KR19990044760A - Method for Purifying Waste Organic Solvent or Kerosene - Google Patents

Abstract

(Objective) It aims to provide a technique for removing impurities dissolved and dispersed in waste organic solvents or kerosene.

(Composition) After repeating the step of adding the inorganic acid to the waste organic solvent or kerosene and stirring for a predetermined time, and then repeat the step of washing with water and then oxidizing, bleaching solution to oxidize, bleaching and then alkaline aqueous solution After passing through the step of neutralization, water is added and washed with water, and then the organic solvent or kerosene is purified by adding a desiccant to dehydration.

Description

Method for Purifying Waste Organic Solvent or Kerosene

The present invention relates to a method for purifying waste organic solvent or kerosene generated from an existing industrial degreasing agent and detergent, laundry detergent for clothes, and the like.

Conventionally, waste organic solvents have been recovered by filtration, distillation, etc., or added to existing low-quality fuel for recycling, incineration or landfill.

This method has the following problems.

① In case of filtration method, impurity removal is not perfect, so it could not be applied to the first use as an organic solvent and lacks economic efficiency due to high treatment cost for filtration and adsorbent.

② Distillation is difficult to purify high-purity, high risk and high cost of energy is also economical.

③ By treating expensive organic solvents by incineration or landfill, waste of resources and secondary pollution are caused.

(4) The method of adding recycled fuel to low-quality fuels is also the most desirable method, but faces the unfortunate situation of processing expensive organic solvents cheaply due to lack of recycling technology.

In addition to the above problems, the seriousness of environmental pollution due to the high cost of waste disposal and the frequent illegal treatment of waste disposal companies is increasing day by day.

Most of these industrial waste organic solvents are used as degreasing and cleaning agents, and the main industries include fatty or mineral substances used in the electrical, electronic parts, metals, machinery, precision machine parts, optical machines, medical machines, and garment laundry industries. It is an organic solvent contaminated with waste products and impurities mainly containing oils.

Most of these waste organic solvents are organic chlorine-based solvents such as PCE, TCE, 111-TCE, MC, etc., and petroleum solvents such as paraffin solvents and aromatic solvents. Of these, organic chlorine solvents are the cause of ozone depletion. In March 1985, the VIN Treaty and the Montreal Protocol in September 87 regulated their use globally. Although it is regulated, there is no substitute material, so the intensity of regulation is weak. In the meantime, it is gradually replaced by general petroleum-based organic solvents, and in some cases low-pollution organic chlorine-based solvents have been developed and supplied, but chlorine-based organic solvents are still the mainstream. However, after using any type of solvent, the problem of treatment remains a big concern, and economic and practical technologies for these organic solvents have not been developed at home and abroad. It is requested.

In order to solve the above problems, an object of the present invention is to provide a technique for removing impurities dissolved and dispersed in all waste organic solvents or kerosene.

The present invention, in order to solve the above problems, by adding an inorganic acid to the waste organic solvent, and then vigorously stirred to oxidize or hydrolyze the impurities dissolved and dispersed in the waste organic solvent, solubilized, separated, removed and washed with general water Remove any remaining inorganic acids and impurities. At this time, in the process of washing with water, an oxidation bleach such as peroxide or chlorate such as hydrogen peroxide and alkaline aqueous solution are respectively oxidized or bleached and neutralized to further remove impurities. Finally, the waste organic solvent is purified by removing the moisture by adding or passing the desiccant.

(Embodiment of Detailed Invention)

More detailed description is as follows.

Inorganic acids, such as phosphoric acid, sulfuric acid, nitric acid, etc., may be used in hydrophobic solvents such as organic solvents such as organic chlorine, petroleum, paraffin, and aromatic solvents. 1 to 15% by volume is added to the waste organic solvent and the mixture is strongly stirred to oxidize or hydrolyze the impurities dissolved and dispersed in the waste organic solvent and the impurities contained in the new solvent before use. Phase to remove. This method is repeated one or more times.

