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Method for preparing 2, 6-naphthalic acid through oxidizing 2-methyl-6-propionyl naphthalene

A technology of propionyl naphthalene and naphthalene dicarboxylic acid, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve the problems of high energy consumption, inability to obtain ideal product yield, high equipment requirements, etc., and achieve The effect of low reaction temperature, suppression of product color blackening, and less by-product formation

Inactive Publication Date: 2018-01-30
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the current research requires high temperature and high pressure, which requires relatively high equipment, high energy consumption, and the ideal product yield cannot be obtained.

Method used

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  • Method for preparing 2, 6-naphthalic acid through oxidizing 2-methyl-6-propionyl naphthalene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In the gas-liquid bubbling and stirring high-pressure reactor, the stirring speed is 600r / min, stirring and heating to 175°C, using N 2 Pressurize to 1.8MPa; mix and dissolve 120g of glacial acetic acid, 5.80g of cobalt acetate tetrahydrate, 4.98g of manganese acetate tetrahydrate, 7.14g of potassium bromide, and 8.58g of potassium acetate. Continuous supply of 3.0 liters (standard state) / min; 72.6g of 2-methyl-6-propionylnaphthalene dissolved with 100g of glacial acetic acid is continuously supplied by a metering pump. After the material stays in the reactor for an average of 2 hours, the bottom of the reactor is The height of the outflow pipe is kept at the same height as the liquid level in the reactor, and the material overflows to ensure that there is sufficient solvent and raw materials in the reactor to maintain the reaction; after the reaction liquid is cooled and solid-liquid separated, the mother liquid is reused, as shown in the attached figure 1 shown. The ...

Embodiment 13

[0035] Embodiment 1.3: Recover mother liquor and solvent after centrifugation

[0036] The mother liquor after the centrifugation of Example 1 and the acetic acid after washing are returned in the reactor as raw materials, do not add catalyst and co-catalyst, other are the same as Example 1, carry out oxidation reaction;

[0037] After drying, 60.33 g of khaki solid powder was obtained. The purity and yield of 2,6-naphthalene dicarboxylic acid after liquid phase analysis were 95.6% and 83.1%, respectively.

[0038] After the mother liquor after the secondary centrifugation and the acetic acid after washing are returned in the reactor as a raw material, and the potassium bromide and 2.0g potassium acetate of 2.28g and 2.0g potassium acetate, and 20g glacial acetic acid are supplemented according to the feeding ratio for the first time among the embodiment 1, Others carry out oxidation reaction with embodiment 1;

[0039]After drying, 58.44 g of khaki solid powder was obtained...

Embodiment 2

[0041] In the gas-liquid bubbling and stirring autoclave, the stirring speed is 600r / min, stirring and heating to 170°C, and pressurizing with N2 to 1.6MPa; 200g of glacial acetic acid and 50.0g of propionic acid and 9.93g of cobalt acetate tetrahydrate, 6.73 G manganese acetate tetrahydrate, 9.64g potassium bromide, and 15.82g potassium acetate are mixed and dissolved, and are continuously added to the oxidation reactor by a metering pump; compressed air is continuously supplied to the reactor at 3.0 liters (standard state) / min; 260g glacial acetic acid Dissolved with 111.38g 2-methyl-6-propionylnaphthalene and continuously supplied by metering pump, the material stays in the reactor for an average of 1 hour, and the height of the outflow pipe at the bottom of the reactor is maintained at the same height as the liquid level in the reactor, and the overflow is discharged, so that It can ensure that there are sufficient solvents and raw materials in the reactor to maintain the r...

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Abstract

The invention belongs to the technical field of chemical synthesis, and concretely relates to a method for preparing 2, 6-naphthalic acid through oxidizing 2-methyl-6-propionyl naphthalene. The methodcomprises the steps of adopting the 2-methyl-6-propionyl naphthalene as a raw material, adopting a Co-Mn-Br-based catalyst as a main catalyst in a continuous oxidation reactor, adopting kali salt, sodium salt or nickel salt as a cocatalyst, adopting one of glacial acetic acid or propionic acid or a mixture of the glacial acetic acid and the propionic acid as a solvent, and continuously feeding oxygen-containing gas into the oxidation reactor for continuously oxidizing the 2-methyl-6-propionyl naphthalene to synthesize the 2, 6-naphthalic acid. The method is liquid phase continuous reaction, has less side reaction, stable product quality and simple and controllable process, and can be used for preparing the high-yield high-purity 2, 6-naphthalic acid.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for preparing 2,6-naphthalene dicarboxylic acid by oxidation of 2-methyl-6-propionylnaphthalene. Background technique [0002] 2,6-Naphthalene dicarboxylic acid is an important monomer for the preparation of various polyesters, polyurethane materials and liquid crystal polymers, and is also widely used in the fields of dyes and medicine. The structure of 2,6-naphthalene dicarboxylic acid is highly symmetrical, and polyethylene 2,6-naphthalene dicarboxylate (PEN), which is obtained by reacting with ethylene glycol, has the characteristics of a straight-chain polymer and is a kind of rigid, high-strength, High-performance material with excellent thermal processing properties. Compared with polyethylene terephthalate (PET), PEN has superior properties such as heat resistance, barrier property, mechanical properties, chemical resistance, and UV resistance; in rec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/38C07C51/265
Inventor 靳海波杨索和郭学华何广湘郭晓燕王亚涛
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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