CN101831316A - Polyelement composite heavy oil emulsion splitter and preparation method thereof - Google Patents
Polyelement composite heavy oil emulsion splitter and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyelement composite heavy oil emulsion splitter and a preparation method thereof. The heavy oil emulsion splitter comprises the following components in percentage by weight: 30-55 percent of polyether, 5-15 percent of surface active agent and 40-60 percent of solvent, wherein the polyether is formed by mixing polyethylene polyamine polyoxyethylene polyoxypropylene ether and fatty alcohol polyoxyethylene polyoxypropylene ether, the surface active agent is polyacrylic acid, and the solvent comprises ethanol and deionized water. The heavy oil emulsion splitter is mainly used for the water scrubbing purification of heavy oil of a gas-turbine power plant and has emulsion splitter dosage of 100-300ppm and good emulsion splitting effect; the K and Na total content of purified heavy oil is less than 1ppm, an oil-water interface is clear, and the water content of the purified heavy oil is less than 0.4 percent and has good broad spectrum activity and lower cost. The polyelement composite heavy oil emulsion splitter can also be used for processing inferior crude oil or crude oil mixed with heavy oil with a larger proportion before catalysis and cracking.
Description
Technical field
The present invention relates to a kind of polyelement composite heavy oil emulsion splitter and preparation method thereof, particularly a kind of at the combustion heavy oil demetalization of dynamo-electric factory (potassium, sodium, calcium) use high-efficient demulsifier.
Background technology
Heavy oil also claims residual oil, and being crude oil extracts Residual oil behind the distillate through normal pressure or vacuum distillation apparatus, or by the cracking Residual oil of extracting out at the bottom of the high-temperature pressurizing cracking evaporator tower, or is mixed, also or add the heavy crude fuel that an amount of cracking Residual oil is made by the two.Its viscosity height, detrimental impurity content height, complicated component.Contain detrimental impurity such as S, Na, K, V, Ca in the heavy oil, when heavy oil acts as a fuel high temperature, the SO that S generates
2, SO
3Can generate Na with NaCl, KCl reaction Deng corrosives
2SO
4And K
2SO
4, and V is oxidized to V
2O
5Work as V
2O
5, Na
2SO
4And K
2SO
4Be deposited on the hardware surface with molten state, can bring out serious vanadium corrosion.Na, K in the heavy oil, V equal size are high more, and it can cause the metallic surface havoc to the corrosion that equipment produces in combustion processes.Calcium impurities in the heavy oil forms metal oxide in combustion processes, the serious thermal etching of metallic surface generation to high-temperature part also can fouling produce underdeposit corrosion to equipment.
Along with the day of petroleum resources is becoming tight, the quality of heavy oil worse and worse.Except that nuisance impurity, organic in the heavy oil, asphalt content is high, organic and bituminous matter is natural emulsifying agent, and it can make the emulsion-stabilizing of heavy oil and water formation, so slag is much more difficult than the breakdown of emulsion of crude oil.The K that contains in the heavy oil, the big multipotency of Na salt are water-soluble, and Ca salt exists with organic calcium mostly, is mainly petroleum acid calcium (lipid acid, naphthenic acid etc.), and is water insoluble substantially, therefore, it is very difficult to reach impurity such as the K, the Na that purify simultaneously in the heavy oil, Ca by the washing desalination.Its component of heavy oil and the detrimental impurity difference of the different places of production, different sources are very big, and general emulsion splitter is difficult to reach the effect that purifies impurity and efficient breakdown of emulsion.
Fire dynamo-electric factory detrimental impurity content in the heavy oil of its use is had strict requirement, the K+Na total content is less than 1ppm in the combustion machine inlet heavy oil, Ca content is less than 10ppm, emulsion splitter energy high efficiency separation profit, water-oil interface are clear, the heavy oil water content is less than 0.4%, and existing emulsion splitter can not satisfy its service requirements.
Summary of the invention
For overcoming above-mentioned the deficiencies in the prior art, requirement according to the dynamo-electric factory of combustion counterweight oil purification breakdown of emulsion, primary and foremost purpose of the present invention is to provide a kind of broad spectrum type polyelement composite heavy oil emulsion splitter, and this heavy oil emulsion splitter can effectively be removed detrimental impurity such as heavy oil K+Na and Ca, high efficiency separation profit.