After repeated washing with water at least one time, phase separation of the residual inorganic acid and the water layer containing impurities, followed by removal of one kind of oxidation, bleaching agents, such as hydrogen peroxide or hypochlorous acid or chloric acid and their sodium or potassium salt. It is made into a 10% aqueous solution and 5 to 20% by volume of the waste organic solvent is oxidized, bleached, and removed.Then, water washing is repeated one or more times with ordinary water, followed by alkaline aqueous solution such as sodium carbonate, potassium carbonate and calcium hydroxide. , Sodium hydroxide, potassium hydroxide and the like are made into 1 to 10% aqueous solution, neutralized by adding 5 to 20% by volume to the waste organic solvent, and washed with water several times. Finally, a desiccant such as calcium chloride, calcium oxide, magnesium oxide, potassium carbonate, barium oxide, magnesium sulfate, sodium sulfate, barium oxide, molecular sieve 4Å is immersed in the purified organic solvent or filled with a tube Pass through to remove moisture to complete purification.

For example, it will be described in detail as follows. However, this embodiment does not limit the present invention. (The component content unit of the example is "L (volume%)", and the comparative example does not have a conventional method similar to the present invention, and thus the comparison is omitted.

Example 1

(1) Add 2 liters of phosphoric acid (85%) to 100 liters of the waste organic solvent (slightly viscous liquid with a dark brown unpleasant odor) from the degreasing and washing process, and stir vigorously for 30 minutes to remove impurities in the waste organic solvent. After repeating three times,

② After repeating the process of washing twice with strong stirring for 10 minutes by adding 20 liters of general water,

③ Add 5ℓ of hydrogen peroxide (10%) solution and stir vigorously for 20 minutes to oxidize, bleach and remove residual impurities.

④ Add 10 liters of aqueous sodium carbonate solution (10%) and neutralize by stirring vigorously for 20 minutes,

⑤ After repeating the process of washing twice with strong stirring for 10 minutes by adding 20 liters of general water,

⑥ After 10 kg of dry calcium chloride was added to this solution, the water in the solvent was sufficiently removed (if the water was removed sufficiently, the solvent became clear and transparent), and the purification of the waste organic solvent was completed to recover 95 liter of the refined oil.

Results: There was no unpleasant odor like the new solvent, clear clarity and low viscosity like water, and 95 liter of organic solvent with 0.3% water content was obtained.

(It is observed visually that transparency, smell and viscosity are better than original solvent.)

Example 2

In Example 1, 10 liters of nitric acid (70%) was substituted for 2 liters of phosphoric acid, and potassium hydroxide (1%) solution was substituted for sodium carbonate solution (10%) as a neutralizing agent, and Molecular Sieve 4 건조 was used as a desiccant instead of calcium chloride. The same procedure as in Example 1 was performed except for the above.

Results: The same result as in Example 1 was obtained. 93 L of an organic solvent having a water content of 0.1% was recovered.

Example 3

In Example 1, replace kerosene (petroleum) instead of waste organic solvent, replace 15 liters of sulfuric acid (98%) instead of 2 liters of phosphoric acid (85%) and repeat twice instead of three repeated acid treatment, hydrogen peroxide (10%) It carried out similarly to Example 1 except having replaced 15 L of sodium hypochlorite solutions (3%) instead of 5 L of solutions.

Table 1

Test Item Sample Sulfur Powder (PPM) Color (say bolt) Aniline point (℃) Flash Point (° C) (C.O.C) Specific gravity (15/4) Odor (Oil) moisture(%) Example 3 0.3 +29 62.5 52 0.7960 About 10% 0.17 Commercial kerosene 10.0 +30 55.0 45 0.7990 100% 0.64 Test Methods KS M 2027 KS M 2029 KS M 2053 KS M 2010 KS M 2002 Sensory examination Moisture Meter

Example 4

In Example 1, it carried out similarly to Example 1 except having replaced the waste organic chlorine-type solvent instead of the waste organic solvent.

