 2000Pa, again pyrolyzer temperature is increased to 240 ~ 360 DEG C, slow dropping 100 ~ 150g Viscotrol C, control rate of addition make to dropwise in its 60 ~ 90min, then at 240 ~ 360 DEG C cracking 5 ~ 8h; Then split product is put into 2L beaker, add 500 ~ 600mL hot water and regulate pH to 5 ~ 6 with the hydrochloric acid soln that mass concentration is 30%, after paraffin oil and water stratification, be separated and remove paraffin oil reservoir, continue to regulate water layer pH to 2 ~ 3, be warming up to 100 ~ 105 DEG C afterwards, reclaim through fractionation and obtain SA; Next 5 ~ 10mL tetraethoxy is got and 10 ~ 20mL phospho-wolframic acid is dissolved in 100 ~ 200mL ethanol, be placed on magnetic stirrer, warming-in-water to 30 ~ 40 DEG C, move into reflux after stirring 15 ~ 30min with the rotating speed of 100 ~ 200r/min, backflow 1 ~ 2h, ageing 24 ~ 30h after taking out, put into vacuum drying oven afterwards, at 80 ~ 90 DEG C, dry 20 ~ 25min, then puts into retort furnace, 5 ~ 6h is calcined, obtained phosphorus tungsten/silicon dioxide catalyzer at 400 ~ 500 DEG C; Subsequently in the four-hole boiling flask that thermometer, water-and-oil separator and reflux condensing tube are housed, add the above-mentioned system of 100 ~ 200mL the above-mentioned obtained phosphorus tungsten/silicon dioxide catalyzer of SA, the isooctyl alcohol of 10 ~ 20mL, the toluene of 30 ~ 50mL and 2 ~ 5g, refuxing esterification 3 ~ 5h at 60 ~ 70 DEG C; Afterwards the mixed solution after above-mentioned esterification is filtered and remove catalyzer, with moving into single port flask after deionized water wash, put into oil bath pan, be warming up to 190 ~ 200 DEG C, reduce pressure pressure of the inside of a bottle 1000 ~ 2000Pa, water, toluene and isooctyl alcohol are removed in distillation, and the weak yellow liquid obtained is diisooctyl sebacate; By Viscotrol C and diisooctyl sebacate in mass ratio for 2:3 carries out oil based on after mixing, thickening material made by the polyacrylamide adding base oil total mass 1 ~ 3% wherein, add again the calcium mahogany sulfonate of base oil total mass 5 ~ 13%, the aminothio ester of 10 ~ 15%, the boronation polyisobutene succinimide of 25 ~ 35% and 3 ~ 16% alkyl diphenylamine be in harmonious proportion, 40 ~ 60min is stirred at 30 ~ 50 DEG C, mixing speed is 100 ~ 200r/min, obtains lubricating oil head product; Finally above-mentioned lubricating oil head product is put into thickening machine, be decompressed to 1000 ~ 2000Pa, remove the moisture in lubricating oil, then make it from top to bottom by activated carbon column, absorption impurity wherein, finally obtains a kind of biodegradable castor oil-base lubricating oil.

