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Copper-composite molecular sieve catalyst used for synthesis of diethyl carbonate through gas-phase oxidative carbonylation and its preparation method

A composite molecular sieve and diethyl carbonate technology, which is applied in the direction of molecular sieve catalyst, carbonate/haloformate preparation, organic compound preparation, etc., can solve problems such as equipment corrosion, catalyst deactivation, chlorine loss, etc., to avoid Equipment corrosion issues, effects of optimal activity and selectivity

Active Publication Date: 2012-12-12
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the reports of catalysts for this reaction system are increasing year by year, among which CuCl is supported on carbon supports. 2 -PdCl 2 The Wacker-type catalyst has better initial activity and selectivity, but at the same time there are problems of catalyst deactivation and equipment corrosion caused by chlorine loss

Method used

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  • Copper-composite molecular sieve catalyst used for synthesis of diethyl carbonate through gas-phase oxidative carbonylation and its preparation method
  • Copper-composite molecular sieve catalyst used for synthesis of diethyl carbonate through gas-phase oxidative carbonylation and its preparation method
  • Copper-composite molecular sieve catalyst used for synthesis of diethyl carbonate through gas-phase oxidative carbonylation and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0022] The preparation method of the Yβ carrier is as follows: add 4.5g of the template agent tetraethylammonium bromide (TEAB) into 8mL of 25% ammonia (density 0.91g / mL) solution, then add 1mL of water, stir to dissolve, and then Add 0.3g NaAlO 2 and 0.3g NaOH and 7.5mL H 2 After O was stirred until completely dissolved, 13g of silica sol (SiO 2 The mass fraction is 30%) and 2mL H 2 O, a suspension was formed after vigorous stirring for 1 h, in which the n(SiO 2 ) / n(Al 2 o 3 )=36, n(NH 3 +NaOH) / n(SiO 2 )=1.8. Then add 2g of commercially available NaY molecular sieve powder (Nankai Catalyst Factory, n(SiO 2 ) / n(Al 2 o 3 )=5) and 25mL H 2 O, stirred for 0.5h, then moved to a crystallization kettle, hydrothermally crystallized at 140°C for 180h, after the crystallization was completed, filtered and washed until the filtrate was neutral. After drying at 120°C for 8 hours, put it into a muffle furnace to raise the temperature to 590°C at a rate of 2°C / min, keep the tem...

Embodiment 2-4

[0026] In the case that other experimental conditions are exactly the same as in Example 1, the crystallization time in the preparation process of the sodium-type Yβ composite molecular sieve is changed to 160h, 190h, and 200h, wherein the mix state refers to the situation of Comparative Example 1, that is, the two molecular sieves Condition after physical mixing. The XRD spectrogram of the NaYβ molecular sieve that it obtains and the NaY-β molecular sieve that physically mixes is as follows figure 1 As shown (XRD adopts the Rigaku D / max2500v / pc diffractometer of Japan Rigaku, and uses Cu / K-alphal rays as the light source for measurement. The target is a copper target, the 2θ angle measurement range is 20~80°, and the scanning speed is 8° / min, the test samples are all powder, the same below). When the crystallization time is longer than 160h, the crystal phases of Y and β molecular sieves can appear at the same time, indicating that the composite molecular sieve has been suc...

Embodiment 5-7

[0028] In the case that other experimental conditions are exactly the same as in Example 1, change the NaAlO added in the system of the β molecular sieve in the preparation process of the NaYβ composite molecular sieve 2 The mass of SiO, i.e. changing the 2 / Al 2 o 3 The ratio n(SiO 2 ) / n(Al 2 o 3 )=21, 27, 45. The XRD spectrogram of the NaYβ molecular sieve that it obtains and example 1 is as figure 2 shown. When n(SiO 2 ) / n(Al 2 o 3) ratio between 21 and 45, NaYβ composite molecular sieves can be successfully synthesized, and the higher the ratio, the higher the proportion of β crystal phase in the composite molecular sieve. Therefore, by controlling the SiO 2 / Al 2 o 3 The ratio of the β molecular sieve can change the proportion of the crystal phase in the composite molecular sieve.

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Abstract

The invention discloses a catalyst used for synthesis of diethyl carbonate through ethanol gas-phase carbonylation and its preparation method. A composite molecular sieve Ybeta is adopted to prepare a copper-composite molecular sieve catalyst through a solid ion exchange method, and the catalyst is applied in a reaction system for synthesis of diethyl carbonate through oxidative carbonylation. The unique acidity and pore structure of the composite molecular sieve are utilized to improve the catalyst performance. The catalyst prepared by the method has the advantages of high selectivity, long service life, low preparation cost, and relatively simple process.

Description

technical field [0001] The invention belongs to the gas-phase synthesis catalytic technology for synthesizing diethyl carbonate, and more specifically, relates to a catalyst for ethanol gas-phase carbonylation of diethyl carbonate and a preparation method thereof. Background technique [0002] Diethyl carbonate (DEC) is an environmentally friendly and widely used green chemical. Due to its active chemical properties, DEC can be used as an important organic synthesis intermediate and widely used in many fields such as synthetic pesticides, medicines, paints, spices, etc., and has good industrial prospects. DEC can be used as a green solvent, surfactant and lithium battery fluid additive, etc. Electronic-grade pure DEC can be used as a cleaning agent for color TV picture tubes. In addition, as one of the substitutes for MTBE, DEC has more competitive advantages than dimethyl carbonate (DMC) and ethanol, and is the potential maximum use. The existing synthesis processes of D...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/80C07C68/00C07C69/96
Inventor 黄守莹孟庆森闫冰申勇立王胜平马新宾
Owner TIANJIN UNIV
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