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A kind of fluorine-containing modified diallylamine water-soluble polymer and preparation method thereof

A technology of water-soluble polymer and diallylamine, applied in the field of fluorine-modified diallylamine water-soluble polymer and preparation thereof, can solve the problem of difficult to obtain pure polymer, difficult to remove surfactant, harsh reaction conditions, etc. problem, to achieve the effect of improving rigidity, improving hydrophobic association ability, and simple preparation

Active Publication Date: 2014-10-15
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] Traditional hydrophobically associated water-soluble polymers are prepared by emulsion polymerization, but the emulsion polymerization of introducing fluorine-containing segments on macromolecular chains requires the use of expensive fluorosurfactants, and the reaction conditions are harsh, and post-treatment is not easy to completely remove residual Surfactant, it is difficult to obtain pure polymer, which affects the use

Method used

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  • A kind of fluorine-containing modified diallylamine water-soluble polymer and preparation method thereof
  • A kind of fluorine-containing modified diallylamine water-soluble polymer and preparation method thereof
  • A kind of fluorine-containing modified diallylamine water-soluble polymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1, preparation of fluorine-modified diallylamine monomer

[0042] Weigh 5.18g (12mmol) of perfluorohexylethyl acrylate and 30mL of absolute ethanol, add them to a 50mL three-necked flask equipped with a condenser tube and a stirring bar, and start stirring. Then weigh 0.972 g (10 mmol) of diallylamine and add it into a three-necked flask. After the solution is mixed evenly, put it into a constant temperature water bath at 60°C, and react for 6 hours. After the reaction, the residual solvent was removed by rotary evaporation under reduced pressure to obtain a brownish yellow liquid, that is, 5.1346 g of a fluorine-modified diallylamine monomer with the structure shown in formula I, with a yield of 97.5%.

[0043] Fluorine-modified diallylamine monomer shown in formula I 1 H-NMR spectrum as figure 1 As shown, after analysis, the structure of the monomer prepared in this embodiment is correct.

Embodiment 2

[0044] Embodiment 2, preparation of fluorine-containing modified diallylamine water-soluble polymer

[0045] Weigh 0.132g (0.2563mmol) of the fluorine-modified diallylamine monomer shown in Formula I prepared in Example 1, and measure 50mL of dimethyl sulfoxide, add a nitrogen tube, a condenser tube and a 100mL In the three-neck flask, start stirring and feed nitrogen. Then weigh 3.532 g of acrylamide (0.0498 mol, the molar ratio of fluorine-modified diallylamine monomer to acrylamide is 1:194), and add it into a three-necked flask. After the solution is mixed evenly, put it into a constant temperature water bath at 60°C. Weigh 0.41g of azobisisobutyronitrile (the amount added is 0.501% of the total molar weight of fluorine-modified diallylamine monomer and acrylamide), and add it to a three-necked flask. In this reaction body, fluorine-modified diallylamine The total molar concentration of allylamine monomer and acrylamide is 1mol L -1 .

[0046] The reaction ended after ...

Embodiment 3

[0050] Embodiment 3, the preparation of polymer containing fluorinated diallylamine structure

[0051] The specific preparation steps are basically the same as in Example 2, except that the monomer feeding is changed to 3.515 g of acrylamide and 0.264 g of fluorine-modified diallylamine to obtain the fluorine-containing modified diallylamine water-soluble polymer powder products, the 1 H-NMR and 19 The F-NMR spectrogram is substantially the same as the polymer prepared in Example 2; wherein, the weight-average molecular weight is 1.523 × 10 5 g / mol.

[0052] When the concentration of the aqueous solution of the fluorine-containing modified diallylamine aqueous polymer prepared in this example is 10 mg / mL at room temperature, the surface tension test of the hanging plate method shows that the surface tension of the aqueous solution can be reduced to 37 mN / m.

[0053] The fluorine-modified diallylamine aqueous solution polymer prepared in this example has relatively high ther...

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Abstract

The invention discloses a water-soluble polymer containing fluorine modified diallylamine and a preparation method thereof. The water-soluble polymer has a structural formula as represented by a formula II. In the formula II, the weight-average degree m of polymerization is a natural number in a range of 2266 to 3493, and the weight-average degree n of polymerization is a natural number in a range of 2 to 35. The preparation method for the water-soluble polymer represented by the formula II comprises the step of subjecting a fluorine modified diallylamine monomer and acrylamide to free radical polymerization under the catalysis of an initiator so as to obtain the water-soluble polymer represented by the formula II. The water-soluble polymer containing fluorine modified diallylamine can be directly used and has extensive latent use values in fields like oil exploitation, coatings, medicines and daily chemicals.

Description

technical field [0001] The invention relates to a fluorine-containing modified diallylamine water-soluble polymer and a preparation method thereof, belonging to the technical field of water-soluble polymer synthesis. Background technique [0002] The fluorine-modified diallylamine polymerizable monomer is a polymerizable monomer prepared by linking the amine group in diallylamine with a side chain containing a perfluoroalkyl group through a chemical reaction. The fluorine-modified diallylamine water-soluble polymer refers to a class of water-soluble polymers in which a fluorine-modified diallylamine structure is introduced into the hydrophilic macromolecular chain of the polymer. After polymerization, diallylamine will form a nitrogen-containing five-membered ring, which can significantly increase the rigidity of the polymer molecular chain, thereby improving the hydrophobic association ability of the water-soluble polymer; while the perfluoroalkyl chain is compatible with t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/12C07C227/06C08F220/56C08F226/02C08F2/06C08F6/12
Inventor 宋彩雨吕鑫张健梁守成李强谭业邦
Owner CHINA NAT OFFSHORE OIL CORP
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