CN100402563C - Method for preparing temperature-resistant and anti-salt type polyacrylamide - Google Patents
Method for preparing temperature-resistant and anti-salt type polyacrylamide Download PDFInfo
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- CN100402563C CN100402563C CNB2005100458330A CN200510045833A CN100402563C CN 100402563 C CN100402563 C CN 100402563C CN B2005100458330 A CNB2005100458330 A CN B2005100458330A CN 200510045833 A CN200510045833 A CN 200510045833A CN 100402563 C CN100402563 C CN 100402563C
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Abstract
The present invention relates to a preparation method for temperature resistant and salt resistant polyacrylamide. An acrylamide monomer aqueous solution whose weight concentration is from 18% to 30%, a hydrolytic reagent, a composite initiator and an auxiliary agent are added to a polymerization kettle, nitrogen is filled to remove oxygen so as to carry out adiabatic polymerization, and then the processes of hydrolyzing, granulating, baking and crushing are carried out. Thereby, the final product is obtained. The method is characterized in that salt resistant monomers, hydrophobe monomers, anion monomers, inorganic compounds, micro cross-linking agents, etc. are added to the polymerization process to carry out the thermal insulation copolymerization of the aqueous solution in a composite initiation system. The copolymer has high viscosity and high-temperature resistant and salt resistant performance, and the molecular weight of the copolymer is higher than 20000000.
Description
Technical field:
The present invention relates to a kind of temperature-resistant and anti-salt type polyacrylamide, is the preparation method who belongs to multiple copolymer type temperature-tolerant anti-salt polyacrylamide.
Background technology:
At present, in view of reservoir temperature in the tertiary oil recovery and the high characteristics of salinity, make oil-displacing agent reach the ideal effect, polymkeric substance must have good tackifying ability and very strong heatproof, anti-salt and anti-shear ability.For this reason, numerous scholars have made number of research projects, make polymkeric substance have higher thermostability as big side group of introducing or rigidity side group (as styrene sulfonic acid, acrylamido chain alkyl sulfonic acid etc.) on the PAM macromolecular chain, adopt the monomer (as the N-alkyl acrylamide) of hydrolysis and the polymkeric substance that the acrylamide copolymerization obtains the temperature resistant antisalt excellent property; The monomer (as N-ethene-2-Pyrrolidone) that introducing can suppress the amide group hydrolysis improves the temperature resistant antisalt performance of polymkeric substance; In molecular chain, introduce and the temperature resistant antisalt performance of PAM is obviously improved the insensitive sulfonic acid group of salt (as 2-acrylamido-2-methyl propane sulfonic acid etc.); In molecule, introduce hydrophobic grouping (as 2-methylacryoyloxyethyl-dimethyl dodecyl bromination ammonium etc.), the temperature resistant antisalt performance of hydrophobic association improved effect PAM by hydrophobic grouping, but still can not satisfy reservoir temperature＞60 ℃, the tertiary oil recovery requirement of salinity 5000mg/l.
Summary of the invention:
In order to remedy the deficiency that prior art can not satisfy reservoir temperature＞60 ℃, the invention provides a kind of preparation method of multiple copolymer type temperature-tolerant anti-salt polyacrylamide, introducing is to the insensitive sulfonic acid group of salt, ultra-fine inorganic thing and little linking agent, and it can improve the temperature resistant antisalt performance of PAM.
