CN102649831A - Preparation method for non-ionic fluorocarbon modified polyacrylamide - Google Patents
Preparation method for non-ionic fluorocarbon modified polyacrylamide Download PDFInfo
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- CN102649831A CN102649831A CN2012101541301A CN201210154130A CN102649831A CN 102649831 A CN102649831 A CN 102649831A CN 2012101541301 A CN2012101541301 A CN 2012101541301A CN 201210154130 A CN201210154130 A CN 201210154130A CN 102649831 A CN102649831 A CN 102649831A
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Abstract
The invention discloses a preparation method for non-ionic fluorocarbon modified polyacrylamide, which comprises the following steps of: firstly, uniformly mixing fluorine-containing monomer, acrylamide and water; introducing nitrogen for dispersing oxygen, and then adding an initiator; and performing solution polymerization under ultrasonic assistance, thereby obtaining the non-ionic fluorocarbon modified polyacrylamide. Due to the high-efficient dispersive action of ultrasonic wave, the hydrophobic monomer is excellently dispersed in water solution and is copolymerized with hydrophilic monomer, without adding emulsifying agent or surface activity monomer. According to the preparation method provided by the invention, the usage of the emulsifying agent or surface activity monomer is avoided, so that the HAPAM after-treatment is fully eliminated, the preparation process is simplified and the production efficiency is increased.
Description
Technical field
The invention belongs to chemical field, particularly a kind of preparation method of non-ion fluorin carbon modified polyacrylamide.
Background technology
SEPIGEL 305 and verivate thereof are important polymkeric substance, and Application Areas is extensive.In the type of numerous SEPIGEL 305s, the hydrophobic association type SEPIGEL 305 is an important branch.The hydrophobic association type SEPIGEL 305 is introduced a small amount of hydrophobic grouping and is processed on the polyacrylamide main chain; Bunch collection takes place owing to the hydrophobic interaction between the hydrophobic grouping makes the SEPIGEL 305 molecular chain; Thereby significantly change the rheological property of solution, improve effect, broadened application field.At present, the hydrophobic grouping of introducing on the hydrophobic association type SEPIGEL 305 molecular backbone chain mainly is hydrocarbon hydrophobic monomer.Fluorochemical monomer is a kind of strong-hydrophobicity monomer, and its hydrophobic association effect is stronger than hydrocarbon hydrophobic monomer, so have the better application effect by the fluorine-containing polyacrylamide copolymer of nonionic of fluorochemical monomer and acrylic amide copolymerization.
For the uncompatibility that overcomes hydrophobic monomer and hydrophilic monomer, realize both copolymerization, the surface active monomer method had appearred again more in the micelle assay that adopt in recent years during preparation hydrophobic association type SEPIGEL 305.Micelle assay is in polymerization system, to add a large amount of emulsifying agents, with after the hydrophobic monomer emulsification again with copolymerization such as hydrophilic monomer, but the raising that adds affiliation impact polymer molecular weight of emulsifying agent, increase the problems such as complexity of multipolymer aftertreatment.Surface active monomer is claimed polymerisable surfactant again, is one type of tensio-active agent that contains polymerizable groups, has both had surfactivity, can under certain initiation conditions, can produce all (being total to) polyreactions again, can eliminate the aftertreatment of HAPAM fully.At present, be applicable to that the surface active monomer preparation of HAPAM is complicated, with high costs, so the research work of surface active monomer method is carried out seldom.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of preparation method who does not use the non-ion fluorin carbon modified polyacrylamide of emulsifying agent and surface active monomer is provided.
The technical scheme that adopts for the present invention that achieves the above object is:
1) at first, with fluorochemical monomer, acrylic amide and water by 1: (10-200): mass ratio (10-10000) mixes and makes mixing solutions;
2) in mixing solutions, led to nitrogen 10-60 minute then, with the speed of 20mL/min-200mL/min;
3) secondly, the initiator of adding monomer total mass 0.1%-1.0% stirs;
4) last, transfer at 20 ℃-90 ℃ and to place ultrasonic generator to carry out ultrasonic polymerization, ultrasonic power 80W-200W reacts and obtains non-ion fluorin carbon modified polyacrylamide after 0.5-5 hour.
Said fluorochemical monomer is vinylformic acid trifluoro ethyl ester, trifluoroethyl methacrylate, vinylformic acid hexafluoro butyl ester, methylacrylic acid hexafluoro butyl ester, dodecafluorhe-ptylacrylate or methylacrylic acid ten difluoro heptyl esters.
Said nitrogen is liquid nitrogen or gasiform nitrogen.
