CN109134751A - A kind of novel heatproof anti-salt polyacrylamide and its synthetic method - Google Patents
A kind of novel heatproof anti-salt polyacrylamide and its synthetic method Download PDFInfo
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- CN109134751A CN109134751A CN201710464462.2A CN201710464462A CN109134751A CN 109134751 A CN109134751 A CN 109134751A CN 201710464462 A CN201710464462 A CN 201710464462A CN 109134751 A CN109134751 A CN 109134751A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
Abstract
The present invention proposes a kind of novel heatproof anti-salt polyacrylamide and its synthetic method, and structure includes sulfonic group and pyrrolidone-base, and for temperature-tolerant anti-salt polyacrylamide anti-salt property up to 20,000 salinities, calcium ions and magnesium ions total amount reaches 504mg/L, 85 DEG C of temperature.Its synthetic method includes the following steps: the first step, in redox and azo composite initiation system, purification acrylamide monomer AM, function monomer AMPS and vinylpyrrolidone is reacted to obtain colloid at -2-0 DEG C of initiation temperature；Second step is granulated, hydrolysis, dry, crushing, sieving.The present invention is polymerize under ultralow temperature using redox and azo composite initiation system, sulfonic group water base group and introducing pyrrolidone-base by force are introduced into polyacrylamide, homemade mixed stabilizer is added while hydrolysis again, both the saline-alkaline tolerance for having improved polyacrylamide in turn ensures super high molecular weight shear degradation and heat-resisting property.
Description
Technical field
The present invention relates to high-molecular compound technical field, particularly relate to a kind of novel heatproof anti-salt polyacrylamide and its
Synthetic method.
Background technique
Polymer displacement of reservoir oil, binary complex oil displacing (alkali-polymer), ternary composite oil-displacing (alkali, surfactant and polymer)
Etc. ternary oil recoveries technology be widely used, and achieve significant oil increasing precipitation effect and good economic benefit.Its
In, polymer displacement of reservoir oil mainly uses polyacrylamide, and common Polyacrylamides For Enhanced Oil Recoveries are due to the quick effect of salt, in high mineralising
It spends lower solubility property to be deteriorated, marine displacement of reservoir oil polyacrylamide requirement is not achieved in viscosity.Moreover, acid, alkali or temperature are super
Rapid hydrolysis can occur under conditions of crossing 70 DEG C, polyacrylamide strand is caused to crimp, or even generate precipitating,
Lose oil-displacement capacity.The structure for how improving polyacrylamide makes it have good temperature-resistant anti-salt performance, to meet marine drive
The needs of oil, are the current technical issues that need to address.
Summary of the invention
To solve the above the deficiencies in the prior art, the invention proposes a kind of novel heatproof anti-salt polyacrylamide and its conjunctions
At method.
The technical scheme of the present invention is realized as follows:
A kind of novel heatproof anti-salt polyacrylamide, including sulfonic group and pyrrolidone-base, temperature-tolerant anti-salt polyacrylamide salt resistance
Performance is up to 20,000 salinities, and calcium ions and magnesium ions total amount is up to 504mg/L or so, and 85 DEG C of temperature.
The synthetic method of above-mentioned novel heatproof anti-salt polyacrylamide, includes the following steps:
The first step, in redox and azo composite initiation system, will purification acrylamide monomer AM, function monomer AMPS and
Vinylpyrrolidone is reacted to obtain colloid at -2-0 DEG C of initiation temperature, and composite initiation system includes by tert-butyl hydroperoxide
The redox initiation system and drawn by the azo that azobisisoheptonitrile forms that hydrogen-oxygen agent is formed with iron ammonium sulfate reducing agent
Hair system；
Second step is granulated, hydrolysis, dry, crushing, sieving.
Preferably, by mass fraction, composition of raw materials in 100 parts of polyblend are as follows: 3.5-5 parts of function monomer AMPS,
18-20 parts of acrylamide monomer AM of purification, 0.05-0.1 parts of vinylpyrrolidone, tert-butyl hydroperoxide 0.0002-0.0005
Part, 0.0006-0.001 parts of iron ammonium sulfate, 0.01-0.02 parts of azobisisoheptonitrile, remaining is water.
It is further preferred that in the first step, it first will purification acrylamide monomer AM, function monomer AMPS and vinyl pyrrolidine
Ketone is configured to aqueous solution, and adjusting PH with sodium hydroxide is 12-12.5；Add 0.1-0.15 parts of sodium chloride, urea 0.1-
0.15 part, at a temperature of -2-0 DEG C, 0.001-0.005 parts of metal ion screener EDTA are added after drum nitrogen deoxygenation 10min,
Azobisisoheptonitrile is added after continuing deoxygenation 20min, is further continued for that tert-butyl hydroperoxide is first added after deoxygenation 20min, after 2min
Iron ammonium sulfate is added, then leads to nitrogen until solution seals after becoming viscous.