The preparation method of temperature-tolerant anti-salt polyacrylamide of the present invention, for non-ionic monomer, hydrolytic reagent, salt tolerant monomer, anionic monomer, hydrophobic monomer, inorganics, little linking agent, auxiliary agent carry out the adiabatic copolymerization of the aqueous solution in composite initiation system, obtain temperature-resistant and anti-salt type polyacrylamide through hydrolysis, granulation, oven dry, pulverizing again.Described non-ionic monomer is preferably acrylamide, and add-on is 70～90% of a monomer weight; Described salt tolerant monomer is a kind of in 2-acrylamido-2-methyl propane sulfonic acid, the 2-acrylamido-2-dodecyl ethyl sulfonic acid, and add-on is 5～20% of a monomer weight; Described anionic monomer is a kind of in vinylformic acid, methacrylic acid, butene dioic acid, methylene-succinic acid, the butenoic acid, and add-on is 0.1～10% of a monomer weight; Described hydrophobic monomer is a kind of in methylacryoyloxyethyl trimethyl ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac, N,N-DMAA, the dimethyl diallyl ammonium chloride, and add-on is 0.01～1% of a monomer weight; Described mineral compound is a kind of (1000～3000 order) in kaolin, wilkinite, atlapulgite, talcum powder, magnesium oxide, colloid silica, molecular sieve, the colloidal aluminium hydroxide, and add-on is 0.01～1% of a monomer weight; Described little linking agent be oxalic dialdehyde, a kind of in the vinyl acetate, urotropine, add-on is 0.001～0.1% of a monomer weight.The multicomponent system that the oxidation-reduction trigger system that composite initiator is made up of organic amine reductive agent and persulfate oxidation agent and ammoniacal liquor, water-soluble type azo class are formed, wherein said oxygenant, a kind of in Potassium Persulphate, ammonium persulphate, the Sodium Persulfate, add-on is 0.005～0.05% of a monomer weight; The organic amine reductive agent, a kind of in thanomin, diethylamine, quadrol, pyridine, the 4-cyanopyridine, add-on is 0.01～1% of a monomer weight; Azo-initiator, be 2,2 '-two (2-amidine propane) dihydrochlorides, 4 of azo, a kind of in 4 '-azo two (4-cyanopentanoic acid), add-on is 0.001～0.5% of a monomer weight; Hydrolytic reagent is Na
2CO
3, add-on is 18～30% of a monomer weight; The add-on of ammoniacal liquor is 0.005～0.2% of a monomer weight.Auxiliary agent is chain propagation agent β-dimethylamino butyronitrile, and add-on is 0.006～0.2% of a monomer weight; Tensio-active agent, a kind of in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, OP class, peregal class, Tweens, the spans, to prevent crosslinked polymer, add-on is 0.08～1% of a monomer weight.Be added with urea outside also having, make polymkeric substance instant, add-on is 1～10% of a monomer weight.
The adiabatic copolymerization mix monomer of aqueous solution concentration is 10～30% among the present invention, and kick off temperature is 10～25 ℃, and the adiabatic polymerisation time is 5～10h.Adiabatic polymerisation is finished post-heating and is warming up to 95～120 ℃, and hydrolysis 5～9h obtains temperature-resistant and anti-salt type polyacrylamide through granulation, oven dry, pulverizing.
Characteristics of the present invention are to add the insensitive salt tolerant monomer of high temperature and high salt, ultra-fine inorganic thing and little linking agent, can obtain the temperature resistant antisalt polyacrylamide of desired viscosity.
Further specify the present invention below by embodiment.
Specific embodiment:
Embodiment 1, the 111.41kg deionized water is put into still, under agitation add 4.4kg yellow soda ash successively, 23.2kg acrylamide, 2.5kg urea, 4.9kg2-acrylamido-2-methyl propane sulfonic acid, 1.02kg methacrylic acid, 0.02kg dimethyl diallyl ammonium chloride, 0.05kg magnesium oxide, 1% oxalic dialdehyde 0.5kg, 2% sodium lauryl sulphate 8.0kg, 1% ammoniacal liquor 5.0kg, 1%4, two (4-cyanopentanoic acid) 12.0kg of 4-azo, 2% β-dimethylamino butyronitrile 2.5kg, 2%4-cyanopyridine 12.0kg, adjust 22 ℃ of kick off temperatures, feed nitrogen to remove the dissolved oxygen in the reaction system, add 0.1% ammonium persulphate 12.5kg behind the logical 30min, crossing the interior material of 20min still approximately begins to be clamminess, and begin to heat up, temperature in the kettle reaches 78 ℃ behind the 5h, heat to 115 ℃, hydrolysis 6h, granulation then, oven dry, it is 1,900 ten thousand that pulverizing obtains molecular weight, is 9763.94mg/l in salinity, temperature is that 65 ℃ salt solution medium viscosity is the temperature resistant antisalt polyacrylamide of 53mpas.
