Method for preparing 1-methoxy-2-acetone with catalytic oxidation of 1-methoxy-2-propyl alcohol

A catalytic oxidation, methoxyl technology, applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the complex reactor design and operation process, raw material 1-methoxy-2-propane Problems such as low alcohol conversion rate, to achieve the effects of easy operation, fast reaction rate and simple equipment

Inactive Publication Date: 2008-12-03
江苏天音化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction needs to be carried out in a tubular reactor, the reactor design and operation process are complicated, and the conversion rate of raw material 1-methoxyl-2-propanol is low

Method used

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  • Method for preparing 1-methoxy-2-acetone with catalytic oxidation of 1-methoxy-2-propyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: 18.0g (0.2mol) 1-methoxy-2-propanol and 0.312g (0.002mol) TEMPO catalyst were added to a 500mL polytetrafluoro-lined autoclave, magnetic stirring was started, and 0.138g dissolved in (0.002mol)NaNO 2 And 0.238g (0.002mol) KBr aqueous solution 1.2g, airtight reactor, fills with O 2 To a gauge pressure of 0.4 MPa, the temperature was raised to 80° C. and kept for 4 hours to complete the reaction. After the temperature was lowered and the pressure was carefully released, samples were taken for GC-MS analysis. The conversion rate of 1-methoxy-2-propanol was 89%, and the selectivity of the product 1-methoxy-2-propanone was 83%.

Embodiment 2

[0015] Example 2: 18.0g (0.2mol) 1-methoxy-2-propanol and 0.312g (0.002mol) TEMPO catalyst were added to a 500mL polytetrafluoro-lined autoclave, magnetic stirring was started, and 0.138g dissolved in (0.002mol)NaNO 2 And 0.238g (0.002mol) KBr, 0.168g of NaHCO 3 2.2 g of the aqueous solution, the reactor was sealed, filled with air to a gauge pressure of 0.7 MPa, and heated to 100 ° C for 4 hours to complete the reaction. After the temperature was lowered and the pressure was carefully released, samples were taken for analysis. The conversion rate of 1-methoxy-2-propanol was 85%, and the selectivity of 1-methoxy-2-acetone was 83%.

Embodiment 3

[0016] Example 3: 18.0g (0.2mol) 1-methoxy-2-propanol and 0.312g (0.002mol) TEMPO catalyst were added to a 500mL polytetrafluoro-lined autoclave, magnetic stirring was started, and 0.104g dissolved in (0.0015mol)NaNO 2 And 0.206g (0.002mol) NaBr, 0.168g of NaHCO 3 Add 1.2 g of aqueous solution of 1.2 g of liquid bromine, 36.0 g of 1,2-dichloroethane, seal the reaction vessel, fill it with air to 0.4 MPa (gauge pressure), raise the temperature to 80 ° C, keep the temperature for 4 hours to complete the reaction, evaporate After the dichloroethane solvent, sampling was carried out for gas chromatography analysis, the conversion rate of 1-methoxyl-2-propanol was 90%, and the selectivity of product 1-methoxyl-2-propanone was 67%.

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Abstract

The invention relates to a method for preparing 1-methoxyl-2-acetone through 1- methoxyl -2-propanol by means of catalytic oxidation, which is characterized in that: the catalytic oxidation is performed under the condition of taking 2, 2, 6, 6-tetramethyl piperidine -1-oxygen-derived free radicals or piperidinol compounds and nitrite or nitrate as catalysts, one or mixture among phosphate (hydrophosphate), halides, halate, borate, molybdate, carbonate (supercarbonate), sulfate and acetate as auxiliary catalyst, and halogen, hypo halite, hydrogen peroxide solution, oxygen, air or organic peroxide as oxidant. Compared with the prior art, the method has the advantages that: main parts of the catalysts do not use transition metals, and the catalysts are low-price and easily obtained and can be reused; the reaction condition is mild, and the reaction can be performed under normal temperature and normal pressure and also can be performed under high temperature and high pressure; equipment is simple and easy to operate; the reaction rate is quick, and the product conversion rate is high and can reach 90 percent; and the method is suitable for continuous industrialized production.

Description

technical field [0001] The invention relates to a method for preparing 1-methoxy-2-propanone by catalytic oxidation of 1-methoxy-2-propanol. Background technique [0002] 1-Methoxy-2-acetone (methoxyacetone) is an excellent organic solvent and pesticide intermediate, which can be widely used in the manufacture of various products such as paints, cleaning agents, dyes, pesticides, and herbicides. In industrial production, 1-methoxy-2-propanol (1,2-propanediol monomethyl ether) is generally synthesized by reaction of methanol and propylene oxide, and then further catalytic oxidation of 1-methoxy-2-propanol is obtained 1-methoxy-2-propanone. Its reaction process is: [0003] [0004] Wherein in the 2nd step, 1-methoxyl-2-propanol is catalyzed and oxidized to prepare 1-methoxyl-2-propanone in the process, usually with the transition metals of 8~10 groups such as palladium, ruthenium, rhodium as catalyst , Copper, platinum, etc. as promoters. As disclosed in U.S. Patent US...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/175C07C45/39B01J31/02
Inventor 秦旭东杨建伟何强蒋大智张学君
Owner 江苏天音化工有限公司
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