Example 1

First get 100g paraffin oil and put into pyrolyzer, be heated to 80 DEG C, slowly add the sodium hydroxide solution that 60mL mass concentration is 50% while stirring, dehydration technology process is carried out after being decompressed to 1000Pa, again pyrolyzer temperature is increased to 240 DEG C, slow dropping 100g Viscotrol C, control rate of addition make to dropwise in its 60min, then at 240 DEG C cracking 5h; Then split product is put into 2L beaker, add 500mL hot water and by mass concentration be 30% hydrochloric acid soln adjustment pH to 5, after paraffin oil and water stratification, be separated and remove paraffin oil reservoir, continue to regulate water layer pH to 2, be warming up to 100 DEG C afterwards, reclaim through fractionation and obtain SA; Next 5mL tetraethoxy is got and 10mL phospho-wolframic acid is dissolved in 100mL ethanol, be placed on magnetic stirrer, warming-in-water to 30 DEG C, moves into reflux after stirring 15min with the rotating speed of 100r/min, backflow 1h, ageing 24h after taking out, put into vacuum drying oven afterwards, at 80 DEG C, dry 20min, then puts into retort furnace, 5h is calcined, obtained phosphorus tungsten/silicon dioxide catalyzer at 400 DEG C; Subsequently in the four-hole boiling flask that thermometer, water-and-oil separator and reflux condensing tube are housed, add the above-mentioned system of 100mL the above-mentioned obtained phosphorus tungsten/silicon dioxide catalyzer of SA, the isooctyl alcohol of 10mL, the toluene of 30mL and 2g, refuxing esterification 3h at 60 DEG C; Afterwards the mixed solution after above-mentioned esterification being filtered and remove catalyzer, with moving into single port flask after deionized water wash, putting into oil bath pan, be warming up to 190 DEG C, reduce pressure pressure of the inside of a bottle 1000Pa, and water, toluene and isooctyl alcohol are removed in distillation, and the weak yellow liquid obtained is diisooctyl sebacate; By Viscotrol C and diisooctyl sebacate in mass ratio for 2:3 carries out oil based on after mixing, get 100g base oil, thickening material made by the polyacrylamide adding 2g wherein, the alkyl diphenylamine adding the calcium mahogany sulfonate of 10g, the aminothio ester of 20g, the boronation polyisobutene succinimide of 50g and 6g is again in harmonious proportion, 40min is stirred at 30 DEG C, mixing speed is 100r/min, obtains lubricating oil head product; Finally above-mentioned lubricating oil head product is put into thickening machine, be decompressed to 1000Pa, remove the moisture in lubricating oil, then make it from top to bottom by activated carbon column, absorption impurity wherein, finally obtains a kind of biodegradable castor oil-base lubricating oil.

During this example operation, the lubricating oil obtained by the present invention is added during factory operates machines, lubricating oil 8mL is added with drip irrigation in every platform machine wheel shaft, after using, for periphery crowd and environment without any harm, 5 months are extended than the Use Limitation of plain oil, and decrease the infringement of machine friction generation, extend machine service life.

Example 2

First get 250g paraffin oil and put into pyrolyzer, be heated to 90 DEG C, slowly add the sodium hydroxide solution that 80mL mass concentration is 50% while stirring, dehydration technology process is carried out after being decompressed to 1500Pa, again pyrolyzer temperature is increased to 300 DEG C, slow dropping 120g Viscotrol C, control rate of addition make to dropwise in its 80min, then at 300 DEG C cracking 7h; Then split product is put into 2L beaker, add 550mL hot water and by mass concentration be 30% hydrochloric acid soln adjustment pH to 5.5, after paraffin oil and water stratification, be separated and remove paraffin oil reservoir, continue to regulate water layer pH to 2.5, be warming up to 103 DEG C afterwards, reclaim through fractionation and obtain SA; Next 8mL tetraethoxy is got and 15mL phospho-wolframic acid is dissolved in 150mL ethanol, be placed on magnetic stirrer, warming-in-water to 35 DEG C, moves into reflux after stirring 20min with the rotating speed of 150r/min, backflow 1.5h, ageing 28h after taking out, put into vacuum drying oven afterwards, at 85 DEG C, dry 23min, then puts into retort furnace, 5.5h is calcined, obtained phosphorus tungsten/silicon dioxide catalyzer at 450 DEG C; Subsequently in the four-hole boiling flask that thermometer, water-and-oil separator and reflux condensing tube are housed, add the above-mentioned system of 150mL the above-mentioned obtained phosphorus tungsten/silicon dioxide catalyzer of SA, the isooctyl alcohol of 150mL, the toluene of 40mL and 4g, refuxing esterification 4h at 65 DEG C; Afterwards the mixed solution after above-mentioned esterification being filtered and remove catalyzer, with moving into single port flask after deionized water wash, putting into oil bath pan, be warming up to 195 DEG C, reduce pressure pressure of the inside of a bottle 1500Pa, and water, toluene and isooctyl alcohol are removed in distillation, and the weak yellow liquid obtained is diisooctyl sebacate; By Viscotrol C and diisooctyl sebacate in mass ratio for 2:3 carries out oil based on after mixing, get 200g base oil, thickening material made by the polyacrylamide adding 4g wherein, the alkyl diphenylamine adding the calcium mahogany sulfonate of 20g, the aminothio ester of 26g, the boronation polyisobutene succinimide of 60g and 24g is again in harmonious proportion, 50min is stirred at 40 DEG C, mixing speed is 150r/min, obtains lubricating oil head product; Finally above-mentioned lubricating oil head product is put into thickening machine, be decompressed to 1500Pa, remove the moisture in lubricating oil, then make it from top to bottom by activated carbon column, absorption impurity wherein, finally obtains a kind of biodegradable castor oil-base lubricating oil.