Embodiment 2, the 78.55kg deionized water is put into still, under agitation add 8.5kg yellow soda ash, 39.1kg acrylamide, 3.0kg urea, 7.5kg2-acrylamido-2-dodecyl ethyl sulfonic acid, 4.31kg methylene-succinic acid, 0.24kg acrylyl oxy-ethyl-trimethyl salmiac, 0.3kg talcum powder, 1% vinyl acetate 2.0kg, 2%OP successively
1025.0kg, 1% ammoniacal liquor 6.0kg, 1%2,2 '-two (2-amidine propane) the dihydrochloride 8.0kg of azo, 2% β-dimethylamino butyronitrile 2.5kg, 2% pyridine 5.0kg, adjust 15 ℃ of kick off temperatures, feed nitrogen to remove the dissolved oxygen in the reaction system, add 0.1% Potassium Persulphate 10.0kg behind the logical 30min, crossing the interior material of 20min still approximately begins to be clamminess, and begin to heat up, temperature in the kettle reaches 72 ℃ behind the 8h, heat to 100 ℃, hydrolysis 5h, granulation then, oven dry, it is 2,100 ten thousand that pulverizing obtains molecular weight, is 9763.94mg/l in salinity, temperature is that 65 ℃ salt solution medium viscosity is the temperature resistant antisalt polyacrylamide of 58mpas.
Embodiment 3, the 114.02kg deionized water is put into still, under agitation add 7.1kg yellow soda ash successively, 48.5kg acrylamide, 1.0kg urea, 4.5kg2-acrylamido-2-methyl propane sulfonic acid, 0.15kg butene dioic acid, 0.54kg N, the N-DMAA, 0.55kg kaolin, 1% vinyl acetate 5.3kg, 1% peregal 15.0kg, 1% ammoniacal liquor 0.5kg, 1%4, two (4-cyanopentanoic acid) 0.24kg of 4-azo, 2% β-dimethylamino butyronitrile 0.2kg, 2% thanomin 0.4kg, adjust 18 ℃ of kick off temperatures, feed nitrogen to remove the dissolved oxygen in the reaction system, add 0.1% Sodium Persulfate 2.0kg behind the logical 30min, crossing the interior material of 20min still approximately begins to be clamminess, and begin to heat up, temperature in the kettle reaches 68 ℃ behind the 10h, heat to 95 ℃, hydrolysis 8h, granulation then, oven dry, it is 2,012 ten thousand that pulverizing obtains molecular weight, is 9763.94mg/l in salinity, temperature is that 65 ℃ salt solution medium viscosity is the temperature resistant antisalt polyacrylamide of 60mpas.
Embodiment 4, the 106.55kg deionized water is put into still, under agitation add 6.0kg yellow soda ash successively, 34.5kg acrylamide, 6.0kg urea, 5.7kg2-acrylamido-2-dodecyl ethyl sulfonic acid, 1.02kg butenoic acid, 0.03kg methylacryoyloxyethyl trimethyl ammonium chloride, 0.2kg colloid silica, 1% urotropine 2.0kg, 2% tween 10.0kg, 1% ammoniacal liquor 6.0kg, 1%2,2 '-two (2-amidine propane) the dihydrochloride 5.0kg of azo, 2% β-dimethylamino butyronitrile 2.0kg, 2% quadrol 5.0kg, adjust 12 ℃ of kick off temperatures, feed nitrogen to remove the dissolved oxygen in the reaction system, add 0.1% Potassium Persulphate 10.0kg behind the logical 30min, crossing the interior material of 20min still approximately begins to be clamminess, and begin to heat up, temperature in the kettle reaches 75 ℃ behind the 6h, heat to 110 ℃, hydrolysis 8h, granulation then, oven dry, it is 2,300 ten thousand that pulverizing obtains molecular weight, is 9763.94mg/l in salinity, temperature is that 65 ℃ salt solution medium viscosity is the temperature resistant antisalt polyacrylamide of 65mpas.
