CN113772903B - Microemulsion for reducing oil content of oily sludge and its preparation method and application - Google Patents

Abstract

The invention belongs to the technical field of microemulsion, and particularly relates to a microemulsion for reducing the oil content of oil-containing sludge, and a preparation method and application thereof. The microemulsion for reducing the oil content of the oil-containing sludge comprises the following raw materials in parts by weight: 1 part of ionic liquid type surfactant, 25-30 parts of cosurfactant, 20-25 parts of oil-soluble component and 45-50 parts of water. The microemulsion for reducing the oil content of the oil-containing sludge is oil-in-water type, saves cost, has great solubilization capacity on crude oil, and improves the removal rate of crude oil in the oil-containing sludge. The application of the microemulsion for reducing the oil content of the oil-containing sludge adopts a thermochemical washing method to pretreat the oil-containing sludge, and then the microemulsion is combined with the ionic liquid microemulsion, so that the recycling treatment of the oil-containing sludge can be realized, and the oil resource in the oil-containing sludge can be extracted efficiently.

Description

Microemulsion for reducing oil content of oily sludge and its preparation method and application

technical field

The invention belongs to the technical field of microemulsions, and in particular relates to a microemulsion for reducing the oil content of oily sludge and its preparation method and application.

Background technique

Petroleum is the blood of industry and an important source of power to drive the industry. Oil plays an important role in the industrialization of world powers. The entire production process of petroleum is accompanied by the generation of oily sludge. Oily sludge, referred to as oily sludge, is oily solid waste produced in the process of oil exploitation, transportation, refining, etc. Emulsion systems that stick together.

The oil resources on the earth are limited, not inexhaustible. In today's increasingly scarce oil resources, under the social environment where the country vigorously advocates environmental protection, resource conservation, and waste recycling and reuse, the recycling and recycling of oily sludge not only meets the requirements of national environmental protection, but also reduces the follow-up treatment of oil sludge pollution , It can also create economic value and play the residual value of oil sludge.

At present, the treatment methods of oily sludge include thermochemical washing method, foam flotation method, mechanical separation method, freeze-thaw method, solvent extraction method, biological treatment method, etc. Due to the different treatment technical conditions and equipment used, each method has its own advantages and disadvantages. Its pros and cons. The thermochemical washing method is simple and easy to implement, with low cost, and can recover most oil products; microemulsion has extremely low interfacial tension, has strong penetration ability to oily sludge, and can effectively improve the extraction ability of the oil phase. However, the traditional microemulsion has low thermal stability, and the increase of temperature will cause the microemulsion to break. Therefore, it is urgent to explore a new type of microemulsion, combined with other oily sludge treatment methods, to achieve efficient extraction of oil resources in oily sludge.

Contents of the invention

The purpose of the present invention is to provide a microemulsion that reduces the oil content of oily sludge; the microemulsion is oil-in-water type and has the ability to solubilize crude oil; the present invention also provides its preparation method and application.

The microemulsion for reducing the oil content of oily sludge according to the present invention is composed of the following raw materials in parts by weight: 1 part of ionic liquid surfactant, 25-30 parts of co-surfactant, 20-30 parts of oil-soluble component 25 parts and 45-50 parts of water.

in:

The ionic liquid surfactant is one of 1-hexadecyl-3-methylimidazolium chloride or 1-hexadecyl-3-methylimidazolium bromide.

The ionic liquid-type surfactant is 1-hexadecyl-3-methylimidazole chloride or 1-hexadecyl chloride synthesized from N-methylimidazole and halogenated alkanes as raw materials and ethyl acetate as a solvent. -3-Methylimidazole bromide; wherein, the halogenated alkane is hexadecane chloride or hexadecane bromide; the molar ratio of N-methylimidazole to the halogenated alkane is 1:1～1:3; N-methylimidazole The volume ratio of the mixture with halogenated alkanes to ethyl acetate is 1:1 to 1:3.

Preferably, the preparation method of described 1-hexadecyl-3-methylimidazolium chloride or 1-hexadecyl-3-methylimidazolium bromide consists of the following steps:

(1) Put N-methylimidazole, hexadecane chloride or hexadecane bromide in ethyl acetate solvent, transfer to a round bottom flask, heat and reflux at 60-80°C for 24-48h to obtain Golden yellow crude product;

(2) Use a rotary evaporator at 50°C for ≥30min to remove ethyl acetate in the crude product, and dry the product in vacuum at 60-80°C for 12-24h to obtain 1-hexadecyl-3-methylimidazole Chlorine or 1-hexadecyl-3-methylimidazolium bromide.

Described cosurfactant is ethylene glycol.

The oil-soluble component is one of n-heptane, n-hexane, toluene or naphtha.

