CN112915593A - Emulsion type reverse demulsifier for offshore oil field and preparation method thereof - Google Patents
Emulsion type reverse demulsifier for offshore oil field and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an emulsion type reverse demulsifier for offshore oilfields and a preparation method thereof. The emulsion type reverse demulsifier for offshore oil fields is prepared by compounding cationic polyacrylamide and diethanol amine resin polyether serving as raw materials and adding a solubilizer and a stabilizer. The reverse demulsifier has good treatment effect when treating oily sewage generated by a high-water-content oil field.
Description
Technical Field
The invention belongs to the technical field of petroleum industry, and particularly relates to an emulsion type reverse demulsifier for offshore oil fields and a preparation method thereof.
Background
At present, reverse demulsifiers developed for O/W type emulsions at home and abroad mainly comprise three categories of low-molecular electrolytes, alcohols, surfactants and high-molecular polymers. The high molecular polymer reverse demulsifier is used in many cases, and can be classified into cationic, anionic and nonionic reverse demulsifiers according to their chargeability. The cationic high-molecular polymer reverse demulsifier is mainly a cationic polyquaternary ammonium salt type, and takes a polymerizable quaternary ammonium salt monomer as a main raw material to carry out free radical polymerization so as to obtain the polyquaternary ammonium salt reverse demulsifier. Common polymerizable quaternary ammonium salt monomers comprise DAC, DMC and DBC, common comonomers comprise Acrylamide (AM), and a cationic polyquaternary ammonium salt type reverse demulsifier is a main type of the prior reverse demulsifier for treating oily sewage. Because the cationic clear water agent has the characteristics of widest application range, high oil removal speed and high oil removal rate, the cationic clear water agent can effectively destroy double electric layers and cause oil drops to be gathered by electrostatic attraction, but the cationic polyquaternary ammonium salt type reverse demulsifier cannot destroy an oil-water interface, so that the oil removal efficiency can be improved only by improving the molecular weight and enhancing the rolling and sweeping capacity, and the flocculation is tight and easy to hang on the wall.
The nonionic reverse demulsifier for demulsification of O/W type emulsion mainly comprises block polyethers, coalescence of oil droplets is realized by reducing the strength of an interface film, and the nonionic reverse demulsifier has the characteristics of high oil removal efficiency, good oil-water interface, good fluidity of upper oil droplets and no adhesion to walls, but the polyether reverse demulsifier has the characteristics of low molecular weight and incapability of quickly rolling and sweeping coalesced oil droplets on the coalescence of the oil droplets, so that the oil-water separation speed and the deep water purification effect are not as good as those of the cationic polyquaternary ammonium salt reverse demulsifier. When the cationic polyquaternium reverse demulsifier and the nonionic polyether reverse demulsifier are used together, the appearance of flocs can be effectively improved, but the cationic polyquaternium reverse demulsifier and the nonionic polyether reverse demulsifier are difficult to compound and easy to delaminate, stirring and mixing are required to be started before use, and the offshore oil field application is difficult due to the limited treatment space of the offshore oil field.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an emulsion type reverse demulsifier for offshore oil fields and a preparation method thereof.
The invention is realized by the following technical scheme:
an emulsion type reverse demulsifier for offshore oilfields is prepared by the following steps:
step one, compounding and dissolving cationic polyacrylamide and alcohol amine resin polyether
Dripping cationic polyacrylamide into the alcohol amine resin polyether solution, and stirring for dissolving; the mass ratio of the cationic polyacrylamide to the alcohol amine resin polyether is 0.1-2.0;
step two, preparation of emulsion reverse demulsifier
Firstly, adding a solubilizer into the product prepared in the first step, and adding a stabilizer after the solubilizer is completely dissolved, wherein the mass part of the solubilizer is 7.8-12.5%; the mass portion of the stabilizer is 4.3-8.5%.
In the technical scheme, in the first step, distilled water is poured into a four-neck flask, stirring is started after the temperature is controlled to be 30-50 ℃, then the molten alcohol amine resin polyether dry agent is slowly dripped into the four-neck flask, stirring is continued for 3 hours after dripping is finished, then cationic polyacrylamide is added, and stirring is continued for 2 hours.
In the technical scheme, in the step one, the cationic degree of the cationic polyacrylamide is 10% -40%, and the mass fraction of the comonomer is 15% -25%;
in the above technical solution, in the step one, the cationicity of the cationic polyacrylamide is preferably 35%; the mass fraction of comonomer is preferably 19%.
