Catalyst for synthesizing ethylidene diacetate and application of catalyst

A technology of diethylene acetate and catalyst, which is applied in the direction of physical/chemical process catalyst, carboxylate preparation, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of low yield of diacetate, Low selectivity and other issues, to achieve the effect of improving yield and selectivity, improving activity and stability

Active Publication Date: 2015-04-29

CHINA PETROLEUM & CHEM CORP +1

7 Cites 0 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0005] One of the technical problems to be solved by this invention is the problem of low yield and selectivity of ethylene d...

Abstract

The invention relates to a catalyst for synthesizing ethylidene diacetate, a preparation method of the catalyst for synthesizing ethylidene diacetate and application of the catalyst in the synthesis of ethylidene diacetate. According to the catalyst, the preparation method and the application, the problems that a catalyst for synthesizing ethylidene diacetate in the prior art is relatively low in activity and selectivity are mainly solved. The catalyst comprises a carrier as well as ruthenium, chromium and alkaline earth metal which are loaded to the carrier, wherein the content of ruthenium is 3.0g/L-15.0g/L, the content of chromium is 1.0g/L-5.0g/L, and the content of alkaline earth metal 0.5g/L-5.0g/L; the carrier is selected from at least one of silicon oxide and aluminum oxide. According to the technical scheme, the technical problems are well solved. The catalyst can be applied to the industrial production of vinyl acetate.

Application Domain

Organic compound preparationCarboxylic acid esters preparation +1

Technology Topic

ChemistryEthylidene diacetate +7

Image

Examples

Experimental program(11)
Comparison scheme(3)

Example Embodiment

[0024] [Example 1]

[0025] Preparation of the catalyst: the Ru(OAc) containing 5.80gRu, 2.50gCr and 1.25gBe 3 ·3H 2 O, Cr (OAc) 3 ·6H 2 O and BeO are thoroughly mixed and dissolved in hydrochloric acid to obtain 500ml of immersion liquid, and 1.0L of spherical SiO with a diameter of 5.6mm 2 The carrier is immersed in the above-mentioned impregnating solution, and allowed to stand for 3h to dry at 100℃. 2 The temperature is increased to 500° C. and calcined for 5 hours to obtain the catalyst.

[0026] Synthesis of ethylene diacetate: Add 1.5 mol acetic acid, 0.05 mol catalyst and 0.45 mol methyl acetate into a 1.5L titanium reactor, first vent the air in the kettle with argon, then pressurize to 2.0MPa, and then pass in carbon monoxide And hydrogen until the pressure is 7.8MPa, increase the stirring speed to 1500rpm, while stirring and heating to increase the reaction temperature, control the reaction temperature to 181℃, the molar ratio of carbon monoxide to hydrogen is 2:1, continue the reaction for 8.0h, stop the reaction.

[0027] Product analysis: The reaction mixture obtained from the above reaction is cooled, decompressed, and separated, and the liquid phase is analyzed by gas chromatography-mass spectrometry (GC-MASS).

[0028] The Ru content of the catalyst is 5.74 g/L, the Cr content is 2.48 g/L, and the Be content is 1.24 g/L. The calculated yield of ethylene diacetate is 60.34%, and the selectivity is 87.79%. For ease of illustration and comparison, the preparation conditions, reaction conditions, yield and selectivity of ethylene diacetate are listed in the table respectively. 1 and Table 2.

Example Embodiment

[0048] [Example 2]

[0049] The preparation of the catalyst: will contain 5.80gRu, 2.50gCr and 1.25gM Ru(NO 3 ) 3 ·3H 2 O, Cr(NO 3 ) 3 ·9H 2 O and MgSO 4 ·H 2 O is thoroughly mixed and dissolved in pure water to obtain 500ml of immersion liquid, and 1.0L of spherical Al with a diameter of 5.6mm 2 O 3 The carrier is immersed in the above-mentioned impregnating solution, allowed to stand for 3 hours and dried at 80° C., and then heated to 400° C. for 5 hours in a He atmosphere to obtain the catalyst.

