CN107841334B - Synthetic method of novel crude oil demulsifier suitable for complex incoming liquid - Google Patents
Synthetic method of novel crude oil demulsifier suitable for complex incoming liquid Download PDFInfo
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- CN107841334B CN107841334B CN201711216253.2A CN201711216253A CN107841334B CN 107841334 B CN107841334 B CN 107841334B CN 201711216253 A CN201711216253 A CN 201711216253A CN 107841334 B CN107841334 B CN 107841334B
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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 synthetic method of a novel crude oil demulsifier suitable for complex incoming liquid. Mainly solves the problems of narrow application range, small molecular weight and high requirement on operating conditions of the oil-water separation of the prior demulsifier. The method is characterized in that: the method comprises the following steps: (1) synthesizing polyether C: adding epichlorohydrin into raw materials polyether A and B, and controlling the temperature at 70-90 ℃ under the action of a catalyst to generate polyether C with the molecular weight of 10000-; (2) synthesizing polyether D: under the action of a catalyst, fatty alcohol and propylene oxide are subjected to polymerization reaction at 130-180 ℃, and then are subjected to polymerization reaction with ethylene oxide at 120-150 ℃ to synthesize block polyether D with the molecular weight of 2000-2800; (3) synthesizing an oil field demulsifier: methanol is added into polyether C and polyether D to synthesize the oil field demulsifier with the molecular weight of 5000-13000. The synthetic method can meet the requirements of oil-water separation under various conditions, greatly reduces the using amount and the difficulty of on-site oil-water separation operation, and simultaneously reduces the crude oil recovery cost.
Description
Technical Field
The invention relates to the field of chemical treatment agents for oil field development produced liquid, in particular to a synthesis method of a novel crude oil demulsifier suitable for incoming liquid under various complex conditions such as polymer flooding, well flushing, sand washing, acidification, flowback and the like.
Background
A demulsifier is a surfactant that breaks emulsions. Demulsifiers break emulsions primarily by the action of partially displacing the stabilizing membrane. The dehydrating agent is used for dehydrating crude oil and heavy oil to ensure that the water content of the crude oil and the heavy oil meets the requirement; can be used in oil well to reduce the viscosity of crude oil and prevent oil well from blocking.
At present, the oil-water separation of crude oil in an oil field mainly adopts a non-ionic demulsifier, and the non-ionic demulsifier does not dissociate ions after being dissolved in water, so that the non-ionic demulsifier has no electric charge. The non-ionic demulsifier mainly comprises a block polyether taking amines as an initiator, a block polyether taking alcohols as an initiator, an alkyl phenolic resin block polyether, a phenolic amine aldehyde resin block polyether, a silicon-containing demulsifier, an ultrahigh relative molecular mass demulsifier, polyphosphate, a modified product of the block polyether and a zwitterionic demulsifier represented by an imidazoline crude oil demulsifier.
Disclosure of Invention
The invention provides a synthetic method of a novel crude oil demulsifier suitable for complex incoming liquid, aiming at overcoming the problems of narrow application range of oil-water separation, small molecular weight, short branched chain, high requirement on operating conditions, large dosage and incapability of coping with the complex incoming liquid of the existing demulsifier in the background art. The synthetic method of the novel crude oil demulsifier suitable for the complex incoming liquid can meet the requirements of oil-water separation under various conditions, greatly reduces the using amount and the difficulty of on-site oil-water separation operation, and simultaneously reduces the crude oil recovery cost.
The invention can solve the problems by the following technical scheme: a synthetic method of a novel crude oil demulsifier adapting to complex incoming liquid comprises the following steps:
the method comprises the following steps:
(1) synthesizing a demulsification dehydration main agent polyether C:
the raw materials are polyether A and polyether B, epichlorohydrin is added into the raw materials polyether A and polyether B, the temperature is controlled to be 70-90 ℃ under the action of a catalyst KOH, and polyether C with the molecular weight of 10000-16000 is generated;
(2) synthesizing a demulsification water purification main agent polyether D:
under the action of a catalyst KOH, fatty alcohol and propylene oxide are subjected to polymerization reaction at the temperature of 130-180 ℃, and then are subjected to polymerization reaction with ethylene oxide at the temperature of 120-150 ℃ to synthesize block polyether D with the molecular weight of 2000-2500;
(3) and (3) synthesis of a crude oil demulsifier:
adding a certain amount of methanol and desalted water into the two raw materials of the demulsification dehydration main agent polyether C and the synthetic demulsification water purification main agent polyether D synthesized in the steps (1) and (2), and fully mixing at 40-50 ℃ to synthesize the novel crude oil demulsifier with the molecular weight of 5000-13000.
