Novel clay mineral demulsifier, preparation method thereof, and method for demulsifying and recycling oil-in-water crude oil emulsion

Abstract

The invention relates to a novel clay mineral demulsifier, a preparation method thereof, and a method for demulsifying and recycling an oil-in-water crude oil emulsion. The preparation method comprises the following steps: mixing pretreated clay mineral with iron chloride, sodium citrate, ethylene glycol and polyethylene glycol, performing ultrasonic dispersing to uniformity, placing the obtainedmixture in a reactor with a PTFE lining, raising the reaction temperature in the reactor to 200-240 DEG C, carrying out a constant temperature reaction for 20-28 h, and cooling the obtained reaction product to obtain the demulsifier. The novel clay mineral demulsifier prepared in the invention is used for the demulsification and dehydration treatment of the oil-in-water crude oil emulsion, the demulsification efficiency on the water-in-oil crude oil emulsion reaches up to 99.0% or more, and the water content of removed water is less than 10 mg / L, and basically meets the discharge standards ofsecondary water. The demulsifier provides an inexpensive and efficient method for the demulsification and dehydration treatment of the oil-in-water crude oil emulsion, and has an excellent applicationprospect.

Description

technical field

[0001] The invention belongs to the demulsification and dehydration treatment technology of crude oil emulsion in the fields of crude oil exploitation and heavy oil emulsification and viscosity reduction, and specifically relates to a novel clay mineral demulsifier and its preparation method, as well as the demulsification treatment and recycling of oil-in-water emulsion method. Background technique

[0002] Water flooding / steam flooding of crude oil, emulsification and viscosity reduction of heavy oil, water-based extraction of oil sands, and hydraulic fracturing or steam injection of oil shale all use a large amount of water or steam for treatment. Water treatment technology has gradually become one of the important strategies for enhancing the recovery of traditional crude oil and unconventional oil and gas resources. However, a large amount of oil-water emulsion is inevitably produced in the water treatment method and the subsequent gathering and transpo...

Examples

Embodiment 1

[0048] The preparation method of the novel attapulgite clay demulsifier of the present embodiment, described method comprises the steps:

[0049] (1) Purification of attapulgite clay: crush attapulgite raw ore and pass through a 200-mesh sieve. Add 1kg of attapulgite clay to 50L of water, and add 6g of sodium hexametaphosphate, under the condition of 3000rpm, mechanically stir for 2h; let it stand for 2-8h, take out the upper layer of clay minerals by siphon method, centrifuge at 5000rpm, freeze-dry. Purified attapulgite clay from impurities such as quartz is obtained.

[0050] (2) Acidification treatment of attapulgite clay: Add 100g of purified attapulgite clay minerals into 500mL of deionized water and ultrasonically disperse for 1 hour, add the dispersed suspension into the reaction vessel, add 1mol / L dilute hydrochloric acid, and react at 60°C After 1 h of reaction, the attapulgite clay was centrifuged, washed three times with deionized water, and freeze-dried to obtain ...

Embodiment 2

[0054] The preparation method of the novel attapulgite clay demulsifier of the present embodiment, described method is basically the same as embodiment 1, difference only is: the solvothermal synthesis of step (4) novel clay mineral demulsifier: 1g ferric chloride is dissolved in 20ml In the ethylene glycol solution, then add 1 g of modified attapulgite clay obtained in step (3), 3 g of sodium citrate and 0.5 g of polyethylene glycol, stir for two minutes, and ultrasonically disperse for 10 min with an ultrasonic cleaner, and stir evenly The mixture was transferred to a hydrothermal synthesis reaction kettle and reacted at a constant temperature of 200°C for 28 hours. The product was taken out, centrifuged and washed to obtain a new attapulgite clay demulsifier.

