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Preparation method and application of magnetic demulsifier capable of simultaneously achieving efficient oil-water separation of O/W and W/O emulsions

A technology of oil-water separation and demulsifier, applied in the field of preparation of magnetic nanoparticles

Active Publication Date: 2019-12-27
HANGZHOU DIANZI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to overcome the deficiencies of the existing magnetic nanoparticles in the field of emulsified oil-water separation, the present invention uses hydrolysis and condensation reactions on Fe 3 o 4 @SiO 2 Hydrophobic alkylsilane and relatively hydrophilic aminosilane with cationic properties are simultaneously introduced on the surface of nanoparticles to construct a magnetic nanoparticle with cationic properties and excellent interfacial activity that can be well dispersed in both the water phase and the oil phase, so that To achieve efficient oil-water separation of O / W emulsion and W / O emulsion at the same time

Method used

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  • Preparation method and application of magnetic demulsifier capable of simultaneously achieving efficient oil-water separation of O/W and W/O emulsions
  • Preparation method and application of magnetic demulsifier capable of simultaneously achieving efficient oil-water separation of O/W and W/O emulsions
  • Preparation method and application of magnetic demulsifier capable of simultaneously achieving efficient oil-water separation of O/W and W/O emulsions

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Experimental program
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Effect test

Embodiment 1-1

[0030] Example 1-1: Fe 3 O 4 @SiO 2 Nanoparticle preparation

[0031] In a 500mL reactor equipped with a stirrer and a temperature control device, 250mL of 1.5mol / L sodium hydroxide aqueous solution was added, and the temperature was raised to 80℃; then 10.8g of FeCl 3 ·6H 2 O, 4.0g FeCl 2 ·4H 2 O was dissolved in 50 mL of 0.5 mol / L hydrochloric acid aqueous solution, and the solution was added dropwise to the above reactor within 30 minutes under the protection of a nitrogen atmosphere, and the reaction was continued for 1 hour to obtain Fe 3 O 4 Nanoparticles. Take 1.5g of the above Fe 3 O 4 The nanoparticles were dispersed in 300mL deionized water, heated to 80℃ under the protection of nitrogen, and 30mL sodium silicate aqueous solution (1.0mol / L) was added at a constant speed within 2h, and then the reaction was continued for 3h to obtain Fe 3 O 4 @SiO 2 Nanoparticles. The pH value of the whole reaction process is controlled at about 6.0.

Embodiment 2-1

[0042] Take 5.0g Fe 3 O 4 @SiO 2 Nanoparticles were dispersed in 200g ethanol, 0.003mol octyltrimethoxysilane and 0.0015mol aminopropyltriethoxysilane were added under the protection of argon, adjusted the pH value to 12, and reacted for 6h at 40℃ to obtain alkylsilane Mixed and modified magnetic nanoparticles with aminosilane. Add the above-mentioned magnetic nano demulsifier to the O / W emulsion (oil phase is diesel oil, pH=7, oil content is 1.0g / L, average oil droplet size is about 0.5μm), when the demulsifier dosage reaches 200mg / L , The oil removal rate can reach more than 99%. Add the above-mentioned magnetic demulsifier to W / O emulsion (oil phase is diesel oil, water content is 140g / L, and the average size of water droplets is 10.8μm), when the demulsifier dosage reaches 500mg / L, the water removal rate can reach 99% or more . After washing with ethanol, the magnetic nano demulsifier can be recycled up to 7 times.

Embodiment 2-2

[0044] Take 5.0g Fe 3 O 4 @SiO 2 Nanoparticles are dispersed in a mixed solution of 160g ethanol and 40g water, add 0.003375mol butyltrimethoxysilane and 0.001125mol aminopropyltriethoxysilane under the protection of argon, adjust the pH value to 7, and react at 50℃ For 48 hours, the magnetic nanoparticles modified by mixing alkylsilane and aminosilane are obtained. Add the above-mentioned magnetic nano demulsifier to the O / W emulsion (oil phase is soybean oil, pH=11, oil content is 1.0g / L, average oil droplet size is about 0.4μm), when the demulsifier dosage reaches 310mg / L When, the oil removal rate can reach more than 99%. Add the above magnetic demulsifier to the W / O emulsion (oil phase is soybean oil, water content is 140g / L, and the average water droplet size is 6.8μm). When the demulsifier dosage reaches 710mg / L, the water removal rate can reach 99% the above. After washing with n-hexane and ethanol, the magnetic nano demulsifier can be recycled up to 6 times.

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Abstract

The invention relates to a preparation method and application of a magnetic demulsifier capable of simultaneously achieving efficient oil-water separation of O / W and W / O emulsions. According to the method, alkyl silane and amino silane are anchored on the surfaces of Fe3O4@SiO2 magnetic nanoparticles through a hydrolytic condensation reaction, so that the magnetic particles are endowed with excellent interfacial activity and cationic characteristics. The magnetic particles modified with the alkyl siloxane and the amino siloxane can be uniformly dispersed in a water phase or an oil phase; afterbeing added into an emulsified oil-water system, the modified magnetic particles can be efficiently adsorbed to an oil-water interface under the driving of interfacial activity and electrostatic attraction, emulsified oil drops or water drops are quickly separated under the action of a magnetic field, and finally, efficient oil-water separation in O / W and W / O emulsions can be realized at the sametime. The obtained magnetic nano material is excellent in demulsification efficiency, and has a very wide application prospect in the field of oil-water separation of O / W and W / O emulsions.

Description

Technical field [0001] The invention relates to the synthesis of a magnetic nano demulsifier that can be well dispersed in both water and oil phases, has cationic characteristics and excellent interfacial activity, and specifically relates to a simultaneous realization of "water-in-oil" emulsion (W / O emulsion) Preparation and application of magnetic nanoparticles modified by mixing aminosilane and alkylsilane with "oil-in-water" emulsion (O / W emulsion) for high efficiency oil-water separation. Background technique [0002] With the continuous advancement of petroleum exploration, storage, transportation and processing, as well as the continuous development of machinery and food processing industries, a large number of W / O emulsions and O / W emulsions have been produced. The water and salt in W / O emulsion will increase the load of pumps, pipelines and storage tanks, cause corrosion and fouling on metal surfaces, and even cause catalyst poisoning in the subsequent processing of oils...

Claims

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Application Information

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IPC IPC(8): B01D17/05
CPCB01D17/048
Inventor 吕挺吴艳张栋赵红挺
Owner HANGZHOU DIANZI UNIV
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