Compared with the background technology, the invention has the following beneficial effects: the crude oil demulsifier produced by the invention is a novel crude oil demulsifier which is suitable for incoming liquid under various complex conditions such as polymer flooding, well flushing, sand washing, acidification, flowback and the like, and can destroy the structure of emulsified liquid so as to achieve the purpose of separating each phase in the emulsion. The demulsifier separates oil and water in emulsified oil-water mixed liquid, so that the purpose of crude oil dehydration is achieved, the standard of water output of crude oil is ensured, the use amount is reduced to the minimum, the original recovery ratio is improved, and the cost is reduced.
Description of the drawings:
FIG. 1 is a usage graph of the product of the present invention for field use;
FIG. 2 is a graph of dosing concentration for field application of the product of the present invention;
FIG. 3 is a graph of water content of export crude oil applied to the product of the present invention on site;
FIG. 4 is a graph showing the oil content of sewage at the inlet of a sedimentation tank for on-site application of the product of the present invention;
FIG. 5 is a graph showing the oil content of sewage at the outlet of a sedimentation tank in the field application of the product of the present invention.
The specific implementation mode is as follows:
the invention will be further illustrated with reference to specific examples:
example 1
1. Preparing base polyether A and base polyether B:
preparation of base polyether a: polyether A is phenolic resin type basic polyether, 1% of phenolic resin and 73.8% of propylene oxide are subjected to polymerization reaction at the temperature of 140-135 ℃ under the action of 0.2% of catalyst KOH to generate an oil head, and then are subjected to polymerization reaction with 25% of ethylene oxide at the temperature of 125-135 ℃ to synthesize block polyether with a branch structure, wherein the molecular weight is about 2200; wherein the dosage of the phenolic resin, the potassium hydroxide, the propylene oxide and the ethylene oxide is calculated by taking the total amount of the phenolic resin, the potassium hydroxide, the propylene oxide and the ethylene oxide as the total amount.
Preparation of base polyether B: polyether B is phenol amine resin type basic polyether, 1% of phenol amine resin and 64.8% of propylene oxide are subjected to polymerization reaction at the temperature of 140-150 ℃ under the action of 0.2% of catalyst KOH to generate an oil head, and then the oil head and 34% of ethylene oxide are subjected to polymerization reaction at the temperature of 125-135 ℃ to synthesize block polyether with the molecular weight of about 2800 and a branch structure; wherein the dosage of the phenolic amine resin, the potassium hydroxide, the propylene oxide and the ethylene oxide is calculated by taking the total amount of the phenolic amine resin, the potassium hydroxide, the propylene oxide and the ethylene oxide as the total amount.
2. Synthesizing a demulsification dehydration main agent polyether C:
mixing 40% of polyether A and 58.4% of polyether B (accounting for the total amount), then using 1% of epoxy chloropropane as a cross-linking agent, and under the action of a catalyst of 0.6% of KOH, controlling the temperature to be 75-85 ℃, so that the hydroxyl of a part of hydrophilic sections of the block polyether is connected with the epoxy chloropropane through ether bonds to form a net structure, and generating novel polyether C with the molecular weight of about 10000; wherein the use amounts of the polyether A, the polyether B, the epichlorohydrin and the potassium hydroxide are calculated by taking the polyether A, the polyether B, the epichlorohydrin and the potassium hydroxide as total amounts.
3. Polyether D as main agent for synthetic demulsifying water purification
Under the action of 0.2 percent of catalyst KOH, 0.1 percent of C18 fatty alcohol and 64.7 percent of propylene oxide are polymerized at the temperature of 140-150 ℃, and then are polymerized with 35 percent of ethylene oxide at the temperature of 125-135 ℃ to synthesize block polyether D, and the polyether has a linear structure, the molecular weight is about 2000, and has better water purification capacity; wherein the use amount of the fatty alcohol, the propylene oxide and the ethylene oxide is calculated by taking the fatty alcohol, the propylene oxide and the ethylene oxide as the total amount.
