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Method for producing alicyclic polycarboxylic acid

A polycarboxylic acid, alicyclic technology, applied in the direction of ozone oxidation to prepare carboxylic acid, organic chemistry, etc., can solve the problems of precipitation, adhesion, heat transfer efficiency reduction, etc., and achieve the effect of simple temperature control

Active Publication Date: 2016-10-12
MITSUBISHI RAYON CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if such a method of cooling through the heat transfer surface is used, the raw materials or reaction products are usually precipitated and attached to the heat transfer surface, and the heat transfer efficiency is rapidly reduced.

Method used

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  • Method for producing alicyclic polycarboxylic acid
  • Method for producing alicyclic polycarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070]

[0071] use as figure 1 In the reaction device with the shown configuration, terephthalic acid (TPA) is hydrogenated to prepare 1,4-cyclohexanedicarboxylic acid (CHDA).

[0072] First, in a raw material preparation tank at normal temperature, 1599 kg / h of TPA at 20°C was mixed and dispersed in 6397 kg / h of water at 20°C to prepare a slurry with a TPA concentration of 20% by weight (TPA / water (weight ratio)=20 / 80).

[0073] The pressure was raised to 6.1 MPa G (gauge pressure, the same below), and the above-mentioned slurry was supplied to a reactor with a stirrer at a supply rate of 7996 kg / h. A heat exchanger regulates the temperature to 91°C and maintains it at 170°C.

[0074] In the reactor, the catalyzer (Pd / C catalyzer) of supporting palladium on the activated carbon of 2% by weight is flowing, while maintaining 6.1MPa G in the stirring tank, with 2664Nm 3 / h Hydrogen gas (6.1 MPa·G) at 114°C was supplied to the reactor.

[0075] While filtering the Pd / C ca...

Embodiment 2

[0106] It was carried out in the same manner as in Example 1 except that the following points were changed.

[0107] That is, in a raw material preparation tank at room temperature, 800 kg / h of TPA at about 20°C was mixed and dispersed in 7196 kg / h of water at 20°C to prepare a slurry with a TPA concentration of 10% by weight (TPA / water (weight ratio) = 10 / 90). The pressure is increased to 6.1MPa·G (gauge pressure, the same below) by hydrogen gas, and the slurry is supplied to the reactor with a stirrer at a supply rate of 7996kg / h. The heat exchanger regulates the temperature to 113°C and maintains it at 170°C.

[0108] In the reactor, flow the catalyzer (Pd / C catalyst) of palladium on the active carbon of 2% by weight, keep 6.1MPa G in the stirred tank simultaneously, with 1342Nm 3 / h Hydrogen gas (6.1 MPa·G) at 74°C was supplied to the reactor. While filtering the Pd / C catalyst, 160,789kg / h of reaction product liquid and 951Nm of hydrogen containing saturated water vapor...

Embodiment 3

[0125] It was carried out in the same manner as in Example 1 except that the following points were changed.

[0126] That is, in a raw material preparation tank at room temperature, 2399 kg / h of TPA at about 20° C. was mixed and dispersed in 5,597 kg / h of water at 20° C. to prepare a slurry with a TPA concentration of 30% by weight (TPA / water (weight ratio) = 30 / 70). The pressure is increased to 6.1MPa·G (gauge pressure, the same below) by hydrogen gas, and the slurry is supplied to the reactor with a stirrer at a supply rate of 7996kg / h. The heat exchanger regulates the temperature to 58°C and maintains it at 170°C.

[0127] In the reactor, the catalyzer (Pd / C catalyst) of supporting palladium on the activated carbon of 2% by weight is flowing, while maintaining 6.1MPa G in the stirring tank, with 3990Nm 3 / h Hydrogen gas (6.1 MPa·G) at 128°C is supplied to the reactor. While filtering the Pd / C catalyst, the reaction product liquid 161924kg / h and the hydrogen gas 2391Nm co...

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Abstract

The present invention provides a method for producing an alicyclic polycarboxylic acid capable of keeping the heat removal performance of a reaction mixture stable and obtaining stable reaction results over an extended period of time. In this method for producing an alicyclic polycarboxylic acid, the aromatic nucleus of an aromatic polycarboxylic acid is hydrogenated in an aqueous medium, and a corresponding alicyclic polycarboxylic acid is continuously produced, wherein the reaction temperature is controlled by adjusting the temperature of the raw material mixture fed to the reactor; in particular, the reaction temperature is 100-200 DEG C, and the temperature of the raw material mixture fed to the reactor is 40 DEG C to 120 DEG C lower than the reaction temperature.

Description

technical field [0001] The present invention relates to the manufacture method of cycloaliphatic polycarboxylic acid, is to use aromatic polycarboxylic acid as raw material, carry out hydrogenation reaction in the presence of solid catalyst, prepare corresponding cycloaliphatic polycarboxylic acid; Hydrogenation of aromatic polycarboxylic acids such as formic acid (hereinafter referred to as "TPA") (hereinafter referred to as "ring hydrogenation") to prepare 1,4-cyclohexanedicarboxylic acid (hereinafter referred to as "1,4- CHDA" or just "CHDA") and other corresponding cycloaliphatic polycarboxylic acids. [0002] 1,4-CHDA and other alicyclic polycarboxylic acids are raw materials for alicyclic polyhydric alcohols such as 1,4-cyclohexanedimethanol, which are used as polyester-based coatings, polyester-based synthetic fibers, synthetic resins, etc. It is useful as a raw material, especially as a raw material of resin or fiber excellent in heat resistance, weather resistance, a...

Claims

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Application Information

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IPC IPC(8): C07C51/36C07C61/08C07C61/09
CPCC07C51/36C07C61/08C07C61/09
Inventor 田中善幸香川浩哉
Owner MITSUBISHI RAYON CO LTD
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