CN100460448C - Preparation method of multifunctional resistance-reducing polymer suspension - Google Patents
Preparation method of multifunctional resistance-reducing polymer suspension Download PDFInfo
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Abstract
The invention discloses a method of preparing multifunctional drag reduction polymer suspension, which includes steps: mixing alpha-olefin polymer with molecular weight of 4-5 millions, pour-point depressant, viscosity modifier and scale inhibitor, and comminuting the mixture to solid powder under temperature of minus 60 to minus 160 DEG C, mixing the solid powder, surfactant, foam resistant agent, thickening agent and residual alcohol-water mixture to prepare drag reduction polymer suspension. The prepared drag reduction polymer suspension has function of pour point depression, viscosity reduction, scale inhibition and drag reduction, can be widely used for multiple type crude oil transportation pipe, and can greatly increase drag reduction effect of different drag reducing agent in different crude oil.
Description
Technical field
The invention belongs to the preparation method of drag-reduction polymer suspension.
Background technology
When fluid flows in pipeline,, particularly under turbulent state, influence more obvious because the influence of friction resistance causes the pipeline throughput rate to reduce or the energy consumption increase.In the oil product transport pipe, inject a spot of high molecular polymer and just can significantly reduce resistance to flow.Commercial applications is in Alaska crude oil pipeline first for the CDR flow improver of producing from U.S. CONOCO company in 1979, and since achieving success, mainly having developed two kinds is monomeric frictional reducing polymer synthetic method with α-alkene, ie in solution polymerization and mass polymerization.
Initial poly-α-alkene flow improver adopts solution polymerization: monomer and initiator are dissolved in polymerization in the appropriate solvent, and the effective constituent of monomer conversion, frictional reducing polymer molecular weight and flow improver is all very low, and drag-reduction effect is poor; And the product viscosity of solution polymerization is high, injects very difficult, superseded gradually now.Developed bulk polymerization the nineties in 20th century, and it does not introduce other medium, and have only monomer this carries out polymerization under the initiator effect, and this method has improved the molecular weight of monomeric transformation efficiency and polymkeric substance greatly.But the mass polymerization product is the viscoelastic solid material, and directly flow in pipes must make its fluidify state through postprocessing working procedures.Postprocessing working procedures generally includes two steps: at first with the visco-elasticity frictional reducing polymer of solid state the powder that is ground into certain fineness under the condition of ultralow temperature (for the polymkeric substance after preventing to pulverize agglomerated together again, need to add an amount of dispersion agent, comprise: calcium stearate, aluminum oxide, talcum powder, clay, calcium phosphate, Zinic stearas, graphite and various stearic amide classes etc.), generally be not less than 100 orders.Dispersion agent itself there is no promoter action to drag-reduction effect, therefore, under the UA prerequisite of maintenance polymer powder, should add less as far as possible, and dispersion agent shared weight in polymkeric substance does not surpass 50%, preferably less than 30%.Make in the mixture of its mixture that is suspended in pure water or several alcohol by various chemical additives then, form the paste-like fluid as product, the purpose that adds chemical additive is to improve the stability of suspension.This flow improver product is the concentration height not only, and flow improver can be dissolved in the oil product fast, has improved the drag-reduction effect of flow improver.But postprocessing working procedures is loaded down with trivial details and complicated, and the production cost height because dispersant particle is very thin, causes environmental pollution (dust pollution) simultaneously in process of production easily.
