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A kind of amorphous fluoropolymer and its preparation method

A polymer and amorphous technology, applied in the direction of organic chemistry, can solve the problems of inability to effectively control material properties, limit the large-scale industrialization and wide application of perfluorinated amorphous polymer materials, and high cost

Active Publication Date: 2020-10-09
上海丰阜投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Currently, with AF and The synthesis process of several amorphous polymers and monomers represented by them are very complicated and the cost is very high
In addition, there are great differences in the mechanical properties, thermal stability, light transmittance and gas separation selectivity of polymers, which cannot simultaneously meet the special properties required in some application fields, or cannot effectively control the properties of materials. These factors limit the large-scale industrialization and wide application of perfluoroamorphous polymer materials.

Method used

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  • A kind of amorphous fluoropolymer and its preparation method
  • A kind of amorphous fluoropolymer and its preparation method
  • A kind of amorphous fluoropolymer and its preparation method

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preparation example Construction

[0045] The present invention also provides a method for preparing the above-mentioned amorphous fluoropolymer, comprising:

[0046] The fluorine-containing monomer shown in the formula (2) is polymerized with the fluorine-containing olefin in the initiator to obtain the amorphous fluorine-containing polymer shown in the formula (I);

[0047]

[0048] The present invention has no special limitation on the sources of all raw materials, which can be commercially available or self-made.

[0049] Wherein, the fluorine-containing monomer shown in formula (2) is preferably prepared according to the following method: a) methyl pyruvate and 2,4-pentanediol are reacted to obtain 2-methyl ester-2,4,6-trimethyl -1,3-dioxane; b) 2-methyl ester -2,4,6-trimethyl-1,3-dioxane is fluorinated and neutralized to obtain fluorine-containing carboxylic acid alkali metal salt; c) decomposing an alkali metal salt of a fluorine-containing carboxylic acid to obtain a fluorine-containing monomer repr...

Embodiment 1

[0069] Mix 102g of methyl pyruvate (1mol) and 104g of 2,4-pentanediol (1mol) in a 500mL three-necked flask, add 150ml of toluene and 5g of p-toluenesulfonic acid, reflux for 24 hours and evaporate the system through a water separator The water and the solvent were distilled under reduced pressure to obtain 35 g of the fluorinated precursor 2-methyl ester-2,4,6-trimethyl-1,3-dioxane. 5 grams of the obtained precursor were mixed in 200 ml of FC-75, 10% concentration of fluorine gas was passed through, and the reaction was carried out at 20° C. for 24 hours, and the reaction was tracked by GC-MS. After the reaction was completed, 5M aqueous sodium hydroxide solution was added to the reaction solution until the pH value was neutral, the aqueous phase was separated, concentrated and freeze-dried to obtain the sodium salt of perfluorocarboxylic acid. The obtained perfluorocarboxylic acid sodium salt was heated to 200°C in a nitrogen atmosphere to carry out a thermal decomposition re...

Embodiment 2

[0075] In a 100mL autoclave, 1.72g perfluoro(2-methylene-4,6-dimethyl-1,3-dioxane), 1.22g perfluoro(2-methylene-4-methyl- 1,3-dioxolane), perfluorodibutyryl peroxide (15mg) was dissolved in perfluorobenzene (10mL), cooled in acetone-dry ice bath, the system was evacuated and high-purity argon was circulated three times, 50 The reaction was heated at °C for 3 hours, and then heated at 60°C for 2 hours. After the system was cooled, the reaction solution was poured into acetone, and a colorless transparent solid precipitated out. The resin was washed three times with acetone, filtered, and vacuum-dried at 50° C. for 12 hours to obtain 2.83 g of white powder, which was an amorphous fluoropolymer.

[0076] Utilize nuclear magnetic resonance to detect the amorphous fluoropolymer obtained in embodiment 2, obtain 19 As a result of FNMR detection, the A / W ratio in the copolymer is 47 / 53.

[0077] Utilize differential scanning calorimetry (DSC) to detect the amorphous fluoropolymer ob...

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Abstract

The invention provides an amorphous fluorine-containing polymer. The amorphous fluorine-containing polymer is shown as a formula (I) and a formula (II). Compared with the prior art, a large-steric-hindrance six-membered ring unit structure is introduced into a high molecular framework; properties including the solubility, mechanical strength, transparency, gas separation selectivity and the like of the polymer are effectively regulated and controlled through adjusting the ratio of the large-steric-hindrance six-membered ring unit structure in the amorphous fluorine-containing polymer and typesof fluorine-containing olefins. The formula (I) and the formula (II) are shown in the description.

Description

technical field [0001] The invention relates to the technical field of amorphous fluoropolymer materials, in particular to an amorphous fluoropolymer and a preparation method thereof. Background technique [0002] Amorphous fluoropolymers have excellent solubility properties in many fluorinated solvents, allowing them to be easily processed into homogeneous coatings or thin film morphologies with nanoscale thickness. In addition, due to their high transmittance and low refractive index, amorphous polymers are used in high-bandwidth and low-loss graded-index distributed plastic optical fibers. Other potential applications include lens protection films, anti-reflection coatings, microwave and radar protection films, and optoelectronic components. In the field of electronics industry, amorphous fluoropolymers can also be used in the passivation layer and packaging layer required for integrated circuit packaging, and the dielectric layer of hybrid integrated circuits. In recen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F224/00C08F214/24C08F216/00C08F214/26C08F214/18C08F216/14C08F124/00C07D319/06
CPCC07D319/06C08F124/00C08F216/00C08F216/14C08F224/00C08F214/24C08F214/26C08F214/182
Inventor 温乐乐张浩李丹
Owner 上海丰阜投资有限公司
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