CN103819606A - Preparation method for salt-tolerant ultra-high molecular weight thickening agent - Google Patents
Preparation method for salt-tolerant ultra-high molecular weight thickening agent Download PDFInfo
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- CN103819606A CN103819606A CN201410092419.4A CN201410092419A CN103819606A CN 103819606 A CN103819606 A CN 103819606A CN 201410092419 A CN201410092419 A CN 201410092419A CN 103819606 A CN103819606 A CN 103819606A
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Abstract
The invention relates to a preparation method for a salt-tolerant ultra-high molecular weight thickening agent. The preparation method comprises the following steps: placing a certain amount of 2-methyl-2-acrylamido propane sulfonic acid and acrylamide into a reaction vessel, and using ammonia water or sodium hydroxide to adjust the pH value to 6.5-7.0; adding a kerosene solution in which Span-80 and a hydrophobic monomer are dissolved, adding an initiator after emulsification, introducing nitrogen, heating for reaction, and adding Tween-80 for invert-emulsion to obtain the salt-tolerant ultra-high molecular weight thickening agent. According to the agent, the octadecyl acrylate hydrophobic monomer is used as a functional monomer for improving the salt tolerance of the thickening agent, the preparation method is simple, and the industrialized production is facilitated.
Description
Technical field
The present invention relates to a kind of preparation method of salt-resistant type thickening material, the acrylamide based terpolymers that this thickening material is ultra-high molecular weight, belongs to chemical technology field.
Background technology
Macromolecule thickener refers to viscosity for improving product or a class new functional macromolecule material of denseness, there is the features such as consumption is little, thickening is obvious, easy to use, be widely used in the industries such as medicine, printing and dyeing, makeup, foodstuff additive, derived energy chemical.Acrylic polymer thickening material is a class efficient thickeners of developing in recent years, its thickening effectiveness and over-all properties are all better, but in hypersaline environment, polymer molecular chain is because the quick property of salt can be subsided, cause the reduction of ydrodynamics volume, thereby thickening effectiveness is weakened.
If with 2-methyl-2-acrylamido propanesulfonic acid and acrylamide copolymerization, make like this on polymer molecular chain with sulfonate ion, will have than other carboxylate anion polymkeric substance and there is larger ydrodynamics volume, thus the salt tolerance of increase polymkeric substance.Meanwhile, we introduce hydrophobic monomer in polymkeric substance preparation process.Due to its structural performance, under the effect of salt adding, be more conducive to outside intermolecular generation association and form meshed super molecular structure, structural viscosity will further increase.The present invention adopts reversed emulsion polymerization to prepare a kind of acrylamide based terpolymers of salt-resistant type ultra-high molecular weight, on polymer molecular chain with both positive and negative electric charge group, in the aqueous solution, because making molecular chain, attracting each other of negative ions shrink, in the time adding small molecule salt, due to anti-ionization, compression double electric layer, magnetism weakens, polymer chain is stretched gradually, and its solution viscosity goes up not down, and shows fairly obvious " anti-polyelectrolyte effect ".
Summary of the invention
The object of the invention is to adopt the method for inverse emulsion polymerization to prepare acrylamide based terpolymers, its molecular weight reaches more than 1,000 ten thousand, by the interaction of the hydrophobic grouping on polymer lateral chain, zwitterion group, thereby there is good salt resistant character.This multipolymer can be used as salt-resistant type thickening material and is applied to oil production, phase-change accumulation energy equal energy source chemical field.