Another object of the present invention is to the preparation method that provides above-mentioned.
For achieving the above object, the invention provides following technical scheme: a kind of polyelement composite heavy oil emulsion splitter, described heavy oil emulsion splitter is made up of following component by weight percentage:
Polyethers 30~55%,
Tensio-active agent 5~15%,
Solvent 40~60%,
Described polyethers is that polyethylene polyamine polyoxyethylene poly-oxygen propylene aether and aliphatic alcohol polyethenoxy polyethenoxy ether mix, and described tensio-active agent is a polyacrylic acid, and described solvent is ethanol and deionized water.
The weight ratio of described polyethylene polyamine polyoxyethylene poly-oxygen propylene aether and aliphatic alcohol polyethenoxy polyethenoxy ether is 1: 1~3.5: 1; Described tensio-active agent is the polyacrylic acid of molecular weight 2000~5000; The weight ratio of described ethanol and deionized water is 0.08~0.20: 1.
The preparation of described polyethylene polyamine polyoxyethylene poly-oxygen propylene aether is initiator with the triethylene tetramine; The preparation of described aliphatic alcohol polyethenoxy polyethenoxy ether is an initiator with ethylene glycol or propylene glycol.
Following operation steps is pressed in the preparation of described polyethylene polyamine polyoxyethylene poly-oxygen propylene aether: add initiator polyethylene polyamine and basic catalyst in pressure reaction still, drip propylene oxide (PO), 120~140 ℃ of controlled temperature treat that pressure reduces to less than continuing reaction 30~60min behind the 0.4MPa; Open pressure reaction still, drip oxyethane (EO), treat that pressure reduces to less than continuing reaction 30~60min behind the 0.4MPa, be cooled to 40~45 ℃ and open pressure reaction still, reactant pH value is adjusted to neutrality, obtain the polyethylene polyamine polyoxyethylene poly-oxygen propylene aether.
The mol ratio of described propylene oxide, oxyethane and triethylene tetramine is (50~80): (100~130): 1; The preferred potassium hydroxide of described basic catalyst (KOH), consumption are 0.1~0.4% of total raw material quality; It is to adopt Glacial acetic acid to regulate that described pH value is adjusted to neutrality.
Following operation steps is pressed in the preparation of described aliphatic alcohol polyethenoxy polyethenoxy ether: add initiator and basic catalyst in pressure reaction still, drip propylene oxide, 120~140 ℃ of controlled temperature treat that pressure reduces to less than continuing reaction 30~60min behind the 0.4MPa; Open pressure reaction still, drip oxyethane, treat that pressure reduces to less than continuing reaction 30~60min behind the 0.4MPa, be cooled to 40~45 ℃, open pressure reaction still, reactant pH value is adjusted to neutrality, obtain the aliphatic alcohol polyethenoxy polyethenoxy ether.
The mol ratio of described propylene oxide, oxyethane and initiator is (8~15): (20~35): 1; The preferred potassium hydroxide of described basic catalyst (KOH), consumption are 0.1~0.4% of total raw material quality; It is to adopt Glacial acetic acid to regulate that described pH value is adjusted to neutrality.
Described polyacrylic preparation is by following operation steps: after deionized water, vinylformic acid, chain-transfer agent and initiator are mixed, place 60~65 ℃ of water-baths to react 3~4h, obtain polyacrylic acid.
Described chain-transfer agent is a Virahol; Described initiator is an ammonium persulphate; Described chain-transfer agent and acrylic acid weight ratio are 0.02~0.08: 1; Described initiator and acrylic acid weight ratio are 0.02~0.04: 1; It is 25~45% that described vinylformic acid, chain-transfer agent and initiator are dissolved in the monomer concentration that forms in the deionized water.
The preparation method of above-mentioned polyelement composite heavy oil emulsion splitter comprises following operation steps: polyethers, tensio-active agent and solvent are obtained polyelement composite heavy oil emulsion splitter after evenly.
Above-mentioned polyelement composite heavy oil emulsion splitter is applied to the water washing cleaning of internal combustion turbine power plant heavy oil or the processing before the crude oil with poor quality catalytic cracking.When this heavy oil emulsion splitter was used to fire the water washing cleaning processing of dynamo-electric factory heavy oil, heavy oil and deionized water temperature were 85~95 ℃, and the profit weight ratio is 9: 1.
