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Synthesis method of 2-propyl-2-heptenal

A synthetic method and technology of heptenal, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of low conversion rate of raw materials, difficulty in separation and purification, increase in production costs, etc., and achieve catalytic performance Good, high yield and purity, avoiding pollution effect

Active Publication Date: 2015-02-04
CHAMBROAD CHEM IND RES INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the industry uses liquid alkali catalyst sodium hydroxide to synthesize 2-propyl-2-heptenal, and its deficiency mainly lies in that a large amount of by-products will be generated, resulting in low conversion rate of raw materials, and due to the existence of a large amount of by-products, subsequent Difficulty in the separation and purification of lye, resulting in low product yield; at the same time, the liquid alkali catalyst will generate a large amount of waste water during the post-treatment process, causing great pollution to the environment, and the lye is highly corrosive to the equipment, which greatly increases the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Mix 120g of calcium nitrate aqueous solution with 200g of aluminum hydroxide dry glue, 6g of extrusion aid, 6g of pore expander, and 7.5g of binder, knead and extrude on the extruder, and then dry at 100°C for 4 hours, 600 Calcined at ℃ for 6 hours to obtain CaO / Al 2 o 3 180g of solid base catalyst, wherein the active ingredient calcium oxide accounts for 24% by mass of the catalyst.

[0032] A kind of synthetic method of 2-propyl group-2-heptenal, concrete steps comprise:

[0033] (1) In the reactor, add 500g of n-valeraldehyde and 100g of CaO / Al 2 o 3 Solid base catalyst, control the reaction temperature at 80°C, feed nitrogen at the same time, maintain the system pressure at 1MPa, react under heterogeneous conditions for 4 hours, and filter after the reaction to obtain filtrate and filter residue;

[0034] (2) Wash the filter residue obtained in step (1) with ethanol to obtain a catalyst, roast at 300°C for 4 hours for regeneration treatment, and set aside;

[0...

Embodiment 2

[0037] Mix 1.82Kg of sodium nitrate solution with 2.4Kg of aluminum hydroxide dry glue, 0.072Kg of extrusion aid, 0.048Kg of pore expander, and 0.084Kg of binder, knead and extrude on the extruder, and then dry at 80°C for 6 hour, calcination at 800°C for 4 hours to obtain Na 2 O / Al 2 o 3 The solid base catalyst is 1.89Kg, wherein the active component sodium oxide accounts for 20% by mass of the catalyst.

[0038] A kind of synthetic method of 2-propyl group-2-heptenal, concrete steps comprise:

[0039] (1) In the reactor, add 10Kg n-valeraldehyde and 1Kg Na 2 O / Al 2 o 3 Solid base catalyst, control the reaction temperature to 120°C, feed nitrogen at the same time, maintain the system pressure at 0.1MPa, react under heterogeneous conditions for 10 hours, filter after the reaction, and obtain filtrate and filter residue;

[0040] (2) Wash the filter residue obtained in step (1) with ethanol to obtain a catalyst, roast at 300°C for 4 hours for regeneration treatment, and s...

Embodiment 3

[0043] Mix 116g of magnesium nitrate solution with 142.5g of aluminum hydroxide dry glue and 7.5g of silicon dioxide, 3g of extrusion aid, 4.5g of pore-enlarging agent, and 4.5g of binder, knead and extrude on the extruder, and then pass through 100 ℃ drying for 4 hours, 450 ℃ calcination for 10 hours to get MgO / Al 2 o 3 -SiO 2 97g of solid base catalyst, wherein the active ingredient magnesium oxide accounted for 5% by mass of the catalyst.

[0044] A kind of synthetic method of 2-propyl group-2-heptenal, concrete steps comprise:

[0045] (1) In the reactor, add 500g n-valeraldehyde and 25g MgO / Al 2 o 3 -SiO 2 Solid base catalyst, control the reaction temperature at 180°C, feed nitrogen at the same time, maintain the system pressure at 2MPa, react under heterogeneous conditions for 0.5 hours, filter after the reaction, and obtain filtrate and filter residue;

[0046] (2) Wash the filter residue obtained in step (1) with ethanol to obtain a catalyst, roast at 300°C for 4...

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Abstract

The invention discloses a synthesis method of 2-propyl-2-heptenal, which is implemented through carrying out dimerization reaction by using a solid base catalyst at a specific mass ratio of a raw material n-valeraldehyde and the catalyst under the conditions of specific reaction temperature, reaction time and reaction pressure, wherein the reaction conditions are relatively mild, the requirements on equipment are low, the occurrence of side reaction can be reduced, and a target product 2-propyl-2-heptenal is produced, the conversion rate is as high as 98%, the product yield is over 95%, and the purity is above 98%. The catalyst adopted by the invention is the solid base catalyst; compared with a liquid catalyst, the post-treatment process of the solid base catalyst is simple, and reaction liquid is neutralized without an acid solution, thereby avoiding the environment pollution caused by spent acid wastewater; and the solid base catalyst can be repeatedly used after being subjected to regeneration treatment, thereby reducing the production cost.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a method for synthesizing 2-propyl-2-heptenal by using a solid base catalyst to catalyze n-valeraldehyde. Background technique [0002] 2-Propyl-2-heptenal is an important intermediate for the synthesis of 2-propylheptanol (2-PH). With the improvement of people's safety awareness, 2-PH has attracted more and more attention, and will become a production The preferred synthetic raw material for plasticizers. At present, the industry uses liquid alkali catalyst sodium hydroxide to synthesize 2-propyl-2-heptenal, and its deficiency mainly lies in that a large amount of by-products will be generated, resulting in low conversion rate of raw materials, and due to the existence of a large amount of by-products, subsequent Separation and purification of lye is difficult, resulting in low product yield; at the same time, the liquid alkali catalyst will generate a large amount of waste wate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/21C07C45/74
CPCY02P20/584
Inventor 姜雪丽侯晓峰刘振学牟庆平栾波姚刚
Owner CHAMBROAD CHEM IND RES INST CO LTD
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