Preparation method of catalyst for synthesizing diphenyl carbonate

Abstract

The invention discloses a preparation method of a catalyst for synthesizing diphenyl carbonate, and belongs to the technical field of catalyst synthesis. The catalyst is obtained by modifying a transition metal oxide by poly-electrolyte until the transition metal oxide is positively or negatively charged, and wrapping a layer of metal organic framework (MOFs) on the outer surface of the transition metal oxide by an electrostatic layer-by-layer self-assembling method, namely the oxide is used as a core, and the MOFs is used as a shell; the catalyst is MalphaObeta@MOFs fort short (M is one of transition metal elements, and alpha and beta are valences). The catalyst is enabled to react with ammonia chloride with a certain concentration to convert the core MalphaObeta into corresponding chloramine salt M(NH3)nClbeta (n is the number of ammonia molecules and is equal to 1 to 8); after ammonia is removed by low-temperature roasting, the catalyst MClbeta@MOFs is obtained. The catalyst can be used in a system for generating diphenyl carbonate by transesterification between urea or carbamic acid ester and phenol; new coordination adsorption is performed on the catalyst and ammonia generated by the reaction system to push the reaction to move rightwards; the yield of a diphenyl carbonate product is up to 90 percent or above; after the catalyst is used for 5 times, the catalysis effect is still good.

Description

technical field

[0001] The invention relates to a preparation method of a catalyst for synthesizing diphenyl carbonate, belonging to the technical field of catalyst synthesis. Background technique

[0002] The "green" intermediate of organic compounds and polymer materials, diphenyl carbonate (Diphenyl Carbonate, referred to as DPC) molecular formula is C 6 h 5 OCOOC 6 h 5 , mainly used in the plastics industry, one of its most notable uses is polycondensation reaction with bisphenol A to synthesize polycarbonate (PC), polycarbonate has good optical properties, high impact strength, high-quality thermal stability It has a wide range of applications due to its excellent properties such as anti-corrosion properties, such as in glasses, aerospace, automobile manufacturing, pesticides, medical treatment, construction and other fields. At present, the total consumption of PC is second only to polyamide (PA) in engineering plastics. The total global consumption in 2005 has ex...

Examples

Embodiment 1

[0021] The method for preparing the chromium chloride catalyst coated with ZIF-8 is as follows:

[0022] (1) Refer to "Powders of chromium and chromium carbides of different morphology and narrow size distribution" published by S Loubiere, C Laurent, JP Bonino, A Rousset to prepare spherical chromium oxide powders with a particle size of 1-5 microns, using conventional Zeta potential The analyzer determines that the chromium oxide solid surface is negatively charged;

[0023] (2) Synthesis of metal-organic framework porous material ZIF-8.

[0024] ① The mass is 1.17 g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 8 g deionized water, and this solution was recorded as A;

[0025] ② Dissolve 22.70 g of 2-methylimidazole in 80 g of deionized water, and call this solution B;

[0026] ③ Mix A and B solutions at room temperature to obtain the initial ZIF-8 reaction solution, stir and mix for 5 minutes, and the mixed solution is in the form of a silky gel at this time; centrifuge the obt...

Embodiment 2

[0034] The method for preparing the MOF-2 coated cadmium chloride catalyst is as follows:

[0035] (1) Refer to "Formation and properties of Cd (OH)" published by M Ristić, S Popović, S Musić, etc. 2 and CdO particles" to prepare spherical cadmium oxide powder with a particle size of 1-5 microns, and use a conventional Zeta potential analyzer to determine that the solid surface of cadmium oxide is negatively charged;

[0036] (2) The metal-organic framework porous material MOF-2 was synthesized by referring to the existing literature: 0.73g of Zn(NO 3 ) 2 ·6H 2 O was dissolved in 10mL N,N-dimethylformamide, 0.48g terephthalic acid was also dissolved in 10mL N,N-dimethylformamide, the two solutions were mixed in a 250mL beaker under stirring, and mixed with 80mL toluene To dilute, add 50mL toluene and 0.5mL triethylamine to a 1L beaker, put the 250mL beaker into a 1L beaker, seal the beaker, and let it stand at room temperature for 7 days to obtain the initial reaction liqu...

