JPH0657285A - Method of recycling used or contaminated lubricating oil - Google Patents

Abstract

PURPOSE: To obtain a reusable finished product by removing an acid waste by a few process steps and reducing a treating time.

CONSTITUTION: A specific amount of a spent or a contaminated lubricating oil is introduced into an autoclave reactor; to add about 15% refined clay, fuller's earth, montimolinote or bentonite, about 1-2% water with an active sulfur base catalyst diluted, and about 2% filtration auxiliary materials such as diatomite; to heat them for about 5 hours; to continuously inject steam under a pressure of 6-10 kg/cm² and to continue distillation at high temperature for about 3 hours while being occasionally under vacuum of 550 mm Hg, until a contact treatment and regulation of the ignition point (the flash point) are completed. The reaction product is heat-treated while collecting samples for laboratory test of whether the product become a state to be filterable. And after confirming transfer of the total carbon waste being in burning oil to a filtered cake by the test of recovered material from a pressure filter, the reaction product, if necessary, is sent to the second step.

COPYRIGHT: (C)1994,JPO

Description

Detailed Description of the Invention

The present invention relates to a novel process for the recycling of used or contaminated lubricating oils, and more particularly not only for its novelty: development of processing through a smaller number of steps and Significant reductions in processing time; elimination of acid waste and improvement of residual products by providing reusable end products: particularly relevant to economic and ecological results. , And in particular to methods that are distinguished when compared to commonly used techniques because of the significant benefits that the present invention brings to the planetary ecosystem.

The general movement of the whole world related to ecological problems, which is fundamentally related to the overall survival of our planet and humanity, is getting faster every day. Are well known to those skilled in the art. In support of this ecology, the "cruzard (cruzad
As a result of e) ', the normal invaders of our environment, the fauna, flora and the air we breathe, are more likely to continue performing these invasions naturally as before. We are discovering great difficulties.

Clearly, the efforts developed to date have been
To protect their own interests, forgetting that future generations will suffer moderately long periods of time, the first and smallest by those who have always used and benefited from our environment and its natural resources. As soon as there were signs of deprecation, it could easily be considered useless.

Furthermore, with the utmost dedication, they are some scientists trying a technical approach to find new ways to control the problem of environmental pollution by gases and chemicals thrown into reservoirs etc. And commend the achievements and efforts developed by the entrepreneur.

An important segment of this movement relates to recycled materials, especially due to the fact that the mineral resources of our planet do not last forever. While struggling with any possible waste, maximizing the use of finite resources and prolonging their use, humankind must learn how to use the resources, which can be done by recovery or recycling.

Clearly, the problem of recycling used materials is an international problem, and all countries are serious about their research, seeking both ideal solutions and realistic solutions in the region. is necessary. In the special case of Brazil, emphasize that it is time to wake up and turn the recycling of used materials into a priority goal, as has already happened in other countries, especially in Eastern Europe. is necessary. This will prevent any further damage to the environment, which plagued Europe as aggression, especially after the Industrial Revolution.

The direct and immediate importance of this prioritization is
It means that the ultimate funding, which is usually aimed at fighting the consequences of pollution, can be directed to more lofty directions, such as social assistance.

Therefore, it cannot be denied that the elimination of any invasion of our environment is necessarily the basis of the recycling industry.

Furthermore, in view of environmental problems in particular, it is inevitable to give examples of the most harmful materials not only to the environment and the ecosystem but also to the overall economy. It is easily acknowledged that the decline of the Berlin Wall a few years ago revealed to the West some serious problems that resulted from Eastern European countries paying little attention to the environment. Will. Examples of such problems are: -The use of low quality, highly pollutant coal in outdated industries. This requires three to four times more energy than similar industries in Western countries. -In Moscow, the level of air pollution is about 50 times higher than what is considered acceptable in Western standards. -Abuse of fertilizers and pesticides. It reaches dozens of times more than the amount that can be tolerated in Western countries, and it defeats the relevance of agricultural exports. -The Bohemian region of Czechoslovakia is always covered with yellow smog clouds, 15% of children have skin disorders or are in the respiratory system, with a life expectancy of 52 years. -In Poland, 95% of natural river water is not suitable for human consumption due to uncontrolled use of fertilizers and pesticides, and 50% is polluted and unusable for agriculture. -High levels of lead, mercury and cadmium are found in the placenta of pregnant women.

