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Method used for preparing epoxy compound via chlorohydrine intermediate cyclization catalyzed by supported solid base

A technology of alkali-catalyzed chlorohydrin and solid alkali catalyst, which is applied in the field of green chemistry, can solve the problems of ecological environment impact and cumbersome treatment, and achieve the effect of less environmental pollution

Inactive Publication Date: 2015-07-08
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, liquid alkali catalyst is used in the closed-loop process, and the after-treatment after the reaction is relatively cumbersome, which will generate a large amount of industrial wastewater and have a great impact on the ecological environment.

Method used

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  • Method used for preparing epoxy compound via chlorohydrine intermediate cyclization catalyzed by supported solid base
  • Method used for preparing epoxy compound via chlorohydrine intermediate cyclization catalyzed by supported solid base
  • Method used for preparing epoxy compound via chlorohydrine intermediate cyclization catalyzed by supported solid base

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 5g of NaOH solid, add a small amount of water to configure NaOH aqueous solution. Weigh another 5gTiO 2 Put it in a beaker, add the above-mentioned prepared NaOH aqueous solution to it, and immerse in an equal volume at room temperature for 24 hours. Then dry it at 100~110°C to remove moisture, put it in a crucible, then bake it in a muffle furnace at 500°C for 5 hours, cool to room temperature and grind to get NaOH / TiO 2 Solid base catalyst with 50% NaOH loading. The alkali strength H was measured by the Hammett indicator method. - It is 15.0~18.4.

[0034] figure 2 For the prepared NaOH / TiO 2 The FT-IR spectrogram of solid base catalyst, by figure 2 It can be seen that NaOH / TiO 2 After solid alkali roasting, at 517cm -1 TiO 2 The absorption peak disappears at 670 cm -1 、876cm -1 There is an absorption peak at , so it can be judged that NaOH has been loaded on TiO 2 superior.

[0035] Add 1.66g of terephthalic acid, 14.8g of epichlorohydrin, and 0....

Embodiment 2~6

[0037] Except that the solid base catalyst type is different, all the other operations are the same as in Example 1, and the experimental results are shown in Table 1:

[0038] Table I:

[0039]

[0040] image 3 For the prepared NaOH / Al 2 o 3 The FT-IR spectrogram of solid base catalyst, by image 3 It can be seen that NaOH / Al 2 o 3 After solid alkali roasting, at 470 cm -1 O-Na-O absorption peak appears at 560cm -1 、617cm -1 Al-O absorption peak appears at 818cm -1 The O-O absorption peak appears at , so it can be judged that NaAlO is formed 2 ;1630 cm -1 、3000~3500cm -1 at OH - Absorption peak; 1450 cm -1 for CO 2 Absorption peak, and after roasting, this peak is obviously weakened.

Embodiment 7~10

[0042] According to the solid base preparation method described in Example 1, the loading capacity is respectively 10%, 20%, 30%, 40% solid base catalyst NaOH / TiO 2 , in the preparation process of diglycidyl terephthalate product, add above-mentioned different load capacity solid base catalyst respectively, all the other operations are identical with embodiment 1, experimental result sees table two:

[0043] Table II:

[0044]

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Abstract

The invention discloses a method used for preparing an epoxy compound via chlorohydrine intermediate cyclization catalyzed by a supported solid base; wherein the chlorohydrine intermediate specifically refers to terephthalic acid-di(3-chloro-2-hydroxypropyl)ester which is obtained via esterification ring-opening of terephthalic acid with epoxy chloropropane, and the epoxy compound refers to p-phthalic diglycidyl ester. The invention belongs to the technical field of green chemistry. The method comprises following steps: the chlorohydrine intermediate obtained via ring-opening of terephthalic acid with epoxy chloropropane is subjected to cyclization reaction in the presence of the supported solid base catalyst; after reaction, the supported solid base catalyst is removed via filteration; and the epoxy compound is obtained by removing solvents via distillation. Advantages of the method are that: liquid base catalysis in the cyclization reaction is avoided, generation of a large amount of saline wastewater is avoided, the solvents can be recycled, and the technology is simple. And in addition, the supported solid base catalyst is simple to prepare, is simple to separate, and is friendly to the environment; and the method belongs to a green chemical technology.

Description

technical field [0001] The invention relates to the technical field of green chemistry, in particular to a method for preparing epoxy compounds through the cyclization of chlorohydrin intermediates catalyzed by a supported solid base. Background technique [0002] At present, the main variety of weather-resistant powder coating curing agent in the domestic and foreign markets is triglycidyl isocyanurate (TGIC), but it has been found to be ecologically toxic, and its use has been gradually restricted in Europe, Australia and other places. At the same time, researchers are also actively developing alternatives with comparable performance, among which the hydroxyalkylamide curing agent Primid XL552 launched by Rohm & Hass and the polyglycidyl benzoate PT910 / 912 developed by Huntsman are The most important species. However, for Primid XL552 curing agent, small molecular compounds will be generated during the curing process, pinholes will appear, and its yellowing resistance...

Claims

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Application Information

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IPC IPC(8): C07D303/16C07D301/26
CPCC07D303/16C07D301/26
Inventor 方志杰吴晖陶小东
Owner NANJING UNIV OF SCI & TECH
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