KR20180113866A - Ion refining oil manufacturing method - Google Patents

Abstract

The present invention relates to a method for manufacturing ion refined oil. More particularly, the present invention relates to a method for manufacturing ion refined oil comprising the steps of: filtering the waste oil with activated carbon to remove solid matter; reacting the filtered waste oil with a coagulant in a reaction tank so that foreign matters in the waste oil are coagulated; centrifuging the coagulated reacted oil; removing water from the centrifuged reacted oil; and filtering the reacted oil from which moisture is removed by activated carbon, wherein the coagulant is a mixture of ammonium phosphate dibasic, which is the main coagulant, and an inorganic coagulant and an organic coagulant, which are auxiliary coagulants. According to the present invention, ion refined oil of high purity can be manufactured by a simple method, and thus environmental pollution due to waste oil can be prevented and energy recycling can be increased.

Description

ION REFINING OIL MANUFACTURING METHOD [0002]

The present invention relates to a method for producing an ionic purified oil, and more particularly, to a method for producing an ionic purified oil having high purity by subjecting waste oil to coagulation treatment with various flocculants and centrifugation.

Waste oil is based on industries related to the production and distribution of petroleum products such as petrochemical plants, stockpiling bases, and refueling stations, and is used in all industries that handle oil, such as electricity, steel, machinery, .

When such waste oil is discharged without being treated, it seriously pollutes soil, ground water, river, hose, and ocean, and causes environmental pollution problem, resulting in a great socioeconomic loss. Therefore, And the Water Quality and Environment Protection Act.

Therefore, since the waste oil is recycled through purification, the recycled refined oil is largely divided into ion refining oil such as bunker oil regenerated by the ion purification method and pyrolysis oil which is recovered by pyrolysis in the furnace by pyrolysis .

The method for producing the ionic refined oil is a method of separating a metal ion suspended in a waste oil by precipitation using a chemical agent, that is, a coagulant, by making the metal ion suspended in the waste oil an insoluble metal salt with a large specific gravity.

Conventionally, only dibasic ammonium phosphate was used as the coagulant. As such a coagulant, the removal efficiency of the metal salt was limited, and the removal efficiency of the residual carbon was poor due to the waste oil having high viscosity and tensile strength.

In addition, since the use of a single flocculant induces the use of a large amount of coagulant, the unreacted chemical and heavy metal ions after the process react and precipitate in the produced ionic refining oil, thereby causing the production of ionic refining oil having a low purity.

KR 10-2015-0132941 A

Accordingly, an object of the present invention is to prepare a high-purity ion-refined oil by purifying a phenol by a simple method using various flocculants.

In addition, fine aggregate air is injected to increase the removal efficiency of residual carbon.

In order to accomplish the above object, the present invention provides a process for preparing ionic refined oil, comprising the steps of filtering waste oil with activated carbon to remove solid matter, and reacting the filtered waste oil with a coagulant in a reaction tank so that foreign matters in the waste oil are coagulated A step of centrifugally separating the coagulated reaction oil, a step of removing moisture from the centrifuged reaction channel, and a step of filtering the reacted oil from which moisture has been removed with activated charcoal, And ammonium bicarbonate and an inorganic coagulant and an organic coagulant which are auxiliary coagulants.

The flocculant is added to 100 parts by weight of dibasic ammonium phosphate which is the main flocculant, 5 to 10 parts by weight of aluminum sulfate, the first auxiliary flocculant, 5 to 10 parts by weight of ferrous sulfate which is the second flocculent flocculant, And 5 to 10 parts by weight of a polymer flocculant.

Wherein the surfactant is further reacted with the coagulant in the step of reacting the filtered waste oil and the coagulant in the reaction tank so that the foreign matter in the waste oil is coagulated, wherein the surfactant comprises sodium hydroxide and calcium chloride mixed at a ratio of 1: 0.5 to 1.5 .

The method may further include the step of centrifugally separating the reaction fluid in which the foreign matter is agglomerated, followed by mixing the micro-air into the centrifugal reaction oil.

The activated carbon is treated with steam of 0.083 to 0.013 g H ₂ O / g activated carbon at a temperature of 400 to 1000 ° C. for 5 to 10 minutes and then continuously fed at a temperature of 400 to 1000 ° C. in an amount of 0.0085 to 0.015 g NH ₃ / Of ammonia for 10 to 20 minutes.

And filtering the waste oil and the flocculant in the reaction tank so that the foreign substances in the waste oil are flocculated, the foreign substances are flocculated while introducing the fine air into the reaction tank.

According to the present invention, it is possible to produce ion refined oil of high purity by a simple method, and it is possible to prevent environmental pollution due to waste oil and to increase energy recycling.