In order to avoid these damages, all the metals, plastics, solvents, rubbers, papers, glasses, textiles and especially lubricating oils used, as well as many other products, are recycled or recovered as many times as possible. There must be. Urban waste and protection must be reasonably pioneered with all recyclable materials prior to the recovery of plants and equipment. The economic and ecological benefits that result from establishing a global policy for recycling domestically used or polluted materials can be astonishing and, while protecting the environment, the economic development we all expect. It will surely be put in.

Among the advantages of recycling used or polluted materials may be mentioned the following: a significant reduction in environmental pollution due to industrial, agricultural and municipal waste; an increase in the useful life of natural sources; recycling. Reduced energy consumption by needing less than 85% energy of primary production of products; much less capital investment in the recycling industry than would otherwise be required for primary products industry; reduction of imports and exports A substantial saving of currency due to the increase of; to generate taxes and work on substances that are considered "unusable"; to reduce public spending or to recover and remove pollutants; to induce without making people useless;
Agricultural reform by saving natural sources.

In view of all the above issues, it is important not only to cite Brazil but also to urgently propose to other countries to save the environment and avoid reaching the pollution levels mentioned above. Is. While most countries do not have the economic resources necessary to repair the damage caused to ecology or the environment, avoiding these damages from the incident of recycling used materials is far more viable. This problem is of great relevance when we think of it.

In some national laws there is a risk of legal problems, especially with regard to recycling, and these laws will be amended to promote conservation of the natural environment.

In accordance with this spirit, what can be recycled is recycled, and as many times as possible, the material is discarded only when it cannot be recycled any more, and further after being disposed so as not to have an adverse effect on the environment. The basic motto that it should be made was created.

Furthermore, in addition to the above motto,
It requires the unyielding will of everyone else, who can take legal steps to achieve the goals from the industrial and economic or environmental standpoints.

[0016] Especially with regard to the recycling of mineral oils, several recyclings are already relatively common in some countries and, despite each developing their own technology, are relatively new activities, eg in Brazil. .
Therefore, at the Japanese level, the recycling of mineral oil has become an important issue both economically and environmentally since the first oil shock in 1973.

Due to the unusual environment of the time, the recycling of mineral oils has led to government, especially Conselhonacional
do Petroleo (National Oil
Counsil's attention, and on this issue, the Law was made by Resolution CNP-18 / 77 and then amended by Resolution CNP-02 / 85.

Furthermore, recycling of used or dirty lubricants is necessary for two reasons: environmental protection and economic asset protection.

Before addressing what is known as a method of recycling used or dirty lubricating oil, no one denies that many industries are throwing large amounts of used or dirty oil into the environment. I should point out that you cannot do it. It is also an open fact that even more car owners simply throw away used or dirty oil in drains when they change the oil in their cars.

10,000 in France, 1983
According to a public survey of car owners in
28% of car owners changed their oil by themselves, and most of the used or dirty oil was simply dumped in drains.

All of this waste is at least 30,0
It is a serious pollutant of 00 tons / year and is extremely harmful to human health. The dumping of used or contaminated oil into the natural environment has a serious impact on soil oxigenation and the surrounding water sources. In addition, it is extremely harmful to the flora and fauna that live there. It is also necessary to point out that the oil dumped in the sewer will seriously damage the water treatment plant. That is, the biological purification process reduces the oxygenation of activated waste, reduces the precipitation of solid waste in the decanter, and introduces many problems to mechanical dehydration precipitation of residual waste.

Thus, such dumping of used or contaminated mineral oil is a crime against people's water sources and interferes with the practice of water-utilizing sports. It is not possible to dump 5 liters of used or contaminated oil into a lake.
It is contaminating up to 00 m ³ of water, and furthermore, a film with a thickness of a few microns is sufficient to kill all living things.

Burning used or contaminated mineral oils has been practiced by several companies, but has been
Sent by resolution 7/90. It emits many harmful substances, especially lead. Five liters of used or contaminated lubricating oil contains as much as 20 g of lead. That is, it is as heavy as a hunting round, and lead causes chronic lead poisoning with concomitant gallbladder edema, anemia, finger paralysis and nephritis.

Therefore, it is important to eliminate pollution sources. Because this solution is very simple and represents a significant saving of resources, it is necessary to recycle the used or contaminated oil.

