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Catalyst for continuously preparing 3,5-dimethyl piperidine and preparation method and application thereof

A technology of dimethylpiperidine and lutidine, which is applied in the field of catalytic hydrogenation of heterocyclic compounds, can solve the problems that the product yield cannot reach 99%, the cis-trans ratio is difficult to control, and the production efficiency is low. Effects of low cost, high catalytic activity and stability, and few by-products

Active Publication Date: 2017-05-31
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is relatively mature, but there are some problems: the conversion rate of raw materials is less than 99%, the product yield is less than 99%, rectification is required, and the cis-trans ratio is not easy to control; the production efficiency is low and the catalytic cost is high; autoclave hydrogenation reaction , poor safety; the raw materials and products are toxic and harmful compounds with strong pungent smell, and the kettle operation is very harmful to people and not environmentally friendly

Method used

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  • Catalyst for continuously preparing 3,5-dimethyl piperidine and preparation method and application thereof
  • Catalyst for continuously preparing 3,5-dimethyl piperidine and preparation method and application thereof
  • Catalyst for continuously preparing 3,5-dimethyl piperidine and preparation method and application thereof

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Embodiment 1

[0034] The catalyst of the present embodiment comprises activated carbon carrier, Ru, Rh and K loaded on the activated carbon carrier; the mass percentage composition of Ru is 1.5% in the described catalyst, the mass percentage composition of Rh is 1%, the mass percentage composition of K The content is 1.2%; the average particle diameter of the activated carbon carrier is 1.5mm, and the specific surface area is 920m 2 / g.

[0035] The preparation method of the catalyst of the present embodiment is:

[0036] Step 1, dissolving ruthenium trichloride containing 1.5g of ruthenium in dilute hydrochloric acid with a mass concentration of 2.5%, to obtain solution A;

[0037] Step 2, dissolving rhodium trichloride containing 1g of rhodium in dilute hydrochloric acid with a mass concentration of 3%, to obtain solution B;

[0038] Step 3. Mix the solution A described in step 1 and the solution B described in step 2 evenly to obtain solution C. Soak 96.3g of activated carbon carrier i...

Embodiment 2

[0044] The catalyst of the present embodiment includes activated carbon carrier, Ru, Rh and K loaded on the activated carbon carrier; the mass percentage of Ru in the catalyst is 2.5%, the mass percentage of Rh is 0.5%, and the mass percentage of K The content is 0.7%; the average particle diameter of the activated carbon carrier is 1.5mm, and the specific surface area is 1020m 2 / g.

[0045] The preparation method of the catalyst of the present embodiment is:

[0046] Step 1, dissolving ruthenium trichloride containing 2.5g ruthenium in dilute hydrochloric acid with a mass concentration of 3.5%, to obtain solution A;

[0047] Step 2, dissolving rhodium trichloride containing 0.5g rhodium in dilute hydrochloric acid with a mass concentration of 2.5%, to obtain solution B;

[0048] Step 3. Mix the solution A described in step 1 and the solution B described in step 2 evenly to obtain solution C. Soak 96.3g of activated carbon carrier in solution C, heat it to 40°C, keep it war...

Embodiment 3

[0054] The catalyst of the present embodiment includes activated carbon carrier, Ru, Rh and K loaded on the activated carbon carrier; the mass percentage of Ru in the catalyst is 5.0%, the mass percentage of Rh is 0.05%, and the mass percentage of K is The content is 0.1%; the average particle diameter of the activated carbon carrier is 2.5mm, and the specific surface area is 1200m 2 / g.

[0055] The preparation method of the catalyst of the present embodiment is:

[0056] Step 1, dissolving ruthenium trichloride containing 5.0 g of ruthenium in dilute hydrochloric acid with a mass concentration of 5%, to obtain solution A;

[0057] Step 2, dissolving rhodium trichloride containing 0.05g rhodium in dilute hydrochloric acid with a mass concentration of 2.5%, to obtain solution B;

[0058] Step 3. Mix the solution A described in step 1 and the solution B described in step 2 evenly to obtain solution C. Soak 94.85g of activated carbon carrier in solution C, heat it to 40°C, kee...

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Abstract

The invention discloses a catalyst for continuously preparing 3,5-dimethyl piperidine. The catalyst is prepared from an activated carbon carrier, Ru, Rh and M, wherein the Ru, the Rh and the M are loaded on the activated carbon carrier, the mass percent content of the Ru in the catalyst is 1% to 5%, the mass percent content of the Rh is 0.05% to 1%, the mass percent content of the M is 0.05% to 1.5%, and the M is Pt, K, Ce or Sn. In addition, the invention further discloses a preparation method of the catalyst and a method for continuously preparing the 3,5-dimethyl piperidine. The catalyst disclosed by the invention has the characteristics of high activity, high selectivity and high stability and can can realize high-efficient catalysis to prepare the 3,5-dimethyl piperidine in high efficiency; the converting rate of a raw material of 3,5-dimethyl pyridine is 100%, the yield of a product of the 3,5-dimethyl piperidine is larger than 99%, and cis-trans isomerism ratio is (87 : 13) to ( 83 : 17).

Description

technical field [0001] The invention belongs to the technical field of catalytic hydrogenation process of heterocyclic compounds, and in particular relates to a catalyst for continuous preparation of 3,5-dimethylpiperidine, a preparation method and application thereof. Background technique [0002] 3,5-Dimethylpiperidine is mainly used in the synthesis of pharmaceutical intermediates, veterinary drug tilmicosin, etc., wherein tilmicosin is a hydrolyzate of tylosin and 3,5-dimethylpiperidine Synthetic special antibiotics for livestock and poultry, and its phosphate for medicinal use is mainly used to prevent and treat livestock pneumonia (caused by infections such as Actinobacillus pleuropneumoniae, Pasteurella, Mycoplasma, etc.), avian mycoplasma disease and mastitis of lactating animals. The dosage is very large . Therefore, the market prospect of 3,5-dimethylpiperidine is very broad. [0003] At present, the synthesis of 3,5-dimethylpiperidine is mainly based on the batc...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J23/58B01J23/62B01J23/63C07D211/12
Inventor 万克柔林涛程杰李霖曾永康曾利辉张之翔
Owner XIAN CATALYST NEW MATERIALS CO LTD
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