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Catalyst for preparing 5-aminoisophthalic acid as well as preparation method and application of catalyst

An aminoisophthalic acid and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem that the reaction process is difficult to precisely control, batch products Problems such as poor stability and long auxiliary operation time are beneficial to safety control, high stability of product quality, and avoidance of quality differences.

Pending Publication Date: 2020-02-28
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis of 5-aminoisophthalic acid mainly relies on kettle-type hydrogenation. The disadvantages of the current process mainly include: 5-aminoisophthalic acid hydrogenation kettle-type process, there are auxiliary operations such as loading and unloading, which have long time and labor High strength, difficult to control independently, slow mass and heat transfer, easy to cause problems such as uneven temperature and concentration, low space-time yield, poor stability of batch products, difficult to accurately control the reaction process, and large safety hazards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. A catalyst for preparing 5-aminoisophthalic acid is made up of carrier and Pt, Pd and Sn loaded on the carrier, and the carrier is an activated carbon carrier; according to weight percentage 100%, the content of Pt is 0.35%, the content of Pd is 0.15%, the content of Sn is 0.2%, and the rest is carrier;

[0031] The activated carbon carrier is a columnar activated carbon carrier, and the average outer diameter of the carrier is 2.5mm, and the specific surface area is 890m 2 / g, axial compressive strength 43N.

[0032] 2. the preparation method of described catalyst, comprises the following steps:

[0033] (1) Dissolve stannous chloride dihydrate containing 0.2g Sn in 0.5wt% dilute nitric acid to obtain solution A, then add 30mL of absolute ethanol which is one-third of the volume of solution A to it, and mix well Submerge the carrier in it, stir for 2 hours, let it stand for 8 hours, and filter to obtain solid material B. Dry the solid material B at 60°C for 8 hour...

Embodiment 2

[0037] 1. A catalyst for preparing 5-aminoisophthalic acid is made up of carrier and Pt, Pd and Sn loaded on the carrier, and the carrier is an activated carbon carrier; according to weight percentage 100%, the content of Pt is 0.5%, the content of Pd is 0.05%, the content of Sn is 0.1%, and the rest is carrier;

[0038] The activated carbon carrier is a columnar activated carbon carrier, and the average outer diameter of the carrier is 2.5mm, and the specific surface area is 890m 2 / g, axial compressive strength 43N.

[0039] 2. the preparation method of described catalyst, comprises the following steps:

[0040] (1) Dissolve stannous chloride dihydrate containing 0.1g Sn in 0.5wt% dilute nitric acid to obtain solution A, then add 30mL of absolute ethanol which is one-third of the volume of solution A to it, and mix well Submerge the carrier in it, stir for 3 hours, let it stand for 4 hours, and filter to obtain solid material B. The solid material B was first vacuum-dried at...

Embodiment 3

[0044] 1. A catalyst for preparing 5-aminoisophthalic acid is made up of carrier and Pt, Pd and Sn loaded on the carrier, and the carrier is an activated carbon carrier; according to weight percentage 100%, the content of Pt is 0.8%, the content of Pd is 0.2%, the content of Sn is 0.3%, and the rest is carrier;

[0045] The activated carbon carrier is a columnar activated carbon carrier, and the average outer diameter of the carrier is 2.5mm, and the specific surface area is 890m 2 / g, axial compressive strength 43N.

[0046] 2. the preparation method of described catalyst, comprises the following steps:

[0047] (1) Dissolve tin protochloride dihydrate containing 0.3g Sn in 0.5wt% dilute nitric acid to obtain solution A, then add 30mL of absolute ethanol, which is one-third of the volume of solution A, and mix well Submerge the carrier in it, stir for 3 hours, let it stand for 4 hours, and filter to obtain solid material B. The solid material B was first vacuum-dried at 70°...

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Abstract

The invention discloses a catalyst for preparing 5-aminoisophthalic acid, the catalyst consists of a carrier, Pt, Pd and metal M, the Pt, Pd and metal M are loaded on the carrier, the metal M is Sn, Ba or Ni, and the carrier is an activated carbon carrier; the catalyst is prepared from, by weight, 0.05%-1% of the Pt, 0.05%-1% of the Pd, 0.05%-1% of the metal M and the balance of the carrier. Meanwhile, the invention also discloses a preparation method of the catalyst and application of the catalyst in continuous preparation of the 5-aminoisophthalic acid by using a 5-nitroisophthalic acid fixed bed. The catalyst provided by the invention is high in catalytic activity, selectivity and stability, when the catalyst is used for preparing the 5-aminoisophthalic acid, the molar conversion rate of raw material 5-nitroisophthalic acid is greater than 96.9%, the molar yield of the product 5-aminoisophthalic acid is greater than 96%, and the accumulated operation time of the catalyst is long.

Description

technical field [0001] The invention belongs to the technical field of catalytic hydrogenation and nitro hydrogenation process, and in particular relates to a catalyst for preparing 5-aminoisophthalic acid, a preparation method and application thereof. Background technique [0002] 5-Aminoisophthalic acid is an important organic synthesis intermediate, which is widely used in chemical reagents, pigments, dyes, non-ionic X-CT contrast agents and other chemical products, such as the synthesis of iohexol, iopamidol, Ioversol and the like all need 5-aminoisophthalic acid, which can form complexes with metals as light-emitting materials, and the synthesis of some macromolecular compounds also requires it as a linking intermediate. Therefore, 5-aminoisophthalic acid is used as a raw material for chemical intermediates, and its synthetic method has attracted much attention. [0003] At present, the synthesis of 5-aminoisophthalic acid mainly relies on kettle-type hydrogenation. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/62B01J35/10B01J23/58C07C227/06C07C229/62
CPCB01J23/626B01J23/58C07C227/06B01J35/617B01J35/618B01J35/647C07C229/62Y02P20/584
Inventor 万克柔程杰张炳亮林涛张力高明明赵茁然张之翔
Owner XIAN CATALYST NEW MATERIALS CO LTD
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