In recent years, people improve to some extent again on the postprocessing working procedures of polymkeric substance, as " drag-reduction polymer suspension " patent disclosure of the US6399676 of CONOCO company and WO03029330 application when polymkeric substance carries out pulverize at low temperature, by adding a kind of material as grinding aid, as: ice, carbohydrate, starch, solid carbon acid esters etc., to improve the crushing effect of polymkeric substance, reduce the waste of liquid nitrogen.Dispersion agent is still selected stearate for use, and also not minimizing of add-on, and grinding aid and dispersion agent itself there is no promoter action to final drag-reduction effect." drag-reduction polymer suspension " patent disclosure of US6765053 application when polymkeric substance carries out pulverize at low temperature, by adding wax crystal modifier, as: the multipolymer of alkene and vinyl cyanide, the multipolymer of alkene and vinyl acetate, alkene, vinyl cyanide and carbon monoxide terpolymer, alkene, vinyl acetate and carbon monoxide terpolymer, multipolymers such as alkene and maleic anhydride.Wax crystal modifier plays two effects: (1) stops polymer powder to condense again as dispersion agent: (2) have reduced the zero pour of crude oil.The adding of wax crystal modifier, not only saved the stearate that drag reduction be there is no promoter action, and, make final suspension product in the higher crude oil of wax content, also can reach good drag-reduction effect by reducing the condensation point of crude oil, enlarged the scope of application of flow improver.But crude oil is the mixture of various hydro carbons and non-hydrocarbons, the rerum natura of crude oil is not inequality yet simultaneously for various components contents, contain the many former oil freezing point height of normal paraffin, and contain colloid, viscosity of crude height that bituminous matter is high, simultaneously, deposition of dirt etc. also has very big influence to the drag-reduction effect of flow improver in the pipe-line transportation, and this just causes with a kind of frictional reducing polymer its resistance reducing performance in the crude oil of different rerum naturas very big difference.
Summary of the invention
The present invention be directed to the existing bad shortcoming of flow improver drag-reduction effect, and provide a kind of preparation method of new multifunctional resistance-reducing polymer suspension, multiple functions such as frictional reducing polymer collection pour point depression, visbreaking, scale inhibition and drag reduction with this method preparation, can be widely used in polytype crude oil pipeline, improve the drag-reduction effect of flow improver in dissimilar crude oil greatly.
The invention provides a kind of preparation method of multifunctional resistance-reducing polymer suspension, its method may further comprise the steps:
1) preparation alpha-olefin polymer: at least a C
4～20Linear alpha-alkene be TiCl at catalyzer
3Perhaps metallocene compound, auxiliary agent are to carry out mass polymerization under the condition of lithium alkylide and/or aluminum alkyls, generate molecular weight and be 400～5,000,000 alpha-olefin polymer, and the alkyl carbon number is C in lithium alkylide and the aluminum alkyls
1～C
6
2) solid mixture powder: in the mix powder gross weight, the Scale inhibitors of alpha-olefin polymer in 40～60% the step 1), 10～30% pour point depressant, 10～20% viscosity modifiers and 5～10% is mixed, under-60～-160 ℃ of temperature, pulverize under best-50～-130 ℃ temperature, obtain greater than 60 orders, more preferably greater than 100 purpose solid mixture powder.
3) suspension preparation: in the suspension gross weight, the alcohol-water mixture of solid mixture powder the step 2 with 30～50%), 0.1～1% tensio-active agent, 0～0.01% kilfoam, 0～0.05% thickening material and surplus stirs at normal temperatures and makes multifunctional resistance-reducing polymer suspension, and wherein the optimum content of tensio-active agent is 0.01%～0.1%.
Aforementioned pour point depressant is that molecular weight is 1000～5000 olefin copolymer, as: alkene and acrylonitrile copolymer, alkene and vinyl acetate copolymer, alkene, vinyl cyanide and carbon monoxide terpolymer, alkene, vinyl acetate and carbon monoxide terpolymer, the multipolymer of alkene and maleic anhydride derivative, when pour point depressant adopted two or more olefin copolymer, each material mixed with arbitrary proportion.
Aforementioned viscosity modifier is that molecular weight is 2000～10000 acrylic copolymer, as: vinylformic acid and stearyl alcohol copolymer, the copolymer of methacrylic acid and stearyl alcohol, vinylformic acid, maleic anhydride and styrene copolymer, vinylformic acid, maleic anhydride and stearyl alcohol terpolymer, when adopting two or more acrylic copolymer, each material mixes with arbitrary proportion.
