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Carboxylate/phosphate dual dynamic covalent polymer network material and preparation method thereof

A technology of phosphate and carboxylate, applied in the field of crystallizable carboxylate/phosphate dual dynamic covalent polymer network materials and its preparation, can solve the problems of slow remodeling and complicated preparation process, and achieve operability Strong, simple preparation process, and improved remodeling efficiency

Pending Publication Date: 2021-11-05
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Existing literature discloses a kind of preparation method of dynamic transfer autocatalytic transesterification type dynamic covalent polymer network, the first step makes maleic anhydride (succinic anhydride) and trimethylolpropane monoesterification reaction, the second step The synthesized polycarboxy compound is cured with bisphenol A epoxy, and the obtained transesterified dynamic network can be reshaped by hot pressing without catalyst, but the preparation process of this method is complicated, and the remodeling is still slow

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  • Carboxylate/phosphate dual dynamic covalent polymer network material and preparation method thereof
  • Carboxylate/phosphate dual dynamic covalent polymer network material and preparation method thereof
  • Carboxylate/phosphate dual dynamic covalent polymer network material and preparation method thereof

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preparation example Construction

[0019] Specifically, as an aspect of the technical solution of the present invention, the preparation method of a carboxylate / phosphate ester double dynamic covalent polymer network material includes: making a cyclic acid anhydride containing a long-chain side group, a ring Oxygen monomers and phosphoric acid group-containing compounds are pre-reacted in a uniformly mixed reaction system, and then undergo a curing reaction to obtain carboxylate / phosphate ester dual dynamic covalent polymer network materials (also denoted as "long-chain side group-containing Crystalline Carboxylate / Phosphate Dual Dynamic Covalent Polymer Network Materials").

[0020] The reaction mechanism of the present invention is: the present invention proposes the preparation method of the crystallizable carboxylate / phosphate dual dynamic covalent polymer network material containing long-chain side groups. The ring-opening curing reaction of the cyclic anhydride and the phosphoric acid group-containing com...

Embodiment 1

[0038] Mix diglycidyl hexahydrophthalate, dodecenyl succinic anhydride, and N-(phosphorylmethyl) glycine in a single-necked flask at a molar ratio of 1:1.33:0.34; place the mixed system at 120 Pre-react in an oil bath at ℃ for 1 h; pour the pre-reaction product into a polytetrafluoroethylene mold, put the mold into a vacuum oven, and vacuumize; the control system is cured under vacuum conditions, and the curing process is 15 °C for 2 h, 190 ℃ for 2 hours; after natural cooling, the solidified product was taken out of the oven to obtain a transparent light yellow film material (ie, the aforementioned crystallizable transesterification-type dynamic covalent polymer network material containing long-chain side groups).

[0039] After the polymer network material prepared in this example was cut into pieces, it was hot-pressed at 160°C for 10 minutes using a flat vulcanizer, and the complete material ( figure 1 ). Also, the material has a glass transition temperature of 47°C ( f...

Embodiment 2

[0041] Mix diglycidyl hexahydrophthalate, dodecyl succinic anhydride, and N-(phosphorylmethyl) glycine in a single-necked flask at a molar ratio of 1:1.33:0.34; place the mixed system in Pre-react in an oil bath at 120°C for 2 hours; pour the pre-reaction product into a polytetrafluoroethylene mold, put the mold into a vacuum oven, and vacuumize; the control system is cured under vacuum conditions, and the curing process is 150°C for 1 hour , React at 190°C for 2 hours; after natural cooling, take the solidified product out of the oven to obtain a transparent light yellow film material.

[0042] After the polymer network material prepared in this example is cut into pieces, it can be hot-pressed at 130°C for 20 minutes with a flat vulcanizer, and the complete material can be obtained again. Please refer to figure 1 shown. Moreover, the glass transition temperature of the material is 55°C, the crystalline melting temperature is 67°C, the elongation at break is 150%, the Young'...

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Abstract

The invention discloses a carboxylate / phosphate dual dynamic covalent polymer network material and a preparation method thereof. The preparation method comprises the following steps: carrying out pre-reaction on a uniformly mixed reaction system of cyclic anhydride containing a long-chain side group, an epoxy monomer and a compound containing a phosphate group, and then carrying out curing reaction to obtain the carboxylate / phosphate dual dynamic covalent polymer network material. The carboxylate / phosphate dual dynamic covalent polymer network material prepared by the invention not only has excellent thermal, mechanical, intrinsic flame retardant and degradation properties, but also can realize autocatalytic rapid remodeling processing; and meanwhile, the preparation process is simple, operability is high, industrial production is easy to achieve, the problems that existing epoxy resin is inflammable and difficult to degrade are hopefully solved, and the problem that improvement of thermal and mechanical properties and acceleration of the autocatalytic remodeling rate contradict is solved.

Description

technical field [0001] The invention relates to a carboxylate / phosphate dual dynamic covalent polymer network material and its preparation method, in particular to a crystallizable carboxylate / phosphate double dynamic covalent polymer network material containing long-chain side groups The preparation method and application thereof belong to the technical field of sustainable thermosetting resin preparation. Background technique [0002] Compared with thermoplastic resins, thermosetting resins have better thermal and mechanical properties and dimensional stability, so they are widely used in coatings, adhesives, composite materials, electronic packaging and other fields. However, traditional thermosetting materials are difficult to recycle after being discarded. Dynamic covalent bonds can endow thermoset resins with remodelability, thus solving the problem of their inability to be recycled. [0003] Among the reported dynamic covalent bonds such as ester bonds, disulfide bon...

Claims

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Application Information

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IPC IPC(8): C08G59/24C08G59/42C08G59/58
CPCC08G59/24C08G59/4284C08G59/58
Inventor 刘艳林马松琪朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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