Mix oil-soluble components, ionic liquid surfactants, and water evenly, and then add co-surfactants to the system to form clear and transparent microemulsions within a certain ratio range. Among them, the ionic liquid can be used as a surfactant to reduce the interfacial tension of oil and water, and the role of the co-surfactant is to cooperate with the surfactant to reduce the interfacial tension of oil and water, improve the flexibility of the interface, and make it easy to bend to form a microemulsion. Along with the increase of cosurfactant carbon chain, the volume of alcohol molecule increases successively, the resistance of its embedding interfacial film increases, the flexibility of interfacial film reduces, and rigidity strengthens, and is unfavorable for the bending of interfacial film, so the present invention selects carbon chain more Short, more hydrophilic ethylene glycol.

The appearance of the microemulsion of the present invention is a transparent liquid, and the droplets are spherical, uniform in size, and have good stability.

The preparation method of the microemulsion that reduces the oily sludge oil content of the present invention, consists of the following steps:

(1) mixing the oil-soluble component with water to prepare a mixed solution;

(2) adding the ionic liquid surfactant to the mixed solution prepared in step (1) and heating in a water bath to dissolve;

(3) Add co-surfactant dropwise to the mixed solution prepared in step (2), and mix it by hand shaking until the last drop of co-surfactant is added to make the mixed solution clear and transparent, which is the prepared Microemulsions for treatment of oily sludge.

in:

The water described in step (1) is distilled water.

The temperature of the water bath described in step (2) is 30-50°C.

Add dropwise cosurfactant in the mixed solution that step (2) prepares described in step (3), can make oil-in-water microemulsion; If oil-soluble component, cosurfactant and ionic liquid Adding water thereinto after the type surfactant mixes, easily forms water-in-oil type microemulsion, does not meet the requirement of the present invention.

The application of the microemulsion that reduces the oil content of oily sludge of the present invention consists of the following steps:

(1) First use sodium carbonate solution to stir and mix with oily sludge, and then leave it to stand to obtain pretreated oily sludge;

(2) Stir and mix the pretreated oily sludge and the microemulsion at a certain volume-to-mass ratio, react at 40-70°C for 10-50min, and let stand for ≥24h to remove oil from the oily sludge and simultaneously measure the oily sludge Medium crude oil removal rate.

in:

The mass fraction of the sodium carbonate solution is 10%, the mixing temperature of the sodium carbonate solution and the oily sludge is 60° C., the stirring speed is 350 r/min, and the stirring time is 30 min.

The volume-to-mass ratio of sodium carbonate solution to oily sludge is 10:1, and the unit is ml:g.

The standing time described in step (1) is ≥24h.

The volume-to-mass ratio of the microemulsion to the pretreated oily sludge is 7.5:2-17.5:2, and the unit is ml/g.

The stirring speed described in step (2) is 350-500r/min.

Preferably, the application of the microemulsion that reduces the oil content of oily sludge according to the present invention first uses a mass ratio of 10% sodium carbonate solution to mix with oily sludge at 60°C, wherein the volume of sodium carbonate solution and oily sludge The ratio is 10ml:1g, stirring at a rotating speed of 350r/min for 30min, and after standing for 24 hours, the pretreated oily sludge is obtained; weigh a certain amount of pretreated oily sludge in a beaker, add a certain volume of microemulsion, The ratio of the microemulsion to the pretreated oily sludge is 7.5ml:2g～17.5ml:2g, stirred with an electric stirrer, the speed is 350-500r/min, the temperature is 40°C-70°C, the reaction is 10min-50min, static After standing for 24 hours, the crude oil removal rate of the oily sludge was measured.

Compared with the prior art, the present invention has the following beneficial effects:

(1) The microemulsion of the present invention that reduces the oil content of oily sludge, the microemulsion is an oil-in-water type, the appearance is a transparent liquid, and the droplets are spherical, uniform in size, and have good stability; adopt the microemulsion While saving costs, it has a great solubilizing ability for crude oil and improves the removal rate of crude oil in oily sludge.

(2) The microemulsion for reducing the oil content of oily sludge according to the present invention is added with ionic liquid, and the ionic liquid-stabilized microemulsion can exist stably at a higher temperature, and has stronger solubilizing ability for both inorganic and organic matter.

(2) The preparation method of the microemulsion for reducing the oil content of oily sludge according to the present invention has the advantages of simple method, less addition of surfactant, simple operation, wide application range, and easy application in industrial applications.

(3) The application of the microemulsion of the present invention that reduces the oil content of oily sludge can realize the treatment of oily sludge under simple process conditions by this microemulsion, extract the oil in the oily sludge, and reduce the oily sludge. The difficulty of sludge subsequent treatment has realized the resource utilization of oil sludge treatment.

(4) The application of the microemulsion for reducing the oil content of oily sludge according to the present invention, using thermochemical washing method to pretreat the oily sludge, and then combining with ionic liquid microemulsion, can realize the resource utilization of oily sludge treatment to efficiently extract oil resources from oily sludge.