Scale inhibitors of the present invention is selected from a kind of in phosphorus derivant, polyalkenyl thiophosphatephosphorothioate, sulphur class and the guanidine Scale inhibitors of polymerase chain alkenyl succinimide, polymerase chain alkenyl succinimide at least, when adopting two or more to mix, each material mixes with arbitrary proportion.
Kilfoam of the present invention is silicone oil or dimethyl silicone oil.
Tensio-active agent of the present invention be in alkyl sodium sulfonate, oxyethane, the pure and mild alkyl aryl polyether alcohol of Resins, epoxy (as NP-4, NP-7 or NP-10 etc.) one or more, when adopting two or more to mix, each material mixes with arbitrary proportion.
Alcohol-water mixture of the present invention is the mixture of one or more and water in methyl alcohol, ethanol, Virahol, isooctyl alcohol, ethylene glycol, propylene glycol, the glycerol, and when selecting two or more alcohol for use, the ratio between the described alcohols material is any.
Described thickening material is at least a in water soluble starch, Walocel MT 20.000PV, polyacrylamide and the carboxymethyl cellulose macromolecular water-soluble polymkeric substance, and when adopting two or more to mix, each material mixes with arbitrary proportion.
The present invention compared with prior art, not only eliminated the dispersion agent that when pulverize at low temperature, must add calcium stearate, Zinic stearas and the finished product drag-reduction effect be there is no promoter action, reduced environmental pollution, and by reducing zero pour, viscosity and the dirt deposition of crude oil, thereby significantly improve drag-reduction effect; Multiple functions such as the drag reducing suspensions product collection pour point depression, visbreaking, scale inhibition and the drag reduction that obtain can be widely used in polytype crude oil pipeline, improve the drag-reduction effect of flow improver in dissimilar crude oil greatly; Adopt the inventive method synthetic multifunctional resistance-reducing polymer suspension product in dissimilar crude oil, all to have good drag-reduction effect, and the stable in properties of suspension, not stratified, be easy to transportation, filling is convenient.
Embodiment
Describe the present invention in detail with specific embodiment below, but embodiment does not limit the scope of the invention.
Embodiment 1 (Comparative Examples)
1) preparation alpha-olefin polymer:
Learnt from else's experience refinement treatment, be chilled to 1-octene 1000g of 0 ℃ in advance, add the triethyl aluminum hexane solution of 18 milliliter 15% (quality), under 0 ℃ of condition, stirred 30 minutes, add TiCl then
3Catalyzer 0.45g mixes.Along with the carrying out of reaction, reaction system viscosity increases to catalyzer not during redeposition gradually, puts it in the low temperature environment (-20 ℃～30 ℃) reaction 4～7 days.The polymkeric substance weight-average molecular weight that obtains like this is about 4.6 * 10
6, the monomer conversion of 1-octene is 95.2%, is designated as polymer A.
Learnt from else's experience refinement treatment, be chilled to 0 ℃ 1-octene and 1-decene (mol ratio 4:1) 1000g in advance, add the triethyl aluminum hexane solution of 20 milliliter 15% (quality), under 0 ℃ of condition, stirred 30 minutes, add TiCl then
3Catalyzer 0.5g mixes.Along with the carrying out of reaction, reaction system viscosity increases to catalyzer not during redeposition gradually, puts it in the low temperature environment (-20 ℃～30 ℃) reaction 4～7 days.The polymkeric substance weight-average molecular weight that obtains like this is about 4.5 * 10
6, the monomer conversion of mixed olefins reaches 95.3%, is designated as polymer B.
2) get 1) synthetic alpha-olefin polymer B30g, coarse crushing becomes the particle less than 1 centimetre under the normal temperature, adds the 20g calcium stearate again, and they are put into refrigeration formula Lowtemperaturepulverizer, under-130～-140 ℃ environment, pulverized 5 minutes, obtain greater than 80 purpose mix powders;
3) 2) mix powder in add 2g NP-10 nonionogenic tenside, 0.01g dimethyl silicone oil, 17g methyl alcohol, the 30g pure water, the carboxymethyl cellulose of 1g (can be dissolved in the water in advance) stirs in agitator and forms the steady suspension product, is called sample I.