During this example operation, the lubricating oil obtained by the present invention is added during factory operates machines, lubricating oil 13mL is added with drip irrigation in every platform machine wheel shaft, after using, for periphery crowd and environment without any harm, 7 months are extended than the Use Limitation of plain oil, and decrease the infringement of machine friction generation, extend machine service life.

Example 3

First get 400g paraffin oil and put into pyrolyzer, be heated to 100 DEG C, slowly add the sodium hydroxide solution that 100mL mass concentration is 50% while stirring, dehydration technology process is carried out after being decompressed to 2000Pa, again pyrolyzer temperature is increased to 360 DEG C, slow dropping 150g Viscotrol C, control rate of addition make to dropwise in its 90min, then at 360 DEG C cracking 8h; Then split product is put into 2L beaker, add 600mL hot water and by mass concentration be 30% hydrochloric acid soln adjustment pH to 6, after paraffin oil and water stratification, be separated and remove paraffin oil reservoir, continue to regulate water layer pH to 3, be warming up to 105 DEG C afterwards, reclaim through fractionation and obtain SA; Next 10mL tetraethoxy is got and 20mL phospho-wolframic acid is dissolved in 200mL ethanol, be placed on magnetic stirrer, warming-in-water to 40 DEG C, moves into reflux after stirring 30min with the rotating speed of 200r/min, backflow 2h, ageing 30h after taking out, put into vacuum drying oven afterwards, at 90 DEG C, dry 25min, then puts into retort furnace, 6h is calcined, obtained phosphorus tungsten/silicon dioxide catalyzer at 500 DEG C; Subsequently in the four-hole boiling flask that thermometer, water-and-oil separator and reflux condensing tube are housed, add the above-mentioned system of 200mL the above-mentioned obtained phosphorus tungsten/silicon dioxide catalyzer of SA, the isooctyl alcohol of 20mL, the toluene of 50mL and 5g, refuxing esterification 5h at 70 DEG C; Afterwards the mixed solution after above-mentioned esterification being filtered and remove catalyzer, with moving into single port flask after deionized water wash, putting into oil bath pan, be warming up to 200 DEG C, reduce pressure pressure of the inside of a bottle 2000Pa, and water, toluene and isooctyl alcohol are removed in distillation, and the weak yellow liquid obtained is diisooctyl sebacate; By Viscotrol C and diisooctyl sebacate in mass ratio for 2:3 carries out oil based on after mixing, get 300g base oil, thickening material made by the polyacrylamide of 9g wherein, the alkyl diphenylamine adding the calcium mahogany sulfonate of 39g, the aminothio ester of 30g, the boronation polyisobutene succinimide of 70g and 32g is again in harmonious proportion, 60min is stirred at 50 DEG C, mixing speed is 200r/min, obtains lubricating oil head product; Finally above-mentioned lubricating oil head product is put into thickening machine, be decompressed to 2000Pa, remove the moisture in lubricating oil, then make it from top to bottom by activated carbon column, absorption impurity wherein, finally obtains a kind of biodegradable castor oil-base lubricating oil.

