CN113522182A - A kind of preparation method of waste oil collector for low-rank coal flotation - Google Patents
A kind of preparation method of waste oil collector for low-rank coal flotation Download PDFInfo
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- CN113522182A CN113522182A CN202110818455.4A CN202110818455A CN113522182A CN 113522182 A CN113522182 A CN 113522182A CN 202110818455 A CN202110818455 A CN 202110818455A CN 113522182 A CN113522182 A CN 113522182A
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- 239000002699 waste material Substances 0.000 title claims abstract description 55
- 239000003245 coal Substances 0.000 title claims abstract description 49
- 238000005188 flotation Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000007789 gas Substances 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 13
- 238000005273 aeration Methods 0.000 claims abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000013049 sediment Substances 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 17
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract 1
- 239000010705 motor oil Substances 0.000 description 34
- 239000010913 used oil Substances 0.000 description 24
- 239000003795 chemical substances by application Substances 0.000 description 21
- 239000003921 oil Substances 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 239000010687 lubricating oil Substances 0.000 description 5
- 150000001335 aliphatic alkanes Chemical group 0.000 description 4
- 239000002283 diesel fuel Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical group CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003250 coal slurry Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000010710 diesel engine oil Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
- B01J10/002—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor carried out in foam, aerosol or bubbles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/008—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0016—Working-up used lubricants to recover useful products ; Cleaning with the use of chemical agents
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Dispersion Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
本发明公开了一种用于低阶煤浮选的废机油捕收剂的制备方法，包括以下步骤：(1)通过臭氧发生器生产氧气、臭氧的混合气体；(2)将步骤(1)得到的混合气体通过加压罐和气泵通入接触反应室内，通过设置在接触反应室内的曝气盘和废机油原料进行接触反应；(3)接触反应完成后，反应后的废机油产品排出，通过滤网滤去固体沉淀物和杂质，得到所述废机油捕收剂。本发明制备的废机油捕收剂具有良好的捕收性和选择性。本发明“变废为宝”有效地将废机油转化为高效低阶煤浮选捕收剂，具有效果好、成本低和污染小的优点，实现了资源的循环利用。
The invention discloses a preparation method of a waste oil collector for low-rank coal flotation, comprising the following steps: (1) producing a mixed gas of oxygen and ozone through an ozone generator; (2) combining step (1) The obtained mixed gas is passed into the contact reaction chamber through a pressurized tank and an air pump, and the contact reaction is carried out through the aeration plate arranged in the contact reaction chamber and the waste oil raw material; (3) after the contact reaction is completed, the reacted waste oil product is discharged, The solid sediment and impurities are filtered out through a filter screen to obtain the waste oil collector. The waste oil collector prepared by the invention has good collection performance and selectivity. The invention "turns waste into treasure" effectively converts waste oil into a high-efficiency low-rank coal flotation collector, has the advantages of good effect, low cost and low pollution, and realizes the recycling of resources.
Description
Technical Field
The invention belongs to the technical field of mineral flotation, and relates to a preparation method of a used oil collecting agent for low-rank coal flotation.
Background
Coal is the main energy source in China, accounts for 60-70% of the total energy consumption in China in an energy structure of nearly 10 years, and is the main energy source for the current development in China. The efficient clean utilization of coal is the current foot point of energy development in China, and the status of the coal as a main energy source cannot be changed for a long time. The low rank coal resource occupies about half of the reserves of the coal resources in China. The low-rank coal has low coalification degree and rich surface oxygen-containing functional groups. For coal slime of low-rank coal, the conventional flotation method and flotation collector have low efficiency and poor benefit. The search for the flotation collector of the high-efficiency coal slime is one of effective methods for improving the treatment capacity of the low-rank coal and cleanly producing the high-quality low-rank coal.
The used oil is one of the used lubricating oils, and is a dangerous waste regulated by the state. In 2018, the consumption of the lubricating oil in China is about 880 ten thousand tons, and according to the estimation of the elimination rate of the lubricating oil in China of 60 percent, in China, about 490 ten thousand tons of waste lubricating oil are generated every year. 167 thousands of cars are disassembled and recovered in 2018, 89.5 thousands of cars are disassembled and recovered in the first half of 2019, and the car disassembling industry in China can produce a large amount of waste engine oil every year. The waste engine oil is polluted by high-temperature and high-pressure oxidation, thermal decomposition and impurities in a mechanical motion working environment, and the physicochemical properties of the waste engine oil reach respective oil change standards, so that the waste engine oil becomes a harmful pollutant oil.