Embodiment 2 (Comparative Examples)
1) with embodiment 1;
2) get synthetic alpha-olefin polymer B30g, coarse crushing becomes the particle less than 1 centimetre under the normal temperature, add ethene-vinyl acetate 20g again, about 6 millimeters of diameter, to put into refrigeration formula Lowtemperaturepulverizer after their mixing, under-130～-140 ℃ environment, pulverized 5 minutes, obtain greater than 80 purpose mix powders;
3) 2) mix powder in add 2g NP-7 nonionogenic tenside, 0.01g silicone oil, 17g methyl alcohol, the 30g pure water, the carboxymethyl cellulose of 1g (can be dissolved in the water in advance) stirred in agitator 0.5～1 hour, the final steady suspension product that forms is called sample II.
Embodiment 3 (example)
1) with embodiment 1;
2) get embodiment 1 synthetic alpha-olefin polymer B40g, add ethene-vinyl acetate 13g again, polyoctodecyl acrylate 13g, polymerase chain alkenyl succinimide 6.5g, their coarse crushings at first at normal temperatures become the particle less than 1 centimetre, put into refrigeration formula Lowtemperaturepulverizer after they being mixed again, and pulverize 6 minutes under less than-130～-140 ℃ environment, obtain greater than 80 purposes, can free-pouring mix powder;
3) 2) mix powder in add 3gNP-10,0.01g dimethyl silicone oil, 16g methyl alcohol, the 40g pure water, the carboxymethyl cellulose of 0.7g (can be dissolved in the water in advance) stirred in agitator 0.5～1 hour, the final steady suspension product that forms is called sample III.
Embodiment 4 (example)
1) with embodiment 1;
2) get embodiment 1 synthetic alpha-olefin polymer B45g, add ethene-vinyl acetate 15g again, polymethyl acrylic acid octadecyl ester 15g, polymerase chain alkenyl succinimide 7.5g, their coarse crushings at first at normal temperatures become the particle less than 1 centimetre, again their are put into refrigeration formula Lowtemperaturepulverizer after mixing, pulverizing is 5 minutes under-130～-140 ℃ environment, obtain greater than 80 purposes, can free-pouring mix powder;
3) 2) mix powder in add 3.0gNP-10, the 0.01g dimethyl silicone oil, 18g methyl alcohol, the 45g pure water, the carboxymethyl cellulose of 0.75g (can be dissolved in the water in advance) stir to form the steady suspension product in agitator, be called sample IV.
Embodiment 5 (example)
1) with embodiment 1;
2) get embodiment 1 synthetic alpha-olefin polymer B45g, add ethene-vinyl acetate-carbon monoxide multipolymer 15g again, vinylformic acid-maleic acid anhydride-phenylethylene terpolymer 15g, polymerase chain alkenyl succinimide 7.5g, their coarse crushings at first at normal temperatures become the particle less than 1 centimetre, again their are put into refrigeration formula Lowtemperaturepulverizer after mixing, pulverizing is 5 minutes under-130～-140 ℃ environment, obtain greater than 80 purposes, can free-pouring mix powder;
3) 2) mix powder in add 3.5gNP-7, the 0.01g dimethyl silicone oil, 15g methyl alcohol, the 30g pure water, the carboxymethyl cellulose of 0.5g (can be dissolved in the water in advance) stir to form the steady suspension product in agitator, be called sample V.
Embodiment 6 (application examples)
The suspension product that makes is dissolved in toluene or the diesel oil, is added in the used oil product, on annular drag reduction experimental installation, estimate the drag-reduction effect of suspension product.Select three kinds of oil products of different nature as base oil:
Oil product A:0
#Finished diesel fuel, density is 0.8285g/cm in the time of 20 ℃
3, kinematic viscosity 4.645mm
2/ s.