Said initiator is ammonium persulphate, Potassium Persulphate, azo diisobutyl amidine hydrochloride, ammonium persulphate-S-WAT, ammonium persulfate-sodium bisulfite, Potassium Persulphate-S-WAT, Potassium Persulphate-sodium sulfite anhy 96, ammonium persulphate-Sulfothiorine or Potassium Persulphate-Sulfothiorine, and wherein the mass ratio of oxygenant and reductive agent is 2: 1 in the oxidation-reduction trigger system.
Because the dissemination of ultrasonic high-efficiency need not to add emulsifying agent or surface active monomer and just can make hydrophobic monomer be dispersed in well in the aqueous solution, carries out copolymerization with hydrophilic monomer.Adopt preparation method of the present invention can avoid the use of emulsifying agent or surface active monomer,, simplify preparation technology, enhance productivity to eliminate the aftertreatment of HAPAM fully.
Embodiment
Embodiment 1,1) at first, fluorochemical monomer vinylformic acid trifluoro ethyl ester, acrylic amide and water mixed by 1: 10: 10 mass ratio make mixing solutions;
2) then, in mixing solutions, led to nitrogen 60 minutes with the speed of 20mL/min;
3) secondly, the initiator ammonium persulfate that adds monomer total mass 1.0% stirs;
4) last, transfer at 20 ℃ and to place ultrasonic generator to carry out ultrasonic polymerization, ultrasonic power 80W reacts and obtains non-ion fluorin carbon modified polyacrylamide after 5 hours.
Embodiment 2,1) at first, fluorochemical monomer methylacrylic acid ten difluoro heptyl esters, acrylic amide and water mixed by 1: 200: 10000 mass ratio make mixing solutions;
2) then, in mixing solutions, led to nitrogen 10 minutes with the speed of 200mL/min;
3) secondly, the initiator azo diisobutyl amidine hydrochloride that adds monomer total mass 0.1% stirs;
4) last, transfer at 90 ℃ and to place ultrasonic generator to carry out ultrasonic polymerization, ultrasonic power 200W reacts and obtains non-ion fluorin carbon modified polyacrylamide after 0.5 hour.
Embodiment 3,1) at first, fluorochemical monomer trifluoroethyl methacrylate, acrylic amide and water mixed by 1: 50: 100 mass ratio make mixing solutions;
2) then, in mixing solutions, led to nitrogen 10 minutes with the speed of 50mL/min;
3) secondly, the initiator ammonium persulfate-Sulfothiorine that adds monomer total mass 0.3% stirs;
4) last, transfer at 50 ℃ and to place ultrasonic generator to carry out ultrasonic polymerization, ultrasonic power 100W reacts and obtains non-ion fluorin carbon modified polyacrylamide after 2 hours.
Embodiment 4,1) at first, fluorochemical monomer dodecafluorhe-ptylacrylate, acrylic amide and water mixed by 1: 100: 1000 mass ratio make mixing solutions;
2) then, in mixing solutions, led to nitrogen 30 minutes with the speed of 100mL/min;
3) secondly, the initiator azo diisobutyl amidine hydrochloride that adds monomer total mass 0.5% stirs;
4) last, transfer at 60 ℃ and to place ultrasonic generator to carry out ultrasonic polymerization, ultrasonic power 140W reacts and obtains non-ion fluorin carbon modified polyacrylamide after 3 hours.
Embodiment 5,1) at first, fluorochemical monomer methylacrylic acid hexafluoro butyl ester, acrylic amide and water mixed by 1: 150: 5000 mass ratio make mixing solutions;
2) then, in mixing solutions, led to nitrogen 30 minutes with the speed of 100mL/min;
3) secondly, the initiator azo diisobutyl amidine hydrochloride that adds monomer total mass 0.4% stirs;
4) last, transfer at 50 ℃ and to place ultrasonic generator to carry out ultrasonic polymerization, ultrasonic power 160W reacts and obtains non-ion fluorin carbon modified polyacrylamide after 3 hours.
Claims (4)
1. the preparation method of a non-ion fluorin carbon modified polyacrylamide is characterized in that:
1) at first, with fluorochemical monomer, acrylic amide and water by 1: (10-200): mass ratio (10-10000) mixes and makes mixing solutions;
2) in mixing solutions, led to nitrogen 10-60 minute then, with the speed of 20mL/min-200mL/min;
3) secondly, the initiator of adding monomer total mass 0.1%-1.0% stirs;
4) last, transfer at 20 ℃-90 ℃ and to place ultrasonic generator to carry out ultrasonic polymerization, ultrasonic power 80W-200W reacts and obtains non-ion fluorin carbon modified polyacrylamide after 0.5-5 hour.
2. the preparation method of non-ion fluorin carbon modified polyacrylamide according to claim 1 is characterized in that: said fluorochemical monomer is vinylformic acid trifluoro ethyl ester, trifluoroethyl methacrylate, vinylformic acid hexafluoro butyl ester, methylacrylic acid hexafluoro butyl ester, dodecafluorhe-ptylacrylate or methylacrylic acid ten difluoro heptyl esters.