4. Demulsifier for synthetic crude oil
And mixing the synthesized 30% of demulsification and dehydration main agent polyether C and 20% of demulsification and water purification main agent polyether D, adding 20% of methanol and 30% of desalted water, and fully mixing at 40 ℃ to synthesize the demulsifier with the molecular weight of about 7200, wherein the dosage of the polyether C, the polyether D, the methanol and the desalted water is calculated by taking the polyether C, the polyether D, the methanol and the desalted water as the total amount.
Example 2
1. Preparing base polyether A and base polyether B: the same as example 1;
2. synthesizing a demulsification dehydration main agent polyether C:
mixing 40% of polyether A and 58.08% of polyether B, then using 1.2% of epoxy chloropropane as a cross-linking agent, and under the action of 0.72% of catalyst KOH, controlling the temperature to be 75-85 ℃, so that the hydroxyl of partial hydrophilic segment of block polyether is connected with epoxy chloropropane through ether bond to form a net structure, and generating demulsification dehydration main agent polyether C with the molecular weight of about 12000; wherein the use amounts of the polyether A, the polyether B, the epichlorohydrin and the potassium hydroxide are calculated by taking the polyether A, the polyether B, the epichlorohydrin and the potassium hydroxide as total amounts.
3. Polyether D as main agent for synthetic demulsifying water purification
Under the action of 0.2 percent KOH of catalyst, 0.15 percent C18 fatty alcohol and 59.65 percent propylene oxide are polymerized at the temperature of 140-150 ℃, and then polymerized with 40 percent ethylene oxide at the temperature of 125-135 ℃ to synthesize block polyether D, which has a linear structure, the molecular weight of about 2200 and better water purification capacity; wherein the use amount of the fatty alcohol, the propylene oxide, the ethylene oxide and the potassium hydroxide is calculated by taking the total amount of the fatty alcohol, the propylene oxide, the ethylene oxide and the potassium hydroxide as the total amount.
4. Synthetic oil field demulsifier
Mixing 40% of synthesized dehydrated main agent polyether C and 10% of synthesized purified water main agent D, then adding 20% of methanol and 30% of desalted water, and fully mixing at 40 ℃ to synthesize the demulsifier with the molecular weight of about 9600, wherein the dosage of the polyether C, the polyether D, the methanol and the desalted water is the total amount of the polyether C, the polyether D, the methanol and the desalted water.
The structural formula of the main molecules of the crude oil demulsifier product synthesized by the invention is as follows:
demulsifying and dehydrating main agent C:
wherein m is 2-4, n is 12-16, and p is 2-3; p is 2-3; x is 3-15, y is 4-12
Demulsifying and water purifying main agent D:
R(PO)x(EO)y(PO)zH
wherein, R is C16-C18 fatty alcohol, x is 3-15, y is 4-12, z is 5-181, the main index of the crude oil demulsifier product of the invention
The method comprises the following steps: brown yellow viscous liquid
The molecular weight is as follows: 5000 to 13000
The quality indexes of the third step are shown in table 1:
TABLE 1
Fourth, an experimental method: taking liquid by adopting a separating funnel, adding a medicament, oscillating, standing and heating the water bath kettle for 40 minutes at a constant temperature of 45 ℃, turning and standing for 1 minute, taking an upper layer oil sample to detect the water content, taking a lower layer water sample to detect the oil content, and observing the interface condition.
Experiment of medicament EN129 used on site and demulsifier prepared in example 1
TABLE 2
As can be seen from the table 2, under the condition that the field agent and the demulsifier in the embodiment 1 have the same concentration, various detection indexes show that the oil-water separation effect of the demulsifier in the embodiment 1 is obviously better than that of the field agent, when the chemical concentration of the demulsifier in the embodiment 1 is 6-8 ppm, the incoming liquid treatment effect is the best, and the transition layer is obviously reduced and leveled.
2. The crude oil demulsifier product of the invention is actually produced on site
And the southern-quintuplet station is used as a field experiment module. The daily liquid is about 17500m3, and the daily crude oil yield is about 1800 tons. At present, 200kg of demulsifier product EN129 produced by the Tangjie chemical industry is added every day, and the adding concentration is about 12ppm for continuously adding the medicine.
Test time
The experimental time of the patent is as follows: 11 month, 7 days 11: 00-11 month, 17 days 11: 00 for a total of 10 days.
A process of field testing
The southern quintet station has been tested with an existing dosing system. Firstly, closing a dosing system valve and a pump, leading the agent (the oil-water separating agent) used in Tangjie out of a dosing tank and cleaning the tank; the DQD series demulsifier was then injected into the dosing tank. And (4) restarting a dosing system pump and a valve, and inspecting the optimal use concentration of the test medicament by changing the dosing concentration.