Embodiment 3

[0056] The preparation method of the novel attapulgite clay demulsifier of the present embodiment, described method is basically the same as embodiment 1, difference only is: the solvothermal synthesis of step (4) novel clay mineral demulsifier: 2g ferric chloride is dissolved in 60ml In ethylene glycol solution, then add the modified attapulgite clay that 1g step (3) obtains, 4g sodium citrate and the polyethylene glycol of 2g, after stirring for two minutes, ultrasonically disperse 10min with ultrasonic cleaner, after stirring evenly, The mixture was transferred to a hydrothermal synthesis reaction kettle and reacted at a constant temperature of 240°C for 20 hours. The product was taken out, centrifuged and washed to obtain a new attapulgite clay demulsifier.

technical field

[0001] The invention belongs to the demulsification and dehydration treatment technology of crude oil emulsion in the fields of crude oil exploitation and heavy oil emulsification and viscosity reduction, and specifically relates to a novel clay mineral demulsifier and its preparation method, as well as the demulsification treatment and recycling of oil-in-water emulsion method. Background technique

[0002] Water flooding / steam flooding of crude oil, emulsification and viscosity reduction of heavy oil, water-based extraction of oil sands, and hydraulic fracturing or steam injection of oil shale all use a large amount of water or steam for treatment. Water treatment technology has gradually become one of the important strategies for enhancing the recovery of traditional crude oil and unconventional oil and gas resources. However, a large amount of oil-water emulsion is inevitably produced in the water treatment method and the subsequent gathering and transpo...

Examples

Embodiment 1

[0048] The preparation method of the novel attapulgite clay demulsifier of the present embodiment, described method comprises the steps:

[0049] (1) Purification of attapulgite clay: crush attapulgite raw ore and pass through a 200-mesh sieve. Add 1kg of attapulgite clay to 50L of water, and add 6g of sodium hexametaphosphate, under the condition of 3000rpm, mechanically stir for 2h; let it stand for 2-8h, take out the upper layer of clay minerals by siphon method, centrifuge at 5000rpm, freeze-dry. Purified attapulgite clay from impurities such as quartz is obtained.

[0050] (2) Acidification treatment of attapulgite clay: Add 100g of purified attapulgite clay minerals into 500mL of deionized water and ultrasonically disperse for 1 hour, add the dispersed suspension into the reaction vessel, add 1mol / L dilute hydrochloric acid, and react at 60°C After 1 h of reaction, the attapulgite clay was centrifuged, washed three times with deionized water, and freeze-dried to obtain ...

Embodiment 2

[0054] The preparation method of the novel attapulgite clay demulsifier of the present embodiment, described method is basically the same as embodiment 1, difference only is: the solvothermal synthesis of step (4) novel clay mineral demulsifier: 1g ferric chloride is dissolved in 20ml In the ethylene glycol solution, then add 1 g of modified attapulgite clay obtained in step (3), 3 g of sodium citrate and 0.5 g of polyethylene glycol, stir for two minutes, and ultrasonically disperse for 10 min with an ultrasonic cleaner, and stir evenly The mixture was transferred to a hydrothermal synthesis reaction kettle and reacted at a constant temperature of 200°C for 28 hours. The product was taken out, centrifuged and washed to obtain a new attapulgite clay demulsifier.

Embodiment 3

[0056] The preparation method of the novel attapulgite clay demulsifier of the present embodiment, described method is basically the same as embodiment 1, difference only is: the solvothermal synthesis of step (4) novel clay mineral demulsifier: 2g ferric chloride is dissolved in 60ml In ethylene glycol solution, then add the modified attapulgite clay that 1g step (3) obtains, 4g sodium citrate and the polyethylene glycol of 2g, after stirring for two minutes, ultrasonically disperse 10min with ultrasonic cleaner, after stirring evenly, The mixture was transferred to a hydrothermal synthesis reaction kettle and reacted at a constant temperature of 240°C for 20 hours. The product was taken out, centrifuged and washed to obtain a new attapulgite clay demulsifier.

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