CN101050381A - Deemulsifier for lowering oil content in drainage of electrical desalting /dewatering, and preparation method - Google Patents
Deemulsifier for lowering oil content in drainage of electrical desalting /dewatering, and preparation method Download PDFInfo
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Abstract
This invention discloses a method for preparing demulsifier for reducing oil content in water discharged from electrical desalination/dehydration. The demulsifier is composed of: nonionic surfactant 9-50 wt.%, cationic polymer 0.5-20 wt.%, nanoscale water purifier 1-30 wt.%, and alcohol solvent 30-60 wt.%. The method comprises: uniformly mixing nonionic polyether surfactant and solvent at 60-80 deg.C and 500 rpm, cooling to 20-40 deg.C, adding cationic polymer and inorganic nanoscale water purifier, and mixing at 20-40 deg.C and 1500 rpm for 20 min. The demulsifier can change the w/o interfacial tension, and destroy o/w emulsion, w/o emulsion and colloid. The demulsifier can be used in water containing large amounts of w/o emulsion and colloidal impurity particles discharged from electrical desalination/dehydration of crude oil, and have such advantages as low consumption, low oil content in wastewater, clear w/o interface, and high efficiency.
Description
Technical field:
The invention belongs to petrochemical industry, particularly be a kind of emulsion splitter and preparation method who reduces oil-contg in the drainage of electrical desalting/dewatering, both can be used for crude oil demulsification dehydration in the defeated process of oil development collection, can be used for the electric desalting of refinery crude oil again.
Background technology:
The breaking emulsion and dewatering desalination of crude oil emulsion is one of link important in the oil production and the course of processing.The most frequently used crude oil demulsification method of petroleum industry is to add emulsion splitter in crude oil at present, carries out desalting and dewatering under gravity or electric field action, and visible emulsion splitter plays an important role in Desalting and Dewatering from Crude Oil.Along with the continuous intensification of crude oil recovery percent, the well stimulation frequency of utilization of excavating oil field production capacity is also more and more higher, and the composition of oil well produced liquid and character also constantly variation are taking place.Since particularly tertiary oil recovery technology is implemented, polymkeric substance, tensio-active agent, alkali and other chemical have generally been contained in the oil field mining liquid.Medicament self reason (charging property) adds corrosion product and the naturally occurring emulsifying agent that carries in crude oil and the recovered water, influence the type and the stability of water-oil emulsion, except producing water-in-oil emulsion, also produce o emulsion, also there is colloid simultaneously, must influence the result of use of crude oil demulsifier and the normal operation of crude oil electro-chemical dehydrator, the draining oil-containing is exceeded standard.
Petro-chemical corporations such as China part enterprise such as Zhenghai, Nanjing, Guangzhou, Maoming processed some acid-containing raw oils successively, and the acid-containing raw oil price is low, but had than great, characteristics such as condensation point is high, acid number height, brought difficulty for the operation of electric desalting apparatus.Because organic acid and foreign matter content are very high, emulsifying property is very strong, in adding water mixing process, except producing water-in-oil emulsion, also produce o emulsion, the existence owing to charged impurity simultaneously forms colloid, so contains o emulsion in the electric desalting draining, cause the draining oil-containing to exceed standard, bring difficulty to sewage disposal.
