Method for synthesizing 3-methyl-2-buten-1-ol from 3-methyl-3-buten-1-ol through trickle-bed transposition

A technology of isopentenol and trickle bed, which is applied in the direction of chemical instruments and methods, isomerization preparation, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of high reaction temperature and reaction time of gas phase isomerization Harsh conditions, low selectivity, etc., to achieve the effect of simple catalyst components, mild reaction conditions, and high product selectivity

Inactive Publication Date: 2019-11-22
SHANDONG NHU PHARMA
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Problems solved by technology

Simultaneously because prenaldehyde and raw material 3-methyl-3-butene-1-alcohol boiling point are close, be difficult to separate, cause energy consumption to increase when reclaiming 3-methyl-3-butene-1-alcohol, and Affect yield
[0021] In summary, when the existing hydrogen transposition reaction for the synthesis of isopentenol is carried out intermittently in a reactor, isoamyl alcohol is unavoidably generated, and it is difficult to ensure a high selectivity in the isomerization reaction, and The degree of automation is low, the operation is cumbersome, and a large amount of hydrogen will be wasted after the reaction of each kettle; when the fixed bed continuous reaction is adopted, the gas phase isomerization reaction temperature is high, and the liquid phase isomerization activity, selectivity and stability cannot be taken into account
When reacting under an inert atmosphere, the reaction conditions are generally harsh, the catalyst is more complicated, the energy consumption and separation cost are higher, and the competitiveness of the product is reduced
During the oxygen transposition reaction, prenyl aldehyde is generated, and the selectivity of prenol is low and a noble metal catalyst is used, which is more expensive
Therefore, there is no mild reaction condition, simple and cheap catalyst, easy separation, high activity selectivity stability, and continuous 3-methyl-3-butene-1-alcohol transposition synthesis isopentenol method

Method used

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  • Method for synthesizing 3-methyl-2-buten-1-ol from 3-methyl-3-buten-1-ol through trickle-bed transposition
  • Method for synthesizing 3-methyl-2-buten-1-ol from 3-methyl-3-buten-1-ol through trickle-bed transposition
  • Method for synthesizing 3-methyl-2-buten-1-ol from 3-methyl-3-buten-1-ol through trickle-bed transposition

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Add 20g of 10%Ni / Al to a trickle bed reactor with an inner diameter of 12mm and a length of 40cm 2 o 3 Catalyst, the particle size of the catalyst is 10-20 mesh, start filling from the bottom of the reaction tube, the filling height is 25cm, and the filling density is 0.7g / cm 3 . Feed the raw material 3-methyl-3-buten-1-ol and oxygen continuously into the trickle bed reactor equipped with catalyst, at the reaction temperature of 50°C and the space velocity of 1.0 h -1 , the reaction was carried out under the condition that the oxygen-oil ratio was 0.05, and the liquid product was detected and analyzed by gas chromatography, the conversion rate was 70.1%, the selectivity was 98.8%, and the purity of the product prenol was 99.6% after the reaction liquid was rectified. . The catalyst is operated for a long period, and after 1000 hours, the conversion rate is 69.6-70.2%, the selectivity is 98.5-99.0%, and the purity of the product isopentenol is 99.5-99.6%, that is, the...

Embodiment 2-5

[0051] On the basis of Example 1, the type of catalyst was changed, and the results are shown in Table 1. Each catalyst was operated for a long period of time. After 1000 hours, the conversion rate fluctuated by ±0.3%, the selectivity fluctuated by ±0.2%, and the purity of the product isopentenol fluctuated by ±0.1%, that is, the catalyst had good stability.

[0052] Table 1 Effect of catalysts on reaction results

[0053]

Embodiment 6-16

[0055] On the basis of Example 1, with 10%V / TiO 2 As a catalyst, change the reaction conditions (reaction temperature, space velocity, oxygen-oil ratio), and the results are shown in Table 2. The catalysts in Table 2 were operated for a long period of time under different corresponding reaction conditions. After 1000 hours, the conversion rate fluctuated ±0.3%, the selectivity fluctuated ±0.2%, and the purity of the product prenol fluctuated ±0.1%, that is, the catalyst had Very good stability.

[0056] Table 2 Effect of reaction conditions on reaction results

[0057]

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Abstract

The invention provides a method for synthesizing 3-methyl-2-buten-1-ol from 3-methyl-3-buten-1-ol through trickle-bed transposition. The method comprises the following steps: introducing 3-methyl-3-buten-1-ol and an oxygen-containing atmosphere into a reactor, and carrying out a transposition reaction under the action of a non-noble metal supported catalyst. The catalytic reaction system is mild in reaction condition, high in raw material conversion rate, high in product selectivity and high in yield; wherein the raw material conversion rate is 62.7%-72.2%, the selectivity is 94.9%-99.2%, andthe yield is 59.5%-70.8%, and preferably, the raw material conversion rate is 69.8%-72.2%, the selectivity is 97.7%-99.2%, and the yield is 68.8%-70.8%. The catalyst is simple in component, is a non-noble metal catalyst and is low in cost; the reaction activity, selectivity and stability of the catalyst can be considered simultaneously.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and relates to a method for synthesizing isopentenol by trickle bed transposition of 3-methyl-3-buten-1-ol. Background technique [0002] Prenol, namely 3-methyl-2-buten-1-ol, is a colorless, transparent liquid with a strong ester aroma. It is mainly used for the synthesis of pyrethroids, the intermediates of pyrethroid insecticides with high efficiency and low toxicity, and its downstream products, permethrin and permethrin; in addition, it can also be used as an intermediate for the production of lemon Various fine chemical products and pharmaceuticals such as aldehydes, floral fragrances and vitamin A. [0003] According to the difference of reaction raw materials, the synthetic routes of isopentenol mainly contain following three kinds. [0004] Acetone method: through the alkynylation reaction of acetone and acetylene, in an alkaline system, ethynyl isopropanol is generat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/56C07C33/03B01J23/755B01J23/745B01J23/75B01J23/22B01J29/48
CPCB01J23/22B01J23/745B01J23/75B01J23/755B01J29/48C07C29/56C07C33/03
Inventor 李浩然马啸张玉霞陈志荣王勇于明马慧娟方万军
Owner SHANDONG NHU PHARMA
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