Generally, used or contaminated oils have two major sources of lubricating oil. That is, oils used in automobiles and oils used in industry. It is necessary to explain that the significant amount of lubricating oil used is consumed during its use or lost by its use. These are the oils used to make lubricating greases, the oils used to form soluble oils, the oils used in the textile industry and the white oils used to make petroleum jelly and the like.

Clean oil used in power converters, turbines and hydraulic transfer systems can be recovered. However, due to their high commercial value, these oils are of particular interest. In fact, these oils can be easily recycled and, through suitable recovery processes,
It can be reused for the same purpose as described above. At this time, it is also possible to reuse those for less valuable applications (such as grease and molding oil). Other industrial oils can be recovered as well.

[0027] Generally, used or contaminated oil is combusted for use as fuel or recovered. Burning used or contaminated oil is not legal and uneconomical. On the other hand, recovering used or contaminated oil does not violate the law and brings further significant advantages. Combusting 1 ton of used and polluted oil will yield 0.62 tonnes of recycle gas. It can be returned to the recycling center for reprocessing after use.

At present, lubricating oils for the automotive industry include mineral oils; additives that exhibit the following special characteristics due to the presence of significant amounts of sulfur in the heat enhancer or fuel. Improve the level of viscosity; add washing and dispersion properties to the oil; lower the freezing point (temperature); improve oxidation resistance; adapt the oil to special requirements.

It is the additive, not the mineral oil, that actually determines the performance and price of the lubricating oil. By collecting and recycling used or contaminated oil,
A basic oil can be obtained with properties similar to those of the new oil. By a person skilled in the art,
It is impossible to recognize the difference between oil that has been once recycled and new oil in the laboratory.

Generally speaking, recycling spent and contaminated oil means water, solid particles, by-products resulting from dilution, duplicates resulting from oxidation and additions that have already been added. Treatment of used and contaminated lubricating oil in a series of treatments to completely remove all contaminants, including agents.

The lubricant does not wear out. In other words, the lubricant does not lose its lubricating properties. It only gets dirty with use or over time. Unfortunately, most people are also unaware that used lubricants can be cleaned and that disposal of them can have very serious adverse ecological and environmental consequences.

Spent or polluted oils are feedstocks that, due to the nature of the oils, make little difference in composition, just as crude oils do. In fact, just as refineries can produce gas and base oils among other products,
A recycling center for recycling used or contaminated oil can cycle the used or contaminated oil to obtain a base oil. The basic operation in both plants is basically the same.

As mentioned above, base oils for use as lubricating oils in the automobile industry are usually modified with additives to reduce the need for regular oil changes,
The most important of such additives, along with some of the most common contaminants, are listed below: Additives for viscosity improvement (polymers); Cleaning and dispersion additives. Antioxidant and antiwear additives; Water resulting from engine operation or engine seal failure (free or in combination with other substances); Lighter oil (fuel) or gaseous oil; Resulting from oxidation By-products (generally caused by engine operation); Lead, an explosion-proof agent found in light oils; Metal particles from engines; Carbon particles resulting from incomplete combustion of oil;

At present, several recycling methods are known, of which the following can be mentioned: acid / clay (Bernd Meiken process); solvent extraction (French Petroleum Institute); distillation / clay; distillation. / Hydrogenation; Thin film evaporator.

In general, the recycling processes, in particular those carried out with sulfuric acid as in the acid / clay process, consist of the same principles and a few differences, which principles are based on Decantation; atmospheric distillation; treatment with sulfuric acid; neutralization; treatment with activated clay; distillation under reduced pressure; filtration; retreatment.

The decantation treatment is a rough treatment in which used or contaminated oil is preheated to 50 to 60 ° C. in a collection container, whereby a part of the water content is removed in the form of colored sludge.

The atmospheric distillation, which is carried out under slight pressure, separates the emulsified water from some of the lighter hydrocarbon fractions.

During the treatment with sulfuric acid, the partially purified oil, free of its water component, is treated with sulfuric acid at temperatures in the region of 35 ° C. The hydrocarbon molecules present in the used or contaminated oil, when not oxidized, even when heated to a certain temperature, await the property of countering high concentrations of sulfuric acid. On the other hand, when the hydrocarbon molecule is oxidized, it is attacked by the acid and combined with it.
ne) to form a dense sludge by-product (commonly referred to as tar sulfate). Suitable for decanting impurities, this by-product is separated from its used or contaminated oil in a suitable facility and this treatment is used or contaminated. It requires the use of an amount of sulfuric acid equal to 6-7% of the initial volume of oil. At this stage in the process, insoluble precipitates, metallic particles, metallic acids,
Unwanted soluble compounds, oxidation products, additives, sulphonated aromatic products and the like are removed from this used or contaminated oil.

