CN113717750A - Demulsifier suitable for crude oil with high wax content - Google Patents
Demulsifier suitable for crude oil with high wax content Download PDFInfo
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- CN113717750A CN113717750A CN202111190075.7A CN202111190075A CN113717750A CN 113717750 A CN113717750 A CN 113717750A CN 202111190075 A CN202111190075 A CN 202111190075A CN 113717750 A CN113717750 A CN 113717750A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/04—Dewatering or demulsification of hydrocarbon oils with chemical means
Abstract
The invention relates to a demulsifier suitable for crude oil with high wax content, which is characterized by comprising an amine demulsifier, a phenolic demulsifier and mixed benzene.
Description
Technical Field
The invention relates to a demulsifier suitable for crude oil with high wax content.
Background
Petroleum is composed of many components, typically containing waxes. Since the time that mankind has been extracting oil, it has never been in the way of wax. The accumulation of wax in oil pipes is a headache-causing problem in the oil industry. Petroleum wax is a solid hydrocarbon, the main component of which is paraffin wax, which exists in crude oil, distillate oil and residual oil, has the molecular structure of wax, and the melting point is higher than 30 ℃.
Under the condition that the oil contains more wax, the crude oil is condensed along with the reduction of the temperature from the ground bottom to the road surface in the process of exploitation, and an oil well is blocked. Based on incomplete statistics in the late 80's of the 20 th century, the annual cost of removing oil well wax in the united states alone is as high as $ 600 million. In the united station, crude oil needs to be dehydrated, and when the temperature is low when the wax content in the crude oil is high, the crude oil does not flow or has poor fluidity. Not easy to combine with demulsifier. Resulting in difficulty in dehydration. The demulsifier with strong penetrability can enable crude oil with high wax content to be easily dehydrated.
Patent number CN 111454745a prepared by my company discloses a demulsifier, which has the advantages of high dehydration speed and good water purification effect, and its use condition is that the temperature is higher than 55 ℃, however, under the condition that the wax content in the oil is more, the oil condenses with the decrease of the temperature of the crude oil from the ground to the road surface in the process of mining, the temperature of the crude oil to the road surface is lower than 50 ℃, and at this time, the oil with higher wax content causes no flow of the raw material or poor fluidity when the temperature is low, which causes the mismatch between the temperature of the oil with higher wax content and the use condition temperature of the demulsifier prepared by CN 111454745a, therefore, the demulsifier prepared by CN 111454745a cannot meet the dehydration problem of the oil with higher wax content, and needs to be solved urgently.
Disclosure of Invention
The invention provides a demulsifier suitable for crude oil with high wax content, and solves the technical problem that crude oil with high wax content is not easy to dehydrate.
In order to solve the technical problems, the invention adopts the following technical scheme:
the demulsifier suitable for crude oil with high wax content consists of amine demulsifier, phenolic demulsifier and mixed benzene;
the amine demulsifier takes potassium hydroxide as a catalyst, and polyethylene polyamine, ethylene oxide and propylene oxide are polymerized to form a block copolymer;
the phenolic demulsifier takes potassium hydroxide as a catalyst, and makes nonyl phenol, ethylene oxide and propylene oxide polymerize to form a copolymer;
the mixed benzene is a mixture of benzene, toluene and xylene.
The mass ratio of the amine demulsifier to the phenolic demulsifier to the mixed benzene is 25-30: 10-15: 50-65.