The emulsion splitter of electrical desalting/dewatering commonly used mainly is to destroy water-in-oil emulsion at present, does not destroy o emulsion and colloidal component and contain simultaneously.Chinese patent CN1186710 discloses a kind of polymer type crude oil demulsifier that is used for crude oil gathering and transferring process processed.This kind emulsion splitter adopts vinylbenzene, methyl methacrylate, methyl acrylate, butyl acrylate, Isooctyl acrylate monomer, vinylformic acid and methacrylic acid synthetic according to a certain ratio, this kind polymer type crude oil demulsifier and crude oil particularly viscous crude affinity are good, utilize it can obtain good breaking emulsion and dewatering effect.Chinese patent CN1600835 discloses a kind of multifunctional crude oil demulsifying agent preparation method who is used for the refinery crude oil upgrading and products thereof, multifunctional crude oil demulsifying agent has the trimethyl-glycine molecular structure, belong to zwitterionics, this crude oil demulsifier is to be initiator with the organic amine, and propylene oxide, generate polyethers with ethylene oxide polymerization, generate the betaine type molecular structure with the alpha-halogenated carboxylic acids reaction again, this emulsion splitter has efficient breakdown of emulsion and dewatering, simultaneously, carboxyl and quaternary ammonium group and deposit on the molecule, has fabulous wetting effect, it is good calcium dispersion agent that alkaline-earth metal in the crude oil is had fabulous complexing stabilising effect, to the magnesium in the crude oil, iron also has removal effect preferably.It is the crude oil demulsification additive of main active component and the method that is used for crude oil demulsification dehydration thereof with water-soluble organic cationic polymer and inorganic polyaluminium salts that Chinese patent CN1253984 discloses a kind of.This additive and the present general senior alcohol ether of crude oil demulsifier polyoxyethylene polyoxypropylene are used and can under the prerequisite that reduces the emulsion splitter cost breaking emulsion and dewatering ability be improved 10～30%.Though these emulsion splitters can be used for oil field electro-dewatering and refinery electric desalting, do not have function and the broken glue function of destroying water-in-oil emulsion and o emulsion simultaneously.
Summary of the invention
The objective of the invention is at having water-in-oil emulsion, o emulsion and colloidal problem in the oil-water mixture simultaneously, adopt nonionic polyoxyalkylene tensio-active agent, cationic polymers that destroys oil-in-water emulsion that destroys water-in-oil emulsion and the method for destroying colloidal inorganic cation combination of polymers, reduce electric desalting/dewatering device draining oil-contg, thus solve that electric desalting/dewatering device deviates from contain a large amount of oils and bring the problem of difficulty to oily water treatment.
A kind of emulsion splitter that reduces oil-contg in the drainage of electrical desalting/dewatering, comprise nonionic polyoxyalkylene tensio-active agent, cationic polymers, inorganic nano water purification agent and solvent, the weight percent content of its component is: nonionogenic tenside 9-50%, cationic polymers 0.5-20%, inorganic nano water purification agent 1-30%, alcoholic solvent 30-60%.
Described nonionic polyoxyalkylene tensio-active agent is mainly the tetrahydroglyoxaline polyether surfactant, also can be polyvalent alcohol ethylene oxide propylene oxide polymer or polyamine ethylene oxide propylene oxide polymer.
The tetrahydroglyoxaline polyether surfactant has following structural formula:
A is that 20-150, b are that 20-200, c are that 20-150, m are the integer of 2-8 in the formula, and n is the integer of 12-18.
Molecular-weight average gpc measurement value is 3000-9000.
Cationic polymers of the present invention is that commercially available molecular weight is 120,000 to 500,000, ion degree is greater than 20% cationic acrylamide polymer.
Inorganic nano water purification agent of the present invention is that commercially available Al13 content reaches 70%, Al concentration greater than 1mol/l polymeric aluminum solution.
Described solvent of the present invention is for lower-molecular substance commonly used, as methyl alcohol, ethanol etc.
Preparation method of the present invention is: nonionic polyoxyalkylene class tensio-active agent, the solvent of metering are mixed at 60-80 ℃, under the 500rpm rotating speed, mix, be cooled to 20-40 ℃, add cationic acrylamide polymer and inorganic nano water purification agent then, control reaction temperature is not higher than 20-40 ℃, mixes getting final product in 20 minutes under the 1500rpm rotating speed.