The preparation of this ultra-high molecular weight terpolymer is divided into three steps, specific as follows:
(1) preparation of kerosin: emulsifying agent Span-80 is mixed with the ratio of 1:4～5 with kerosene, and stir, after Span-80 is dissolved in kerosene completely, slowly add a certain amount of hydrophobic monomer, stir and make its dissolving;
Described hydrophobic monomer is octadecyl acrylate;
Wherein, the mass ratio of hydrophobic monomer and kerosene is 1:1～2;
(2) preparation of the aqueous solution: 2-methyl-2-acrylamido propanesulfonic acid and acrylamide are dissolved in the water with certain mass ratio, then under condition of ice bath, hierarchy of control temperature is 0～10 ℃, slowly drip while stirring a certain amount of ammoniacal liquor or aqueous sodium hydroxide solution, make the pH value of system be controlled at 6.5-7.0;
Wherein, the mass ratio of 2-methyl-2-acrylamido propanesulfonic acid, acrylamide, water is (1～2): (1～4): (4～9);
(3) step (1) gained kerosin is added to step (2) obtained aqueous solution with the mass ratio of 1:1.5～2; emulsification 30-45 minute under the condition of normal temperature and low whipping speed 1200-1500 rev/min; then add a certain amount of initiator; be warming up to 60-70 ℃; under nitrogen protection, react 2-3h; finally add the reverse emulsification 40-60 minute of a certain amount of Tween-80, discharging obtains salt-resistant type ultra-high molecular weight thickening material.
Wherein, the mass ratio of Tween-80 and kerosene is 1:1～1.5;
Described initiator is the one in ammonium persulphate, Sodium Persulfate, Potassium Persulphate, and the mass ratio of initiator and kerosene is 1:120-140.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of embodiment 1 gained salt-resistant type ultra-high molecular weight thickening material;
Fig. 2 is that in embodiment 2, to embodiment 1 gained salt-resistant type ultra-high molecular weight thickening material, the viscosity under different salt concn changes.
Embodiment
Below by embodiment, the present invention is specifically described.Be necessary to be pointed out that at this; following examples are only for the invention will be further described; can not be interpreted as limiting the scope of the invention, some nonessential improvement and adjustment that the professional and technical personnel in this field content according to the present invention is made, still belong to protection scope of the present invention.
The preparation of embodiment 1 salt-resistant type ultra-high molecular weight thickening material
2-methyl-2-acrylamido propanesulfonic acid and acrylamide are dissolved in the water with the mass ratio of 1:1:4, and then, under condition of ice bath, hierarchy of control temperature is 5 ℃, slowly drips while stirring ammonia soln, makes the pH value of system be controlled at 6.5; Emulsifying agent Span-80 is mixed with the ratio of 1:4 with kerosene again, and stir, after Span-80 is dissolved in kerosene completely, the octadecyl acrylate that slowly to add with the mass ratio of kerosene be 1:1, stirs and makes its dissolving; Kerosin is joined in the aqueous solution neutralizing; emulsification 40 minutes under the condition that normal temperature and low whipping speed are 1200 revs/min; then the ammonium persulphate that to add with the mass ratio of kerosene be 1:140; be warming up to 60 ℃; under nitrogen protection, react 2 hours; the Tween-80 that finally to add with the mass ratio of kerosene be 1:1, oppositely emulsification 50 minutes, discharging obtains salt-resistant type ultra-high molecular weight thickening material.
The salt resistant character of embodiment 2 thickening materials is measured
Embodiment 1 gained salt-resistant type ultra-high molecular weight thickening material is applied to containing sal glauberi (Na
2sO
4 .10H
2o) in 0～20% phase change material system.Take 1 gram of salt-resistant type ultra-high molecular weight thickening material, it is slowly joined in 100 ml waters, and stirring at normal temperature 2 hours under the condition of 1500 revs/min of low whipping speeds, then its airtight water-bath of putting into 50 ℃ is heated swelling 2 hours, be finally cooled to 25 ℃.Be 1 s by the solution preparing in shearing rate
-1condition under, measure its viscosity number with Anton Paar MCR501 rotational rheometer.Then, in solution, add respectively 2%, 5%, 10% and 20% sal glauberi, continue to measure its corresponding viscosity number.Fig. 2 is the curve that the soltion viscosity that records changes with salt concn, and the viscosity of this thickening material is subject to the variation of salt concn less, has good salt tolerance.