Compared with prior art, the present invention has following beneficial effect: polyelement composite heavy oil emulsion splitter of the present invention is when being applied to fire the water washing cleaning processing of dynamo-electric factory heavy oil, and have advantage: (1) emulsion splitter consumption is little.The emulsion splitter consumption is at 100~300ppm, and demulsification is good, and water-oil interface are clear; (2) purify back heavy oil K+Na total content less than 1ppm, Ca content is less than 10ppm; (3) the self-cleaning oil water content is less than 0.4%; (4) broad spectrum is good, and cost is lower; Purify back heavy oil and satisfy the user demand of the dynamo-electric factory of combustion fully.The broken broad spectrum of polyelement composite heavy oil emulsion splitter is better, and consumption is few, and cost is lower.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed description, but embodiments of the present invention are not limited thereto.
Embodiment 1
Add initiator polyethylene polyamine and catalyzer KOH in pressure reaction still, drip propylene oxide (PO), 120~140 ℃ of controlled temperature treat that pressure reduces to less than continuing reaction 30min behind the 0.4MPa; Open pressure reaction still, drip oxyethane (EO), treat that pressure reduces to less than continuing reaction 30min behind the 0.4MPa, pressure reaction still is opened in cooling, and reactant pH value is adjusted to neutrality with Glacial acetic acid, obtains the polyethylene polyamine polyoxyethylene poly-oxygen propylene aether.
Concrete proportioning raw materials is as shown in table 1, and the consumption of KOH is 0.3% of a total raw material quality, obtains polyethylene polyamine polyoxyethylene poly-oxygen propylene aether D1 and polyethylene polyamine polyoxyethylene poly-oxygen propylene aether D2 respectively.
The preparation raw material of table 1 polyethylene polyamine polyoxyethylene poly-oxygen propylene aether
The polyethylene polyamine polyoxyethylene poly-oxygen propylene aether | PO: EO: initiator (mol ratio) | Initiator |
??D1 | ??55∶110∶1 | Triethylene tetramine |
??D2 | ??70∶95∶1 | Triethylene tetramine |
Embodiment 2
Add initiator and catalyzer KOH in pressure reaction still, drip propylene oxide, 120~140 ℃ of controlled temperature treat that pressure reduces to less than continuing reaction 30min behind the 0.4MPa; Open pressure reaction still, drip oxyethane, treat that pressure reduces to less than continuing reaction 30min behind the 0.4MPa, pressure reaction still is opened in cooling, and reactant pH value is adjusted to neutrality with Glacial acetic acid, obtains the aliphatic alcohol polyethenoxy polyethenoxy ether.
Concrete proportioning raw materials is as shown in table 2, and the consumption of initiator is 0.3% of a total raw material quality, obtains polyethylene polyamine polyoxyethylene poly-oxygen propylene aether Z1 and polyethylene polyamine polyoxyethylene poly-oxygen propylene aether Z2 respectively.
The preparation raw material of table 2 aliphatic alcohol polyethenoxy polyethenoxy ether
The aliphatic alcohol polyethenoxy polyethenoxy ether | PO: EO: initiator (mol ratio) | Initiator |
??Z1 | ??9∶22∶1 | Ethylene glycol |
??Z2 | ??12∶28∶1 | Propylene glycol |
Embodiment 3
After deionized water, vinylformic acid, chain-transfer agent Virahol and initiator ammonium persulfate mixed, place 60~65 ℃ of water-baths to react 3~4h, obtain polyacrylic acid.
Concrete proportioning raw materials is as shown in table 3, obtains polyacrylic acid B1 and polyacrylic acid B2 respectively.
The polyacrylic preparation raw material of table 3
Polyacrylic acid | Vinylformic acid/g | Virahol/g | Ammonium persulphate/g | Deionized water/g |
??B1 | ??30 | ??1.2 | ??0.9 | ??70 |
??B2 | ??40 | ??2.0 | ??1.2 | ??60 |
Embodiment 4
With 35g polyethers (25g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether D1 and 10g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether Z2), 5g polyacrylic acid B1, after mixing, 60g solvent (6g ethanol and 54g deionized water) obtains polyelement composite heavy oil emulsion splitter.