1 is a view showing a process for producing an ionic purified oil according to the present invention.

Hereinafter, the present invention will be described in detail.

Conventional ionic refining oil generally used only diphosphoric acid ammonium flocculant to aggregate foreign matter in waste oil. However, when only ammonium diphosphate is used, the removal efficiency of the foreign matter is not high and refined oil of high purity can not be produced.

Accordingly, the present invention proposes a method for producing purified oil of high purity by using ammonium phosphate as a main coagulant and using an inorganic coagulant as an auxiliary coagulant together with an organic coagulant to increase the efficiency of removing foreign matter.

More specifically, the method for producing ionic purified oil according to the present invention comprises the steps of purifying and collecting the collected waste oil, filtering the waste oil with activated carbon to remove the solid matter, and reacting the filtered waste oil and the flocculant in the reaction tank A step of centrifugally separating the reaction oil in which the foreign matter is agglomerated, a step of removing moisture from the centrifugally separated reaction channel, a step of filtering the reacted oil from which the moisture has been removed, Wherein the coagulant is a mixture of dibasic ammonium phosphate as a primary coagulant and an inorganic coagulant as an auxiliary coagulant and an organic coagulant.

Hereinafter, the present invention will be described in detail with reference to FIG.

And filtering the waste oil with activated carbon to remove the solid matter.

First, the solids such as sludge in the collected waste oil are removed by filtration with an activated carbon filtration apparatus. The collected waste oil refers to waste oil collected after being used in various industrial sites or everyday life, such as waste lubricating oil, waste fish oil, waste cutting oil, waste abrasive oil, and waste cooking oil. The collected waste oil is mixed with oil, solid matter, moisture, dissolved minerals, residual carbon, metal ions and the like, and when it is filtered with activated carbon, a bulky solids can not pass through the activated carbon but are adsorbed and filtered.

Here, the activated carbon filtration apparatus means a filter filled with a plurality of activated carbons. In this method, waste oil drawn into the activated carbon filtration apparatus passes through the activated carbon layer and then is discharged to the lower portion. Only through the passage between the activated carbons exhibits excellent filtration efficiency. At this time, the particle size of the activated carbon is not limited, but may be in the range of 8 to 40 mesh. Further, it is of course possible to apply the pressure during filtration to pass the waste oil.

The filtered waste oil and coagulant In the reaction tank  Thereby causing the foreign matter in the waste oil to coagulate.

Next, the filtered waste oil is charged into a reaction tank, and a coagulant is added thereto and reacted to cause foreign matters such as dissolved minerals, residual carbon, and metal ions in the waste oil to coagulate. Here, the reaction tank may be equipped with a stirring device, and a high-temperature atmosphere of about 80 to 110 ° C is established through indirect heat, and the reaction is performed for 1 to 2 hours. At this time, the method of supplying the indirect heat is not limited. The reaction is allowed to stand for about 2 to 3 hours for precipitation after the reaction.

The amount of the waste oil and the flocculant to be filtered is preferably about 100: 1 to 3: 1 by weight. If the amount of the coagulant is small, the flocculant is not sufficiently flocculated. When the amount of the flocculant is excessive, Of refined oil can not be produced.

In the present invention, dibasic ammonium phosphate is used as the main coagulant and an inorganic coagulant and an organic coagulant are used as auxiliary coagulants, instead of using only dibasic ammonium which is usually used as the coagulant. More specifically, 5 to 10 parts by weight of aluminum sulfate, a first auxiliary coagulant, 5 to 10 parts by weight of ferrous sulfate, a second auxiliary coagulant, and a second auxiliary coagulant are added to 100 parts by weight of dibasic ammonium phosphate as the main coagulant, And 5 to 10 parts by weight of a cationic organic polymer flocculant as a flocculant. The flocculant is used in combination to increase the removal efficiency of heavy metals and residual carbon.

That is, generally, only one kind or two kinds of coagulants do not sufficiently coagulate, and in the present invention, the coagulation efficiency is increased by using all four coagulants. Here, the coagulant may be used by dissolving it in water as a solvent for an effective reaction, and its use is not limited.

When the foreign matter is agglomerated Reactive oil  Centrifuging step.

Then, the reaction oil in which the foreign matter is agglomerated is centrifuged again to remove the remaining foreign matter, that is, the sludge. The centrifugal separation is also performed according to a conventionally published method, and a detailed description thereof will be omitted.

The centrifuged From the reaction channel  Removing moisture.

Next, the centrifuged reaction oil is put into a water still and is indirectly heated to 100 to 110 ° C to distill water. Here, distilled water and gas are recovered through separate purification and condensation facilities to prevent environmental pollution. At this time, the heating time is not limited.