The amine demulsifier is prepared according to the following steps:
1) weighing polyethylene polyamine, potassium hydroxide, propylene oxide and ethylene oxide;
2) adding polyethylene polyamine and potassium hydroxide into a reaction kettle, and closing the reaction kettle;
3) introducing nitrogen into the reaction kettle, stopping introducing the nitrogen when the pressure is 0.5-0.7 MPa, and keeping for 20-40 min;
4) if the pressure in the reaction kettle is unchanged, releasing nitrogen and introducing new nitrogen, and repeating at least once;
5) when the pressure in the reaction kettle changes, releasing nitrogen and introducing new nitrogen, and repeating until the pressure in the reaction kettle does not change; repeating the step 4);
6) opening the reaction kettle, and reacting for 0.5-1.5 h under the conditions that the temperature is 90-100 ℃, the stirring speed is 180-200 r/min, and the pressure is-0.1-0 MPa;
7) heating to 125-150 ℃, and adding propylene oxide until the pressure is 0.3-0.5 MPa;
8) continuously preserving the heat for 2 hours at the temperature of 125-150 ℃ until the pressure in the reaction kettle is-0.098-0 Mpa;
9) adjusting the temperature in the reaction kettle to 110-120 ℃, and adding ethylene oxide;
10) under the condition that the temperature is 110-120 ℃, and the pressure in the reaction kettle is-0.098-0 Mpa, continuously preserving the heat for 0.5 h;
11) adjusting the temperature to 130-150 ℃, and adding propylene oxide until the pressure is 0.4 MPa;
12) continuously preserving heat for 2 hours at the temperature of 123-150 ℃ until the pressure in the reaction kettle is negative;
13) cooling to 90 ℃, sampling, and obtaining the amine demulsifier after the amine demulsifier is qualified through detection; named WD-2631 dry agent;
the mass ratio of the polyethylene polyamine to the potassium hydroxide to the propylene oxide to the ethylene oxide is 150-170: 4-6: 550-650: 300-400.
Step 7), the addition amount of the propylene oxide is 30-40% of the total amount of the propylene oxide; the adding amount of the propylene oxide in the step 11) is 60-70% of the total amount of the propylene oxide.
The phenolic demulsifier is carried out according to the following steps:
a) weighing nonyl phenol, potassium hydroxide, propylene oxide, ethylene oxide and formaldehyde;
b) closing an emptying valve and a kettle bottom valve of the polymerization kettle, opening a vacuum valve, starting a vacuum pump, adding nonyl phenol, formaldehyde and potassium hydroxide into the polymerization kettle when the pressure in the kettle reaches-0.06-0.1 MPa, and closing the kettle bottom valve, the vacuum pump and the vacuum valve;
c) flushing nitrogen until the pressure is 0.5-0.7 MPa, heating to 65 ℃ under the condition that the rotating speed is 180-200 r/min, and keeping for 10 min; continuously heating to 80-85 ℃, and keeping for 30 min; heating to 90-95 ℃ again, and keeping for 1 h;
d) starting a heat exchanger to cool water, volatilizing water generated by the system reaction, condensing the water by the heat exchanger, heating to 150 ℃, and keeping the temperature for 30 min; cooling to 130 deg.C, and dehydrating under-0.04 Mpa for 30 min;
e) under the condition that the temperature is 130 ℃, adding propylene oxide, controlling the temperature to be 140-150 ℃, controlling the temperature to be 135-145 ℃ after the temperature and the feeding are stable, and keeping the temperature for 1h after the propylene oxide is fed;
h) cooling to 110-120 ℃, and keeping for 30min under the condition that the pressure is-0.04 Mpa;
i) adding ethylene oxide at the temperature of 120-130 ℃, and preserving the temperature for 30min when the pressure in the polymerization kettle is reduced to-0.04 MPa;
j) cooling, and keeping the temperature at 110-120 ℃ and the pressure at-0.04 Mpa for 30 min;
k) cooling to 90 ℃, sampling, and obtaining the phenolic demulsifier after the detection is qualified; named WD-1-2 dry agent;
the nonyl phenol, the potassium hydroxide, the propylene oxide, the ethylene oxide and the formaldehyde are mixed according to the mass ratio of 28.5:0.5:42.8:26.4: 1.8;
the stable feeding means that the fluctuation range of the temperature is 2 ℃ between 140 ℃ and 150 ℃, the feeding speed is 500kg/h, and the pressure is 0.1-0.3 MPa.
A preparation method of a demulsifier suitable for crude oil with high wax content comprises the steps of adding an amine demulsifier, a phenolic demulsifier and mixed benzene into a reaction kettle, and uniformly mixing to obtain the demulsifier suitable for crude oil with high wax content, which is named as a WD-666 type demulsifier.