Description of drawings

Fig. 1 is embodiment 1 synthetic 1-hexadecyl-3-methylimidazolium chloride ionic liquid proton nuclear magnetic resonance spectrogram;

Fig. 2 is embodiment 1 preparation microemulsion apparent figure;

Fig. 3 is the effect diagram of embodiment 1 processing oily sludge;

Fig. 4 is the scanning electron micrograph of solid particle after embodiment 3 is processed;

Fig. 5 is the effect drawing of embodiment 3 processing oily sludge;

Fig. 6 is the effect drawing of embodiment 4 processing oily sludge;

Fig. 7 is embodiment 5 processing oily dirt effect figure;

Fig. 8 is embodiment 6 processing oily dirt effect figure;

Fig. 9 is embodiment 7 processing oily dirt effect figure;

Fig. 10 is a diagram showing the effect of treating oily sludge in Example 2.

Detailed ways

The present invention will be further described below in conjunction with embodiment.

Example 1

The microemulsion for reducing the oil content of oily sludge described in Example 1 is composed of the following raw materials in parts by weight: 0.1 g of ionic liquid surfactant, 3.0 g of co-surfactant, and 2.5 g of oil-soluble components and water 5.0g.

in:

The ionic liquid surfactant is 1-hexadecyl-3-methylimidazolium chloride.

Described cosurfactant is ethylene glycol.

The oil-soluble component is n-hexane.

The preparation method of the ionic liquid type surfactant described in the present embodiment 1 is made up of the following steps:

Put 0.08mol of N-methylimidazole and 0.08mol of hexadecane chloride in a round bottom flask, add 45ml of ethyl acetate as a solvent, and heat to reflux at 80°C for 24h to obtain a golden yellow crude product. Use a rotary evaporator at 50°C for 30 minutes to remove a large amount of ethyl acetate in the crude product, and dry the product in a vacuum oven at 80°C for 12 hours to obtain 1-hexadecyl-3-methylimidazolium chloride ionic liquid , and its NMR characterization is shown in Figure 1.

The preparation method of the microemulsion that reduces the oil content of oily sludge described in the present embodiment 1 is made up of the following steps:

Mix 2.5g of n-hexane with 5.0g of distilled water, add 0.1g of 1-hexadecyl-3-methylimidazolium chloride ionic liquid synthesized in Example 1, and mix 1-hexadecyl-3- Dissolve methylimidazole chloride in the mixed solution, add 3.0 g of ethylene glycol to the mixed solution, and mix it by hand to obtain a clear and transparent microemulsion for treating oily sludge. The appearance of the prepared microemulsion is shown in the figure 2.

The application of the microemulsion that reduces the oily sludge oil content described in present embodiment 1 is made up of the following steps:

(1) Prepare an aqueous solution of sodium carbonate with a mass fraction of 10%, weigh 1g of oily sludge in a beaker, add medium sodium carbonate solution to it, the added volume is 10ml, the reaction temperature is 60°C, the rotating speed is 350r/min, and the stirring time is 30min , stood still for 24 hours to obtain pretreated oily sludge, and the measured crude oil removal rate was 52.21%.

(2) Weigh 2g of oily sludge pretreated at 60°C in a beaker, add meso-emulsion to it, the volume is 7.5ml, the reaction temperature is 50°C, the rotation speed is 350r/min, the stirring time is 30min, and stand After 24 hours, the treated product was obtained, as shown in Figure 3, and the measured crude oil removal rate was 98.07%.

Example 2

The microemulsion for reducing the oil content of oily sludge described in Example 2 is composed of the following raw materials in parts by weight: 0.1 g of ionic liquid surfactant, 2.7 g of co-surfactant, and 2.0 g of oil-soluble component and water 4.5g.

in:

The ionic liquid surfactant is 1-hexadecyl-3-methylimidazolium chloride.

Described cosurfactant is ethylene glycol.

The oil-soluble component is n-hexane.

The preparation method of the ionic liquid type surfactant described in the present embodiment 2 is made up of the following steps:

Put 0.08mol of N-methylimidazole and 0.10mol of hexadecane chloride in a round bottom flask, add 75ml of ethyl acetate as a solvent, and heat to reflux at 70°C for 36h to obtain a golden yellow crude product. Use a rotary evaporator at 60°C for 35 minutes to remove a large amount of ethyl acetate in the crude product, and dry the product in a vacuum oven at 70°C for 16 hours to obtain the ionic liquid 1-hexadecyl-3-methylimidazolium chloride .

The preparation method of the microemulsion that reduces the oily sludge oil content described in present embodiment 2, is made up of the following steps:

Mix 2.0 g of n-hexane with 4.5 g of distilled water, add 0.1 g of the 1-hexadecyl-3-methylimidazolium chloride ionic liquid synthesized in Example 1, and mix 1-hexadecyl-3- Methylimidazole chloride was dissolved in the mixed solution, 2.7 g of ethylene glycol was added to the mixed solution, and it was mixed by hand shaking to obtain a clear and transparent microemulsion for treating oily sludge.

