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Preparation method of diphenoxy methane
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A technology of diphenoxymethane and phenol, which is applied in the field of preparation of diphenoxymethane, can solve problems such as complex synthesis process and treatment process, and achieve the effects of easy industrial production, improved conversion selectivity, and reduced production cost
Inactive Publication Date: 2017-05-10
HUANGSHAN UNIV
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Problems solved by technology
[0005] For this reason, the technical problem to be solved by the present invention is to provide a kind of preparation method of diphenoxymethane, to solve the complex problem of the synthesis technique and follow-up treatment process of diphenoxymethane in the prior art
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Embodiment 1
[0024] The preparation method of the diphenoxymethane described in the present embodiment comprises the steps:
[0026] (2) Add 4 g of D001 type macroporous cation exchange resin catalyst, stir and react at 60-100° C. for 4-5 h;
[0027] (3) The reactant is filtered to remove the catalyst, and after distillation, the required diphenoxymethane is obtained.
[0028] The resulting product is detected by GC and GC-MS, and its detection spectrum is shown in the attached figure 1 As shown, the analysis of the detection data proves that the compound obtained in this example is diphenoxymethane. The conversion of the reaction to the product was calculated to be 95%.
Embodiment 2
[0030] The preparation method of the diphenoxymethane described in the present embodiment comprises the steps:
[0032] (2) Add 10 g of 732 styrene cation exchange resin as a catalyst, and stir and react at 60-100 °C for 4-5 hours;
[0033] (3) The reactant is filtered to remove the catalyst, and after distillation, the required diphenoxymethane is obtained.
[0034] The obtained product is detected and compared by GC and GC-MS, and the obtained product is diphenoxymethane. The conversion of the reaction to the product was calculated to be 94%.
Embodiment 3
[0036] The preparation method of the diphenoxymethane described in the present embodiment comprises the steps:
[0037] (1) Get paraformaldehyde 30g under stirring condition, join in the phenol raw material of 188g molten state and stir and mix;
[0038] (2) Add D001 type macroporous cation exchange resin as catalyst 4g, stir and react at 60-100°C for 4-5h;
[0039] (3) The reactant is filtered to remove the catalyst, and after distillation, the required diphenoxymethane is obtained.
[0040] The obtained product is detected and compared by GC and GC-MS, and the obtained product is diphenoxymethane. The conversion of the reaction to the product was calculated to be 95%.
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Abstract
The invention belongs to the technical field of chemical synthesis and particularly relates to a preparation method of diphenoxy methane. The preparation method of the diphenoxy methane uses paraformaldehyde and phenol in a molten state as raw materials and uses storng acid cation exchange resin as a catalyst, solvent-free diphenoxy methane synthesis is achieved, and meanwhile product separation is easy. The reaction can be completely performed at low temperature without phase transfer catalyst adding, and the prepared diphenoxy methane is high in purity and good in stability. The raw materials for the whole reaction are low in cost, no side product is produced, the production cost of the diphenoxy methane is obviously reduced, industrialized production is easy, and the requirement for green process is met.
Description
technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of diphenoxymethane. Background technique [0002] Diphenoxymethane is a kind of acetal compound. It is a light yellow oily liquid at room temperature with a boiling point of 122°C / 1.6mmHg. It is miscible with most organic solvents such as alcohol, ether, and acetone. Acetal compounds are important intermediates in organic synthesis and important chemical raw materials. They can be used as oil additives without environmental problems; and under suitable catalyst conditions, they can be directly oxidized to synthesize carbonates with molecular oxygen. [0003] The traditional method of synthesizing diphenoxymethane is to use phenol and diiodomethane, dibromomethane or dichloromethane as raw materials, use dimethyl sulfoxide as solvent, and add phase transfer under alkaline conditions in the presence of sodiumhydroxide. The catalyst rea...
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