And uniformly mixing at 40 ℃, wherein the stirring speed is 190r/min, and the time is 30-60 min.
The invention has the following beneficial technical effects:
the crude oil with higher wax content can better perform dehydration.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
The demulsifier suitable for crude oil with high wax content consists of amine demulsifier, phenolic demulsifier and mixed benzene;
the amine demulsifier takes potassium hydroxide as a catalyst, and polyethylene polyamine, ethylene oxide and propylene oxide are polymerized to form a block copolymer;
the phenolic demulsifier takes potassium hydroxide as a catalyst, and makes nonyl phenol, ethylene oxide and propylene oxide polymerize to form a copolymer;
the mixed benzene is a composition of benzene, toluene and xylene according to a mass ratio of 3:2: 1.
The mass ratio of the amine demulsifier to the phenolic demulsifier to the mixed benzene is 28:12: 60.
The amine demulsifier is prepared according to the following steps:
1) weighing polyethylene polyamine, potassium hydroxide, propylene oxide and ethylene oxide;
2) adding polyethylene polyamine and potassium hydroxide into a reaction kettle, and closing the reaction kettle;
3) introducing nitrogen into the reaction kettle, stopping introducing nitrogen when the pressure is 0.6MPa, and keeping for 30 min;
4) if the pressure in the reaction kettle does not change, releasing nitrogen and introducing new nitrogen, and repeating twice;
5) when the pressure in the reaction kettle changes, releasing nitrogen and introducing new nitrogen, and repeating until the pressure in the reaction kettle does not change; repeating the step 4);
6) opening the reaction kettle, and reacting for 1h at the temperature of 100 ℃, the stirring speed of 190r/min and the pressure of-0.1 MPa;
7) heating to 135 deg.C, and adding propylene oxide to pressure of 0.4 MPa;
8) keeping the temperature for 2 hours at 140 ℃ until the pressure in the reaction kettle is-0.088 Mpa;
9) adjusting the temperature in the reaction kettle to 115 ℃, and adding ethylene oxide;
10) keeping the temperature for 0.5h under the condition that the temperature is 115 ℃ and the pressure in the reaction kettle is-0.088 Mpa;
11) adjusting the temperature to 140 ℃, and adding propylene oxide until the pressure is 0.4 MPa;
12) keeping the temperature for 2 hours under the condition that the temperature is 1350 ℃ until the pressure in the reaction kettle is negative;
13) cooling to 90 ℃, sampling, and obtaining the amine demulsifier after the amine demulsifier is qualified through detection; named WD-2631 dry agent;
the mass ratio of the polyethylene polyamine, the potassium hydroxide, the propylene oxide and the ethylene oxide is 160:5:580: 350.
Step 7), the addition amount of the propylene oxide is 35 percent of the total amount of the propylene oxide; and step 11), adding 65% of propylene oxide.
The phenolic demulsifier is carried out according to the following steps:
a) weighing nonyl phenol, potassium hydroxide, propylene oxide, ethylene oxide and formaldehyde;
b) closing an emptying valve and a kettle bottom valve of the polymerization kettle, opening a vacuum valve, starting a vacuum pump, adding nonyl phenol, formaldehyde and potassium hydroxide into the polymerization kettle when the pressure in the kettle reaches 0.08MPa, and closing the kettle bottom valve, the vacuum pump and the vacuum valve;
c) flushing nitrogen until the pressure is 0.6MPa, heating to 65 ℃ under the condition that the rotating speed is 190r/min, and keeping for 10 min; continuously heating to 82 deg.C, and maintaining for 30 min; raising the temperature to 92 ℃ again, and keeping the temperature for 1 h;
d) starting a heat exchanger to cool water, volatilizing water generated by the system reaction, condensing the water by the heat exchanger, heating to 150 ℃, and keeping the temperature for 30 min; cooling to 130 deg.C, and dehydrating under-0.04 Mpa for 30 min;
e) adding propylene oxide at 130 ℃, controlling the temperature to be 145 ℃, controlling the temperature to be 140 ℃ after the temperature and the feeding are stable until the propylene oxide is fed, and preserving the temperature for 1 h;
h) cooling to 115 deg.C, and maintaining under-0.04 Mpa for 30 min;
i) adding ethylene oxide at 125 deg.C, and maintaining the pressure in the polymerization kettle at-0.04 MPa for 30 min;
j) cooling, and maintaining at 115 deg.C and-0.04 Mpa for 30 min;
k) cooling to 90 ℃, sampling, and obtaining the phenolic demulsifier after the detection is qualified; named WD-1-2 dry agent;
the nonyl phenol, the potassium hydroxide, the propylene oxide, the ethylene oxide and the formaldehyde are mixed according to the mass ratio of 28.5:0.5:42.8:26.4: 1.8;
the stable feeding means that the temperature is 145 ℃, the fluctuation range is +/-2 ℃, the feeding speed is 500kg/h, and the pressure is 0.2 MPa.
