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A kind of epoxy-terminated hyperbranched polyphosphate and preparation method thereof

A technology of polyphosphate and epoxy-terminated polyphosphate, which is applied in the field of epoxy-terminated hyperbranched polyphosphate and its preparation, can solve problems such as low viscosity, high molecular weight, and reduce production costs, and achieve good compatibility and high product quality. The effect of high quality and reduced production energy consumption

Active Publication Date: 2020-12-01
SHANDONG RUNKE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the deficiencies of the above-mentioned prior art, and to provide a resin with high molecular weight, corrosion resistance, low viscosity, mild reaction conditions, reduced production energy consumption, no by-product generation, and no need for curing. Epoxy-terminated hyperbranched polyphosphate with reduced production cost and no environmental pollution and preparation method thereof

Method used

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  • A kind of epoxy-terminated hyperbranched polyphosphate and preparation method thereof
  • A kind of epoxy-terminated hyperbranched polyphosphate and preparation method thereof
  • A kind of epoxy-terminated hyperbranched polyphosphate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A kind of preparation method of epoxy-terminated hyperbranched polyphosphate:

[0038] 1) Synthesis of Triglycidyl Trimetaphosphate (B3)

[0039] At room temperature, dissolve 100g of sodium trimetaphosphate with 300g of water, add 180g of organic solvent I dichloroethane, heat up to 50°C under stirring, add 1g of catalyst I tetraethylammonium bromide and stir until dissolved; then drop Add 100g of epichlorohydrin, control the reaction temperature at 40°C, keep warm, check the pH value of the system with a pH meter at intervals of 0.5h, adjust the pH to 7-8 with 10% sodium hydroxide solution, until the end of the reaction, the tricyclic trimetaphosphate is obtained The crude oxypropyl ester (B3) was washed with water and dried in vacuum to obtain the trimetaphosphate (B3) product.

[0040] 2) Synthesis of epoxy-terminated hyperbranched polyphosphate

[0041] Get 140g of triglycidyl trimetaphosphate prepared in step 1), add to 840g organic solvent II toluene and dissol...

Embodiment 2

[0043] A preparation method of epoxy-terminated hyperbranched polyphosphate, comprising the following steps:

[0044] At room temperature, dissolve 100g of sodium trimetaphosphate in 500g of water, and after 750g of organic solvent I chloroform, raise the temperature to 60°C under stirring, then add 15g of catalyst I: 5g of tetraethylammonium bromide, 5g of tetrabutyl Ammonium bromide and 5g benzyltriethylammonium chloride were stirred until dissolved; then 200g epichlorohydrin was added dropwise, the reaction temperature was controlled at 60°C, and the temperature was kept at 0.5h intervals to detect the pH value of the system with a pH meter. Sodium hydroxide solution adjusts the pH to make it stable at pH 7-8, until the end of the reaction, the crude product of triglycidyl trimetaphosphate B3 is obtained, washed with water, and dried in vacuum to obtain the product of triglycidyl trimetaphosphate B3 .

[0045] 2) Synthesis of epoxy-terminated hyperbranched polyphosphate

...

Embodiment 3

[0048] A kind of preparation method of epoxy-terminated hyperbranched polyphosphate:

[0049] 1) Synthesis of Triglycidyl Trimetaphosphate (B3)

[0050] At room temperature, dissolve 100g of sodium trimetaphosphate with 400g of water, then add 465g of organic solvent I: 100g of dichloroethane, 120g of chloroform, 245g of carbon tetrachloride, heat up to 55°C under stirring, and add 8g of catalyst Ⅰ: Stir 4g of tetrabutylammonium bromide and 4g of benzyltriethylammonium chloride until dissolved; then add 150g of epichlorohydrin dropwise, keep the reaction temperature at 50°C, keep warm, and measure the pH of the system with a pH meter at intervals of 0.5h Value, adjust pH 7~8 with 20% sodium hydroxide solution, until reaction finishes, get trimetaphosphate trimetaphosphate (B3) crude product, wash with water, vacuum dry, get trimetaphosphate trimetaphosphate (B3) crude product, B3) Products.

[0051] 2) Synthesis of epoxy-terminated hyperbranched polyphosphate

[0052] Get ste...

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Abstract

The invention relates to epoxy-terminated hyperbranched polyphosphate and a preparation method thereof, aiming at solving the technical problems that in the prior art, epoxy resin is lower in relativemolecular mass, poorer in corrosion resistance, higher in viscosity and troublesome in construction, the toxicity of curing agent varieties for the epoxy resin is larger, and the epoxy resin is moreaffected by the environment. The epoxy-terminated hyperbranched polyphosphate provided by the invention is prepared adding a branching agent into tri-epichloropropyl trimetaphosphate (B3), and enabling the tri-epichloropropyl trimetaphosphate (B3) and the branching agent to be subjected to an epoxide ring-opening reaction so as to obtain the epoxy-terminated hyperbranched polyphosphate. Furthermore, the invention also provides the preparation method of the epoxy-terminated hyperbranched polyphosphate. The epoxy-terminated hyperbranched polyphosphate and the preparation method thereof can be widely applied to the technical field of organic synthesis.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to an epoxy-terminated hyperbranched polyphosphate and a preparation method thereof. Background technique [0002] The structure of hyperbranched polymers is dendritic and hyperbranched. From the perspective of synthesis, generally, two or more monomers with active groups are synthesized separately and reacted in the presence of a catalyst to form a polymer, and the structure of the product changes due to the feed ratio of the monomers. Since the topological structure of a polymer has a great influence on its properties, the preparation of polymers with specific topological structures has always been a research hotspot in the field of polymer chemistry. [0003] Epoxy resins generally refer to organic polymer compounds containing two or more epoxy groups in their molecules. Except for a few, their relative molecular weights are not high; generally, amine curing agents are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/04
CPCC08G79/04
Inventor 吴多坤秦善宝王桂福
Owner SHANDONG RUNKE CHEM
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