The water- Reactive oil  Filtration with activated charcoal.

The reacted oil from which the moisture has been removed is filtered again with activated carbon. At this time, the filtration method using the activated carbon is the same as the method described above, and a detailed description thereof will be omitted.

The ion-purified oil purified by the above-described method has an advantage that purity is much higher than that of refined oil which was conventionally treated with only ammonium diphosphate, and since a separate treatment facility is not required, manufacturing cost is low, .

On the other hand, in order to produce ion refined oil of higher purity, in the step of reacting the filtered waste oil and the flocculant in the reaction tank so that the foreign substances in the waste oil are flocculated, a surfactant may be added to the reaction tank together with the flocculant to react .

At this time, as the surfactant, sodium hydroxide and calcium chloride are mixed in a weight ratio of 1: 0.5 to 1.5, more preferably 1: 1, and the amount of the filtered waste oil and the surfactant used in the reaction tank is 100 : 1 to 2 weight ratio.

That is, the surfactant is used to provide an emulsifying force to uniformly disperse the particles of the viscous waste oil into small particles, and various stabilizers (antioxidants, dispersants, etc.) contained in the waste oil prevent the solidification of the generated residues. By treating the surfactant with the flocculant, it is possible to easily flocculate such foreign matter.

Further, the method may further include a step of centrifugally separating the reactant oil in which the foreign matter is agglomerated, followed by the step of mixing fine air into the centrifuged reaction oil.

This is to rapidly remove water during the post-process water removal step by mixing the fine air to lower the viscosity of the centrifugal reaction oil. That is, the reactive oil having a high viscosity and particle tension is not easy to distill water, and thus the water removal efficiency is low as well as the time is long and the efficiency of the process is poor. In the present invention, This disadvantage is solved.

At this time, the fine air is injected by injecting fine air through micropores such as a perforated plate or a punching plate used in the air injection method, and mixing the filtered air with the filtered reaction oil through the gas-liquid mixing means. The size of the fine pores, the amount of air injected, and the like are not limited.

Meanwhile, the activated carbon used in the filtration may be generally used ordinary activated carbon. However, the activated carbon may be treated with steam of 0.083-0.013 g H ₂ O / g activated carbon at a temperature of 400-1000 ° C. for 5-10 minutes, and it is more preferred to use that one for 10 ~ 20 minutes at a rate of 0.0085 ~ 0.015g of ammonia NH ₃ / g of activated carbon at a temperature of 400 ~ 1000 ℃. This is because this treatment effectively improves the adsorption ability of the activated carbon to the residual carbon, thereby helping to produce a high-purity ion-refined oil.

Also, in the step of reacting the filtered waste oil and the flocculant in the reaction tank so that the foreign substances in the waste oil are flocculated, the foreign matter may be flocculated while the fine air is introduced into the reaction tank. This is because the waste oil charged into the reaction tank has a high viscosity, so that the residual carbon can not be easily removed only by the coagulant. Therefore, when the foreign substances are agglomerated while introducing the fine air, it is easy to remove the residual carbon.

Here, as described above, the injection of the fine air suffices to inject fine air through the fine pores. The size of the fine pores, the amount of air injected, and the like are not limited.

The method for producing ionic refined oil of the present invention as described above has an advantage that purified refined oil can be produced with a simple process without requiring a separate manufacturing apparatus and facilities.

In the meantime, although not described in the present invention, it is natural that the above-described process can be performed while controlling the flow rate through a flow rate regulator by continuous purification, so long as it is commonly used in the field to which this technology belongs .

Hereinafter, the present invention will be described in more detail with reference to the accompanying examples.

(Example 1)

100 kg of the waste oil stored in the waste oil storage tank was filtered with an activated carbon filter device to remove the solid matter. Then, 2 kg of the coagulant was added to the filtered waste oil, heated to 80 ° C. by indirect heat, and reacted for 60 minutes while stirring at 200 rpm. The reaction was continued for 30 minutes while stirring at 30 rpm and then settled for 180 minutes. Aluminum sulfate (Al ₂ (SO ₄ ) ₃ .14 to 18H ₂ O: DC Chemical) was added to 100 parts by weight of dibasic ammonium phosphate (Di-Ammonium Phosphate, , 5 parts by weight of ferrous sulfate (FeSO ₄ .7H ₂ O: DC Chemical), and 5 parts by weight of an organic coagulant, Copolymer Acridid and Cationic acrylate (Nalco 855: Nalco Korea).