Coal slime flotation is to separate coal from impurities by utilizing the difference of the surface hydrophobicity of the coal and gangue, and the addition of a collecting agent plays a crucial role in the process. The collecting agent selectively acts on the surface of coal through physical or chemical adsorption, and the surface hydrophobicity difference between the coal and gangue is improved. The coal adsorbing the collecting agent is easier to adhere to the bubbles, so that the separation of the coal and the gangue can be completed. The selectivity and the collector performance of the collector are two important indexes for measuring the performance of the collector. Coal is heterogeneous organic matter, and the lower the coalification degree, the more alkane side chains and oxygen-containing functional groups are on the surface of the coal. Therefore, the collector is preferably a reasonably composed mixture of various nonpolar hydrocarbon oils. The oxygen-containing functional groups on the surface of the low-rank coal are rich in impurities, so that the effect of using the oxygen-containing organic oil as the collecting agent is better. The waste engine oil can strengthen the flotation effect of the low-rank coal to a certain extent. The used oil is mainly composed of a large amount of aromatic hydrocarbon components and alkane components. The proportion of the oxidation substances such as carboxylic acid, ester, ketone, alcohol and the like is reported to be lower and less than 20 percent. The waste engine oil has high content of heavy metal ions, mechanical impurities and solid impurities, and the environment can be polluted by directly using the waste engine oil as a flotation collector.
The waste engine oil is deeply oxidized by a controllable oxidation method, so that the content of various oxygen-containing organic matters can be improved, and the performance of the waste engine oil as a low-rank coal flotation collector is further enhanced; various metal ions and solid impurities in the waste engine oil form precipitates under the oxidation reaction, so that the precipitates can be separated from the waste engine oil more easily, and the pollution of the waste engine oil is reduced.
Disclosure of Invention
The invention aims to provide a preparation method of a used oil collecting agent for low-rank coal flotation, which is used for reducing the pollution degree of used oil and enhancing the effect of the used oil in the application of the low-rank coal collecting agent. Aiming at waste engine oil and waste lubricating oil, ozone is used for carrying out controllable deep oxidation on oil, and the components of the waste oil are improved.
A preparation method of a used oil collector for low-rank coal flotation comprises the following steps:
(1) producing mixed gas of oxygen and ozone by an ozone generator;
(2) introducing the mixed gas obtained in the step (1) into a contact reaction chamber through a pressurizing tank and an air pump, and carrying out contact reaction on the mixed gas and the waste oil raw material through an aeration disc arranged in the contact reaction chamber;
(3) and after the contact reaction is finished, discharging the reacted waste engine oil product, and filtering out solid precipitates and impurities through a filter screen to obtain the waste engine oil collecting agent.
Further, in the step (1), the concentration of ozone in the ozone generator is monitored in real time through an ultraviolet light analyzer and a gas flowmeter, and the concentration of ozone is controlled to be 20-50 mg/L.
Furthermore, in the step (2), 1.0-1.5kg/h of ozone is correspondingly used for each 1kg of used oil raw material, and the contact reaction time is 3-5 h.
Further, in the step (2), during the contact reaction, stirring is performed by a ribbon stirrer.
Further, in the step (2), the content of ozone overflowing from the contact reaction chamber is monitored by an ultraviolet light analyzer, and when the concentration of the overflowing ozone is higher than 10-20mg/L, the overflowing gas is circulated and refilled into the contact reaction chamber; when the concentration of the overflowed ozone is lower than 10mg/L and the reaction time is longer than 3h, the overflowed gas is treated as tail gas.
Furthermore, the aperture of the aeration discs is 10-40 μm, and the aeration discs are uniformly distributed on the bottom and the side wall of the contact reaction chamber.
Furthermore, the lining of the contact reaction chamber is made of polytetrafluoroethylene material.
Furthermore, the aperture of the filter screen is 200-400 meshes, and 1-2 channels are arranged on the filter screen.
The invention has the beneficial effects that: the improved collecting agent is waste engine oil, and is a secondary utilization of waste resources; compared with the traditional collecting agents such as kerosene, diesel oil and the like, the waste engine oil has better flotation effect and lower economic cost. In the composition of the waste engine oil oxidized by ozone, long-chain alkane and cyclane can interact with the side chain of organic alkane on the surface of coal; the functional groups of aldehyde, ketone, carboxylic acid and alcohol formed by oxidation can react with the oxygen-containing functional groups on the surface of the coal. The organic matter composition of the used oil collecting agent produced by the method is complex, so that the method has good collecting property and selectivity on heterogeneous coal. Heavy metal ions and solid impurities in the waste engine oil are easy to coalesce to form solid precipitates after the strong oxidation of ozone, and the pollution of the waste engine oil can be reduced through subsequent filtering removal.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
As shown in figure 1, the device used in the preparation method of the used oil collecting agent for low-rank coal flotation comprises an ozone generator and a contact reaction chamber, wherein an aeration disc is arranged in the contact reaction chamber, an outlet of the ozone generator is connected with the aeration disc through a pressurizing tank and an air pump, a used oil raw material inlet and a tail gas discharge outlet are arranged at the upper part of the contact reaction chamber, a product outlet is arranged at the lower part of the contact reaction chamber, and the product outlet is connected with a filter screen. The ozone generator is provided with a first flowmeter and a first ultraviolet light analyzer, and the contact reaction chamber is provided with a second flowmeter and a second ultraviolet light analyzer. The contact reaction chamber is internally provided with a helical ribbon stirrer, and the lining of the contact reaction chamber is made of polytetrafluoroethylene material.