In the above technical solution, in the step one, the cationic monomer is one of dimethyldiallylammonium chloride, acryloyloxyethyldimethylbenzylammonium chloride, methacryloyloxyethyldimethylbenzylammonium chloride, acryloyloxyethyltrimethylammonium chloride, and methacryloyloxyethyltrimethylammonium chloride, preferably dimethyldiallylammonium chloride.
In the technical scheme, in the step one, the molecular weight of the cationic polyacrylamide is 50-200 ten thousand.
In the above technical solution, in the first step, the alcohol amine resin polyether is prepared by using dimethylethanolamine, N dimethylpropylenediamine, and N, N dimethylethylenediamine as an initiator to synthesize 3 and 2 block polyoxyethylene polyoxypropylene polymers:
according to (starter: propylene oxide): ethylene oxide: polyether is synthesized by propylene oxide with different mass ratios, wherein the ratio of (initiator: propylene oxide) is 1: 1-1: 9, (initiator: propylene oxide): ethylene oxide: propylene oxide is 1: m: n (m is between 1 and 9, n is between 1 and 9);
according to (starter: propylene oxide): propylene oxide: synthesizing block polyoxyethylene polyoxypropylene polymer by using ethylene oxide in different mass ratios, wherein the ratio of (initiator: propylene oxide) is 1: 1-1: 9, (initiator: propylene oxide): ethylene oxide: propylene oxide is 1: m: n (m is between 1 and 9, n is between 1 and 9).
In the technical scheme, in the second step, the product obtained in the first step is added into a four-neck flask, then the four-neck flask is placed in a water bath kettle, and a stirrer and a constant-pressure dropping funnel are connected with the four-neck flask; starting stirring when the water bath is heated to 40-60 ℃, dropwise adding the solubilizer into the aqueous phase solution, and continuing stirring for 2 hours after dropwise adding is finished; and then adding a stabilizer into the aqueous phase solution, and continuously stirring for 3 hours after the stabilizer is completely dissolved to obtain the emulsion reverse demulsifier.
In the above technical scheme, in the second step, the solubilizer is one of ethylene glycol methyl ether, ethylene glycol dimethyl ether, ethylene glycol ethyl ether, ethylene glycol diethyl ether, ethylene glycol butyl ether, diethylene glycol butyl ether, dipropylene glycol methyl ether or propylene glycol methyl ether.
In the above technical solution, in the second step, the stabilizer is one of ammonium sulfate, ammonium carbonate, or sodium sulfate.
The invention has the advantages and beneficial effects that: the emulsion type reverse demulsifier for offshore oil fields is prepared by compounding cationic polyacrylamide and diethanol amine resin polyether serving as raw materials and adding a solubilizer and a stabilizer. The reverse demulsifier has good treatment effect when treating oily sewage generated by a high-water-content oil field.
Drawings
FIG. 1 is a graph (one) showing the effect of different agents on the oil removal rate of oily wastewater in the examples.
FIG. 2 is a graph showing the effect of different agents on the oil removal rate of oily wastewater in the example (II).
For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention is further described below with reference to specific examples.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
EXAMPLE 1 preparation of emulsion-type reverse demulsifier
Firstly, 50g of distilled water is poured into a four-neck flask, stirring is started after the temperature is controlled to be 40 ℃, then 35g of melted diethanol amine resin polyether dry agent is slowly dripped into the four-neck flask, stirring is continued for 6 hours after dripping is finished, then 25g of copolymer (with the effective content of 19%) of dimethyl diallyl ammonium chloride and acrylamide is added, and stirring is continued for 2 hours; starting stirring when the water bath is heated to 55 ℃, dropwise adding 10g of ethylene glycol monobutyl ether into the aqueous phase solution, and continuing stirring for 2 hours after dropwise adding is finished; then 8.5g of ammonium sulfate is added into the aqueous phase solution, and after the ammonium sulfate is completely dissolved, the mixture is continuously stirred for 3 hours to obtain the emulsion reverse-phase demulsifier 1.
EXAMPLE 2 preparation of emulsion-type reverse demulsifier
Firstly, 50g of distilled water is poured into a four-neck flask, stirring is started after the temperature is controlled to be 40 ℃, then 40g of melted diethanol amine resin polyether dry agent is slowly dripped into the four-neck flask, stirring is continued for 6 hours after dripping is finished, then 20g of copolymer (with the effective content of 19%) of dimethyl diallyl ammonium chloride and acrylamide is added, and stirring is continued for 2 hours; starting stirring when the water bath is heated to 55 ℃, dropwise adding 10g of ethylene glycol monobutyl ether into the aqueous phase solution, and continuing stirring for 2 hours after dropwise adding is finished; then 8.5g of ammonium sulfate is added into the aqueous phase solution, and after the ammonium sulfate is completely dissolved, the mixture is continuously stirred for 3 hours to obtain the emulsion reverse-phase demulsifier 2.