Embodiment 3

[0044] The method for preparing the ferric chloride catalyst covered by MOF-70 is as follows:

[0045] (1) Refer to "Mechanism and controlled growth of shape and size variant core / shell FeO / Fe" published by H Khurshid, W Li, S Chandra, MH Phan 3 o 4 "Spherical iron oxide powder with a particle size of 1-5 microns was prepared, and a conventional Zeta potential analyzer was used to determine that the iron oxide solid surface was negatively charged;

[0046] (2) The metal-organic framework porous material MOF-70 was synthesized by referring to the existing literature: 0.12g of Pb(NO 3 ) 2 Dissolve in 18mL absolute ethanol, 0.06g terephthalic acid is also dissolved in 2mL N,N-dimethylformamide, mix the two solutions in a 100mL beaker with stirring and add 0.2mL hydrogen peroxide; add in a 500mL beaker 10mL N,N-dimethylformamide and 0.8mL triethylamine, put a 100mL beaker in the middle of a 500mL large beaker, seal the large beaker, and let it stand at room temperature for 7 da...

technical field

[0001] The invention relates to a preparation method of a catalyst for synthesizing diphenyl carbonate, belonging to the technical field of catalyst synthesis. Background technique

[0002] The "green" intermediate of organic compounds and polymer materials, diphenyl carbonate (Diphenyl Carbonate, referred to as DPC) molecular formula is C 6 h 5 OCOOC 6 h 5 , mainly used in the plastics industry, one of its most notable uses is polycondensation reaction with bisphenol A to synthesize polycarbonate (PC), polycarbonate has good optical properties, high impact strength, high-quality thermal stability It has a wide range of applications due to its excellent properties such as anti-corrosion properties, such as in glasses, aerospace, automobile manufacturing, pesticides, medical treatment, construction and other fields. At present, the total consumption of PC is second only to polyamide (PA) in engineering plastics. The total global consumption in 2005 has ex...

Examples

Embodiment 1

[0021] The method for preparing the chromium chloride catalyst coated with ZIF-8 is as follows:

[0022] (1) Refer to "Powders of chromium and chromium carbides of different morphology and narrow size distribution" published by S Loubiere, C Laurent, JP Bonino, A Rousset to prepare spherical chromium oxide powders with a particle size of 1-5 microns, using conventional Zeta potential The analyzer determines that the chromium oxide solid surface is negatively charged;

[0023] (2) Synthesis of metal-organic framework porous material ZIF-8.

[0024] ① The mass is 1.17 g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 8 g deionized water, and this solution was recorded as A;

[0025] ② Dissolve 22.70 g of 2-methylimidazole in 80 g of deionized water, and call this solution B;

[0026] ③ Mix A and B solutions at room temperature to obtain the initial ZIF-8 reaction solution, stir and mix for 5 minutes, and the mixed solution is in the form of a silky gel at this time; centrifuge the obt...

Embodiment 2

[0034] The method for preparing the MOF-2 coated cadmium chloride catalyst is as follows:

[0035] (1) Refer to "Formation and properties of Cd (OH)" published by M Ristić, S Popović, S Musić, etc. 2 and CdO particles" to prepare spherical cadmium oxide powder with a particle size of 1-5 microns, and use a conventional Zeta potential analyzer to determine that the solid surface of cadmium oxide is negatively charged;

[0036] (2) The metal-organic framework porous material MOF-2 was synthesized by referring to the existing literature: 0.73g of Zn(NO 3 ) 2 ·6H 2 O was dissolved in 10mL N,N-dimethylformamide, 0.48g terephthalic acid was also dissolved in 10mL N,N-dimethylformamide, the two solutions were mixed in a 250mL beaker under stirring, and mixed with 80mL toluene To dilute, add 50mL toluene and 0.5mL triethylamine to a 1L beaker, put the 250mL beaker into a 1L beaker, seal the beaker, and let it stand at room temperature for 7 days to obtain the initial reaction liqu...

Embodiment 3

[0044] The method for preparing the ferric chloride catalyst covered by MOF-70 is as follows:

[0045] (1) Refer to "Mechanism and controlled growth of shape and size variant core / shell FeO / Fe" published by H Khurshid, W Li, S Chandra, MH Phan 3 o 4 "Spherical iron oxide powder with a particle size of 1-5 microns was prepared, and a conventional Zeta potential analyzer was used to determine that the iron oxide solid surface was negatively charged;

[0046] (2) The metal-organic framework porous material MOF-70 was synthesized by referring to the existing literature: 0.12g of Pb(NO 3 ) 2 Dissolve in 18mL absolute ethanol, 0.06g terephthalic acid is also dissolved in 2mL N,N-dimethylformamide, mix the two solutions in a 100mL beaker with stirring and add 0.2mL hydrogen peroxide; add in a 500mL beaker 10mL N,N-dimethylformamide and 0.8mL triethylamine, put a 100mL beaker in the middle of a 500mL large beaker, seal the large beaker, and let it stand at room temperature for 7 da...