The application of the microemulsion that reduces the oily sludge oil content described in present embodiment 2 is made up of the following steps:

(1) Prepare an aqueous solution of sodium carbonate with a mass fraction of 10%, weigh 1g of oily sludge in a beaker, add medium sodium carbonate solution to it, the added volume is 10ml, the reaction temperature is 60°C, the rotating speed is 350r/min, and the stirring time is 30min , stood still for 24 hours to obtain pretreated oily sludge, and the measured crude oil removal rate was 52.21%.

(2) Weigh 2g of sludge pretreated at 60°C in a beaker, add a microemulsion to it, the volume of addition is 10ml, the reaction temperature is 60°C, the rotation speed is 350r/min, the stirring time is 30min, and stand for 24 hours , the processed product was obtained, as shown in Figure 10, and the measured crude oil removal rate was 98.14%.

Example 3

The microemulsion for reducing the oil content of oily sludge described in Example 3 is composed of the following raw materials in parts by weight: 0.1 g of ionic liquid surfactant, 2.8 g of co-surfactant, and 2.2 g of oil-soluble component and water 4.6g.

in:

The ionic liquid surfactant is 1-hexadecyl-3-methylimidazolium chloride.

Described cosurfactant is ethylene glycol.

The oil-soluble component is n-heptane.

The preparation method of the ionic liquid type surfactant described in the present embodiment 3 is made up of the following steps:

Put 0.10 mol of N-methylimidazole and 0.20 mol of hexadecane chloride in a round bottom flask, add 100 ml of ethyl acetate as a solvent, and heat to reflux at 60° C. for 48 hours to obtain a golden yellow crude product. Use a rotary evaporator at 50°C for 40 minutes to remove a large amount of ethyl acetate in the crude product, and dry the product in a vacuum oven at 80°C for 12 hours to obtain the ionic liquid 1-hexadecyl-3-methylimidazolium chloride .

The preparation method of the microemulsion that reduces the oil content of oily sludge described in the present embodiment 3 is made up of the following steps:

Mix 2.2 g of n-heptane with 4.6 g of distilled water, add 0.1 g of the 1-hexadecyl-3-methylimidazolium chloride ionic liquid synthesized in Example 1, and 1-hexadecyl-3 Dissolve methylimidazole chloride in the mixed solution, add 2.8 g of ethylene glycol to the mixed solution, and mix it by hand to obtain a clear and transparent microemulsion for treating oily sludge.

The application of the microemulsion that reduces the oily sludge oil content described in present embodiment 3 is made up of the following steps:

(1) Prepare an aqueous solution of sodium carbonate with a mass fraction of 10%, weigh 1g of oily sludge in a beaker, add medium sodium carbonate solution to it, the added volume is 10ml, the reaction temperature is 60°C, the rotating speed is 350r/min, and the stirring time is 30min , stood still for 24 hours to obtain pretreated oily sludge, and the measured crude oil removal rate was 52.21%.

(2) Weigh 2g of pretreated sludge at 60°C in a beaker, add meso-emulsion to it, the added volume is 15ml, the reaction temperature is 60°C, the rotation speed is 400r/min, the stirring time is 20min, and stand for 24 hours , the processed product was obtained, the scanning electron microscope picture of the oily sludge particles after drying is shown in Figure 4, and the effect diagram of the oily sludge treatment is shown in Figure 5, and the measured crude oil removal rate was 98.84%.

Example 4

The microemulsion for reducing the oil content of oily sludge described in Example 4 is composed of the following raw materials in parts by weight: 0.1 g of ionic liquid surfactant, 2.9 g of co-surfactant, and 2.3 g of oil-soluble components and water 4.8g.

in:

The ionic liquid surfactant is 1-hexadecyl-3-methylimidazolium chloride.

Described cosurfactant is ethylene glycol.

The oil-soluble component is n-hexane.

The preparation method of the ionic liquid type surfactant described in the present embodiment 4 is made up of the following steps:

Put 0.20 mol of N-methylimidazole and 0.30 mol of hexadecane chloride in a round bottom flask, add 160 ml of ethyl acetate as a solvent, and heat to reflux at 80° C. for 30 h to obtain a golden yellow crude product. Use a rotary evaporator at 50°C for 40 minutes to remove a large amount of ethyl acetate in the crude product, and dry the product in a vacuum oven at 80°C for 16 hours to obtain the ionic liquid 1-hexadecyl-3-methylimidazolium chloride .

The preparation method of the microemulsion that reduces the oil content of oily sludge described in the present embodiment 4 is made up of the following steps:

Mix 2.3g of n-hexane with 4.8g of distilled water, add 0.1g of the 1-hexadecyl-3-methylimidazolium chloride ionic liquid synthesized in Example 1, and mix 1-hexadecyl-3- Methylimidazole chloride was dissolved in the mixed solution, 2.9 g of ethylene glycol was added to the mixed solution, and mixed by hand to obtain a clear and transparent microemulsion for treating oily sludge.