A preparation method of a demulsifier suitable for crude oil with high wax content comprises the steps of adding an amine demulsifier, a phenolic demulsifier and mixed benzene into a reaction kettle, and uniformly mixing to obtain the demulsifier suitable for crude oil with high wax content, which is named as a WD-666 type demulsifier.
And uniformly mixing at 40 ℃, wherein the stirring speed is 190r/min, and the time is 40 min.
Example 2
The demulsifier suitable for crude oil with high wax content consists of amine demulsifier, phenolic demulsifier and mixed benzene;
the amine demulsifier takes potassium hydroxide as a catalyst, and polyethylene polyamine, ethylene oxide and propylene oxide are polymerized to form a block copolymer;
the phenolic demulsifier takes potassium hydroxide as a catalyst, and makes nonyl phenol, ethylene oxide and propylene oxide polymerize to form a copolymer;
the mixed benzene is a mixture of benzene, toluene and xylene.
The mass ratio of the amine demulsifier to the phenolic demulsifier to the mixed benzene is 26:14: 60.
The amine demulsifier is prepared according to the following steps:
1) weighing polyethylene polyamine, potassium hydroxide, propylene oxide and ethylene oxide;
2) adding polyethylene polyamine and potassium hydroxide into a reaction kettle, and closing the reaction kettle;
3) introducing nitrogen into the reaction kettle, stopping introducing nitrogen when the pressure is 0.7MPa, and keeping for 20 min;
4) if the pressure in the reaction kettle does not change, releasing nitrogen and introducing new nitrogen, and repeating for three times;
5) when the pressure in the reaction kettle changes, releasing nitrogen and introducing new nitrogen, and repeating until the pressure in the reaction kettle does not change; repeating the step 4);
6) opening the reaction kettle, and reacting for 0.8 h at the temperature of 92 ℃, the stirring speed of 180r/min and the pressure of-0.001 MPa;
7) heating to 130 ℃, and adding propylene oxide until the pressure is 0.3 MPa;
8) keeping the temperature for 2 hours under the condition that the temperature is 130 ℃ until the pressure in the reaction kettle is-0.025 Mpa;
9) adjusting the temperature in the reaction kettle to 110 ℃, and adding ethylene oxide;
10) keeping the temperature for 0.5h under the condition that the temperature is 110 ℃ and the pressure in the reaction kettle is-0.032 Mpa;
11) adjusting the temperature to 140 ℃, and adding propylene oxide until the pressure is 0.4 MPa;
12) continuously preserving the heat for 2 hours at the temperature of 135 ℃ until the pressure in the reaction kettle is negative;
13) cooling to 90 ℃, sampling, and obtaining the amine demulsifier after the amine demulsifier is qualified through detection; named WD-2631 dry agent;
the mass ratio of the polyethylene polyamine, the potassium hydroxide, the propylene oxide and the ethylene oxide is 155:4:620: 320.
Step 7), the adding amount of the propylene oxide is 32 percent of the total amount of the propylene oxide; and step 11), adding the propylene oxide in an amount of 66% of the total amount of the propylene oxide.
