Fluorinated isocyanate and method for preparing fluorinated isocyanate-acrylate copolymer emulsion

A technology for isocyanate and isocyanate is applied in the field of new fluorinated isocyanate monomers, which can solve the problems of poor monomer compatibility, poor stability, and complicated operation, and achieve the effect of stable reaction system, good stability, and easy reaction

Active Publication Date: 2014-08-20
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although the organosilicon and / or organofluorine modification methods reported in the aforementioned patent documents have improved polyurethane-acrylate water resistance, solvent resistance, corrosion resistance, weather resistance and other properties to varying degrees, due to the applied organosilicon, The polarity difference between the organic fluorine monomer and the monomer for synthesizing polyurethane-acrylate is very large, the compatibility between the monomers is poor, the reaction system is uneven, the stability of the reaction mixture is poor, and the synthesized fluorosilicon modified The stability of the polyurethane-acrylate copolymer emulsion is also poor, and more condensates are produced during the reaction, resulting in less stable performance of the synthesized fluorosilicon modified copolymer coating
In addition, some methods (such as the method reported by CN1951968A) are complicated to operate, and the reaction conditions are not easy to control

Method used

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  • Fluorinated isocyanate and method for preparing fluorinated isocyanate-acrylate copolymer emulsion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] In Example 1, vinyl-containing fluorinated isocyanate monomers were prepared by sequentially reacting toluene diisocyanate (TDI) with hexafluorobutanol (HFB) and hydroxyethyl methacrylate (HEMA).

[0062] Wherein, the molar ratio of TDI, HFB and HEMA is 2:1:1.2.

[0063] With butyl acetate as solvent, its consumption is 40wt% based on reactant total amount;

[0064] The consumption of catalyst (DBT) is based on 0.3wt% of reactant total amount;

[0065] The amount of polymerization inhibitor (hydroquinone) is based on 0.1wt% of the total amount of reactants.

[0066] like figure 1 As shown, a four-necked bottle 2 equipped with a thermometer 4, a condensation tube 5 and an electric stirrer 3 is placed in the oil bath 1, and an A dropping funnel is installed on the first bottle mouth 2A (for dropping and initiating agent aqueous solution), a B dropping funnel (for dropping the pre-emulsion of the monomer mixture) is installed on the fourth bottle mouth 2D.

[0067]The ...

Embodiment 2

[0078] In Example 2, vinyl-containing fluorinated isocyanate monomers were prepared by reacting toluene diisocyanate (TDI) sequentially with dodecafluoroheptanol (DFH) and hydroxyethyl methacrylate (HEMA).

[0079] Wherein, the molar ratio of TDI, DFH and HEMA is 2:1:1.2.

[0080] With xylene as solvent, its consumption is 60wt% based on reactant total amount;

[0081] Taking zinc naphthenate as a catalyst, its consumption is based on 0.5wt% of the total amount of reactants;

[0082] The amount of polymerization inhibitor (hydroquinone) is based on 0.1wt% of the total amount of reactants.

[0083] like figure 1 As shown, a four-necked bottle 2 equipped with a thermometer 4, a condensation tube 5 and an electric stirrer 3 is placed in the oil bath 1, and an A dropping funnel is installed on the first bottle mouth 2A (for dropping and initiating agent aqueous solution), a B dropping funnel (for dropping the pre-emulsion of the monomer mixture) is installed on the fourth bottl...

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Abstract

The invention discloses a vinyl-containing fluorinated isocyanate monomer. The preparation method of the fluorinated isocyanate monomer comprises the following steps: reacting diisocyanate with fluorinated alcohol to prepare a fluorinated isocyanate intermediate and then reacting the fluorinated isocyanate intermediate with (meth) hydroxyalkyl acrylate to obtain the fluorinated isocyanate monomer. The organic fluorine-modified polyurethane-acrylate copolymer emulsion with the characteristics of organic fluorine, polyurethane and acrylate resin is synthesized by carrying out emulsion polymerization on the fluorinated isocyanate monomer and the conventional (meth) acrylate. Compared with the prior art, the method for preparing fluorinated isocyanate-acrylate copolymer emulsion has the advantages that since the fluorinated isocyanate monomer is prepared in advance, when an emulsion copolymerization reaction is carried out on the fluorinated isocyanate monomer and acrylates monomer in an aqueous system, the compatibility between the monomers is better, the reaction system is more stable, the reaction is controlled easier and the synthesized copolymer emulsion has better stability.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and specifically provides a novel vinyl-containing fluorinated isocyanate monomer, a preparation method of the monomer, a copolymer emulsion of the monomer and a (meth)acrylic acid ester monomer, and its resolve resolution. Background technique [0002] Acrylic resin has many outstanding advantages, such as light color, transparency, excellent light resistance and outdoor aging resistance, strong outdoor exposure durability, not easy to decompose and turn yellow under ultraviolet light, and can maintain the original luster and color for a long time. Acrylic resin coatings have both excellent decorative properties and good protective properties. However, acrylic resin alone has poor high and low temperature resistance, and poor hydrophobicity and corrosion resistance in some applications. [0003] Fluorocarbons are both hydrophobic and oleophobic, exhibiting excellent chemical stabili...

Claims

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Application Information

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IPC IPC(8): C07C269/02C07C271/28C08F220/18C08F220/14C08F220/28C08F220/36C08F212/08C08F2/30C08F2/26
Inventor 陈贻炽唐伟明李卫平刘慧丛朱立群
Owner BEIHANG UNIV
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