Firstly, 11 am on 11 months, 7 days, the demulsifier produced by the invention is used (no medicine is left in the system for 3 hours because of pump stopping, tank cleaning and medicine changing), and the knob of the medicine feeding pump is adjusted to 100% of discharge capacity;
adjusting the knob of the dosing pump to 50% of discharge capacity when 11 am on 9 months of 11 months;
③ 11 months, 11 am, the dosing pump knob is adjusted to 35% displacement.
The production and operation conditions are as follows:
the product field production operation record report of the invention is shown in the table 3:
TABLE 3
As can be seen from the production operation condition table, the demulsifier of the invention is applied for 10 days totally, the treated liquid amount is 173846m3, the output pure oil amount is 18363 tons, the back flushing is carried out for 4 days in the period, the production fluctuation is small, the cumulative dosage is 1800kg in 10 days, the average dosage concentration is 10.2ppm, the dosage concentration is reduced to 7ppm in the last 6 days, the average water content of the output oil is 0.09%, the average oil content of the sewage at the inlet of the settling tank is 516.5mg/l, and the average oil content of the sewage at the outlet of the settling tank is 184.3 mg/l.
Fourth use condition analysis
Firstly, the chemical adding condition is analyzed
FIG. 1 is a usage amount chart of the product of the invention applied on site, and as can be seen from FIG. 1, the dosage of the medicament used in normal production is 200 kg/day, the stable production period of 6 scales after the medicament of the invention is adopted is kept at 125 kg/day, 75kg of the medicament is used less every day, and 24.75 tons of the medicament can be used less every year according to 330 days production.
FIG. 2 is a dosing concentration graph of the product of the invention applied on site, and it can be seen from FIG. 2 that the concentration of the drug of the invention in the stable production period of 6 balances after dosing concentration is controlled at 7ppm, which is 5 ppm lower than the daily rated dosing concentration of 12 ppm.
② analysis of water content of export crude oil
FIG. 3 is a diagram of water content of export crude oil for field application of the product of the present invention, and it can be seen from FIG. 3 that the water content of the export crude oil is below 0.1% and 66% lower than the standard of 0.3%.
Analysis of oil-containing condition of sewage at inlet of settling tank
FIG. 4 is a graph showing the oil content of sewage at the inlet of a settling tank for on-site application of the product of the present invention, and it can be seen from FIG. 4 that the sewage at the inlet of the settling tank is in an adjustment period for 7 days and 8 days, the oil content is high, and the oil content is controlled below the index of 800mg/l all the time from 9 to 17 days. The average value of the oil content of the sewage at the inlet of the settling tank is 516.5mg/l after 10 days of operation, which is 35.4 percent lower than the control index of 800 mg/l; after the operation is stable, the balance 6 is 334mg/l, which is 58.2 percent lower than the control index.
Analysis of oil-containing condition of sewage at outlet of sedimentation tank
Referring to FIG. 5, the oil content of the sewage at the outlet of the settling tank is 184.3mg/l on average, and 175mg/l at the lowest, which are lower than the control index of 240mg/l, as can be seen from FIG. 5.
The results of field experiments of the demulsifier of the invention show that each detection index is superior to the original indexes such as: the concentration of the device in the stable production period is controlled to be 7ppm, and is 5 ppm lower than the daily rated dosing concentration of 12ppm of the demulsifier used in the current production. The dosage of the medicament used in the current production is 200 kg/day, after the demulsifier produced by the invention is adopted, the dosage of the medicament used in the stable production period of the device is 125 kg/day, the medicament is used less by 75kg every day, and the medicament can be used less by 24.75 tons every year according to 330 days production. The average value of the water content of the external oil transportation is 0.09 percent (the control index is 0.3 percent), the average value of the oil content of the sewage at the inlet of the settling tank is 516.5mg/l (the control index is 800mg/l), and the average value of the oil content of the sewage at the outlet of the settling tank is 184.3mg/l (the control index is 240 mg/l).
According to laboratory test indexes and field 10-day actual production application, the demulsifier provided by the invention is greatly improved on the basis of overcoming the defects of the existing demulsifier, not only is the field actual production requirement met, but also each index is obviously superior to the existing demulsifier in detection, and meanwhile, the dosage is greatly reduced, the requirements under various operating conditions are met, and the cost of oil-water separation is also reduced.