The phenolic demulsifier is carried out according to the following steps:
a) weighing nonyl phenol, potassium hydroxide, propylene oxide, ethylene oxide and formaldehyde;
b) closing an emptying valve and a kettle bottom valve of the polymerization kettle, opening a vacuum valve, starting a vacuum pump, adding nonyl phenol, formaldehyde and potassium hydroxide into the polymerization kettle when the pressure in the kettle reaches-0.04 MPa, and closing the kettle bottom valve, the vacuum pump and the vacuum valve;
c) flushing nitrogen until the pressure is 0.7MPa, heating to 65 ℃ under the condition that the rotating speed is 190r/min, and keeping for 10 min; continuously heating to 83 deg.C, and maintaining for 30 min; heating to 94 ℃ again, and keeping for 1 h;
d) starting a heat exchanger to cool water, volatilizing water generated by the system reaction, condensing the water by the heat exchanger, heating to 150 ℃, and keeping the temperature for 30 min; cooling to 130 deg.C, and dehydrating under-0.04 Mpa for 30 min;
e) adding propylene oxide at 130 ℃, controlling the temperature to be 143 ℃, controlling the temperature to be 138 ℃ after the temperature and the feeding are stable, and keeping the temperature for 1h when the feeding of the propylene oxide is finished;
h) cooling to 120 deg.C, and maintaining at-0.04 Mpa for 30 min;
i) adding ethylene oxide at 124 deg.C, and maintaining the pressure in the polymerization kettle to-0.04 MPa for 30 min;
j) cooling, and maintaining at 118 deg.C and-0.04 MPa for 30 min;
k) cooling to 90 ℃, sampling, and obtaining the phenolic demulsifier after the detection is qualified; named WD-1-2 dry agent;
the nonyl phenol, the potassium hydroxide, the propylene oxide, the ethylene oxide and the formaldehyde are mixed according to the mass ratio of 28.5:0.5:42.8:26.4: 1.8;
the stable feeding means that the temperature is 140 ℃, the fluctuation range is +/-2 ℃, the feeding speed is 500kg/h, and the pressure is 0.2 MPa.
A preparation method of a demulsifier suitable for crude oil with high wax content comprises the steps of adding an amine demulsifier, a phenolic demulsifier and mixed benzene into a reaction kettle, and uniformly mixing to obtain the demulsifier suitable for crude oil with high wax content, which is named as a WD-666 type demulsifier.
And uniformly mixing, wherein the temperature is 40 ℃, the stirring speed is 190r/min, and the time is 35 min.
Example 3
The demulsifier suitable for crude oil with high wax content consists of amine demulsifier, phenolic demulsifier and mixed benzene;
the amine demulsifier takes potassium hydroxide as a catalyst, and polyethylene polyamine, ethylene oxide and propylene oxide are polymerized to form a block copolymer;
the phenolic demulsifier takes potassium hydroxide as a catalyst, and makes nonyl phenol, ethylene oxide and propylene oxide polymerize to form a copolymer;
the mixed benzene is a mixture of benzene, toluene and xylene.
The mass ratio of the amine demulsifier to the phenolic demulsifier to the mixed benzene is 29:12: 59.
The amine demulsifier is prepared according to the following steps:
1) weighing polyethylene polyamine, potassium hydroxide, propylene oxide and ethylene oxide;
2) adding polyethylene polyamine and potassium hydroxide into a reaction kettle, and closing the reaction kettle;
3) introducing nitrogen into the reaction kettle, stopping introducing nitrogen when the pressure is 0.7MPa, and keeping for 35 min;
4) if the pressure in the reaction kettle is unchanged, releasing nitrogen and introducing new nitrogen, and repeating at least once;
5) when the pressure in the reaction kettle changes, releasing nitrogen and introducing new nitrogen, and repeating until the pressure in the reaction kettle does not change; repeating the step 4);
6) opening the reaction kettle, and reacting for 1.2 h at the temperature of 100 ℃, the stirring speed of 180r/min and the pressure of-0.09 MPa;
7) heating to 130 ℃, and adding propylene oxide until the pressure is 0.5 MPa;
8) keeping the temperature for 2 hours under the condition that the temperature is 140 ℃ and the pressure in the reaction kettle is-0.008 Mpa;
9) adjusting the temperature in the reaction kettle to 115 ℃, and adding ethylene oxide;
10) keeping the temperature for 0.5h under the condition that the temperature is 110-120 ℃ until the pressure in the reaction kettle is-0.009 Mpa;
11) adjusting the temperature to 140 ℃, and adding propylene oxide until the pressure is 0.4 MPa;
12) continuously preserving the heat for 2 hours at the temperature of 135 ℃ until the pressure in the reaction kettle is negative;
13) cooling to 90 ℃, sampling, and obtaining the amine demulsifier after the amine demulsifier is qualified through detection; named WD-2631 dry agent;
the mass ratio of the polyethylene polyamine to the potassium hydroxide to the propylene oxide to the ethylene oxide is 170:6:620: 340.