The neutralization step following the treatment with sulfuric acid is soda,
Neutralization of recycle oil containing a high content of sulfuric acid containing calcium carbonate or other alkaline compounds.

Activated clay
During this stage of the treatment with y), the post-acid treatment contaminants still present in this recycled oil are removed by adsorption by activated clay. A special purpose at this stage is to provide a cleaner final product, which usually requires the use of granulated clay in amounts ranging from 5-8% of the oil's initial loading weight. And

Vacuum distillation uses oils according to their different viscosities in order to limit their required temperature.
Waiting for the purpose of separation. This vacuum distillation is based on a steam junction equipment (conjunction equipment).
t). The different oils are recovered at different stages or levels in the distillation column. In the upper part of the column, a gaseous oil is recovered after its concentration, which is neutralized together with some non-concentrating gases to be incinerated.

Vacuum distillation can be carried out at the same time as the treatment with activated clay, in which the clay also acts as a catalyst, although it also has an adsorption function.

Depending on the technique used or combined, vacuum distillation can be carried out before or after the steps of neutralization and treatment with activated clay.

The purpose of the filtration is to separate the activated clay containing the adsorbed contaminants from this recycled oil in order to obtain a basic oil.

Regeneration, the final step in this recycling process, is based on the fact that some oils for the automotive industry have gradually increased the amount of organometallic additives, thereby requiring large amounts of sulfuric acid. I have to. Therefore, several regeneration steps have been developed to significantly reduce this acid consumption.

Thermal regeneration, carried out under conditions of tightly controlled time and temperature range, leads to the decomposition of said additives, making the removal of metals easier.

After the decanting step and before the atmospheric distillation step,
Centrifugation performed at the beginning of the recycle process at a temperature in the range of 50-60 ° C removes salt dissolved water, carbon deposits and a considerable amount of insoluble precipitates.

The above-mentioned method, namely the acid / clay method for recycling used or impure oils (one of the most used methods at present), has drawbacks, the main reason being serious economic The formation of what is called an acid effluent that causes problems and ecological problems.

Solvent extraction, distillation / clay, distillation / hydrogenation, and wiped film evaporator developed by the French Oil Institute.
aporator) and some other studied methods (although some of these, especially those that do not use sulfuric acid, do not lead to the formation of acid effluent), they have other drawbacks, For example, there is the disadvantage of the need for industrial equipment, which results in these methods not only being economical but also technically inadequate (in most cases very skilled professionals). Needless to say, there are problems associated with building factories that require the existence of.

Therefore, it is an object of the present invention to satisfy the needs and requirements of both technicians and ecologists, which means that, especially in both, mankind is constantly improving what is unknown. This is due to the fact that they have taken on new challenges. In this sense, humans have spent most of their time discovering new technologies and improving existing ones throughout Earth's history. Its purpose is to improve its way of engaging humanity in productive activities, as an executive and commander in the process of evolution.

This characteristic exclusively for humanity should also be present in this important technical field in the recycling of used materials, for recycling and recovering used or contaminated mineral oils.

With this in mind, the inventor has, for the purpose of making a viable and economical solution to the problem, strictly comply with all the requirements laid down in various specific legislations. The method of the present invention for recycling the produced mineral oil has been developed.

Since the method according to the invention is reduced to only two steps and eventually to a single step, it is very simple compared to the previously described eight steps of the known prior art method: It also makes it easy to recycle used or contaminated oil without the need for any special equipment or elaborate techniques, and the processing time is less than the normal processing time required by the acid / clay process. It is distinguished by the fact that it has been shortened to 1/3 and therefore brings significant technical advantages.

From an economic point of view, the advantages afforded by the method according to the invention are clear, and at the same time, from an ecological point of view, the method of the invention does not form acidic wastes, and thus ecologists It will be pointed out that the important technological advances we have dreamed of have been achieved.

Furthermore, the product obtained from the recycling process according to the invention, commonly referred to as a filter cake, which has hitherto been discarded, is used as a raw material for the production of other products such as carbon black. Thus, it has an important practical application. It can also facilitate the substitution of mineral and / or vegetable charcoal, firewood or other fuels as an energy source. Although this end use is virtually limitless, its use after burning and crushing the filter cake has a high content of manganese, sulfur and other products, which makes it difficult to filter and filter rubber for rubber in tire manufacturing. It can be extended to applications such as nutrients for agricultural purposes.