The sludge was centrifuged by centrifuging at 4000 rpm, and the sludge was removed. Then, the sludge was poured into a water distiller and the water was evaporated at a temperature of 110 ° C for 120 minutes. Next, the moisture removed from the reaction oil was filtered with an activated carbon filter and stored in a storage tank.

(Example 2)

The procedure of Example 1 was repeated,

The sludge was centrifuged by a centrifugal separator to remove fine sludge from the sludge through an air injector, and 0.1 to 0.4 L / l of sludge was removed from the sludge.

(Example 3)

The procedure of Example 1 was repeated,

Fine air was injected into the reaction tank through the air injector as much as 0.1 to 0.4 L / L of filtered waste oil.

(Example 4)

The procedure of Example 1 was repeated,

2 kg of surfactant was added together with the coagulant. Here, as the surfactant, sodium hydroxide and calcium chloride were mixed in a weight ratio of 1: 1.

(Comparative Example 1)

The procedure of Example 1 was repeated,

Only dibasic ammonium phosphate was used as the coagulant.

(Test Example 1)

The quality of the ion-refined oil produced through the above-described Examples and Comparative Examples was evaluated. The results are shown in Table 1, and the evaluation methods are as follows: the petroleum product ash test (KS M ISO 6243: 2003), the petroleum product residual carbon fraction test method (KS M ISO 2017: 2001) Followed by inductively coupled plasma emission spectrometry.

Test Example 1 Results. division Pre-purification waste oil Comparative Example 1 Example 1 Example 2 Example 3 Example 4 Residual carbon (wt%) 2.54 2.47 2.20 2.18 1.25 1.78 Moisture and sediment (vol%) 8.272 1.411 1.235 0.831 1.104 1.213 Ash (wt%) 0.397 0.315 0.041 0.040 0.037 0.036 Pb and its compound (mg / L) 11.25 5.85 1.11 1.03 0.78 0.83

As can be seen from the above Table 1, the ion-purified oil according to the purification method of Examples 1 to 4 according to the present invention has a higher removal rate than that of Comparative Example 1 in all of the residual carbon, ash, water and precipitate, Pb and the compound I can confirm that it is visible.

As compared with Example 1, it was confirmed that the removal efficiency of residual carbon, ash, water, precipitate, Pb and the compounds of Examples 2 to 4, in which fine air was injected or a surfactant was used together, was generally high.

Therefore, according to the present invention, it has been determined that it is possible to produce ion refined oil of high purity.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the scope of the present invention is not limited to the disclosed exemplary embodiments. It will also be appreciated that many modifications and variations will be apparent to those skilled in the art without departing from the scope of the present invention.

Claims (6)

Filtering the waste oil with activated carbon to remove solid matter,
Reacting the filtered waste oil with a flocculant in a reaction tank so that foreign matter in the waste oil is flocculated;
Centrifuging the reaction fluid in which the foreign matter is aggregated,
Removing moisture from the centrifuged reaction channel,
And filtering the reacted oil from which moisture has been removed by activated carbon,
Wherein the coagulant is a mixture of dibasic ammonium phosphate as a primary coagulant and an inorganic coagulant as an auxiliary coagulant and an organic coagulant.
The method according to claim 1,
The flocculant is added to 100 parts by weight of dibasic ammonium phosphate which is the main flocculant, 5 to 10 parts by weight of aluminum sulfate, the first auxiliary flocculant, 5 to 10 parts by weight of ferrous sulfate which is the second flocculent flocculant, And 5 to 10 parts by weight of a polymer flocculating agent is mixed.
3. The method of claim 2,
In the step of reacting the filtered waste oil and the flocculant in a reaction tank so as to cause flocculation of the foreign matter in the waste oil,
Wherein the surfactant is further reacted with the coagulant, wherein the surfactant is a mixture of sodium hydroxide and calcium chloride in a weight ratio of 1: 0.5 to 1.5.
4. The method according to any one of claims 1 to 3,
After the step of centrifuging the reactive oil in which the foreign matters are aggregated,
Further comprising the step of mixing fine air into the centrifugal reaction oil.
The method according to claim 1,
In the activated carbon,
After treatment with steam of 0.083 to 0.013 g H ₂ O / g activated carbon at a temperature of 400 to 1000 ° C. for 5 to 10 minutes, ammonia of 0.0085 to 0.015 g NH ₃ / g activated carbon is continuously added at a temperature of 400 to 1000 ° C., To 20 minutes. ≪ / RTI >
The method according to claim 1,
In the step of reacting the filtered waste oil and the flocculant in a reaction tank so as to cause flocculation of the foreign matter in the waste oil,
So that the foreign matter is agglomerated while introducing fine air into the reaction tank.

Images