Step 7), the adding amount of the propylene oxide is 36 percent of the total amount of the propylene oxide; and step 11), adding 65% of propylene oxide.
The phenolic demulsifier is carried out according to the following steps:
a) weighing nonyl phenol, potassium hydroxide, propylene oxide, ethylene oxide and formaldehyde;
b) closing an emptying valve and a kettle bottom valve of the polymerization kettle, opening a vacuum valve, starting a vacuum pump, adding nonyl phenol, formaldehyde and potassium hydroxide into the polymerization kettle when the pressure in the kettle reaches-0.004 MPa, and closing the kettle bottom valve, the vacuum pump and the vacuum valve;
c) flushing nitrogen until the pressure is 0.6MPa, heating to 65 ℃ under the condition that the rotating speed is 200r/min, and keeping for 10 min; continuously heating to 80 deg.C, and maintaining for 30 min; heating to 90 ℃ again, and keeping for 1 h;
d) starting a heat exchanger to cool water, volatilizing water generated by the system reaction, condensing the water by the heat exchanger, heating to 150 ℃, and keeping the temperature for 30 min; cooling to 130 deg.C, and dehydrating under-0.04 Mpa for 30 min;
e) adding propylene oxide at 130 ℃, controlling the temperature to be 145 ℃, controlling the temperature to be 140 ℃ after the temperature and the feeding are stable until the propylene oxide is fed, and preserving the temperature for 1 h;
h) cooling to 115 deg.C, and maintaining under-0.04 Mpa for 30 min;
i) adding ethylene oxide at 125 deg.C, and maintaining the pressure in the polymerization kettle at-0.04 MPa for 30 min;
j) cooling, and maintaining at 120 deg.C and-0.04 Mpa for 30 min;
k) cooling to 90 ℃, sampling, and obtaining the phenolic demulsifier after the detection is qualified; named WD-1-2 dry agent;
the nonyl phenol, the potassium hydroxide, the propylene oxide, the ethylene oxide and the formaldehyde are mixed according to the mass ratio of 28.5:0.5:42.8:26.4: 1.8;
the stable feeding means that the temperature fluctuates within +/-2 ℃ at 145 ℃, the feeding speed is 500kg/h, and the pressure is 0.2 MPa.
A preparation method of a demulsifier suitable for crude oil with high wax content comprises the steps of adding an amine demulsifier, a phenolic demulsifier and mixed benzene into a reaction kettle, and uniformly mixing to obtain the demulsifier suitable for crude oil with high wax content, which is named as a WD-666 type demulsifier.
And uniformly mixing at 40 ℃, wherein the stirring speed is 190r/min, and the time is 40 min.
The beneficial effects of the present invention are further illustrated below in conjunction with experimental data:
experiment one
1.1 site of experiment: the Wanda group, Inc. of lone Dong I United stations.
1.2 Experimental samples: the demulsifier of WD-666 type prepared in example 1 of this application and the demulsifier of WD-515 type prepared in example 1 of patent CN 111454745A of this company.
1.3 oil sample selection:
1.3.1 sampling time: the sampling time is not more than 24h (ensuring the freshness of the oil sample);
1.3.2 sampling sites: the inlet of the separator is not added with medicine, and the inlet and the outlet of the external delivery pump are added with medicine.