EXAMPLE 3 preparation of emulsion-type reverse demulsifier
Firstly, 50g of distilled water is poured into a four-neck flask, stirring is started after the temperature is controlled to be 40 ℃, then 45g of melted diethanol amine resin polyether dry agent is slowly dripped into the four-neck flask, stirring is continued for 6 hours after dripping is finished, then 15g of copolymer (with the effective content of 19%) of dimethyl diallyl ammonium chloride and acrylamide is added, and stirring is continued for 2 hours; starting stirring when the water bath is heated to 55 ℃, dropwise adding 10g of ethylene glycol monobutyl ether into the aqueous phase solution, and continuing stirring for 2 hours after dropwise adding is finished; then 8.5g of ammonium sulfate is added into the aqueous phase solution, and after the ammonium sulfate is completely dissolved, the mixture is continuously stirred for 3 hours to obtain the emulsion reverse-phase demulsifier 3.
EXAMPLE 4 preparation of emulsion-type reverse demulsifier
Firstly, 50g of distilled water is poured into a four-mouth flask, stirring is started after the temperature is controlled to be 40 ℃, then 40g of melted diethanol amine resin polyether drying agent is slowly dripped into the four-mouth flask, stirring is continued for 6 hours after dripping is finished, then 20g of copolymer (with the effective content of 19%) of acryloyloxyethyl dimethyl benzyl ammonium chloride and acrylamide is added, and stirring is continued for 2 hours; starting stirring when the water bath is heated to 55 ℃, dropwise adding 10g of ethylene glycol monobutyl ether into the aqueous phase solution, and continuing stirring for 2 hours after dropwise adding is finished; then 8.5g of ammonium sulfate is added into the aqueous phase solution, and after the ammonium sulfate is completely dissolved, the mixture is continuously stirred for 3 hours to obtain the emulsion reverse demulsifier 4.
EXAMPLE 5 preparation of emulsion-type reverse demulsifier
Firstly, 50g of distilled water is poured into a four-neck flask, stirring is started after the temperature is controlled to be 40 ℃, then 40g of melted diethanol amine resin polyether drying agent is slowly dripped into the four-neck flask, stirring is continued for 6 hours after dripping is finished, then 20g of copolymer (with the effective content of 19%) of methacryloyloxyethyl dimethyl benzyl ammonium chloride and acrylamide is added, and stirring is continued for 2 hours; starting stirring when the water bath is heated to 55 ℃, dropwise adding 10g of ethylene glycol monobutyl ether into the aqueous phase solution, and continuing stirring for 2 hours after dropwise adding is finished; then 8.5g of ammonium sulfate is added into the aqueous phase solution, and after the ammonium sulfate is completely dissolved, the mixture is continuously stirred for 3 hours to obtain the emulsion reverse-phase demulsifier 5.
Example 6 evaluation of the Performance of the reverse demulsifier for treating oily wastewater
Firstly, 80ml of oily sewage (with the oil content of 1400mg/L) of a certain oil field is poured into a 100ml water removing bottle and is placed at 60 ℃ for heat preservation for 10 min; and finally adding 40mg/L of oil-water separating agent, oscillating 100 times before and after, standing for 5min, taking a lower-layer water sample to measure the oil content and calculating the oil removal rate. The results of the oil removal rates of the different reverse demulsifiers are shown in table 1 and fig. 1 and 2.
TABLE 1 oil removal rates of different agents for oily wastewater
The results of the oil removal rates of the different oil-water separating agents are shown in fig. 1 and 2. The results in the figure show that the reverse demulsifier 2 has high oil removal rate, good transmittance and stable oil droplet state.
Example 7 evaluation of the Performance of the reverse demulsifier for treating oily wastewater
Firstly, 80ml of oily sewage (with the oil content of 1400mg/L) of a certain oil field is poured into a 100ml water removing bottle and is placed at 60 ℃ for heat preservation for 10 min; then, adding different types of reverse demulsifiers, adding the chemical concentration of 30mg/L, oscillating 100 times before and after, standing for 5min, taking a lower-layer water sample to measure the oil content and calculating the oil removal rate. The results in table 2 show that the oil removal rate of reverse demulsifier 2 was the highest.