Embodiment 5
With 40g polyethers (25g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether D2 and 15g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether Z2), 5g polyacrylic acid B1, after mixing, 55g solvent (8g ethanol and 47g deionized water) obtains polyelement composite heavy oil emulsion splitter.
Embodiment 6
With 32g polyethers (20g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether D2 and 12g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether Z1), 8g polyacrylic acid B2, after mixing, 60g solvent (10g ethanol and 50g deionized water) obtains polyelement composite heavy oil emulsion splitter.
Embodiment 7
With 30g polyethers (20g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether D1 and 10g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether Z1), 10g polyacrylic acid B2, after mixing, 60g solvent (5g ethanol and 55g deionized water) obtains polyelement composite heavy oil emulsion splitter.
Embodiment 8
With 32g polyethers (12g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether D2 and 20g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether Z1), 8g polyacrylic acid B1, after mixing, 60g solvent (8g ethanol and 52g deionized water) obtains polyelement composite heavy oil emulsion splitter.
Embodiment 9
With 40g polyethers (30g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether D1 and 10g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether Z1), 15g polyacrylic acid B1, after mixing, 45g solvent (5g ethanol and 40g deionized water) obtains polyelement composite heavy oil emulsion splitter.
Embodiment 10
With 30g polyethers (15g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether D2 and 15g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether Z2), 15g polyacrylic acid B2, after mixing, 55g solvent (5g ethanol and 50g deionized water) obtains polyelement composite heavy oil emulsion splitter.
Embodiment 11
With 30g polyethers (20g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether D1 and 10g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether Z2), 15g polyacrylic acid B1, after mixing, 55g solvent (6g ethanol and 49g deionized water) obtains polyelement composite heavy oil emulsion splitter.
Embodiment 12
With 35g polyethers (22g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether D1 and 13g polyethylene polyamine polyoxyethylene poly-oxygen propylene aether Z1), 12g polyacrylic acid B2, after mixing, 53g solvent (5g ethanol and 48g deionized water) obtains polyelement composite heavy oil emulsion splitter.
Embodiment 13
Recompounded multielement heavy oil emulsion splitter use properties is estimated:
Estimate Recompounded multielement heavy oil emulsion splitter of the present invention below by related experiment several heavy oil from the different places of production are removed K+Na, Ca and demulsification, comprise the emulsion splitter consumption, purify back heavy oil K+Na and Ca content, water-oil interface state, purify the heavy oil water content.
Table 4 polyelement composite heavy oil emulsion splitter performance evaluation of the present invention
10 parts the dried up heavy oil with 90 parts that goes mixes in elder generation, be heated to 90~95 ℃ in the water-bath, stirred 2 minutes with the emulsification pretreatment stirrer, the mixture that emulsification is good stirs and adds a certain amount of emulsion splitter down, a certain amount of to centrifuge tube with the suction pipe taking-up behind the 2min, centrifugal 3 minutes of whizzer (rotating speed 2000rmp) is observed water-oil interface and aquifer yield etc., and get upper strata, centrifugal back oil sample, with the content of metals such as K, Na, Ca in the heavy oil behind the SPECTROIL M spectrograph detection water washing cleaning.
Polyelement composite heavy oil emulsion splitter is as shown in table 4 to the purification breakdown of emulsion result of different places of production heavy oil.Polyelement composite heavy oil emulsion splitter demulsification of the present invention is good, and water-oil interface are clear; Under 130~300ppm consumption, the K+Na total content is reduced to below the 1ppm by 26~39ppm in the heavy oil, and Ca content is reduced to 10ppm by 33~54ppm, and the heavy oil water content purifies back heavy oil and satisfies the user demand of the dynamo-electric factory of combustion fully less than 0.4%.The broken broad spectrum of polyelement composite heavy oil emulsion splitter is better, and consumption is few, and cost is lower.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. polyelement composite heavy oil emulsion splitter, it is characterized in that: described heavy oil emulsion splitter is made up of following component by weight percentage:
Polyethers 30~55%,
Tensio-active agent 5~15%,
Solvent 40~60%,
Described polyethers is that polyethylene polyamine polyoxyethylene poly-oxygen propylene aether and aliphatic alcohol polyethenoxy polyethenoxy ether mix, and described tensio-active agent is a polyacrylic acid, and described solvent is ethanol and deionized water.