[0050] Synthesis of ethylene diacetate: Add 1.5 mol acetic acid, 0.05 mol catalyst and 0.45 mol methyl acetate into a 1.5L titanium reactor, first vent the air in the kettle with argon, then pressurize to 2.0MPa, and then pass in carbon monoxide And hydrogen until the pressure is 7.8MPa, increase the stirring speed to 1500rpm, while stirring and heating to increase the reaction temperature, control the reaction temperature to 181℃, the molar ratio of carbon monoxide to hydrogen is 2:1, continue the reaction for 8.0h, stop the reaction.

[0051] Product analysis: The reaction mixture obtained from the above reaction is cooled, decompressed, and separated, and the liquid phase is analyzed by gas chromatography-mass spectrometry (GC-MASS).

[0052] The Ru content of the catalyst is 5.74 g/L, the Cr content is 2.48 g/L, and the Mg content is 1.25 g/L. The calculated yield of ethylene diacetate is 60.39% and the selectivity is 87.44%. For ease of illustration and comparison, the preparation conditions, reaction conditions, yield and selectivity of ethylene diacetate are listed in the table respectively. 1 and Table 2.

Example Embodiment

[0053] [Example 3]

[0054] Preparation of the catalyst: RuCl containing 5.80gRu, 2.50gCr and 1.25gCa 3 ·3H 2 O, CrCl 3 ·6H 2 O and Ca (NO 3 ) 2 ·4H 2 O. Mix thoroughly and dissolve in hydrochloric acid to obtain 500ml of immersion liquid, and add 1.0L of spherical Al with a diameter of 5.6mm 2 O 3 The carrier is immersed in the above-mentioned impregnating solution, allowed to stand for 3 hours and dried at 120° C., and then heated to 600° C. in an Ar atmosphere and calcined for 5 hours to obtain the catalyst.

[0055] Synthesis of ethylene diacetate: Add 1.5 mol acetic acid, 0.05 mol catalyst and 0.45 mol methyl acetate into a 1.5L titanium reactor, first vent the air in the kettle with argon, then pressurize to 2.0MPa, and then pass in carbon monoxide And hydrogen until the pressure is 7.8MPa, increase the stirring speed to 1500rpm, while stirring and heating to increase the reaction temperature, control the reaction temperature to 181℃, the molar ratio of carbon monoxide to hydrogen is 2:1, continue the reaction for 8.0h, stop the reaction.

[0056] Product analysis: The reaction mixture obtained from the above reaction is cooled, decompressed, and separated, and the liquid phase is analyzed by gas chromatography-mass spectrometry (GC-MASS).

[0057] The Ru content of the catalyst is 5.75 g/L, the Cr content is 2.47 g/L, and the Ca content is 1.25 g/L. The calculated yield of ethylene diacetate is 60.68% and the selectivity is 87.71%. For ease of illustration and comparison, the preparation conditions, reaction conditions, yield and selectivity of ethylene diacetate are listed in the table respectively. 1 and Table 2.

PUM

Property	Measurement	Unit
Diameter	5.6	mm

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.

Classification and recommendation of technical efficacy words

Improve activity and stability
Improve yield and selectivity

Catalyst for synthesizing ethylidene diacetate and application of catalyst

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

Similar technology patents

Catalyst for synergetic dioxin removal and denitration and preparation method thereof

Method for synthesizing vinyl acetate through methyl acetate carbonylation

High-performance catalyst for preparing diol by hydrating epoxyalkane, preparation method and application

Method for producing 1,3-propylene glycol from vinyl acetate

Method for producing vinyl acetate through methyl acetate carbonylation

Classification and recommendation of technical efficacy words

Hydro-fining catalyst roasted at low temperature and preparation method thereof

Method for preventing pore passages from being flooded with water in catalyst layer of fuel cell

Chemical tinning liquid, preparation method thereof and chemical tinning method

Water electrolysis hydrogen production catalyst and preparation method thereof

Preparation method of graphene-multi-element metal positive electrode material

Method for synthesizing ethanol

Catalyst for synthesizing gas and liquid fuel, preparation method and application thereof

Method for producing cyclohexylamine by hydrogenating aniline

Method for synthesizing vinyl acetate

Microchannel gas-liquid reactor with Koch curve structure