The application of the microemulsion that reduces the oily sludge oil content described in present embodiment 4 is made up of the following steps:

(1) Prepare an aqueous solution of sodium carbonate with a mass fraction of 10%, weigh 1g of oily sludge in a beaker, add medium sodium carbonate solution to it, the added volume is 10ml, the reaction temperature is 60°C, the rotating speed is 350r/min, and the stirring time is 30min , stood still for 24 hours to obtain pretreated oily sludge, and the measured crude oil removal rate was 52.21%.

(2) Weigh 2g of pretreated sludge at 60°C in a beaker, add meso-emulsion to it, the added volume is 17.5ml, the reaction temperature is 60°C, the rotating speed is 500r/min, the stirring time is 40min, and stand for 24 After 1 hour, the treated product was obtained. The effect diagram of treating oily sludge is shown in Fig. 6, and the measured crude oil removal rate was 99.07%.

Example 5

The microemulsion for reducing the oil content of oily sludge described in Example 5 is composed of the following raw materials in parts by weight: 0.1 g of ionic liquid surfactant, 2.8 g of co-surfactant, and 2.4 g of oil-soluble component and water 4.8g.

in:

The ionic liquid surfactant is 1-hexadecyl-3-methylimidazolium bromide.

Described cosurfactant is ethylene glycol.

The oil-soluble component is naphtha.

The preparation method of the ionic liquid type surfactant described in present embodiment 5, is made up of the following steps:

Put 0.10 mol of N-methylimidazole and 0.10 mol of hexadecane bromide in a round bottom flask, add 120 ml of ethyl acetate as a solvent, and heat to reflux at 80°C for 30 hours to obtain a reddish-brown crude product. Use a rotary evaporator at 50°C for 40 minutes to remove a large amount of ethyl acetate in the crude product, and dry the product in a vacuum oven at 70°C for 24 hours to obtain the ionic liquid 1-hexadecyl-3-methylimidazolium bromide .

The preparation method of the microemulsion that reduces the oil content of oily sludge described in the present embodiment 5 is made up of the following steps:

Mix 2.4g of naphtha with 4.8g of distilled water, add 0.1g of 1-hexadecyl-3-methylimidazolium bromide ionic liquid synthesized in Example 1, and 1-hexadecyl-3 - Methylimidazolium bromide was dissolved in the mixed solution, 2.8 g of ethylene glycol was added to the mixed solution, and mixed by hand shaking to obtain a clear and transparent microemulsion for treating oily sludge.

The application of the microemulsion that reduces the oily sludge oil content described in present embodiment 5 is made up of the following steps:

(1) Prepare an aqueous solution of sodium carbonate with a mass fraction of 10%, weigh 1g of oily sludge in a beaker, add medium sodium carbonate solution to it, the added volume is 10ml, the reaction temperature is 60°C, the rotating speed is 350r/min, and the stirring time is 30min , stood still for 24 hours to obtain pretreated oily sludge, and the measured crude oil removal rate was 52.21%.

(2) Weigh 2g of pretreated sludge at 60°C in a beaker, add meso-emulsion to it, the added volume is 7.5ml, the reaction temperature is 40°C, the rotating speed is 350r/min, the stirring time is 30min, and stand for 24 hours, the processed product was obtained, as shown in Figure 7, and the measured crude oil removal rate was 97.05%.

Example 6

The microemulsion for reducing the oil content of oily sludge described in Example 6 consists of the following raw materials in parts by weight: 0.1 g of ionic liquid surfactant, 3.0 g of co-surfactant, and 2.5 g of oil-soluble components and water 5.0g.

in:

The ionic liquid surfactant is 1-hexadecyl-3-methylimidazolium bromide.

Described cosurfactant is ethylene glycol.

The oil-soluble component is n-hexane.

The preparation method of the ionic liquid type surfactant described in present embodiment 6 is made up of the following steps:

Put 0.10mol of N-methylimidazole and 0.20mol of hexadecane bromide into a round bottom flask, add 140ml of ethyl acetate as a solvent, and heat to reflux at 70°C for 36h to obtain a reddish-brown crude product. Use a rotary evaporator at 50°C for 30 minutes to remove a large amount of ethyl acetate in the crude product, and dry the product in a vacuum oven at 80°C for 12 hours to obtain the ionic liquid 1-hexadecyl-3-methylimidazolium bromide .

The preparation method of the microemulsion that reduces the oil content of oily sludge described in the present embodiment 6 is made up of the following steps:

Mix 2.5g of n-hexane with 5.0g of distilled water, add 0.1g of 1-hexadecyl-3-methylimidazolium bromide ionic liquid synthesized in Example 1, and mix 1-hexadecyl-3- Methylimidazolium bromide was dissolved in the mixed solution, 3.0 g of ethylene glycol was added to the mixed solution, and mixed by hand shaking to obtain a clear and transparent microemulsion for treating oily sludge.

