Epoxy end group hyperbranched poly (amide-ester) and preparation method

A technology of hyperbranched polyester and hyperbranched polymer, which is applied in the field of epoxy-terminated hyperbranched polymer and its preparation method, can solve the problems of difficult acquisition of reaction raw materials, large-scale preparation and application impact, etc., achieve broad industrial promotion and application prospects, and be easy to use The effect of industrial production

Inactive Publication Date: 2010-03-10
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Swedish patent 94/04440 (Petterson B.et al, SE94/04440, 1994) has reported to react with ethoxy pentaerythritol and 2,2-dimethylol propionic acid earlier, and the preparation terminal functional group is the hyperbranched polye

Method used

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  • Epoxy end group hyperbranched poly (amide-ester) and preparation method

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Embodiment 1

[0034] Embodiment 1.N, the preparation of N-dihydroxyethyl-3-aminopropionic acid ethyl ester monomer

[0035]Using a 250ml three-necked flask reactor equipped with a stirrer and an oil bath and a nitrogen inlet, add 10.51g (0.10mol) diethanolamine and 5ml ethanol, then drop 10.01g in the three-necked flask with a dropping funnel at room temperature (0.10mol) ethyl acrylate, after the dropwise addition, the temperature was raised to 35°C, and the stirring reaction was continued for 4 hours, and then the ethanol was distilled under reduced pressure to obtain a colorless transparent oil, which was N,N-dihydroxyethyl-3- Ethyl aminopropionate monomer.

[0036] The synthesized monomer adopts gas chromatography spectrometer (Agilent 6890N) to analyze its content to be 94.97%; -1 、990cm -1 、910cm -1 The C=C bond peak in ethyl acrylate disappears at 939cm -1 The N-H characteristic peaks of diethanolamine disappeared at 1190.54cm -1 The absorption peak of C-N appears at 1731.93cm ...

Embodiment 2

[0037] Embodiment 2.N, the preparation of N-dimethylol-3-aminopropionic acid methyl ester monomer

[0038] Using a 250ml three-neck flask reactor equipped with a stirrer and an oil bath and a nitrogen inlet, add 8.6g (0.10mol) methyl acrylate, 7.7g (0.10mol) dimethanolamine and 5ml methanol, and the mixture is at room temperature and logical N , Stirring for 30 minutes, then raising the temperature to 35°C for 4 hours, and then vacuuming to remove methanol to obtain a colorless and transparent oil, which is N,N-dimethylol-3-aminopropionic acid methyl ester monomer.

[0039] The synthesized monomer was analyzed by infrared spectroscopy, and at 1445cm -1 、990cm -1 、910cm -1 The C=C bond peak in methyl acrylate disappears at 939cm -1 The N-H characteristic peaks of dimethanolamine all disappeared, and the results of measuring the content of monomer components by CHN-O-RAPID elemental analyzer of German Foss Heraeus company are shown in Table 1:

[0040] Table 1 Analysis resu...

Embodiment 3

[0043] Embodiment 3.N, the preparation of N-dihydroxyphenethyl-3-aminomethyl propionate isooctyl monomer

[0044] Using a 250ml three-neck flask reactor equipped with a stirrer and an oil bath and a nitrogen inlet, add 19.8g (0.10mol) of isooctyl methacrylate, 10.51g (0.10mol) of benzphenylethanolamine and 10ml of methanol, and the mixture is heated at room temperature And pass through N, under the condition of stirring for 30 minutes, then raise the temperature to 35 ° C for 4 hours, then vacuumize to remove methanol, and obtain a colorless and transparent oil, which is N, N-dihydroxyphenethyl-3-amino Isooctyl methylpropionate monomer.

[0045] The synthesized monomer was analyzed by infrared spectroscopy, and at 1445cm -1 The C=C bond peak in isooctyl methacrylate disappears at 939cm -1 The N-H characteristic peaks of dimethanolamine all disappeared, and the results of measuring the content of monomer components by CHN-O-RAPID elemental analyzer of German Foss Heraeus comp...

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Abstract

The invention provides an epoxy end group hyperbranched poly (amide-ester) and a preparation method. The preparation method comprises the following steps: taking dihydroxy amide ester as a chain propagation monomer, adding multifunctionalmolecule polylol as a core, reacting in the presence of a catalyst and inert gases to obtain hydroxyl end group amido hyperbranched poly (amide-ester); and then enabling a hydroxyl end group to react with epoxy chloropropane to generate the epoxy end group hyperbranched poly (amide-ester). The epoxy end group hyperbranched poly (amide-ester) is in an approximately sphere symmetrical three-dimensional structure with high functionality, has the relatively molecular weight as high as 10,000-20,000 and the molecular weight distribution coefficient as much as 1.02-1.35, can be used as a rheologicalproperty regulator or polymer rheological processing modifier, can improve the compatibility when being blended with a polymer containing an epoxy group, improvethe tensile strength by 40 percent compared with a pure polymer, improve the breaking strength by 60 percent compared with the pure polymer and achieve the functions of toughening and strengthening.

Description

technical field [0001] The invention provides an epoxy terminal hyperbranched poly(amine-ester) and a preparation method. Background technique [0002] As a new material, hyperbranched polymers were only developed in the 1980s. Due to their highly dense structure and almost perfect geometric configuration, hyperbranched polymers have become a great choice in topology, biology, and materials. After more than ten years of research, the basic research and application research of hyperbranched polymers have made great progress. International Patent 96 / 07688 ( B, Shi W.F, WO 96 / 07688, 1996) reported to react with polyhydric alcohol and aryl polycarboxylic acid anhydride earlier, the preparation end functional group is the hyperbranched polyester of carboxyl group. This hyperbranched polyester is obtained by the gradual esterification of different compounds, and the polydispersity coefficient increases, so that the degree of branching and the molecular weight are low, and the h...

Claims

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Application Information

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IPC IPC(8): C08G63/91C08G63/685
Inventor 张龙寇大凯
Owner CHANGCHUN UNIV OF TECH
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