Preparation method and application of heterogeneous epoxy catalyst

A technology of oxidation catalyst and phase ring, which is applied in physical/chemical process catalysts, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., to achieve simple preparation process, stable reuse performance, and convenient catalyst recovery. Effect

Inactive Publication Date: 2015-01-07
JIANGNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the preparation of epoxy fatty acid esters from waste edible oils and fats not only solves the problems of waste edible oils recycling and environmental pollution, but also can replace the use of traditional o-benzene plasticizers to a certain extent

Method used

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  • Preparation method and application of heterogeneous epoxy catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) PS-[MoO 2 (H 2 Preparation of FSAP)DMF]:

[0030] ① Ligand H 2 Synthesis of FSAP: 1.66g (10mmol) of 3-formyl salicylic acid and 1.09g (10mmol) of o-aminophenol were mixed and dissolved in 30mL of absolute ethanol, stirred for 6h under reflux to produce orange-red precipitate, filtered and dried , recrystallized in boiling alcohol, filtered and dried to obtain the pure ligand H 2 FSAP.

[0031] ②PS-H 2 Synthesis of FSAP: 1g PS (equivalent to 4.69mmol Cl) microspheres were added to a 100mL three-necked flask, swelled in 10mL DMF for 2h, and 3.6g H 2 A 15 mL DMF solution of FSAP (14 mmol, 1:3 amount of microspheres and ligand) was added to the suspension solution, followed by a 100 mL ethyl acetate solution of 4.5 g triethylamine. React for 15 hours under mechanical stirring at 90°C, filter after cooling down to room temperature, wash with hot DMF and methanol several times, and dry in an oven at 120°C to obtain purple-red PS-H 2 FSAP microspheres.

[0032] ③PS...

Embodiment 2

[0035] (1) PS-[MoO 2 (H 2 FSAP) DMF] preparation: same as Example 1.

[0036] (2) Synthesis of epoxy fatty acid methyl ester: 10g of refined fatty acid methyl ester, 0.5gPS-[MoO 2 (H 2 FSAP)DMF], 10mL of 1,2-dichloroethane were added to a 100mL three-necked flask, ozone was introduced into the reaction system at a flow rate of 0.50mg / min, and the epoxidation reaction was carried out at 80°C. After the reaction, the reaction mixture was depressurized Epoxy fatty acid methyl esters are obtained after distillation. The catalyst can be reused 4 times.

Embodiment 3

[0038] (1) PS-MP-[MoO 2 (H 2 Preparation of FSAP)DMF]:

[0039] ① Ligand H 2 Synthesis of FSAP: same as Example 1.

[0040] ②PS-MP-H 2 Synthesis of FSAP: 1g PS-MP (equivalent to 3.5mmol Cl) was added to a 100mL three-neck flask, swelled in 10mL DMF for 2h, 2.69g H 2 A 15 mL DMF solution of FSAP (10.5 mmol, 1:3 amount of microspheres and ligand) was added to the suspension solution, followed by a 100 mL ethyl acetate solution of 4.5 g triethylamine. React for 15 hours under mechanical stirring at 90°C, filter after cooling down to room temperature, wash with hot DMF and methanol several times, and dry in an oven at 120°C to obtain orange PS-MP-H 2 FSAP microspheres.

[0041] ③PS-MP-[MoO 2 (H 2 FSAP) DMF] synthesis: add 1gPS-MP-H in 100mL there-necked flask 2 FSAP (equivalent to 1.17mmol Schiff base ligand), swell in 15mlDMF for 2h, 0.77gMoO 2 (acac) 2 (2.34mmol, 1:2 the amount of Schiff base ligand and metal) was added to the above suspended state, reacted in an oil ...

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Abstract

A preparation method and application of a heterogeneous epoxy catalyst belong to the technical field of catalyst preparation and application. With a high-molecular polymer as a carrier, the heterogeneous epoxy catalyst is grafted with a molybdenum metal complex after reacting with Schiff base ligand. The heterogeneous epoxy catalyst can be used for catalytic synthesis of epoxy aliphatic ester by using swill-cooked dirty oil as the initial raw material; and the epoxy aliphatic ester obtained is a novel environment-friendly plasticizer. The heterogeneous epoxy catalyst provided by the invention is simple in preparation process, and has the characteristics of high catalytic activity and selectivity, convenience in recovery, stable reusability and the like if applied to the epoxidation reactions. Besides, the waste edible oil is taken as the initial raw material for preparing the epoxy aliphatic ester so that the problems of recycling, environmental pollution and the like of the waste edible oil are solved; moreover, the epoxy aliphatic ester can be used for replacing the traditional orthophthalic plasticizers to a certain extent.

Description

technical field [0001] A preparation method and application of a heterogeneous epoxidation catalyst, the present invention relates to a preparation of a heterogeneous epoxidation catalyst, and its application to a synthetic method for preparing epoxy fatty acid esters using waste edible oil as a starting material, The invention belongs to the technical field of catalyst preparation and application. Background technique [0002] Waste edible oils and fats, including various single or mixed waste edible vegetable oils such as soybean oil, corn oil, sunflower oil, and blended oil, as well as animal fats such as roast duck oil, chicken oil, butter, lard, and animal offal oil. It mainly includes but is not limited to the following three categories: old frying oil, swill oil, and gutter oil (or "gutter oil" in a narrow sense). The main component of waste cooking oil is still triglyceride, but it has many more pathogenic and carcinogenic toxic substances than real cooking oil. my...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07D301/19C07D301/03C07D303/42C11C3/10
Inventor 蒋平平张书源徐玉成冷炎莫贯田
Owner JIANGNAN UNIV
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