The application of the microemulsion that reduces the oily sludge oil content described in present embodiment 6 is made up of the following steps:

(1) Prepare an aqueous solution of sodium carbonate with a mass fraction of 10%, weigh 1g of oily sludge in a beaker, add medium sodium carbonate solution to it, the added volume is 10ml, the reaction temperature is 60°C, the rotating speed is 350r/min, and the stirring time is 30min , stood still for 24 hours to obtain pretreated oily sludge, and the measured crude oil removal rate was 52.21%.

(2) Weigh 2g of pretreated sludge at 60°C in a beaker, add meso-emulsion to it, the added volume is 7.5ml, the reaction temperature is 50°C, the rotating speed is 450r/min, the stirring time is 30min, and stand for 24 hours, the processed product was obtained, as shown in Figure 8, and the crude oil removal rate was measured to be 97.81%.

Example 7

The microemulsion for reducing the oil content of oily sludge described in Example 7 is composed of the following raw materials in parts by weight: 0.1 g of ionic liquid surfactant, 3.0 g of co-surfactant, and 2.3 g of oil-soluble components and water 4.8g.

in:

The ionic liquid surfactant is 1-hexadecyl-3-methylimidazolium bromide.

Described cosurfactant is ethylene glycol.

The oil-soluble component is n-hexane.

The preparation method of the ionic liquid type surfactant described in the present embodiment 7 is made up of the following steps:

Put 0.10 mol of N-methylimidazole and 0.30 mol of hexadecane bromide in a round bottom flask, add 100 ml of ethyl acetate as a solvent, and heat to reflux at 60°C for 48 hours to obtain a reddish-brown crude product. Use a rotary evaporator at 50°C for 50 minutes to remove a large amount of ethyl acetate in the crude product, and dry the product in a vacuum oven at 70°C for 24 hours to obtain the ionic liquid 1-hexadecyl-3-methylimidazolium bromide .

The preparation method of the microemulsion that reduces the oil content of oily sludge described in the present embodiment 7 is made up of the following steps:

Mix 2.3g of n-hexane with 4.8g of distilled water, add 0.1g of the 1-hexadecyl-3-methylimidazolium bromide ionic liquid synthesized in Example 1, and mix 1-hexadecyl-3- Methylimidazolium bromide was dissolved in the mixed solution, 3.0 g of ethylene glycol was added to the mixed solution, and mixed by hand shaking to obtain a clear and transparent microemulsion for treating oily sludge.

The application of the microemulsion that reduces the oily sludge oil content described in present embodiment 7 is made up of the following steps:

(1) Prepare an aqueous solution of sodium carbonate with a mass fraction of 10%, weigh 1g of oily sludge in a beaker, add medium sodium carbonate solution to it, the added volume is 10ml, the reaction temperature is 60°C, the rotating speed is 350r/min, and the stirring time is 30min , stood still for 24 hours to obtain pretreated oily sludge, and the measured crude oil removal rate was 52.21%.

(2) Weigh 2g of pretreated sludge at 60°C in a beaker, add meso-emulsion to it, the added volume is 15ml, the reaction temperature is 60°C, the rotation speed is 500r/min, the stirring time is 40min, and stand for 24 hours , the processed product was obtained, as shown in Figure 9, and the measured crude oil removal rate was 98.80%.

Comparative example 1

Mix Span80 and Tween20 at a mass ratio of 1:1 to obtain a mixed surfactant, weigh 1 g of the mixed surfactant, 1 g of n-heptane, and 9 g of water, and homogenize them at 10,000 r/min for 5 minutes to obtain an emulsion.

Prepare a sodium carbonate aqueous solution with a mass concentration of 10%, weigh 1g of oily sludge in a beaker, add medium sodium carbonate solution to it, the added volume is 10ml, the reaction temperature is 60°C, the rotating speed is 350r/min, the stirring time is 30min, and stand After 24 hours, the pretreated oily sludge was obtained, and the crude oil removal rate was measured to be 52.21%.

Weigh 2g of pretreated sludge at 60°C into a beaker, add 15ml of the emulsion, the reaction temperature is 50°C, the rotation speed is 350r/min, the stirring time is 40min, and stand for 24 hours to obtain the treated product. The removal rate was 83.36%.

Comparative example 2

Span80 and Tween20 were compounded at a mass ratio of 1:1 to obtain a mixed surfactant, and 1 g of the mixed surfactant, 2 g of n-heptane, and 8 g of water were weighed and homogenized at 10,000 r/min for 5 min to obtain an emulsion.