Claims (4)
1. A synthetic method of a novel crude oil demulsifier suitable for complex incoming liquid is characterized by comprising the following steps: the method comprises the following steps:
(1) synthesizing a demulsification dehydration main agent polyether C:
the raw materials are polyether A and polyether B, epichlorohydrin is added into the raw materials polyether A and polyether B, the temperature is controlled to be 70-90 ℃ under the action of a catalyst KOH, and polyether C with the molecular weight of 10000-16000 is generated;
(2) synthesizing a demulsification water purification main agent polyether D:
under the action of a catalyst KOH, fatty alcohol and propylene oxide are subjected to polymerization reaction at the temperature of 130-180 ℃, and then are subjected to polymerization reaction with ethylene oxide at the temperature of 120-150 ℃ to synthesize block polyether D with the molecular weight of 2000-2500; the fatty alcohol is C16-C18 fatty alcohol;
(3) and (3) synthesis of a crude oil demulsifier:
adding a certain amount of methanol and desalted water into the two raw materials of the demulsification dehydration main agent polyether C and the synthetic demulsification water purification main agent polyether D synthesized in the steps (1) and (2), and fully mixing at 40-50 ℃ to synthesize a novel crude oil demulsifier with the molecular weight of 5000-13000;
the polyether A in the step (1) is phenolic resin type basic polyether, which is block polyether with a branch structure, is synthesized by polymerization reaction of phenolic resin and propylene oxide at the temperature of 130-180 ℃ under the action of a catalyst KOH, and then polymerization reaction of the phenolic resin and ethylene oxide at the temperature of 120-150 ℃, and the molecular weight is 2000-2800;
the polyether B is phenol amine resin type basic polyether, and is block polyether which has a molecular weight of 2200-3500 and a branch structure and is synthesized by carrying out polymerization reaction on phenol amine resin and propylene oxide at the temperature of 130-180 ℃ under the action of a catalyst KOH to generate an oil head and then carrying out polymerization reaction on the oil head and ethylene oxide at the temperature of 120-150 ℃;
the total weight of two polyethers A and B for preparing the crude oil demulsifier in the step (1) is calculated by 100 percent, wherein the weight percentage of the polyether A is 20 to 80 percent, the weight percentage of the polyether B is 80 to 20 percent, and the weight percentage of epichlorohydrin is 1 to 2 percent; step (2) taking fatty alcohol, propylene oxide and ethylene oxide as the total weight, wherein the total weight is 100%, the weight percentage of the fatty alcohol is 0.01-0.2%, the weight percentage of the propylene oxide is 50-80%, and the weight percentage of the ethylene oxide is 50-20%; and (3) taking the demulsification dehydration main agent polyether C, the demulsification water purification main agent polyether D, the methanol and the desalted water as the total weight, wherein the total weight is 100%, the weight percentage of the dehydration main agent polyether C is 15-40%, the weight percentage of the water purification main agent polyether D is 35-10%, the weight percentage of the methanol is 20%, and the weight percentage of the desalted water is 30%.
2. The method for synthesizing the novel crude oil demulsifier adapting to complex incoming liquid according to claim 1, wherein the method comprises the following steps: polyether A is prepared from (by weight) phenolic resin 1%, catalyst KOH 0.2%, propylene oxide 73.8%, and ethylene oxide 25%, with the total weight of phenolic resin, catalyst KOH, propylene oxide, and ethylene oxide being 100%; polyether B is prepared from (by weight) phenolic amine resin 1%, catalyst KOH 0.2%, propylene oxide 64.8%, and ethylene oxide 34%, by taking phenolic amine resin, catalyst KOH, propylene oxide, and ethylene oxide as total weight 100%.
3. The method for synthesizing the novel crude oil demulsifier adapting to complex incoming liquid according to claim 1, wherein the method comprises the following steps: the structural formula of the demulsification dehydration main agent polyether C is as follows:
wherein m is 2-4, n is 12-16, and p is 2-3; x is 3-15, and y is 4-12.
4. The method for synthesizing the novel crude oil demulsifier adapting to complex incoming liquid according to claim 1, wherein the method comprises the following steps: the structural formula of the demulsification water purification main agent polyether D is as follows:
R(PO)x(EO)y(PO)zH
wherein, R is fatty alcohol of C16-C18, x is 3-15, y is 4-12, and z is 5-18.
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