Example 5

In Example 1, it carried out similarly to Example 1 except having replaced the waste oil solvent instead of the waste organic solvent.

Example 6

In Example 1, it carried out similarly to Example 1 except having replaced the waste paraffinic solvent instead of the waste organic solvent.

Example 7

In Example 1, it carried out similarly to Example 1 except having replaced the waste aromatic solvent instead of the waste organic solvent.

Example 8

In Example 1, it carried out similarly to Example 1 except having replaced the barium oxide instead of calcium chloride.

Example 9

In Example 1, it carried out similarly to Example 1 except having replaced magnesium oxide instead of calcium chloride.

Example 10

In Example 1, it carried out similarly to Example 1 except having replaced potassium carbonate instead of calcium chloride.

Example 11

In Example 1, it carried out similarly to Example 1 except having replaced barium oxide instead of calcium chloride.

Example 12

In Example 1, it carried out similarly to Example 1 except having replaced magnesium sulfate instead of calcium chloride.

Example 13

It carried out similarly to Example 1 except having replaced sodium sulfate instead of calcium chloride in Example 1.

Example 14

The same procedure as in Example 1 was carried out except that sodium chlorate was replaced with hydrogen peroxide in Example 1.

Example 15

In Example 1, it carried out similarly to Example 1 except having replaced potassium hypochlorite instead of hydrogen peroxide water.

Example 16

In Example 1, it carried out similarly to Example 1 except having replaced potassium carbonate instead of sodium carbonate.

Example 17

It carried out similarly to Example 1 except having replaced sodium hydroxide instead of sodium carbonate in Example 1.

Compared with Example 3 using general petroleum as a comparative example, the sulfur content was reduced by more than 97%, the color became clearer, the flash point and the aniline point were increased, and the safety was increased. In particular, the water content was reduced by more than 70%. In addition, the odor of petroleum is reduced to almost unnoticeable, and thus, the product of the present invention shows a much better effect than the existing product.

In addition, the waste organic solvent is a slightly viscous liquid having a dark brown unpleasant odor, and as shown in Examples 1 and 2, the waste organic solvent can be recovered by the purification method of the present invention, and also prevents secondary pollution. There is an excellent effect that can be done.

Claims (6)

After repeating the step of adding the inorganic acid to the waste organic solvent or kerosene and stirring for a predetermined time, repeating the step of washing with water and then oxidizing and bleaching with oxidizing and bleaching solution, and then adding alkaline aqueous solution After the step of neutralizing, water is added to the water washing and then a drying agent is put into the dehydration method of the waste organic solvent or kerosene characterized in that it is made. The method of claim 1, wherein the waste organic solvent is a waste organic chlorine solvent, a waste petroleum solvent, a waste paraffinic solvent, a waste aromatic solvent, or a mixture thereof. The method for purifying waste organic solvent or kerosene according to claim 1, wherein the inorganic acid is selected from phosphoric acid, nitric acid and sulfuric acid, and the amount thereof is 2 to 15% by volume. The method of claim 1, wherein the desiccant is selected from calcium chloride, calcium oxide, magnesium oxide, potassium carbonate, barium oxide, magnesium sulfate, sodium sulfate, and molecular sieves. The waste organic acid according to claim 1, wherein the oxidizing and bleaching solution is hydrogen peroxide or hypochlorous acid or chloric acid and their sodium or potassium salts, each having 5 to 20 volumes of an aqueous solution of 1 to 10% by volume. Method of making kerosene or kerosene. The waste organic solvent or kerosene according to claim 1, wherein the alkaline aqueous solution is one of sodium carbonate, potassium carbonate, potassium hydroxide, and sodium hydroxide, and each of 1 to 10% by volume aqueous solution is 5 to 20% by volume. Purification method.