Unlock instant, AI-driven research and patent intelligence for your innovation.
Method for preparing p-methylsulfonylbenzoic acid by catalytic oxidation of p-methylsulfonyl toluene through metalloporphyrin
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A technology for methylsulfonylbenzoic acid and methylsulfonyltoluene is applied in the field of metal porphyrin catalytic oxidation of p-methylsulfonyltoluene to prepare p-methylsulfonylbenzoic acid, and can solve the problems of harsh reaction conditions, air pollution, difficult operation and the like, Achieve mild reaction conditions, reduce equipment investment, and eliminate environmental pollution.
Inactive Publication Date: 2013-12-04
BEIJING UNIV OF TECH
View PDF2 Cites 0 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
[0004] (1) Concentrated nitric acid will produce a large amount of NOx gas during the oxidation process, which will not only cause serious waste of nitric acid, but also cause serious air pollution
In order to reduce the impact on the air, it is necessary to add an additional exhaust gas absorption device, which increases equipment investment and complicates the operation
[0005] (2) Due to the generation of gas during the nitric acid oxidation process, and nitric acid is extremely corrosive, not only will the reactor be flushed easily due to excessive pressure, which is not conducive to safety and makes the operation difficult , but also requires the use of equipment made of special materials, which obviously increases the investment in equipment
[0006] (3) The reaction conditions are harsh. Due to the use of highly corrosive concentrated nitric acid, and because the reaction temperature is too high, reaching 200 ° C, and the pressure is also high, there is a great potential safety hazard
[0007] And the method that adopts metalloporphyrin catalytic oxidation p-thiamphenicol toluene to prepare p-thiamphenicol benzoic acid has not been seen bibliographical information yet
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more
Image
Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0026] In a 100mL autoclave, add 2.0g sodium hydroxide, 25mL methanol, 1.7g p-thiamphenyl toluene, 100ppm tetrakis-(4-nitrophenyl)iron porphyrin, that is, a mononuclear compound with the structure of formula (I) Metalloporphyrins (where R 11 = R 12 = H, R 13 = NO 2 , M 1 =Fe), and then 2.0 MPa of oxygen was introduced, and the reaction temperature was controlled to be 100° C., and the reaction was performed for 10 h. After the reaction, dilute the reaction solution with a solvent, take a certain amount of the diluted reaction solution in a 10mL volumetric flask, add dilute hydrochloric acid to acidify, constant volume, and filter. Analysis by liquid chromatography showed that the conversion rate of p-thiamphenicol toluene was 55.6%, and the yield of p-thiamphenicol benzoic acid was 24.2%.
Embodiment 2
[0028] In a 100mL autoclave, add 3.0g sodium hydroxide, 25mL methanol, 1.7g p-thiamphenyl toluene, 100ppm tetrakis-(4-nitrophenyl) manganese porphyrin, that is, a mononuclear compound with the structure of formula (I) Metalloporphyrins (where R 11 = R 12 = H, R 13 = NO 2 , M 1 =Mn), and then 2.0 MPa of oxygen was introduced, and the reaction temperature was controlled to be 100° C., and the reaction was carried out for 10 h. Post-processing steps are the same as in Example 1. Analysis by liquid chromatography showed that the conversion rate of p-thiamphenicol toluene was 60.8%, and the yield was 27.4%.
Embodiment 3
[0030] In a 100mL autoclave, add 3.0g sodium hydroxide, 25mL methanol, 1.7g p-thiamphenyl toluene, 100ppm tetrakis-(4-chlorophenyl) manganese porphyrin, that is, a mononuclear metal with the structure of formula (I) Porphyrin (where R 11 = R 12 = H, R 13 = Cl, M 1 = Manganese), and then 2.0 MPa of oxygen was introduced, and the reaction temperature was controlled to be 90° C., and the reaction was carried out for 10 h. Post-processing steps are the same as in Example 1. Analysis by liquid chromatography showed that the conversion rate of p-thiamphenicol toluene was 56.3%, and the yield of p-thiamphenicol benzoic acid was 23.8%.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More
PUM
Login to View More
Abstract
The invention relates to a method for preparing p-methylsulfonylbenzoic acid by catalytic oxidation of p-methylsulfonyl toluene through metalloporphyrin; the method adopts p-methylsulfonyl toluene as a raw material, adopts methanol or ethanol as a solvent, adopts any one of or a combination of two of 1-300 ppm mononuclear metalloporphyrin and mu-oxo-binuclear metalloporphyrin as a catalyst, and comprises the following steps: introducing 0-3 MPa oxygen into a sodium hydroxide alcoholic solution with a concentration of 0.5-6 mol / L, reacting at a reaction temperature of 50-145 DEG C for 1-12 hours, performing routine separation to obtain the p-methylsulfonylbenzoic acid. The method of the invention adopts clean and cheap oxygen instead of chemical oxidant nitric acid which causes serious environment pollution and is expensive, eliminates the environment pollution caused by NOx waste gas, reduces the cost of raw materials and the preparation process, has relatively mild reaction conditions, has a low reaction temperature, not only saves the energy consumption of the preparation process, but also significantly improves the safety of the preparation process.
Description
technical field [0001] The invention relates to a preparation method of aromatic acid, in particular to a method for preparing p-thiamphenicol benzoic acid by catalyzing the oxidation of p-thiamphenicol toluene by metalloporphyrin. Background technique [0002] The method for preparing p-thiamphenicol benzoic acid from p-thiamphenicol toluene reported in the prior art is mainly a chemical oxidation method. Huang Yinhua et al. (Journal of Zhejiang University of Technology, 2002, 30 (1): 59-62, 67) reported a method for preparing p-thiamphenicol benzoic acid by oxidizing p-thiamphenicol toluene with nitric acid. Using 96% nitric acid as an oxidizing agent, react at 200°C for 70 minutes, and obtain o-nitro-p-thiamphenicol benzoic acid after post-treatment, with a crude yield of 74.4%. [0003] The above-mentioned method for synthesizing p-thiamphenicol mainly has the following problems: [0004] (1) Concentrated nitric acid will produce a large amount of NOx gas during the ox...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More
Application Information
Patent Timeline
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
Login to View More 
Login to View More