Prepare a sodium carbonate aqueous solution with a mass concentration of 10%, weigh 1g of oily sludge in a beaker, add medium sodium carbonate solution to it, the added volume is 10ml, the reaction temperature is 60°C, the rotating speed is 350r/min, the stirring time is 30min, and stand After 24 hours, the pretreated oily sludge was obtained, and the crude oil removal rate was measured to be 52.21%.

Weigh 2g of pretreated sludge at 60°C into a beaker, add 15ml of the emulsion, the reaction temperature is 50°C, the rotation speed is 350r/min, the stirring time is 40min, and stand for 24 hours to obtain the treated product. The removal rate was 85.27%.

Comparative example 3

Mix Span80 and Tween20 at a mass ratio of 1:1 to obtain a mixed surfactant, weigh 1 g of the mixed surfactant, 3 g of n-heptane, and 7 g of water, and homogenize them at 10,000 r/min for 5 minutes to obtain an emulsion.

Prepare a sodium carbonate aqueous solution with a mass concentration of 10%, weigh 1g of oily sludge in a beaker, add medium sodium carbonate solution to it, the added volume is 10ml, the reaction temperature is 60°C, the rotating speed is 350r/min, the stirring time is 30min, and stand After 24 hours, the pretreated oily sludge was obtained, and the crude oil removal rate was measured to be 52.21%.

Weigh 2g of pretreated sludge at 60°C into a beaker, add 15ml of the emulsion, the reaction temperature is 50°C, the rotation speed is 350r/min, the stirring time is 40min, and stand for 24 hours to obtain the treated product. The removal rate was 86.51%.

Comparative example 4

The preparation method and application of the microemulsion that reduces the oil content of oily sludge described in this comparative example 4 are all the same as in Example 1, the only difference is that the ionic liquid type surfactants used in the microemulsion are different, and the ionic liquid type The surfactant is 1-tetradecyl-3-methylimidazolium chloride.

In the preparation of the microemulsion, mix 2.5g of n-hexane with 5.0g of distilled water, add 0.1g of 1-tetradecyl-3-methylimidazolium chloride ionic liquid, and dissolve 1-tetradecyl-3 -Methylimidazolium chloride is dissolved in the mixed solution, ethylene glycol 2.5g is added to the mixed solution, and mixed by hand shaking, it is found that the use of 1-tetradecyl-3-methylimidazolium chloride under this condition Microemulsions are not formed and thus cannot be used to treat oily sludge.

Comparative example 5

The preparation method and application of the microemulsion that reduces the oil content of oily sludge described in this comparative example 5 are all the same as in Example 1, the only difference is that the ionic liquid type surfactants used in the microemulsion are different, and the ionic liquid type The surfactant is 1-dodecyl-3-methylimidazolium chloride.

In the preparation of the microemulsion, mix 2.5g of n-hexane with 5.0g of distilled water, add 0.1g of 1-dodecyl-3-methylimidazolium chloride ionic liquid, and mix 1-dodecyl-3 - Dissolve methylimidazole chloride in the mixed solution, add 2.5 g of ethylene glycol to the mixed solution, and mix it by hand shaking until the mixed solution becomes clear and transparent when the last drop of ethylene glycol is added, and the reduced oil content can be obtained. Sludge oil content using microemulsion.

The application of the microemulsion that reduces the oil content of oily sludge described in this comparative example 5 is made up of the following steps:

(1) Prepare an aqueous solution of sodium carbonate with a mass concentration of 10%, take 1g of oily sludge in a beaker, add medium sodium carbonate solution therein, the added volume is 10ml, the reaction temperature is 60°C, the rotating speed is 350r/min, and the stirring time is 30min , standing for 24 hours to obtain pretreated oily sludge, and the measured crude oil removal rate was 52.21%.

(2) Weigh 2g of pretreated sludge at 60°C in a beaker, add meso-emulsion to it, the added volume is 15ml, the reaction temperature is 50°C, the rotation speed is 350r/min, the stirring time is 30min, and stand for 24 hours , the treated product was obtained, and the crude oil removal rate was measured to be 88.26%.

Comparative example 6

The preparation method and application of the microemulsion that reduces the oil content of oily sludge described in this comparative example 6 are all the same as in Example 1, and the only difference is that the cosurfactant used in the microemulsion is different, and the cosurfactant is ethanol.

In the preparation of the microemulsion, mix 2.5g of n-hexane with 5.0g of distilled water, add 0.1g of 1-hexadecyl-3-methylimidazolium chloride ionic liquid, and dissolve 1-hexadecyl-3 - Dissolve methylimidazole chloride in the mixed solution, add 2.5 g of ethanol to the mixed solution, and mix it by hand shaking. It is found that the microemulsion formed by using ethanol as a co-surfactant is unstable and easy to demulsify, and cannot be used for the treatment of oily sludge.

