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A kind of fluorine-containing polyurethane and preparation method thereof

A technology of polyurethane and sulfonyl fluoride, which is applied in the field of fluorine-containing polyurethane and its preparation, and can solve the problems of high unit price of fluorine-containing monomers, difficult synthesis, and restrictions on wide application

Active Publication Date: 2021-04-27
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since this preparation method needs to go through two-step reactions (prepolymer synthesis first and then chain extension reaction) to obtain thermoplastic fluorine-containing polyurethane elastomers, it has the disadvantages of long reaction cycle, complicated preparation process, and high cost, which greatly limits its use. widely used
[0004] At present, almost all fluorine-containing polyurethanes are synthesized by using fluorine-containing raw materials such as fluorine-containing polyether polyols, fluorine-containing isocyanates, and fluorine-containing chain extenders through conventional polymerization methods. Conventional methods have the advantages of controllable fluorine content and performance , but there are also defects such as high unit price of fluorine-containing monomers, difficulty in synthesis, and complex process and difficult control during the polymerization process. The performance of the synthesized fluorine-containing polyurethane is unstable, which seriously restricts the large-scale application of fluorine-containing polyurethane

Method used

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  • A kind of fluorine-containing polyurethane and preparation method thereof
  • A kind of fluorine-containing polyurethane and preparation method thereof
  • A kind of fluorine-containing polyurethane and preparation method thereof

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preparation example Construction

[0041] The present invention also provides a kind of preparation method of above-mentioned fluorine-containing polyurethane, comprises the following steps:

[0042] A) mixing polyurethane having a structure represented by formula (IV) with a polar solvent to obtain a first mixed solution;

[0043] B) mixing the first mixed solution with the silane coupling agent to obtain the second mixed solution;

[0044] C) mixing the second mixed solution, sulfonyl fluoride and water, and reacting to obtain a fluorine-containing polyurethane having a structure shown in formula (I);

[0045]

[0046] Among them, 10≤n≤20.

[0047] The present invention has no special limitation on the source of the polyurethane having the structure represented by formula (IV). In some embodiments of the present invention, the polyurethane having the structure shown in formula (IV) is prepared according to the following method:

[0048] performing a chain extension reaction on the polyurethane prepolyme...

Embodiment 1

[0102] Have the preparation of the polyurethane of structure shown in formula (IV):

[0103] (1) Dehydration treatment of diisocyanate

[0104] Add 2.55g (0.01mol) MDI into a three-necked flask equipped with mechanical stirring, nitrogen protection, and a constant pressure dropping funnel, heat in an oil bath and vacuumize with a vacuum pump until the dehydration is complete.

[0105] (2) Prepolymerization reaction

[0106] Nitrogen was passed into the three-necked flask in advance, and then the temperature in the three-necked flask was controlled to be 80°C. 5g of PTMG (0.005mol) was added dropwise to the three-necked flask with a constant pressure dropping funnel at a rate of 3 drops / s. After completion, add 9 mL of toluene, the solid content is 49.20%, and react for 3 hours to obtain the polyurethane prepolymer.

[0107] (3) Chain extension reaction

[0108] After the prepolymerization, the NCO% titration was carried out by the di-n-butylamine method, and then the BDO ch...

Embodiment 2

[0117] The preparation method of the polyurethane having the structure shown in formula (IV) is the same as in Example 1.

[0118] Preparation of fluorine-containing polyurethane:

[0119] Weigh 1g of polyurethane (n=13) having the structure shown in formula (IV), place it in a 100mL Erlenmeyer flask, then pour 15mL of N,N-dimethylformamide (DMF), and control the stirring speed to 230r / min, stirred at room temperature for 0.5h.

[0120] Then weigh 0.26g of KH902 and drop it into the conical flask using a constant pressure dropping funnel, control the dropping rate to 1 drop / s, keep the stirring speed constant, and continue stirring at room temperature for 0.4h after the dropping is completed.

[0121] Place the Erlenmeyer flask in a cold water bath, cool to 5°C, weigh 0.45g of perfluorooctanesulfonyl fluoride, drop it into the Erlenmeyer flask using a constant pressure dropping funnel, and control the dropping rate to 2 drops / min. Then 0.03 g of distilled water was added dr...

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Abstract

The invention relates to the technical field of polymer synthesis, in particular to a fluorine-containing polyurethane and a preparation method thereof. The fluorine-containing polyurethane has a segment structure represented by formula (I); wherein, R has a structure represented by formula (II) or (III); wherein, 10≤n≤20. The invention uses sulfonyl fluoride and silane coupling agent to modify ordinary hydroxyl-terminated polyurethane, and the obtained fluorine-containing polyurethane not only has good mechanical properties, but also has good hydrophobicity. The invention directly modifies the polyurethane, avoids the cumbersome monomer synthesis and polyurethane synthesis steps in the conventional synthesis, and the preparation method is simple, convenient and fast.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis, in particular to a fluorine-containing polyurethane and a preparation method thereof. Background technique [0002] Fluorine has strong electronegativity, high C-F bond energy (540KJ / mol) and fluorine’s shielding effect on carbon chains. Therefore, the introduction of fluorine can maintain the excellent mechanical properties and two-phase microstructure characteristics of polyurethane (PU). On the basis of PU, the surface properties of PU can be improved to a large extent, and it can be endowed with excellent heat resistance, weather resistance, corrosion resistance, low surface energy, low friction and biocompatibility, etc., and low surface energy And low friction makes fluorine-containing polyurethane have outstanding hydrophobic and oleophobic properties and anti-adhesion properties. [0003] In 1958, British Patent 797795 reported for the first time that fluorinated polyurethane w...

Claims

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Application Information

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IPC IPC(8): C08G18/83C08G18/76C08G18/66C08G18/48C08G18/32
CPCC08G18/4854C08G18/6674C08G18/7671C08G18/831C08G18/837
Inventor 刘向东张航盛德鲲孙磊熊征蓉周妍郭晓明王军周子侠杨宇明
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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