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Preparation method and application of magnetic inorganic clay-graphene composite demulsifying material

A graphene composite and graphene technology, applied in the field of inorganic materials, can solve the problems of inability to achieve efficient separation of oil-in-water emulsions, limitations in wide application, and large demulsification dose, and achieve excellent demulsification performance and high cycle stability. The effect of sex, efficient separation

Inactive Publication Date: 2020-01-03
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the amount of M-DM used in the demulsification process is relatively large, so its wide application is limited
[0005] It can be seen that the existing modified inorganic clay materials have many shortcomings in the separation of oil-in-water crude oil emulsions, such as large demulsification dose or inability to achieve efficient separation of oil-in-water emulsions with different pH values.

Method used

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  • Preparation method and application of magnetic inorganic clay-graphene composite demulsifying material
  • Preparation method and application of magnetic inorganic clay-graphene composite demulsifying material
  • Preparation method and application of magnetic inorganic clay-graphene composite demulsifying material

Examples

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Effect test

Embodiment 1

[0032] Example 1 Preparation of a magnetic inorganic clay-graphene composite demulsification material, comprising the following steps:

[0033] (1) Disperse graphene oxide in a polyethyleneimine aqueous solution with a concentration of 0.1 wt%, so that the concentration of graphene oxide in the polyethyleneimine aqueous solution is 0.1 wt%. After standing for 2 hours, it was stirred at 60 °C for 8 hours. After the reaction, suction filtration was performed to obtain product A; product A was successively washed with absolute ethanol and deionized water for several times, and freeze-dried at -40 °C for 24 hours to obtain the product graphene oxide. Complex.

[0034] (2) Disperse ferric chloride hexahydrate in 40 mL of ethylene glycol to make Fe in the mixed solution 3+ Then add 1.0 mol of sodium acetate and 1.5 g of polyethylene glycol to 1 L of the mixed solution in sequence, stir for 60 min, and then disperse 0.1 g of silane coupling agent-modified inorganic clay into the mix...

Embodiment 2

[0040] Example 2 Preparation of a magnetic inorganic clay-graphene composite demulsification material, comprising the following steps:

[0041] (1) Disperse graphene oxide in a polyethyleneimine aqueous solution with a concentration of 0.01 wt%, so that the concentration of graphene oxide in the polyethyleneimine aqueous solution is 0.01 wt%. After standing for 1 hour, it was stirred at 70 °C for 4 hours. After the reaction, suction filtration was performed to obtain product A; product A was successively washed with anhydrous ethanol and deionized water for several times, and freeze-dried at -30 °C for 36 hours to obtain the product graphene oxide. Complex.

[0042] (2) Disperse ferric chloride hexahydrate in 30 mL of ethylene glycol to make Fe in the mixed solution 3+ Then add 1.5 mol of sodium acetate and 1.0 g of polyethylene glycol in sequence to 1 L of the mixed solution, stir for 30 min, and then disperse 0.5 g of the inorganic clay modified by the silane coupling agent...

Embodiment 3

[0048] Example 3 Preparation of a magnetic inorganic clay-graphene composite demulsification material, comprising the following steps:

[0049] (1) Disperse graphene oxide in a polyethyleneimine aqueous solution with a concentration of 0.05wt%, so that the concentration of graphene oxide in the polyethyleneimine aqueous solution is 0.5wt%. After standing for 5 hours, it was stirred at 80 °C for 6 hours. After the reaction was completed, suction filtration was performed to obtain product A; the product A was successively washed with absolute ethanol and deionized water for several times, and freeze-dried at -20 °C for 48 hours to obtain product oxidation. Graphene composites.

[0050] (2) Disperse ferric chloride hexahydrate in 50 mL of ethylene glycol to make Fe in the mixed solution 3+ Then add 0.1mol sodium acetate and 0.5g polyethylene glycol in sequence to 1L mixture, stir for 40min, and then disperse 0.05g silane coupling agent-modified inorganic clay in the mixture, sti...

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Abstract

The invention relates to a preparation method of a magnetic inorganic clay-graphene composite demulsifying material. The preparation method comprises the following steps: (1) dispersing graphene oxidein an aqueous polyethyleneimine solution, standing the obtained solution, stirring the solution, and carrying out suction filtration, washing and freeze drying to obtain a graphene oxide compound; (2) dispersing ferric chloride hexahydrate in ethylene glycol, sequentially adding sodium acetate, polyethylene glycol and silane coupling agent-modified inorganic clay, performing stirring, carrying out a reaction in a reaction kettle, and washing and drying the obtained reaction product to obtain a ferroferric oxide-inorganic clay compound; (3) dispersing the graphene oxide compound in deionized water to obtain a 10-100 mg / L solution; and (4) adding the ferroferric oxide-inorganic clay compound into the solution, and performing stirring, washing and drying to obtain the magnetic inorganic clay-graphene composite demulsifying material. The invention also discloses a separation application of the material in an oil-in-water crude oil emulsion. The method has the advantages of simplicity, andlow cost, and the obtained material can simultaneously realize efficient separation of oil-in-water crude oil emulsions with different pH values and recycling of demulsifying materials.

Description

technical field [0001] The invention relates to the technical field of inorganic materials, in particular to the preparation and application of a magnetic inorganic clay-graphene composite demulsification material. Background technique [0002] At present, petroleum extraction and processing, textile industry, mechanical processing, solid fuel thermal processing and other industries (S.Bratskaya, V. Avramenko, S. Schwarz, Colloid Surface A , 2006, 275, 168-176) will produce a large number of oil-water emulsions, of which the emulsions produced during oil extraction and processing account for the vast majority. The direct discharge of such emulsions will cause serious environmental pollution, so demulsification must be carried out before discharge. [0003] The study found that graphene oxide (J. Liu, X. Li, W. Jia, Energ. Fuel. , 2015, 29(7):4644-4653) and carbon nanotubes (J. Liu, X. Li, W. Jia, J. Disper. Sci. Technol. , 2015, 37(9): 1294-1302) can achieve high-effici...

Claims

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Application Information

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IPC IPC(8): B01D17/05
CPCB01D17/047
Inventor 王金清徐海燕杨生荣
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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