Claims (2)
1. a preparation method for salt-resistant type ultra-high molecular weight thickening material, is characterized in that comprising the steps:
(1) preparation of kerosin: emulsifying agent Span-80 is mixed with the ratio of 1:4～5 with kerosene, and stir, after Span-80 is dissolved in kerosene completely, slowly add a certain amount of hydrophobic monomer, stir and make its dissolving;
Wherein, the mass ratio of hydrophobic monomer and kerosene is 1:1～2;
(2) preparation of the aqueous solution: 2-methyl-2-acrylamido propanesulfonic acid and acrylamide are dissolved in the water with certain mass ratio, then under condition of ice bath, hierarchy of control temperature is 0～10 ℃, slowly drip while stirring a certain amount of ammoniacal liquor or aqueous sodium hydroxide solution, make the pH value of system be controlled at 6.5-7.0; Wherein, the mass ratio of 2-methyl-2-acrylamido propanesulfonic acid, acrylamide, water is (1～2): (1～4): (4～9);
(3) step (1) gained kerosin is added to step (2) obtained aqueous solution with the mass ratio of 1:1.5～2, emulsification 30-45 minute under the condition of normal temperature and low whipping speed 1200-1500 rev/min, then add a certain amount of initiator, be warming up to 60-70 ℃, under nitrogen protection, react 2-3 hour, finally add the reverse emulsification 40-60 minute of a certain amount of Tween-80, discharging obtains salt-resistant type ultra-high molecular weight thickening material; Wherein, the mass ratio of Tween-80 and kerosene is 1:1～1.5;
Described initiator is the one in ammonium persulphate, Sodium Persulfate, Potassium Persulphate; Wherein, the mass ratio of initiator and kerosene is 1:120-140.
2. the preparation method of a kind of salt-resistant type ultra-high molecular weight thickening material according to claim 1, is characterized in that: described hydrophobic monomer is octadecyl acrylate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106279523A (en) * | 2015-06-25 | 2017-01-04 | 中国石油天然气股份有限公司 | A kind of thickening agent and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1772778A (en) * | 2005-10-31 | 2006-05-17 | 山东大学 | Inverse emulsion process of preparing amphoteric polymer |
| CN1908026A (en) * | 2006-08-17 | 2007-02-07 | 广州市天赐高新材料科技有限公司 | Acrylamide crosslinking copolymer emulsion and preparation method thereof |
| CN101037492A (en) * | 2007-03-28 | 2007-09-19 | 中国石油大学(华东) | Method for preparing propylene amides copolymer with regular branch structure by inverse emulsion method |
| CN103146372A (en) * | 2013-02-28 | 2013-06-12 | 中国石油化工股份有限公司 | Inverse emulsion polymer thickener for fracturing fluid and preparation method thereof |
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2014
- 2014-03-28 CN CN201410092419.4A patent/CN103819606A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1772778A (en) * | 2005-10-31 | 2006-05-17 | 山东大学 | Inverse emulsion process of preparing amphoteric polymer |
| CN1908026A (en) * | 2006-08-17 | 2007-02-07 | 广州市天赐高新材料科技有限公司 | Acrylamide crosslinking copolymer emulsion and preparation method thereof |
| CN101037492A (en) * | 2007-03-28 | 2007-09-19 | 中国石油大学(华东) | Method for preparing propylene amides copolymer with regular branch structure by inverse emulsion method |
| CN103146372A (en) * | 2013-02-28 | 2013-06-12 | 中国石油化工股份有限公司 | Inverse emulsion polymer thickener for fracturing fluid and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106279523A (en) * | 2015-06-25 | 2017-01-04 | 中国石油天然气股份有限公司 | A kind of thickening agent and its preparation method and application |
| CN106279523B (en) * | 2015-06-25 | 2019-03-15 | 中国石油天然气股份有限公司 | A kind of thickener and its preparation method and application |
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Application publication date: 20140528 |