In particular, the method for recycling spent or contaminated lubricating oil according to the present invention is:
Pumping a fixed amount of used or contaminated lubricating oil into the autoclave reactor; about 15% cleaning clay,
Fuller's earth, montimolinote or bentonite is added; about 1-2% water containing active sulfur-based catalyst diluted therein; and about 2% filter aid. Add an agent, eg diatomaceous earth;
It consists of

When these ingredients are added, the first step of the process of the present invention is to heat the material to a predetermined first temperature in the range of 100 to 150 ° C. for about 3 hours, followed by a temperature range of 300 to 300 ° C. 2 more up to a given second temperature in the range of 320 ° C
It consists of raising the temperature for an hour. Here, this temperature range varies according to the type of used or contaminated oil in the recycling operation. After heating the material for about 5 hours, the next step is to permanently inject steam under a certain pressure varying from 6 kg / cm ³ to 10 kg / cm ³ and occasionally apply a vacuum of 550 mmHg to the material. Is a step of distilling at a high temperature. Here, the distillation lasts about 3 hours until the catalytic treatment of the treated product and the adjustment of the ignition point of the product are completely completed.
In this step, to test the product, the material is thermally treated and some samples are taken for laboratory measurements.

By measuring the material recovered from the pressure filter, it is possible to prove that all the waste carbon present in the burned oil has been transferred to the filter cake.

This measurement concludes the first step of the method of the invention, at which time it is possible to continue the method by carrying out the second step of the method. This second step is sometimes not necessary. However, it is not preferred to omit this second step, since further processing of the final product can be achieved in the second step. The second step consists of another amount of clarifying clay (although a smaller amount of 8-10% is used at this time) and the catalyst (0.4%) dissolved in water and a filtration means ( 1%) to the product of the first step. The product is the same as previously used or contaminated.

After that, the Brazilian Rule
To adjust the product specifications to CNP 16/81, the product is reheated for about 2 hours and some samples are taken for laboratory measurements. 6 kg during this process
Permanent injection of steam under a certain pressure varying from / cm ³ to 10 kg / cm ³ and eventually a vacuum of 550 mmHg is adopted. After demonstrating the product, it is pumped to a pressure filter and stored for commercialization.

As can be readily seen from the above specification, the method of recycling used or contaminated lubricating oils developed by the Applicant does not produce so-called acid waste derived from previously known techniques. Therefore, this method is new and deserves the protection of law with respect to its protection and exclusive use.

Claims (2)

[Claims] 1. A method of recycling used or contaminated lubricating oil, comprising the steps of: pumping a quantity of used or contaminated lubricating oil into an autoclave reaction vessel; clarified clay. , Fuller type soil, montimolinote or bentonite about 15%,
Add about 1-2% of water in which the active sulfur-based catalyst is diluted, and about 2% of a filter aid such as diatomaceous earth; add such material to a first predetermined range of 100-150 ° C. Heat to temperature for about 3 hours, then increase the temperature range to 300
Heated to a second predetermined temperature of ~ 320 ° C and heated for a further 2 hours, the temperature range varying depending on the type of oil used or contaminated in the recycling operation;
Continuously injecting steam under a pressure varying in the range of kg / cm ³ and distilling such material at a high temperature while sometimes applying a reduced pressure of 550 mmHg, the distillation is carried out by contact treatment and ignition point (brightness point). The conditioning lasts about 3 hours until complete completion; thermal treatment of such material while taking several samples for laboratory testing to test if the product is ready for filtration. It was possible to confirm that all the carbon waste present in the burned oil had been transferred to the filter cake by testing the material recovered from the pressure filter, where Proceeding to a second step, which may or may not be necessary; 2. A method of reusing used or contaminated lubricating oil, the method comprising the steps of:
Add 10% purified clay, 0.4% catalyst dissolved in water and 1% filtration means to the product of the first step; a number for laboratory tests to adjust the technical details of the product. The product was reheated for about 2 hours while taking a sample of the seed, and such distillation was carried out by continuously injecting steam under a pressure in the range of 6 to 10 kg / cm ³ , and occasionally applying a reduced pressure of 550 mmHg at a high temperature. Carrying out; pumping the product into a pressure filter and storing it for commercial sale after approval;