Tetrahydroglyoxaline polyether surfactant preparation method:
Proportioning raw materials
Ethylene oxide: propylene oxide=3-4: 5-2 (weight ratio),
Tetrahydroglyoxaline: propylene oxide=1: 40-500 (mol ratio);
Catalyst levels: 0.5-1.0 weight %, in the raw material gross weight;
Temperature of reaction: 110-140 ℃.
Preparation process: the tetrahydroglyoxaline and the alkaline earth metal hydroxides catalyzer of metering are added in the stainless steel cauldron of band water coolant and agitator, be warming up to temperature of reaction, slowly be pressed into the propylene oxide of metering with nitrogen, slowly be pressed into the oxyethane of metering then with nitrogen, the last propylene oxide that is pressed into metering again, cooling can obtain the tetrahydroglyoxaline polyether surfactant.
Polyvalent alcohol ethylene oxide propylene oxide polymer preparation method
Proportioning raw materials
Ethylene oxide: propylene oxide=4～6: 6～2 (weight ratios),
Polyvalent alcohol: propylene oxide=1: 80～300 (mol ratio);
Catalyst levels: 0.4-1.0 weight %, in the raw material total amount;
Temperature of reaction: 100-120 ℃.
Preparation process: the polyvalent alcohol and the alkaline earth metal hydroxides catalyzer of metering are added in the stainless steel cauldron of band water coolant and agitator, be warming up to temperature of reaction, slowly be pressed into the propylene oxide of metering with nitrogen, slowly be pressed into the ethylene oxide of metering then with nitrogen, the last propylene oxide that is pressed into metering again, cooling can obtain polyvalent alcohol ethylene oxide propylene oxide polymer.
Polyamine ethylene oxide propylene oxide polymer preparation method:
Proportioning raw materials
Ethylene oxide: propylene oxide=3～4: 5～3 (weight ratios),
Polyamines: propylene oxide=1: 40～550 (mol ratio);
Catalyst levels: 0.5-1.0 weight %, in the raw material gross weight;
Temperature of reaction: 110-140 ℃.
Preparation process: the polyamine and the alkaline earth metal hydroxides catalyzer of metering are added in the stainless steel cauldron of band water coolant and agitator, be warming up to temperature of reaction, slowly be pressed into the propylene oxide of metering with nitrogen, slowly be pressed into the ethylene oxide of metering then with nitrogen, the last propylene oxide that is pressed into metering again, cooling can obtain polyvalent alcohol ethylene oxide propylene oxide polymer.
The present invention can change oil water interfacial tension, destroy water-in-oil emulsion, o emulsion and colloid simultaneously, it is low to have the sewage with oil of deviating from, water-oil interface are clear, dewatering speed is fast, can generally be applicable to the crude oil extraction liquid of various character, be particularly suitable for draining and contain a large amount of oil-in-water emulsions and colloidal state impurity particle crude oil electric desalting/dehydration breakdown of emulsion.
Embodiment
Embodiment 1
A kind of emulsion splitter that reduces oil-contg in the drainage of electrical desalting/dewatering, by nonionic polyoxyalkylene tensio-active agent, cationic polymers, inorganic nano water purification agent and solvent composition, tetrahydroglyoxaline polyether non-ionic surface active agent 9%, cationic polymers 20%, nanometer purifying agent 30%, methanol solvate 31%.Described nonionic polyoxyalkylene tensio-active agent is the tetrahydroglyoxaline polyether surfactant; Cationic polymers is that commercially available molecular weight is 120,000 to 500,000, ion degree is greater than 20% cationic acrylamide polymer; The inorganic nano water purification agent is that commercially available Al13 content reaches 70%, Al concentration greater than 1mol/l polymeric aluminum solution.Solvent is a methyl alcohol.
The preparation method mixes the tetrahydroglyoxaline polyether surfactant of above-mentioned metering, solvent heating for 60 ℃, under the 500rpm rotating speed, mix, be cooled to 30 ℃, add cationic polymers and nanometer purifying agent at last, control reaction temperature is not higher than 35 ℃, mixes getting final product in 20 minutes under the 1500rpm rotating speed.