TABLE 2 oil removal rates of different agents for oily wastewater
In conclusion, the cationic polyacrylamide and the diethanol amine resin polyether are compounded as raw materials, and the solubilizer and the stabilizer are added, so that the emulsion type reverse demulsifier has a good treatment effect on the oily sewage of the oil field.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. An emulsion type reverse demulsifier for offshore oil fields is characterized in that: is prepared by the following steps:
step one, compounding and dissolving cationic polyacrylamide and alcohol amine resin polyether
Dripping cationic polyacrylamide into the alcohol amine resin polyether solution, and stirring for dissolving; the mass ratio of the cationic polyacrylamide to the alcohol amine resin polyether is 0.1-2.0;
step two, preparation of emulsion reverse demulsifier
Firstly, adding a solubilizer into the product prepared in the first step, and adding a stabilizer after the solubilizer is completely dissolved, wherein the mass part of the solubilizer is 7.8-12.5%; the mass portion of the stabilizer is 4.3-8.5%.
2. The emulsion type reverse demulsifier for offshore oil fields according to claim 1, wherein: in the first step, the cationic degree of the cationic polyacrylamide is 10% -40%, and the mass fraction of the comonomer is 15% -25%.
3. The emulsion type reverse demulsifier for offshore oil fields according to claim 1, wherein: in the first step, the cationic monomer is one of dimethyldiallylammonium chloride, acryloyloxyethyldimethylbenzylammonium chloride, methacryloyloxyethyldimethylbenzylammonium chloride, acryloyloxyethyltrimethylammonium chloride or methacryloyloxyethyltrimethylammonium chloride.
4. The emulsion type reverse demulsifier for offshore oil fields according to claim 1, wherein: in the first step, the alcohol amine resin polyether is prepared by synthesizing 3 and 2 block polyoxyethylene polyoxypropylene polymers by taking dimethyl ethanolamine, N dimethyl propylene diamine and N, N dimethyl ethylene diamine as initiators.
5. The emulsion type reverse demulsifier for offshore oil fields according to claim 1, wherein: in the second step, the solubilizer is one of ethylene glycol methyl ether, ethylene glycol dimethyl ether, ethylene glycol ethyl ether, ethylene glycol diethyl ether, ethylene glycol butyl ether, diethylene glycol butyl ether, dipropylene glycol methyl ether or propylene glycol methyl ether; the stabilizer is one of ammonium sulfate, ammonium carbonate or sodium sulfate.
6. A preparation method of an emulsion type reverse demulsifier for offshore oil fields is characterized by comprising the following steps:
step one, compounding and dissolving cationic polyacrylamide and alcohol amine resin polyether
Dripping cationic polyacrylamide into the alcohol amine resin polyether solution, and stirring for dissolving; the mass ratio of the cationic polyacrylamide to the alcohol amine resin polyether is 0.1-2.0;
step two, preparation of emulsion reverse demulsifier
Firstly, adding a solubilizer into the product prepared in the first step, and adding a stabilizer after the solubilizer is completely dissolved, wherein the mass part of the solubilizer is 7.8-12.5%; the mass portion of the stabilizer is 4.3-8.5%.
7. The method for preparing the emulsion type reverse demulsifier for the offshore oilfield according to claim 6, wherein the emulsion type reverse demulsifier comprises the following steps: in the first step, the cationic degree of the cationic polyacrylamide is 10% -40%, and the mass fraction of the comonomer is 15% -25%.
8. The method for preparing the emulsion type reverse demulsifier for the offshore oilfield according to claim 6, wherein the emulsion type reverse demulsifier comprises the following steps: in the first step, the cationic monomer is one of dimethyldiallylammonium chloride, acryloyloxyethyldimethylbenzylammonium chloride, methacryloyloxyethyldimethylbenzylammonium chloride, acryloyloxyethyltrimethylammonium chloride or methacryloyloxyethyltrimethylammonium chloride.
9. The method for preparing the emulsion type reverse demulsifier for the offshore oilfield according to claim 6, wherein the emulsion type reverse demulsifier comprises the following steps: in the first step, the alcohol amine resin polyether is prepared by synthesizing 3 and 2 block polyoxyethylene polyoxypropylene polymers by taking dimethyl ethanolamine, N dimethyl propylene diamine and N, N dimethyl ethylene diamine as initiators.
10. The method for preparing the emulsion type reverse demulsifier for the offshore oilfield according to claim 6, wherein the emulsion type reverse demulsifier comprises the following steps: in the second step, the solubilizer is one of ethylene glycol methyl ether, ethylene glycol dimethyl ether, ethylene glycol ethyl ether, ethylene glycol diethyl ether, ethylene glycol butyl ether, diethylene glycol butyl ether, dipropylene glycol methyl ether or propylene glycol methyl ether; the stabilizer is one of ammonium sulfate, ammonium carbonate or sodium sulfate.
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