1.4 instruments, equipment and reagents: a constant temperature water bath, an analytical balance, a beaker, a reagent bottle, a thermometer, a screening bottle, a pipette, a disposable needle tube, absolute ethyl alcohol and a mixing device.
1.5 summary of Experimental methods
Selecting an experimental fresh oil sample, pouring the oil sample into a screening bottle platform oil sample, respectively placing the screening bottle platform oil sample into water baths at constant temperatures of 60 ℃ and 40 ℃, observing the dehydration rates of the sample for 30min, 60min and 90min under the specified dosing concentration, observing the water color and the interface condition, and calculating the absolute dehydration rate%.
And (3) experimental detection: the output water content and oil production (on a dry basis) after dehydration by the demulsifier.
Experimental detection reference standard: general technical conditions of the Q/SH10201418-2013 crude oil demulsifier.
2 results of the experiment
The dehydration rates of the 60 ℃ water bath tank for 30min, 60min and 90min, the water color, the interface condition and the absolute dehydration rate% are observed and shown in Table 1
TABLE 1
The dehydration rates of the 40 ℃ water bath tank for 30min, 60min and 90min, the water color, the interface condition and the absolute dehydration rate% are observed and shown in Table 2
TABLE 2
As can be seen from Table 1, the experimental temperature is 60 ℃, WD-515 and WD-666 prepared by the company have better dehydration rate, and the WD-666 performance is more excellent; as can be seen from a comparison of the data in Table 2, the experimental temperature of 40 ℃ is very different between the company-produced WD-515 and WD-666 in terms of dehydration, and the WD-515 is not suitable as a demulsifier for crude oil with higher wax content.
Claims (7)
1. The demulsifier suitable for crude oil with high wax content is characterized by comprising an amine demulsifier, a phenolic demulsifier and mixed benzene;
the amine demulsifier takes potassium hydroxide as a catalyst, and polyethylene polyamine, ethylene oxide and propylene oxide are polymerized to form a block copolymer;
the phenolic demulsifier takes potassium hydroxide as a catalyst, and makes nonyl phenol, ethylene oxide and propylene oxide polymerize to form a copolymer;
the mixed benzene is a mixture of benzene, toluene and xylene.
2. The demulsifier suitable for crude oil with high wax content according to claim 1, wherein the mass ratio of the amine demulsifier, the phenolic demulsifier and the mixed benzene is 25-30: 10-15: 50-65.
3. The demulsifier suitable for high wax content in crude oil according to claim 1 or 2, wherein the amine demulsifier is prepared by the following steps:
1) weighing polyethylene polyamine, potassium hydroxide, propylene oxide and ethylene oxide;
2) adding polyethylene polyamine and potassium hydroxide into a reaction kettle, and closing the reaction kettle;
3) introducing nitrogen into the reaction kettle, stopping introducing the nitrogen when the pressure is 0.5-0.7 MPa, and keeping for 20-40 min;
4) if the pressure in the reaction kettle is unchanged, releasing nitrogen and introducing new nitrogen, and repeating at least once;
5) when the pressure in the reaction kettle changes, releasing nitrogen and introducing new nitrogen, and repeating until the pressure in the reaction kettle does not change; repeating the step 4);
6) opening the reaction kettle, and reacting for 0.5-1.5 h under the conditions that the temperature is 90-100 ℃, the stirring speed is 180-200 r/min, and the pressure is-0.1-0 MPa;
7) heating to 125-150 ℃, and adding propylene oxide until the pressure is 0.3-0.5 MPa;
8) continuously preserving the heat for 2 hours at the temperature of 125-150 ℃ until the pressure in the reaction kettle is-0.098-0 Mpa;
9) adjusting the temperature in the reaction kettle to 110-120 ℃, and adding ethylene oxide;
10) under the condition that the temperature is 110-120 ℃, and the pressure in the reaction kettle is-0.098-0 Mpa, continuously preserving the heat for 0.5 h;
11) adjusting the temperature to 130-150 ℃, and adding propylene oxide until the pressure is 0.4 MPa;
12) continuously preserving heat for 2 hours at the temperature of 123-150 ℃ until the pressure in the reaction kettle is negative;
13) cooling to 90 ℃, sampling, and obtaining the amine demulsifier after the amine demulsifier is qualified through detection; named WD-2631 dry agent;
the mass ratio of the polyethylene polyamine to the potassium hydroxide to the propylene oxide to the ethylene oxide is 150-170: 4-6: 550-650: 300-400.