The emulsion splitter that adopts present embodiment production is to density 0.93g/cm
3, acid number is that the Sudan's high-acid crude oil of 3.5mgKOH/g experimentizes, its result is as follows:
But the Sudan high-acid crude oil 50ml injects 100ml added electric field graduated cylinder, adds various chemical demulsifiers (concentration 1%) 0.15ml (30ppm), and graduated cylinder is placed 60 ℃ of waters bath with thermostatic control, back and forth shake 200 times with hand, added electric field 800V/cm 10 minutes leaves standstill graduated cylinder then, and cases of dehydration sees Table 1.
Table 1 emulsion splitter cases of dehydration
| Sequence number | Emulsion splitter | Deviate from water (ml) | Deviate from water oil length ppm | Deviate from the water color |
| 1 | Emulsion splitter of the present invention | 40 | 60 | Clearly |
| 2 | 191 | 25 | 320 | Black |
| 3 | AE-750 | 29 | 450 | Black |
| 4 | AE7920 | 38 | 600 | Black |
| 5 | 204 | 37 | 270 | Yellow |
| 6 | FC96 | 15 | 300 | Black |
| 7 | GT94 | 26 | 400 | Black |
| 8 | ST-141 | 16 | 200 | Yellowish-brown |
| 9 | BP204 | 25 | 380 | Black |
By test-results as can be seen, for the Sudan's high-acid crude oil, demulsification performance of the present invention obviously is better than other emulsion splitter, and oil-contg is reduced to qualified level in the drainage water.
Embodiment 2
The described nonionic polyoxyalkylene tensio-active agent of present embodiment is mainly polyamine ethylene oxide propylene oxide polymer; Described cationic polymers is that commercially available molecular weight is 120,000 to 500,000, ion degree is greater than 20% cationic acrylamide polymer; Described inorganic nano water purification agent is that commercially available Al13 content reaches 70%, Al concentration greater than 1mol/l polymeric aluminum solution.Described solvent is a methyl alcohol.Polyamine ethylene oxide propylene oxide polymer nonionogenic tenside 50%, cationic polymers 0.5%, inorganic nano water purification agent 1%, methanol solvate 48.5%.
The preparation method of present embodiment mixes the polyamine polyether surfactant of above-mentioned metering, solvent heating for 70 ℃, under the 500rpm rotating speed, mix, be cooled to 30 ℃, add cationic polymers and inorganic nano water purification agent at last, control reaction temperature is not higher than 30 ℃, mixes getting final product in 20 minutes under the 1500rpm rotating speed.
The emulsion splitter that adopts present embodiment production is under 50 ℃ of conditions, to density 0.94g/cm
3, acid number experimentizes for the 1.5mgKOH/g lu ning pipeline transportation of crude oil, and its result is as follows:
Pipeline oil 50ml injects 100ml tool plug graduated cylinder, and water filling 10ml adds various chemical demulsifiers (concentration 1%) 0.15ml (10ppm), graduated cylinder is placed 60 ℃ of waters bath with thermostatic control, back and forth shake 200 times, left standstill 20 minutes with hand, leave standstill graduated cylinder then, observe cases of dehydration, cases of dehydration sees Table 2.
Table 2 emulsion splitter cases of dehydration
| Sequence number | Emulsion splitter | Deviate from water ml | Deviate from water oil-containing ppm | Deviate from the water color |
| 1 | Emulsion splitter of the present invention | 10 | 40 | Clearly |
| 2 | 1910 | 6 | 230 | Black |
| 3 | AE-750 | 9 | 350 | Black |
| 4 | AE7920 | 8 | 200 | Black |
| 5 | 204 | 7 | 370 | Black |
| 6 | FC961 | 5 | 100 | Black |
| 7 | GT940 | 6 | 400 | Black |
| 8 | ST-14 | 6 | 200 | Black |
| 9 | BP2040 | 5 | 120 | Black |
By test-results as can be seen, for lu ning pipeline transportation of crude oil, demulsification performance of the present invention and reduction are deviate from water oil-contg aspect and obviously are better than other emulsion splitter.
