Polyether type heteropolyacid temperature control ionic liquid for removing basic nitrides of gasoline and diesel oil and preparation method thereof

A heteropolyacid anion, ionic liquid technology, applied in the treatment of hydrocarbon oil, refined hydrocarbon oil, petroleum industry, etc., can solve the problems of complex adsorption denitrification operation process, large amount of adsorbent, low degree of automation, etc. The effect of separation, efficient removal and loss reduction

Pending Publication Date: 2021-12-07
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the adsorption denitrification operation process is relatively complicated, the degree of automation is low, and the yield of refined oil is low; the adsorbent needs to be regenerated, otherwise the amount of adsorbent will be large

Method used

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  • Polyether type heteropolyacid temperature control ionic liquid for removing basic nitrides of gasoline and diesel oil and preparation method thereof
  • Polyether type heteropolyacid temperature control ionic liquid for removing basic nitrides of gasoline and diesel oil and preparation method thereof
  • Polyether type heteropolyacid temperature control ionic liquid for removing basic nitrides of gasoline and diesel oil and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Synthesis of polyether-type heteropolyacid temperature-controlled ionic liquid

[0035]Add 0.1mol of 1,1,3,3-tetramethylguanidine (cationic liquid) and 20mL of ethanol into the autoclave, place it in the refrigerator for 12 hours, weigh 35mL of ethylene oxide and add it to the autoclave , seal the kettle, and replace the air in the kettle with nitrogen at a pressure of 3.5 MPa for 3 times. Stir and react in a water bath at 30°C for 2 hours, then raise the temperature to 70°C for 6-10 hours, lower the temperature, release the pressure, and open the kettle. The reaction solution was distilled off absolute ethanol in a round-necked flask to constant weight to obtain intermediate I, and the average degree of polymerization n was calculated according to the product weight gain method (see Table 1). Add 0.1mol of 1,3-propane sultone into the autoclave, add 30mL of ethyl acetate to dissolve it completely, add intermediate I dropwise in a water bath at 30°C according to th...

Embodiment 2

[0051] (1) Synthesis of polyether-type heteropolyacid temperature-controlled ionic liquid

[0052] As shown in Table 1, this embodiment is the same as that of Embodiment 1 except for the volume addition of cationic liquid and ethylene oxide. The specific reaction process is:

[0053]

[0054] (2) Removal of basic nitrogen compounds in simulated gasoline and diesel oil

[0055] a) Add 1 g of ionic liquid denitrification agent (n=11) to a reaction flask equipped with magnetic stirring, then add 40 g of the gasoline and diesel simulative oil (1:40) configured in Example 1, seal it, heat it in a water bath and carry out Stir magnetically and react at 50°C for 10 minutes. Stand and separate at room temperature, the upper liquid phase is the gasoline and diesel simulated oil phase after denitrification, the lower layer is the temperature-controlled ionic liquid phase, and the upper simulated oil phase is collected. Quantitative analysis was carried out by gas chromatography, a...

Embodiment 3

[0062] (1) Synthesis of polyether-type heteropolyacid temperature-controlled ionic liquid

[0063] As shown in Table 1, this embodiment is the same as that of Embodiment 1 except for the volume addition of cationic liquid and ethylene oxide.

[0064] (2) Removal of basic nitrogen compounds in simulated gasoline and diesel oil

[0065] a) Add 1 g of ionic liquid denitrification agent (n=49) to a reaction flask equipped with magnetic stirring, then add 30 g of the gasoline and diesel simulant oil (1:30) configured in Example 1, seal it, heat it in a water bath and carry out Stir magnetically and react at 50°C for 20 minutes. Stand and separate at room temperature, the upper liquid phase is the gasoline and diesel simulated oil phase after denitrification, the lower layer is the temperature-controlled ionic liquid phase, and the upper simulated oil phase is collected. Quantitative analysis was carried out by gas chromatography, and the content of basic nitrogen compounds before...

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Abstract

The invention discloses a polyether type heteropolyacid temperature control ionic liquid for removing basic nitrides of gasoline and diesel oil and a preparation method thereof. The temperature control ionic liquid is composed of a polyether group with temperature response capability, a cation skeleton with a strong acidic functional group and heteropolyacid anions. The method comprises the following steps: reacting cationic liquid with ethylene oxide in an inert atmosphere to generate an intermediate I, reacting the intermediate I with 1,3-propane sultone according to a molar ratio of 1:1 to generate an intermediate II, slowly dropwise adding a heteropolyacid aqueous solution into the intermediate II, and performing reacting at 80-85 DEG C for 10-12 hours to obtain the polyether type heteropolyacid temperature control ionic liquid. The acidity of the ionic liquid is regulated and controlled by introducing an acidic group and heteropoly acid, the melting point of the ionic liquid is reduced by introducing polyether groups with different polymerization degrees, the ionic liquid with stable properties is obtained, and the purposes of high-temperature homogeneous reaction and low-temperature two-phase separation are achieved by regulating and controlling solubility response of the polyether type ionic liquid in gasoline and diesel oil.

Description

technical field [0001] The invention belongs to the field of denitrification of oil products, and in particular relates to a polyether type heteropolyacid temperature-controlled ionic liquid for removing basic nitrogen compounds from gasoline and diesel and a preparation method thereof. Background technique [0002] The efficient separation of high value-added compounds in complex systems is one of the important research directions in chemical engineering, and the great challenge comes from the separation of complex systems. Organic nitrogen compounds are one of the high value-added components of complex systems, and they play an extremely important role in people's production and life. Industrially, organic nitrogen compounds are mainly derived from petroleum and coal-based products, among which basic nitrogen compounds include pyridine, aniline, quinoline, etc. and their derivatives. In addition, trace amounts of organic nitrogen compounds also exist in fuel oil products ...

Claims

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Application Information

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IPC IPC(8): C08G65/26C08G65/328C08G65/334C08G65/338C10G21/22
CPCC08G65/328C08G65/3346C08G65/338C08G65/263C08G65/2624C10G21/22C10G2300/202C10G2400/02C10G2400/04
Inventor 张连正李方方徐冬梅高军马艺心赵萍萍
Owner SHANDONG UNIV OF SCI & TECH
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