More preferably, it after sealing after solution temperature rises to peak and Temperature fall 2h, takes out colloid and is granulated,
By mass fraction, 1-3 parts of hydrolytic reagent sodium hydroxide and 0.1-1 parts of reducing agent sulfurous acid is added in every 100 parts of colloidal solid
Hydrogen sodium, 90-92 DEG C, hydrolysis 1-2 hour, later 0.5-1 parts of mixed stabilizer of addition be dried after reaching uniform state, powder
It is broken, it include 0.6 part of thiocarbamide, 0.2 part of anhydrous sodium sulfite, 0.2 part of EDETATE SODIUM in 1 part of mixed stabilizer.
The present invention uses redox and azo composite initiation system, improves polymer molecular weight, by introducing sulfonic acid
Water base group improves the saline-alkaline tolerance of polymer to base by force, and the branched structure of strand is improved by introducing pyrrolidone-base.This
Invention causes polymerization under ultralow temperature, and homemade mixed stabilizer is added while hydrolysis, both improves polyacrylamide
Saline-alkaline tolerance, in turn ensure super high molecular weight shear degradation and heat-resisting property, be worth application.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with the embodiment of the present invention.Obviously, described
Embodiment is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field
Those of ordinary skill's every other embodiment obtained without creative efforts, belongs to protection of the present invention
Range.
Embodiment 1
Distilled water 739.8g is first added into 1L wide-mouth bottle, adds an alkali sodium hydroxide 7g, is slowly added to function after being uniformly dissolved
Energy monomer AMPS 50g, is added vinylpyrrolidone 0.5g after 15 DEG C of water bath with thermostatic control or less dissolutions completely, is stirring evenly and then adding into
Acrylamide monomer AM 200g is refined, adjusting pH value is 12, and sodium chloride 1g, urea 1.5g are added later and cools to -2
℃；It moves into Dewar bottle, is passed through 99.999% or more High Purity Nitrogen deoxygenation 10min, EDTA 0.01g is added, continue logical nitrogen and remove
Tert-butyl hydroperoxide 0.002g is first added after azobisisoheptonitrile 0.2g, then logical nitrogen deoxygenation 20min are added after oxygen 20min,
Iron ammonium sulfate 0.01g is added after 2min, then continues to seal after logical nitrogen becomes viscous to solution.
After solution temperature rises to peak and Temperature fall 2h, colloid is taken out from Dewar bottle, is granulated into diameter 2-3mm
Particle, take out the colloidal solid 100g that has been granulated and be put into beaker, addition hydrolytic reagent grain alkali sodium hydroxide 1.0g and reducing agent
Sodium hydrogensulfite 0.1g, seals after mixing evenly and is put into 90 DEG C of water bath with thermostatic control and hydrolyze 1 hour, and mixed stability is added later
Agent 1g(is including thiocarbamide 0.6g, anhydrous sodium sulfite 0.2g, EDETATE SODIUM 0.2g), dispersing agent (white oil), after mixing evenly
It is put into baking oven and the dry 1.5-2h under the conditions of 65 DEG C, taking-up is got product after pulverizing and sieving.
Embodiment 2
Distilled water 771.3g is first added into 1L wide-mouth bottle, adds an alkali sodium hydroxide 10g, is slowly added to function after being uniformly dissolved
Energy monomer AMPS 35g, is added vinylpyrrolidone 1.0g after 15 DEG C of water bath with thermostatic control or less dissolutions completely, is stirring evenly and then adding into
Acrylamide monomer AM 180g is refined, adjusting pH value is 12.5, and sodium chloride 1.5g, urea 1g are added later and cools to 0
℃；It moves into Dewar bottle, is passed through 99.999% or more High Purity Nitrogen deoxygenation 10min, EDTA 0.05g is added, continue logical nitrogen and remove
Tert-butyl hydroperoxide 0.004g is first added after azobisisoheptonitrile 0.15g, then logical nitrogen deoxygenation 20min are added after oxygen 20min,
Iron ammonium sulfate 0.008g is added after 2min, then continues to seal after logical nitrogen becomes viscous to solution.
After solution temperature rises to peak and Temperature fall 2h, colloid is taken out from Dewar bottle, is granulated into diameter 1-3mm
Particle, take out the colloidal solid 100g that has been granulated and be put into beaker, addition hydrolytic reagent grain alkali sodium hydroxide 3.0g and reducing agent
Sodium hydrogensulfite 1.0g, seals after mixing evenly and is put into 91 DEG C of water bath with thermostatic control and hydrolyze 1.5 hours, and it is steady that mixing is added later
Determine agent 0.5g(including thiocarbamide 0.3g, anhydrous sodium sulfite 0.1g, EDETATE SODIUM 0.1g), dispersing agent (white oil), stirring is equal
It is put into baking oven after even and the dry 1.5-2h under the conditions of 65 DEG C, taking-up are got product after pulverizing and sieving.