Embodiment 3
Present embodiment is by nonionic polyoxyalkylene tensio-active agent, cationic polymers, inorganic nano water purification agent and solvent composition, the weight percent content of its component is: tetrahydroglyoxaline polyether non-ionic surface active agent 40%, cationic polymers 1%, nanometer purifying agent 1%, alcohol solvent 58%.
The preparation method of present embodiment mixes the tetrahydroglyoxaline polyether surfactant of above-mentioned metering, solvent heating for 60 ℃, under the 500rpm rotating speed, mix, be cooled to 30 ℃, add cationic polymers and nanometer purifying agent at last, control reaction temperature is not higher than 35 ℃, mixes getting final product in 20 minutes under the 1500rpm rotating speed.
This emulsion splitter is used at 2,500,000 tons of/year electric desalting apparatus of certain refinery, and processing crude oil is multiple import high-acid crude oil and Bohai Sea commingled crude, this oil density 0.90g/cm
3, acid number is 1.1mgKOH/g, application result such as table 3.
Use before the emulsion splitter of the present invention, draining is a black, and oil-containing has a strong impact on the operation of sewage treatment facility in the draining between 500-2000ppm; Take off the back saliferous at 3-6.5mg/l; It is moisture about 0.2% to take off the back, emulsion splitter consumption 30ppm.
Operational condition: 120 ℃ of service temperatures, strength of electric field 400-1000V/cm.
Table 3 reduces the emulsion splitter application result of electric desalting/dewatering device draining oil-contg
| Treatment capacity t/h | Output voltage KV | Breakdown of emulsion dosage ppm | Temperature ℃ | Water injection rate % | Take off the oily moisture % in back | Salt content in crud oil mg/l | Take off back saliferous mg/l | Deviate from water oil-containing ppm |
| 300 | 19 | 9 | 120 | 3.5 | 0.10 | 45 | 3.0 | 149 |
| 315 | 19 | 10 | 118 | 2.5 | 0.17 | 25 | 2.7 | 113 |
| 310 | 19 | 8 | 109 | 2.5 | 0.14 | 35 | 2.9 | 115 |
| 320 | 19 | 7 | 120 | 2.5 | 0.24 | 55 | 2.6 | 126 |
| 311 | 19 | 8 | 119 | 2.4 | 0.2 | 69 | 2.8 | 99 |
Service data shows that the emulsion splitter of this device device employing reduction oil-contg in the drainage of electrical desalting/dewatering between the oil-containing 99-150ppm, takes off the back saliferous and also obviously reduces in the draining after treatment, takes off the back saliferous 2.6-3.0mg/l (standard is less than 3mg/l); It is moisture about 0.2% (standard is less than 0.3%) to take off the back; Below the emulsion splitter consumption 10ppm.
Claims (5)
1. emulsion splitter that reduces oil-contg in the drainage of electrical desalting/dewatering, comprise nonionic polyoxyalkylene tensio-active agent, cationic polymers, inorganic nano water purification agent and solvent, the weight percent content of its component is: nonionogenic tenside 9-50%, cationic polymers 0.5-20%, inorganic nano water purification agent 1-30%, alcoholic solvent 30-60%, wherein the nonionic polyoxyalkylene tensio-active agent is tetrahydroglyoxaline polyether surfactant or polyvalent alcohol ethylene oxide propylene oxide polymer or polyamine ethylene oxide propylene oxide polymer; Cationic polymers is that commercially available molecular weight is 120,000 to 500,000, ion degree is greater than 20% cationic acrylamide polymer, the inorganic nano water purification agent is that commercially available Al13 content reaches 70%, Al concentration greater than 1mol/l polymeric aluminum solution, alcoholic solvent is methyl alcohol, ethanol class lower-molecular substance.