Wherein the aperture of the aeration discs is 10-40 μm, and the aeration discs are uniformly distributed on the bottom and the side wall of the contact reaction chamber. The aperture of the filter screen is 200-400 meshes, and 1-2 channels are arranged on the filter screen.
The present invention will be further described with reference to the following examples.
Example 1
Used oil and diesel and motor oil were sampled from petrol stations (brand 5W 50). And (3) preparing a collecting agent from the waste engine oil sample. Preparing mixed gas of oxygen and ozone by using an ozone generator, monitoring and controlling the concentration of the ozone to be 30mg/L by using an ultraviolet analyzer, introducing the mixed gas into an aeration disc with the aperture of 40 mu m through a pressurizing tank and a gas pump, introducing the mixed gas into a contact reaction chamber to react with the waste engine oil raw material, stirring the mixed gas in the contact reaction chamber by using a spiral belt type stirrer, controlling the reaction time to be 3 hours, and using 1.0kg/h of ozone for every 1kg of the waste engine oil raw material. The ozone content overflowing from the contact reaction column was monitored using an ultraviolet light analyzer. And after the reaction is finished, the waste engine oil after the reaction passes through a 1-channel 200-mesh filter screen. And after filtering, obtaining the used oil collecting agent.
And filtering the used oil and the used oil collecting agent obtained after the used oil is treated by the method by using slow-speed qualitative filter paper, and measuring the solid content. 10ml of each of the two oil samples were diluted in n-pentane, filtered, dried and weighed for solids content. After the used engine oil is filtered, the solid residue is 8.5 mg; the residual solid amount of the used oil collecting agent treated by the method is 2.4 mg. The content of solid contaminants is greatly reduced.
The dynamic viscosity of the engine oil, the waste engine oil and the waste engine oil collector prepared by the method is measured by using a viscometer. The test conditions and results are listed in table 1.
The waste engine oil, diesel oil, engine oil and the collector prepared by the invention are subjected to laboratory flotation tests of low-rank coal (lignite). The concentration of the flotation coal slurry is 100 g/L. The collector dose was 5 kg/t. The air bubble agent is secondary octanol, and the dosage is 600 g/t. And respectively filtering the obtained flotation clean coal and tail coal, drying, weighing and measuring ash. The test conditions and results are listed in table 2.
TABLE 1
| Sample number | Name of medicament | Dynamic viscosity mPa. multidot.s (25 ℃ C.) |
| 1 | Engine oil | 182.44 |
| 2 | Diesel oil | 6.52 |
| 3 | Waste engine oil | 118.46 |
| 4 | Treated used oil | 85.05 |
TABLE 2
Table 1 shows that the method effectively reduces the dynamic viscosity of the used oil, and shows that the contents of components such as colloid and solid in the used oil are reduced, and the dispersing performance is improved. As can be seen from table 2, the preparation method of the used oil collecting agent provided by the invention can effectively improve the ability of the used oil to recover low-rank coal, and improve the collecting property and selectivity of the used oil. The waste engine oil treated by the method is used as a collecting agent, and compared with the traditional hydrocarbon oil collecting agent and untreated waste engine oil, the yield of clean coal products of low-rank coal is higher, and ash content is lower.
The above description is only a part of the embodiments of the present invention, and not intended to limit the present invention, and it will be apparent to those skilled in the art that several modifications and variations can be made without departing from the principle of the present invention, and these modifications and variations should be construed as the protection scope of the present invention.
Claims (8)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110818455.4A CN113522182A (en) | 2021-07-20 | 2021-07-20 | A kind of preparation method of waste oil collector for low-rank coal flotation |
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| CN202110818455.4A CN113522182A (en) | 2021-07-20 | 2021-07-20 | A kind of preparation method of waste oil collector for low-rank coal flotation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116426307A (en) * | 2023-02-23 | 2023-07-14 | 山西新鸿顺能源有限公司 | Refining method of waste mineral oil overhead oil |
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2021
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