The examples of the present invention use 1-hexadecyl-3-methylimidazolium chloride or 1-hexadecyl-3-methylimidazolium bromide ionic liquid type surfactants to prepare microemulsions and comparative examples 1-3 use common Compared with Tween20, the surfactant Span80 showed comparable or even better treatment effect; using 1-hexadecyl-3-methylimidazolium chloride or 1-hexadecyl-3-methylimidazolium bromide ion Compared with comparative example 4-5 using 1-tetradecyl-3-methylimidazolium chloride and 1-dodecyl-3-methylimidazolium chloride in liquid preparation microemulsion, the former is easier to form microemulsion and has better treatment effect Good; using ethylene glycol as a co-surfactant compared with comparative example 6 using ethanol, the microemulsion system with ethylene glycol participation is more stable. Due to the extremely low interfacial tension of the microemulsion and its great solubilization ability for oil, it can promote the detachment of asphaltene from the surface of oily sludge and improve the removal rate of crude oil in oily sludge. The combination of the microemulsion of the present invention and the treatment process of the oily sludge of the present invention reduces the difficulty of the subsequent treatment of the oily sludge and realizes the resource utilization of the oily sludge treatment.

It should be noted that the specific implementation is only a representative example of the present invention, and obviously the technical solution of the present invention is not limited to the above-mentioned embodiments, and many variations are possible. Those of ordinary skill in the art, based on the disclosure of the present invention or obtained without objection from the written description of the document, should be considered as the protection scope of this patent.

Claims (6)

1. A microemulsion that reduces the oil content of oily sludge is characterized in that: in parts by weight, it is composed of the following raw materials: 1 part of ionic liquid surfactant, 25-30 parts of cosurfactant, oil-soluble component Divide 20-25 parts and 45-50 parts of water; in: The ionic liquid-type surfactant is 1-hexadecyl-3-methylimidazole chloride or 1-hexadecyl chloride synthesized from N-methylimidazole and halogenated alkanes as raw materials and ethyl acetate as a solvent. -3-Methylimidazole bromide; wherein, the halogenated alkane is hexadecane chloride or hexadecane bromide; the molar ratio of N-methylimidazole to the halogenated alkane is 1:1～1:3; N-methylimidazole The volume ratio of the mixture with halogenated alkanes to ethyl acetate is 1:1~1:3; The preparation method of described 1-hexadecyl-3-methylimidazolium chloride or 1-hexadecyl-3-methylimidazolium bromide consists of the following steps: (1) Put N-methylimidazole, hexadecane chloride or hexadecane bromide in ethyl acetate solvent, transfer to a round bottom flask, heat and reflux at 60-80°C for 24-48h to obtain Golden yellow crude product; (2) Use a rotary evaporator at 50°C for ≥30min to remove ethyl acetate in the crude product, and dry the product in vacuum at 60-80°C for 12-24h to obtain 1-hexadecyl-3-methylimidazole Chlorine or 1-hexadecyl-3-methylimidazolium bromide; The co-surfactant is ethylene glycol; the oil-soluble component is one of n-heptane, n-hexane, toluene or naphtha. 2. a method for preparing the microemulsion that reduces the oil content of oily sludge as claimed in claim 1, is characterized in that: consist of the following steps: (1) mixing the oil-soluble component with water to prepare a mixed solution; (2) adding the ionic liquid surfactant to the mixed solution prepared in step (1) and heating in a water bath to dissolve; (3) Add co-surfactant dropwise to the mixed solution prepared in step (2), and mix it by hand shaking until the last drop of co-surfactant is added to make the mixed solution clear and transparent, which is the prepared Microemulsions for treatment of oily sludge. 3. the preparation method of the microemulsion that reduces the oil content of oily sludge according to claim 2, is characterized in that: the water described in step (1) is distilled water; In step (2), water bath temperature is 30-50 ℃ . 4. the application of a microemulsion reducing the oil content of oily sludge as claimed in claim 1, is characterized in that: consist of the following steps: (1) First use sodium carbonate solution to stir and mix with oily sludge, and then leave it to stand to obtain pretreated oily sludge; (2) Stir and mix the pretreated oily sludge and the microemulsion at a certain volume-to-mass ratio, react at 40-70°C for 10-50min, and let stand for ≥24h to remove oil from the oily sludge and simultaneously measure the oily sludge Medium crude oil removal rate. 5. the application of the microemulsion that reduces oily sludge oil content according to claim 4 is characterized in that: the massfraction of sodium carbonate solution is 10%, and the mixing temperature of sodium carbonate solution and oily sludge is 50 ℃, The stirring speed is 350r/min, and the stirring time is 30min; The volume-to-mass ratio of sodium carbonate solution to oily sludge is 10:1, and the unit is ml:g; The standing time in step (1) is ≥24h. 6. The application of the microemulsion reducing the oil content of oily sludge according to claim 4, characterized in that: the volume-to-mass ratio of microemulsion to pretreated oily sludge is 7.5:2-17.5:2, and the unit is ml/ g; the stirring speed in step (2) is 350-500r/min.

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