Embodiment 3
Distilled water 771.3g is first added into 1L wide-mouth bottle, adds an alkali sodium hydroxide 10g, is slowly added to function after being uniformly dissolved
Energy monomer AMPS 35g, is added vinylpyrrolidone 1.0g after 15 DEG C of water bath with thermostatic control or less dissolutions completely, is stirring evenly and then adding into
Refine acrylamide monomer AM 180g, adjust pH value be 12.2, later be added sodium chloride 1.5g, urea 1g and cool to-
1℃；It moves into Dewar bottle, is passed through 99.999% or more High Purity Nitrogen deoxygenation 10min, EDTA 0.05g is added, continue logical nitrogen and remove
Tert-butyl hydroperoxide 0.004g is first added after azobisisoheptonitrile 0.15g, then logical nitrogen deoxygenation 20min are added after oxygen 20min,
Iron ammonium sulfate 0.008g is added after 2min, then continues to seal after logical nitrogen becomes viscous to solution.
After solution temperature rises to peak and Temperature fall 2h, colloid is taken out from Dewar bottle, is granulated into diameter 3-5mm
Particle, take out the colloidal solid 100g that has been granulated and be put into beaker, addition hydrolytic reagent grain alkali sodium hydroxide 2.0g and reducing agent
Sodium hydrogensulfite 0.5g, seals after mixing evenly and is put into 90 DEG C of water bath with thermostatic control and hydrolyze 2 hours, and mixed stability is added later
Agent 0.8g(is including thiocarbamide 0.48g, anhydrous sodium sulfite 0.16g, EDETATE SODIUM 0.16g), dispersing agent (white oil), stirring is equal
It is put into baking oven after even and the dry 1.5-2h under the conditions of 65 DEG C, taking-up are got product after pulverizing and sieving.
Embodiment 4
Distilled water 758.6g is first added into 1L wide-mouth bottle, adds an alkali sodium hydroxide 8g, is slowly added to function after being uniformly dissolved
Energy monomer AMPS 40g, is added vinylpyrrolidone 0.8g after 15 DEG C of water bath with thermostatic control or less dissolutions completely, is stirring evenly and then adding into
Refine acrylamide monomer AM 190g, adjust pH value be 12, later be added sodium chloride 1.2g, urea 1.2g and cool to-
2℃；It moves into Dewar bottle, is passed through 99.999% or more High Purity Nitrogen deoxygenation 10min, EDTA 0.03g is added, continue logical nitrogen and remove
Tert-butyl hydroperoxide 0.003g is first added after azobisisoheptonitrile 0.14g, then logical nitrogen deoxygenation 20min are added after oxygen 20min,
Iron ammonium sulfate 0.009g is added after 2min, then continues to seal after logical nitrogen becomes viscous to solution.
After solution temperature rises to peak and Temperature fall 2h, colloid is taken out from Dewar bottle, is granulated into diameter 2-4mm
Particle, take out the colloidal solid 100g that has been granulated and be put into beaker, addition hydrolytic reagent grain alkali sodium hydroxide 1.8g and reducing agent
Sodium hydrogensulfite 0.8g, seals after mixing evenly and is put into 92 DEG C of water bath with thermostatic control and hydrolyze 2 hours, and mixed stability is added later
Agent 0.6g(is including thiocarbamide 0.36g, anhydrous sodium sulfite 0.12g, EDETATE SODIUM 0.12g), dispersing agent (white oil), stirring is equal
It is put into baking oven after even and the dry 1.5-2h under the conditions of 65 DEG C, taking-up are got product after pulverizing and sieving.
Test characterization is carried out to the product of embodiment 1-4, specific test result is as follows shown in table:
Wherein, the test of solution properties viscosity number and molecular weight is tested according to middle petroleum enterprise mark Q/SY 119-2014, specific to grasp
As: take sample 1g(to give money as a gift) to be slowly uniformly added into (199-1/s) g(s be solid content) in pure water, stirred under 400r/min revolving speed
It is measured after 2 hours；
Wherein, the test method of viscosity specifically: sample 1g(is taken to give money as a gift) slowly it is uniformly added into the mould of 199g, 1.8 ten thousand salinities
In quasi- salt water, calcium ions and magnesium ions content reaches 504mg/L, stirs 1 hour under 400r/min revolving speed, after the closed placement of room temperature 24 hours
It is diluted to 2000ppm, is measured under the conditions of 85 DEG C；
Wherein, water-insoluble according to middle petroleum look forward to mark Q/SY 119-2014 detected, be much better than standard requirements≤0.20%；
Wherein, filterable agent according to middle petroleum look forward to mark Q/SY 119-2014 detected, better than standard requirements≤2.0.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of novel heatproof anti-salt polyacrylamide, it is characterised in that: including sulfonic group and pyrrolidone-base, novel heatproof is anti-
For salt polyacrylamide anti-salt property up to 20,000 salinities, calcium ions and magnesium ions total amount reaches 504mg/L, and 85 DEG C of temperature.
