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Catalyst for synthesizing diphenyl carbonate, preparation method thereof and process

A diphenyl carbonate and catalyst technology, applied in the field of catalytic synthesis of diphenyl carbonate, can solve the problems of deactivation of catalyst active components, low activity or selectivity, and difficulty in repeated use, and achieve high catalytic activity and high catalytic performance Activity, energy barrier lowering effect

Active Publication Date: 2020-07-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Homogeneous catalysts have the problem of difficult separation from products and are not easy to be reused, so heterogeneous catalysts are the main direction of development
Although the heterogeneous catalyst is easy to separate from the product, its activity or selectivity is usually low, and the catalyst is easily deactivated due to the loss of active components

Method used

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  • Catalyst for synthesizing diphenyl carbonate, preparation method thereof and process
  • Catalyst for synthesizing diphenyl carbonate, preparation method thereof and process
  • Catalyst for synthesizing diphenyl carbonate, preparation method thereof and process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Prepare 1mol / L lithium nitrate solution, impregnate 20g ZSM-5 molecular sieves in 1L lithium nitrate solution, stir at room temperature for 6 hours, filter solid-liquid separation, dry the solid at 120°C for 12 hours, and then bake at 550°C for 3 hours . The above steps were repeated 2 more times. Molecular sieve M1 was prepared.

[0052] Molecular sieve M1 was vacuum dried at 120° C. for 4 hours. Prepare a 0.8mol / L tin chloride solution, and impregnate the molecular sieve M1 with equal volume. Dry at room temperature for 12 hours. Molecular sieve M1 was then further vacuum dried at 120°C for 4 hours.

[0053] Prepare a 0.8mol / L zirconium nitrate solution, and impregnate the molecular sieve M1 with equal volume. Dry at room temperature for 12 hours. Precursor P1 is obtained.

[0054] Then the precursor P1 was placed in 1L saturated ammonia water and soaked at room temperature for 4 hours. Dry at room temperature for 12 hours.

[0055] The dried solid was calcin...

Embodiment 2-17

[0058] Change the type of lithium salt, solution concentration, solid-to-liquid ratio, treatment time, drying temperature, drying time, and treatment times, and the rest of the conditions are the same as in Example 1. Obtain LiZSM-5 molecular sieve. As shown in Table 1.

[0059] Table 1.

[0060]

[0061] The type of molecular sieve, the calcination temperature and time were changed, and other conditions were the same as in Example 1 to obtain LiY molecular sieve and Liβ molecular sieve.

[0062] Table 2.

[0063]

[0064] Use the lithium type molecular sieve in table 1 and table 2, change the metal salt solution type, concentration, solid-liquid ratio, drying condition, treatment times of active component, all the other conditions are identical with embodiment 1, obtain catalyst precursor P, as table 3.

[0065] table 3.

[0066]

[0067] Use the catalyst precursor in Table 3, change the soaking time of saturated ammonia water, drying condition, treatment times ...

Embodiment 18

[0071] Weigh 10g of the catalyst C1 prepared in Example 1 above and place it in a 300mL stainless steel reactor, replace the air in the reactor with N2, then fill it with 50.0g of phenol and 64.3g of dibenzyl carbonate, raise the temperature to 175°C, and react for 10 Cool after 1 hour, reaction product is carried out chromatographic analysis, in molar basis, the conversion rate that obtains dibenzyl carbonate (DBC) is 86.3%, the selectivity of diphenyl carbonate (DPC) is 76.5%, benzyl phenyl carbonate (BPC) selectivity was 21.9%.

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Abstract

The invention discloses a catalyst for synthesizing diphenyl carbonate. The catalyst comprises a molecular sieve and a loaded active component, the molecular sieve is an alkali metal modified microporous molecular sieve, and the active component is binary mixed metal oxide AO / B<c>O<d>, wherein A is selected from Sn, Ga or Zn, B is selected from Zr, Cr or La, and a, b, c and d are stoichiometric numbers. Due to the addition of a lithium additive, the energy barrier in the side reaction process is remarkably improved, and the reaction speed of the side reaction is reduced. The tin oxide and other active components obviously lower the energy barrier in the main reaction process, and enhance the reaction speed of the main reaction. The catalyst provided by the invention has very high catalytic activity, effectively realizes diphenyl carbonate synthesis reaction, inhibits the occurrence of ether side reaction, and reduces the energy consumption of the production process.

Description

technical field [0001] The invention relates to a catalytic synthesis method of diphenyl carbonate, in particular to a method for preparing diphenyl carbonate through the transesterification reaction of phenol and dibenzyl carbonate catalyzed by a heterogeneous catalyst. Background technique [0002] Diphenyl carbonate is an important fine chemical intermediate, which can synthesize many organic compounds and polymer materials through reactions such as halogenation, nitration, hydrolysis and ammonolysis, especially can replace highly toxic phosgene and bisphenol A through melt transesterification Polycarbonate with excellent synthetic properties. Diphenyl carbonate is the raw material for the preparation of polycarbonate by non-phosgene method. The traditional preparation method of diphenyl carbonate is the phosgene method, which is subject to policy restrictions due to the potential harm of highly toxic phosgene to the environment and safe production. [0003] Synthesis o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40B01J29/08B01J29/70B01J37/02B01J37/30C07C69/96C07C68/06
CPCB01J29/405B01J29/088B01J29/7057B01J23/002B01J37/0201B01J37/30C07C68/065B01J2229/183B01J2229/186C07C69/96
Inventor 张志智孙潇磊王陶尹泽群刘全杰方向晨
Owner CHINA PETROLEUM & CHEM CORP
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