4. The demulsifier suitable for high wax content crude oil according to claim 3, wherein the propylene oxide is added in the step 7) in an amount of 30-40% of the total amount of propylene oxide; the adding amount of the propylene oxide in the step 11) is 60-70% of the total amount of the propylene oxide.
5. The demulsifier suitable for high wax content crude oil according to claim 1 or 2, wherein the phenolic demulsifier is prepared by the following steps:
a) weighing nonyl phenol, potassium hydroxide, propylene oxide, ethylene oxide and formaldehyde;
b) closing an emptying valve and a kettle bottom valve of the polymerization kettle, opening a vacuum valve, starting a vacuum pump, adding nonyl phenol, formaldehyde and potassium hydroxide into the polymerization kettle when the pressure in the kettle reaches-0.06-0.1 MPa, and closing the kettle bottom valve, the vacuum pump and the vacuum valve;
c) flushing nitrogen until the pressure is 0.5-0.7 MPa, heating to 65 ℃ under the condition that the rotating speed is 180-200 r/min, and keeping for 10 min; continuously heating to 80-85 ℃, and keeping for 30 min; heating to 90-95 ℃ again, and keeping for 1 h;
d) starting a heat exchanger to cool water, volatilizing water generated by the system reaction, condensing the water by the heat exchanger, heating to 150 ℃, and keeping the temperature for 30 min; cooling to 130 deg.C, and dehydrating under-0.04 Mpa for 30 min;
e) under the condition that the temperature is 130 ℃, adding propylene oxide, controlling the temperature to be 140-150 ℃, controlling the temperature to be 135-145 ℃ after the temperature and the feeding are stable, and keeping the temperature for 1h after the propylene oxide is fed;
h) cooling to 110-120 ℃, and keeping for 30min under the condition that the pressure is-0.04 Mpa;
i) adding ethylene oxide at the temperature of 120-130 ℃, and preserving the temperature for 30min when the pressure in the polymerization kettle is reduced to-0.04 MPa;
j) cooling, and keeping the temperature at 110-120 ℃ and the pressure at-0.04 Mpa for 30 min;
k) cooling to 90 ℃, sampling, and obtaining the phenolic demulsifier after the detection is qualified; named WD-1-2 dry agent;
the nonyl phenol, the potassium hydroxide, the propylene oxide, the ethylene oxide and the formaldehyde are mixed according to the mass ratio of 28.5:0.5:42.8:26.4: 1.8;
the stable feeding means that the fluctuation range of the temperature is 2 ℃ between 140 ℃ and 150 ℃, the feeding speed is 500kg/h, and the pressure is 0.1-0.3 MPa.
6. A preparation method of a demulsifier suitable for crude oil with high wax content is characterized in that an amine demulsifier, a phenolic demulsifier and mixed benzene are added into a reaction kettle and mixed uniformly to obtain the demulsifier suitable for crude oil with high wax content, which is named as WD-666 type demulsifier.
7. The demulsifier suitable for crude oil with high wax content according to claim 6, wherein the blending is carried out at 40 ℃ and at a stirring speed of 190r/min for 30-60 min.
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| CN104946298A (en) * | 2015-07-07 | 2015-09-30 | 万达集团股份有限公司 | Crude oil demulsifier and production technology thereof |
| CN111454745A (en) * | 2020-04-02 | 2020-07-28 | 万达集团股份有限公司 | Demulsifier and preparation method thereof |
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| CN102492460A (en) * | 2011-12-21 | 2012-06-13 | 孙安顺 | Preparation method and application of crude oil low-temperature demulsifier |
| CN104946298A (en) * | 2015-07-07 | 2015-09-30 | 万达集团股份有限公司 | Crude oil demulsifier and production technology thereof |
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