2. a kind of synthetic method of novel heatproof anti-salt polyacrylamide as described in claim 1, it is characterised in that: including such as
Lower step:
The first step, in redox and azo composite initiation system, will purification acrylamide monomer AM, function monomer AMPS and
Vinylpyrrolidone is reacted to obtain colloid at -2-0 DEG C of initiation temperature, and the composite initiation system includes by tert-butyl mistake
Hydrogen oxide oxidant and the iron ammonium sulfate reducing agent redox initiation system formed and the idol being made of azobisisoheptonitrile
Nitrogen causes system；
Second step is granulated, hydrolysis, dry, crushing, sieving.
3. synthetic method according to claim 2, it is characterised in that: press mass fraction, 100 parts of polyblend Central Plains
Material formula are as follows: 3.5-5 parts of function monomer AMPS, refine 18-20 parts of acrylamide monomer AM, vinylpyrrolidone 0.05-0.1
Part, 0.0002-0.0005 parts of tert-butyl hydroperoxide, 0.0006-0.001 parts of iron ammonium sulfate, azobisisoheptonitrile 0.01-
0.02 part, remaining is water.
4. synthetic method according to claim 3, it is characterised in that: in the first step, will first refine acrylamide list
Body AM, function monomer AMPS and vinylpyrrolidone are configured to aqueous solution, and adjusting PH with sodium hydroxide is 12-12.5；Again plus
Enter 0.1-0.15 parts of sodium chloride, 0.1-0.15 parts of urea, at a temperature of -2-0 DEG C, drum nitrogen deoxygenation 10min after be added metal from
Azobisisoheptonitrile is added after continuing deoxygenation 20min, after being further continued for deoxygenation 20min in 0.001-0.005 parts of sub- screener EDTA
Tert-butyl hydroperoxide is first added, iron ammonium sulfate is added after 2min, then leads to nitrogen until solution seals after becoming viscous.
5. synthetic method according to claim 4, it is characterised in that: rise to peak and natural to solution temperature after sealing
Cool down after 2h, take out colloid and be granulated, by mass fraction, 1-3 parts of hydrolytic reagent hydroxide is added in every 100 parts of colloidal solid
Sodium and 0.1-1 parts of reducing agent sodium hydrogensulfite, 90-92 DEG C, hydrolysis 1-2 hours, are added 0.5-1 parts of mixed stabilizer later
Reach and be dried after uniform state, crush, includes 0.6 part of thiocarbamide, anhydrous sodium sulfite 0.2 in 1 part of mixed stabilizer
Part, 0.2 part of EDETATE SODIUM.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111925478A (en) * | 2020-07-23 | 2020-11-13 | 天津博弘化工有限责任公司 | Preparation method of differential type multi-component polyacrylamide |
| CN112694882A (en) * | 2020-11-26 | 2021-04-23 | 天津大港油田滨港集团博弘石油化工有限公司 | Low-cost high-temperature high-salinity reservoir binary composite oil displacement system and preparation method thereof |
| CN113736013A (en) * | 2020-05-28 | 2021-12-03 | 中国石油天然气股份有限公司 | Temperature-resistant salt-resistant polyacrylamide with adjustable molecular weight and preparation method thereof |
| CN113943398A (en) * | 2021-12-07 | 2022-01-18 | 东营宝莫环境工程有限公司 | Preparation method of thickening agent for high-temperature-resistant instant acidizing fracturing fluid |
| CN114605576A (en) * | 2022-03-22 | 2022-06-10 | 爱森（中国）絮凝剂有限公司 | Preparation method of polyacrylamide potassium salt for drilling fluid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111925478A (en) * | 2020-07-23 | 2020-11-13 | 天津博弘化工有限责任公司 | Preparation method of differential type multi-component polyacrylamide |
| CN112694882A (en) * | 2020-11-26 | 2021-04-23 | 天津大港油田滨港集团博弘石油化工有限公司 | Low-cost high-temperature high-salinity reservoir binary composite oil displacement system and preparation method thereof |
| CN113943398A (en) * | 2021-12-07 | 2022-01-18 | 东营宝莫环境工程有限公司 | Preparation method of thickening agent for high-temperature-resistant instant acidizing fracturing fluid |
| CN114605576A (en) * | 2022-03-22 | 2022-06-10 | 爱森（中国）絮凝剂有限公司 | Preparation method of polyacrylamide potassium salt for drilling fluid |
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Application publication date: 20190104 |