Oil product B: the land is than crude oil, 24 ℃ of condensation points, 30 ℃ kinematic viscosity 34.2mm
2/ s belongs to the high thin oil that coagulates.
Oil product C: Gudao crude, 32 ℃ of condensation points, 50 ℃ kinematic viscosity 231.4mm
2/ s belongs to the high viscous crude that coagulates.
The drag reduction result is as shown in table 1.
The drag reducing efficiency of table 1 drag reducing suspensions
30 ℃ of experimental temperatures, Reynolds number 6000.
By testing data as can be known, no matter adopt present method synthetic multifunctional resistance-reducing polymer suspension product 0
#In the finished diesel fuel, still in dissimilar crude oil, all have good drag-reduction effect, obviously be better than the simple sample that only adds dispersion agent or pour point depressant.This explanation adopts the inventive method synthetic multifunctional resistance-reducing polymer suspension product application scope wide, can fully be applicable to dissimilar crude oil.And the stable in properties of suspension, leave standstill for a long time also and demixing phenomenon can not occur, be easy to transportation, on-the-spot filling is very convenient.
Claims (6)
1. the preparation method of a multifunctional resistance-reducing polymer suspension.It is characterized in that may further comprise the steps:
1) preparation alpha-olefin polymer: at least a C
4～20Linear alpha-alkene be TiCl at catalyzer
3Perhaps metallocene compound, auxiliary agent are to carry out polymerization under the condition of lithium alkylide and/or aluminum alkyls, generate molecular weight and be 400～5,000,000 alpha-olefin polymer, and the alkyl carbon number is C in lithium alkylide and the aluminum alkyls
1～C
6
2) solid mixture powder: in solid mixture powder gross weight, the Scale inhibitors of the alpha-olefin polymer in 40～60% the step 1), 10～30% pour point depressant, 10～20% viscosity modifiers and 5～10% is mixed, under-60～-160 ℃ of temperature, pulverize, obtain greater than 60 purpose solid mixture powder;
The alcohol-water mixture of the solid mixture powder 3) suspension preparation: in suspension gross weight, the step 2 with 30～50%), 0.1～1% tensio-active agent, 0～0.01% kilfoam, 0～0.05% thickening material and surplus stirs at normal temperatures and makes multifunctional resistance-reducing polymer suspension;
Wherein said pour point depressant is that molecular weight is 1000～5000 olefin copolymer, viscosity modifier is that molecular weight is 2000～10000 acrylic copolymer, Scale inhibitors is in the phosphorus derivant, polyalkenyl thiophosphatephosphorothioate, sulphur class and the guanidine Scale inhibitors that are selected from polymerase chain alkenyl succinimide, polymerase chain alkenyl succinimide at least one or more, when adopting two or more, above-mentioned Scale inhibitors can mix with arbitrary proportion.
2. according to the described preparation method of claim 1, it is characterized in that: the tensio-active agent in the suspension preparation is one or more in alkyl sodium sulfonate, oxyethane, the pure and mild alkyl aryl polyether alcohol of Resins, epoxy, when adopting two or more, above-mentioned tensio-active agent can mix with arbitrary proportion.
3. according to the described preparation method of claim 1, it is characterized in that: the kilfoam in the suspension preparation is silicone oil or dimethyl silicone oil.
4. according to the described preparation method of claim 1, it is characterized in that: the thickening material in the suspension preparation is at least a in water soluble starch, Walocel MT 20.000PV, polyacrylamide and the carboxymethyl cellulose macromolecular water-soluble polymkeric substance, when adopting two or more mixing, each material mixes with arbitrary proportion.
5. according to the described preparation method of claim 1, it is characterized in that: the alcohol-water mixture in the suspension preparation is the mixture that is selected from methyl alcohol, ethanol, Virahol, ethylene glycol, isooctyl alcohol, propylene glycol and the glycerol one or more and water, when adopting two or more alcohol, the ratio between the described alcohols material is any.
6. according to the described preparation method of claim 1, it is characterized in that: the temperature of preparation solid mixture powder is-50～-130 ℃.
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