2. a kind of according to claim 1 emulsion splitter that reduces oil-contg in the drainage of electrical desalting/dewatering, the preparation method who it is characterized in that emulsion splitter is: nonionic polyoxyalkylene class tensio-active agent, the solvent of metering are mixed at 60-80 ℃, under the 500rpm rotating speed, mix, be cooled to 20-40 ℃, add cationic acrylamide polymer and inorganic nano water purification agent then, control reaction temperature is 20-40 ℃, mixes getting final product in 20 minutes under the 1500rpm rotating speed.
3. a kind of as claimed in claim 1 or 2 emulsion splitter that reduces oil-contg in the drainage of electrical desalting/dewatering, what it is characterized in that nonionic polyoxyalkylene class tensio-active agent uses is the tetrahydroglyoxaline polyether surfactant, tetrahydroglyoxaline polyether surfactant preparation method is:
Proportioning raw materials:
Ethylene oxide: propylene oxide=3-4: 5-2, weight ratio,,
Tetrahydroglyoxaline: propylene oxide=1: 40-500, mol ratio;
Catalyst levels: 0.5-1.0 weight %, in the raw material gross weight;
Temperature of reaction: 110-140 ℃;
Preparation process: the tetrahydroglyoxaline and the alkaline earth metal hydroxides catalyzer of metering are added in the stainless steel cauldron of band water coolant and agitator, be warming up to temperature of reaction, slowly be pressed into the propylene oxide of metering with nitrogen, slowly be pressed into the oxyethane of metering then with nitrogen, the last propylene oxide that is pressed into metering again, cooling can obtain the tetrahydroglyoxaline polyether surfactant.
4. a kind of as claimed in claim 1 or 2 emulsion splitter that reduces oil-contg in the drainage of electrical desalting/dewatering is characterized in that nonionic polyoxyalkylene class tensio-active agent is a polyvalent alcohol ethylene oxide propylene oxide polymer, and the preparation method is:
Proportioning raw materials is:
Ethylene oxide: propylene oxide=4～6: 6～2, weight ratio,
Polyvalent alcohol: propylene oxide=1: 80～300, mol ratio,
Catalyst levels: 0.4-1.0 weight %, in the raw material total amount;
Temperature of reaction: 100-120 ℃.
Preparation process: the polyvalent alcohol and the alkaline earth metal hydroxides catalyzer of metering are added in the stainless steel cauldron of band water coolant and agitator, be warming up to temperature of reaction, slowly be pressed into the propylene oxide of metering with nitrogen, slowly be pressed into the ethylene oxide of metering then with nitrogen, the last propylene oxide that is pressed into metering again, cooling can obtain polyvalent alcohol ethylene oxide propylene oxide polymer.
5. a kind of as claimed in claim 1 or 2 emulsion splitter that reduces oil-contg in the drainage of electrical desalting/dewatering is characterized in that nonionic polyoxyalkylene class tensio-active agent is a polyamine ethylene oxide propylene oxide polymer, and the preparation method is:
Proportioning raw materials
Ethylene oxide: propylene oxide=3～4: 5～3, weight ratio,
Polyamines: propylene oxide=1: 40～550, mol ratio,
Catalyst levels: 0.5-1.0 weight %, in the raw material gross weight;
Temperature of reaction: 110-140 ℃;
Preparation process: the polyamine and the alkaline earth metal hydroxides catalyzer of metering are added in the stainless steel cauldron of band water coolant and agitator, be warming up to temperature of reaction, slowly be pressed into the propylene oxide of metering with nitrogen, slowly be pressed into the ethylene oxide of metering then with nitrogen, the last propylene oxide that is pressed into metering again, cooling can obtain polyvalent alcohol ethylene oxide propylene oxide polymer.
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