During this example operation, the lubricating oil obtained by the present invention is added during factory operates machines, lubricating oil 15mL is added with drip irrigation in every platform machine wheel shaft, after using, for periphery crowd and environment without any harm, 8 months are extended than the Use Limitation of plain oil, and decrease the infringement of machine friction generation, extend machine service life.

Claims (1)

1. a preparation method for biodegradable castor oil-base lubricating oil, is characterized in that concrete preparation process is:

(1) get 100 ~ 400g paraffin oil and put into pyrolyzer, be heated to 80 ~ 100 DEG C, slowly add the sodium hydroxide solution that 60 ~ 100mL mass concentration is 50% while stirring, dehydration technology process is carried out after being decompressed to 1000 ~ 2000Pa, again pyrolyzer temperature is increased to 240 ~ 360 DEG C, slow dropping 100 ~ 150g Viscotrol C, control rate of addition make to dropwise in its 60 ~ 90min, then at 240 ~ 360 DEG C cracking 5 ~ 8h;

(2) split product is put into 2L beaker, add 500 ~ 600mL hot water and regulate pH to 5 ~ 6 with the hydrochloric acid soln that mass concentration is 30%, after paraffin oil and water stratification, be separated and remove paraffin oil reservoir, continue to regulate water layer pH to 2 ~ 3, be warming up to 100 ~ 105 DEG C afterwards, reclaim through fractionation and obtain SA;

(3) 5 ~ 10mL tetraethoxy is got and 10 ~ 20mL phospho-wolframic acid is dissolved in 100 ~ 200mL ethanol, be placed on magnetic stirrer, warming-in-water to 30 ~ 40 DEG C, move into reflux after stirring 15 ~ 30min with the rotating speed of 100 ~ 200r/min, backflow 1 ~ 2h, ageing 24 ~ 30h after taking out, put into vacuum drying oven afterwards, at 80 ~ 90 DEG C, dry 20 ~ 25min, then puts into retort furnace, 5 ~ 6h is calcined, obtained phosphorus tungsten/silicon dioxide catalyzer at 400 ~ 500 DEG C;

(4) in the four-hole boiling flask that thermometer, water-and-oil separator and reflux condensing tube are housed, add the above-mentioned system of 100 ~ 200mL the above-mentioned obtained phosphorus tungsten/silicon dioxide catalyzer of SA, the isooctyl alcohol of 10 ~ 20mL, the toluene of 30 ~ 50mL and 2 ~ 5g, refuxing esterification 3 ~ 5h at 60 ~ 70 DEG C;

(5) mixed solution after above-mentioned esterification is filtered removal catalyzer, with moving into single port flask after deionized water wash, put into oil bath pan, be warming up to 190 ~ 200 DEG C, reduce pressure pressure of the inside of a bottle 1000 ~ 2000Pa, water, toluene and isooctyl alcohol are removed in distillation, and the weak yellow liquid obtained is diisooctyl sebacate;

(6) by Viscotrol C and diisooctyl sebacate in mass ratio for 2:3 carries out oil based on after mixing, thickening material made by the polyacrylamide adding base oil total mass 1 ~ 3% wherein, add again the calcium mahogany sulfonate of base oil total mass 5 ~ 13%, the aminothio ester of 10 ~ 15%, the boronation polyisobutene succinimide of 25 ~ 35% and 3 ~ 16% alkyl diphenylamine be in harmonious proportion, 40 ~ 60min is stirred at 30 ~ 50 DEG C, mixing speed is 100 ~ 200r/min, obtains lubricating oil head product;

(7) above-mentioned lubricating oil head product is put into thickening machine, be decompressed to 1000 ~ 2000Pa, remove the moisture in lubricating oil, then make it from top to bottom by activated carbon column, absorption impurity wherein, finally obtains a kind of biodegradable castor oil-base lubricating oil.