3. the preparation method of non-ion fluorin carbon modified polyacrylamide according to claim 1 is characterized in that: said nitrogen is liquid nitrogen or gasiform nitrogen.
4. the preparation method of non-ion fluorin carbon modified polyacrylamide according to claim 1; It is characterized in that: said initiator is ammonium persulphate, Potassium Persulphate, azo diisobutyl amidine hydrochloride, ammonium persulphate-S-WAT, ammonium persulfate-sodium bisulfite, Potassium Persulphate-S-WAT, Potassium Persulphate-sodium sulfite anhy 96, ammonium persulphate-Sulfothiorine or Potassium Persulphate-Sulfothiorine, and wherein the mass ratio of oxygenant and reductive agent is 2: 1 in the oxidation-reduction trigger system.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665262A (en) * | 2013-12-13 | 2014-03-26 | 山东大学 | Water-soluble fluorine-containing modified N-NVP polymer and preparation method thereof |
| CN106386041A (en) * | 2016-08-28 | 2017-02-15 | 山东胜伟园林科技有限公司 | Cultivation method for suaeda salsa used for improvement of saline-alkaline land in Hetao irrigation area |
| CN110342624A (en) * | 2019-07-27 | 2019-10-18 | 重庆工商大学 | A kind of preparation method of oxidisability organic polymer coargulator |
| US11534759B2 (en) | 2021-01-22 | 2022-12-27 | Saudi Arabian Oil Company | Microfluidic chip with mixed porosities for reservoir modeling |
| US11566165B2 (en) | 2019-05-30 | 2023-01-31 | Saudi Arabian Oil Company | Polymers and nanoparticles for flooding |
| US11660595B2 (en) | 2021-01-04 | 2023-05-30 | Saudi Arabian Oil Company | Microfluidic chip with multiple porosity regions for reservoir modeling |
| US11773715B2 (en) | 2020-09-03 | 2023-10-03 | Saudi Arabian Oil Company | Injecting multiple tracer tag fluids into a wellbore |
| US11873353B2 (en) | 2019-05-29 | 2024-01-16 | Saudi Arabian Oil Company | Flow synthesis of polymer nanoparticles |
-
2012
- 2012-05-17 CN CN2012101541301A patent/CN102649831A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 中国石油学会炼制分会等编: "《2002重质油加工利用学术研讨会论文集》", 31 December 2002 * |
| 李刚辉等: "《表面活性含氟单体-丙烯酰胺共聚物溶液性质研究》", 《高分子学报》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665262A (en) * | 2013-12-13 | 2014-03-26 | 山东大学 | Water-soluble fluorine-containing modified N-NVP polymer and preparation method thereof |
| CN103665262B (en) * | 2013-12-13 | 2016-05-11 | 山东大学 | Water solubility copolymer of a kind of fluorine-containing modification NVP and preparation method thereof |
| CN106386041A (en) * | 2016-08-28 | 2017-02-15 | 山东胜伟园林科技有限公司 | Cultivation method for suaeda salsa used for improvement of saline-alkaline land in Hetao irrigation area |
| US11873353B2 (en) | 2019-05-29 | 2024-01-16 | Saudi Arabian Oil Company | Flow synthesis of polymer nanoparticles |
| US11566165B2 (en) | 2019-05-30 | 2023-01-31 | Saudi Arabian Oil Company | Polymers and nanoparticles for flooding |
| US11987749B2 (en) | 2019-05-30 | 2024-05-21 | Saudi Arabian Oil Company | Polymers and nanoparticles for flooding |
| US11987748B2 (en) | 2019-05-30 | 2024-05-21 | Saudi Arabian Oil Company | Polymers and nanoparticles for flooding |
| CN110342624A (en) * | 2019-07-27 | 2019-10-18 | 重庆工商大学 | A kind of preparation method of oxidisability organic polymer coargulator |
| US11773715B2 (en) | 2020-09-03 | 2023-10-03 | Saudi Arabian Oil Company | Injecting multiple tracer tag fluids into a wellbore |
| US11660595B2 (en) | 2021-01-04 | 2023-05-30 | Saudi Arabian Oil Company | Microfluidic chip with multiple porosity regions for reservoir modeling |
| US11534759B2 (en) | 2021-01-22 | 2022-12-27 | Saudi Arabian Oil Company | Microfluidic chip with mixed porosities for reservoir modeling |
| US11911761B2 (en) | 2021-01-22 | 2024-02-27 | Saudi Arabian Oil Company | Microfluidic chip with mixed porosities for reservoir modeling |
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Application publication date: 20120829 |