Embodiment 5, the 123.66kg deionized water is put into still, under agitation add 7.1kg yellow soda ash successively, 39.5kg acrylamide, 3.0kg urea, 4.7kg2-acrylamido-2-methyl propane sulfonic acid, 0.98kg butene dioic acid, 0.05kgN, the N-DMAA, 0.01kg colloidal aluminium hydroxide, 1% vinyl acetate 0.001kg, 1% sapn 5.0kg, 1% ammoniacal liquor 5.0kg, 1%4, two (4-cyanopentanoic acid) 2.5kg of 4 '-azo, 2% β-dimethylamino butyronitrile 1.5kg, 2% diethylamine 4.0kg, adjust 18 ℃ of kick off temperatures, feed nitrogen to remove the dissolved oxygen in the reaction system, add 0.1% Sodium Persulfate 3.0kg behind the logical 30min, crossing the interior material of 20min still approximately begins to be clamminess, and begin to heat up, temperature in the kettle reaches 70 ℃ behind the 9h, heat to 100 ℃, hydrolysis 7h, granulation then, oven dry, it is 2,312 ten thousand that pulverizing obtains molecular weight, is 9763.94mg/l in salinity, temperature is that 65 ℃ salt solution medium viscosity is the temperature resistant antisalt polyacrylamide of 61mpas.
Claims (2)
1. the preparation method of a temperature-resistant and anti-salt type polyacrylamide, for non-ionic monomer, hydrolytic reagent, salt tolerant monomer, anionic monomer, hydrophobic monomer, inorganics, little linking agent, auxiliary agent carry out the adiabatic copolymerization of the aqueous solution in composite initiation system, obtain temperature-resistant and anti-salt type polyacrylamide through hydrolysis, granulation, oven dry, pulverizing again; Described non-ionic monomer is an acrylamide, and add-on is 70～90% of a monomer weight; Described salt tolerant monomer is a kind of in 2-acrylamido-2-methyl propane sulfonic acid, the 2-acrylamido-2-dodecyl ethyl sulfonic acid, and add-on is 5～20% of a monomer weight; Described anionic monomer is a kind of in vinylformic acid, methacrylic acid, butene dioic acid, methylene-succinic acid, the butenoic acid, and add-on is 0.1～10% of a monomer weight; Described hydrophobic monomer is a kind of in methylacryoyloxyethyl trimethyl ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac, N,N-DMAA, the dimethyl diallyl ammonium chloride, and add-on is 0.01～1% of a monomer weight; Described mineral compound is a kind of in kaolin, wilkinite, atlapulgite, talcum powder, magnesium oxide, colloid silica, molecular sieve, the colloidal aluminium hydroxide, and add-on is 0.01～1% of a monomer weight; Described little linking agent be oxalic dialdehyde, a kind of in the vinyl acetate, urotropine, add-on is 0.001～0.1% of a monomer weight; The multicomponent system that the oxidation-reduction trigger system that composite initiator is made up of organic amine reductive agent and persulfate oxidation agent and ammoniacal liquor, water-soluble type azo class are formed, wherein said oxygenant, a kind of in Potassium Persulphate, ammonium persulphate, the Sodium Persulfate, add-on is 0.005～0.05% of a monomer weight; The organic amine reductive agent, a kind of in thanomin, diethylamine, quadrol, pyridine, the 4-cyanopyridine, add-on is 0.01～1% of a monomer weight; Azo-initiator, be 2,2 '-two (2-amidine propane) dihydrochlorides, 4 of azo, a kind of in 4 '-azo two (4-cyanopentanoic acid), add-on is 0.001～0.5% of a monomer weight; Hydrolytic reagent is Na
2CO
3, add-on is 18～30% of a monomer weight; The add-on of ammoniacal liquor is 0.005～0.2% of a monomer weight; Auxiliary agent is chain propagation agent β-dimethylamino butyronitrile and tensio-active agent, chain propagation agent β-dimethylamino butyronitrile add-on is 0.006～0.2% of a monomer weight, tensio-active agent is a kind of in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, OP class, peregal class, Tweens, the spans, and add-on is 0.08～1% of a monomer weight; The kick off temperature of aqueous solution polymerization is 10～25 ℃, and polymerization time is 5～10h, and adiabatic polymerisation is finished post-heating and is warming up to 95～120 ℃, hydrolysis 5～9h.
2. preparation method as claimed in claim 1 is characterized in that: be added with urea outside after the hydrolytic reagent, add-on is 1～10% of a monomer weight.
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