2. a kind of polyelement composite heavy oil emulsion splitter according to claim 1 is characterized in that: the weight ratio of described polyethylene polyamine polyoxyethylene poly-oxygen propylene aether and aliphatic alcohol polyethenoxy polyethenoxy ether is 1: 1~3.5: 1; Described tensio-active agent is the polyacrylic acid of molecular weight 2000~5000; The weight ratio of described ethanol and deionized water is 0.08~0.20: 1; The preparation of described polyethylene polyamine polyoxyethylene poly-oxygen propylene aether is initiator with the triethylene tetramine; The preparation of described aliphatic alcohol polyethenoxy polyethenoxy ether is an initiator with ethylene glycol or propylene glycol.
3. a kind of polyelement composite heavy oil emulsion splitter according to claim 1, it is characterized in that: following operation steps is pressed in the preparation of described polyethylene polyamine polyoxyethylene poly-oxygen propylene aether: add initiator polyethylene polyamine and basic catalyst in pressure reaction still, drip propylene oxide, 120~140 ℃ of controlled temperature treat that pressure reduces to less than continuing reaction 30~60min behind the 0.4MPa; Open pressure reaction still, drip oxyethane, treat that pressure reduces to less than continuing reaction 30~60min behind the 0.4MPa, be cooled to 40~45 ℃ after, open pressure reaction still, reactant pH value is adjusted to neutrality, obtain the polyethylene polyamine polyoxyethylene poly-oxygen propylene aether.
4. a kind of polyelement composite heavy oil emulsion splitter according to claim 3 is characterized in that: the mol ratio of described propylene oxide, oxyethane and triethylene tetramine is (50~80): (100~130): 1; Described basic catalyst is a potassium hydroxide, and consumption is 0.1~0.4% of a reaction raw materials total mass; It is to adopt Glacial acetic acid to regulate that described pH value is adjusted to neutrality.
5. a kind of polyelement composite heavy oil emulsion splitter according to claim 1, it is characterized in that: following operation steps is pressed in the preparation of described aliphatic alcohol polyethenoxy polyethenoxy ether: add initiator and basic catalyst in pressure reaction still, drip propylene oxide, 120~140 ℃ of controlled temperature treat that pressure reduces to less than continuing reaction 30~60min behind the 0.4MPa; Open pressure reaction still, drip oxyethane, treat that pressure reduces to less than continuing reaction 30~60min behind the 0.4MPa, be cooled to 40~45 ℃, open pressure reaction still, reactant pH value is adjusted to neutrality, obtain the aliphatic alcohol polyethenoxy polyethenoxy ether.
6. a kind of polyelement composite heavy oil emulsion splitter according to claim 5 is characterized in that: the mol ratio of described propylene oxide, oxyethane and initiator is (8~15): (20~35): 1; Described basic catalyst is a potassium hydroxide, and consumption is 0.1~0.4% of a reaction raw materials total mass; It is to adopt Glacial acetic acid to regulate that described pH value is adjusted to neutrality.
7. a kind of polyelement composite heavy oil emulsion splitter according to claim 1, it is characterized in that: described polyacrylic preparation is by following operation steps: after deionized water, vinylformic acid, chain-transfer agent and initiator are mixed, place 60~65 ℃ of water-baths to react 3~4h, obtain polyacrylic acid.
8. a kind of polyelement composite heavy oil emulsion splitter according to claim 1 is characterized in that: described chain-transfer agent is a Virahol; Described initiator is an ammonium persulphate; Described chain-transfer agent and acrylic acid weight ratio are 0.02~0.08: 1; Described initiator and acrylic acid weight ratio are 0.02~0.04: 1; It is 25~45% that described vinylformic acid, chain-transfer agent and initiator are dissolved in the monomer concentration that forms in the deionized water.
9. the preparation method of a kind of polyelement composite heavy oil emulsion splitter according to claim 1 is characterized in that comprising following operation steps: polyethers, tensio-active agent and solvent are obtained polyelement composite heavy oil emulsion splitter after evenly.
10. a kind of polyelement composite heavy oil emulsion splitter according to claim 1 is applied to the water washing cleaning of internal combustion turbine power plant heavy oil or the processing before the crude oil with poor quality catalytic cracking.
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