Method for preparing 1,9-decadiene by using fixed-bed reactor

A fixed-bed reactor and decadiene technology, applied in the chemical industry, can solve the problems of expensive catalyst, complex reaction conditions, complex production conditions, etc., and achieve the effects of good industrial application value, high product purity, and high raw material utilization rate.

Active Publication Date: 2021-11-05
宁波永顺精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. Patent US20140155666 report: using unsaturated fatty acid 10-undecylenic acid as raw material, PdCl 2 (PPh 3 ) 2 As a catalyst, a decarboxylation reaction occurs, and the yield of 1,9-decadiene is only 59%, and the catalyst is expensive and the production conditions are complicated
[0005] 2. Literature (Synthesis, 2012, 44(19): 3003-3005) reports: using dodecanedioic acid as raw material, PdCl 2 (PPh 3 ) 2 As a catalyst, decarboxylation reaction occurs above 190 ° C, and the yield of 1,9-decadiene is only 55%. Like the above method, the production cost is high and the reaction conditions are complicated
This method consumes a large amount of catalyst and causes solid waste

Method used

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  • Method for preparing 1,9-decadiene by using fixed-bed reactor
  • Method for preparing 1,9-decadiene by using fixed-bed reactor
  • Method for preparing 1,9-decadiene by using fixed-bed reactor

Examples

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Effect test

example 1

[0036] Example 1, a reaction device, such as figure 1 As shown, it includes a dripping device 1, a connecting pipe 2, a fixed bed reactor 3 and a collection container 4 connected in sequence from top to bottom;

[0037] The collection container 4 is provided with a spherical condensation pipe 41, and the effect of the spherical condensation pipe 41 is to condense the discharge of gas discharged from the bottom of the fixed bed reactor 3; the fixed bed reactor 3 is heated in parallel with electric coils, and the fixed bed reactor 3 is provided There is a thermocouple 31, and this thermocouple 31 is used to display the temperature in the fixed-bed reactor 3 in real time.

[0038] A filler is arranged in the fixed bed reactor 3, and the filler is a glass Raschig ring filler with a particle size of 3±0.5mm. The temperature in the fixed-bed reactor 3 is 350-450°C. The purpose of controlling the temperature in the fixed-bed reactor 3 is to realize the pyrolysis reaction of the est...

Embodiment 1

[0050] Embodiment 1, a kind of method utilizing fixed bed reactor to prepare 1,9-decadiene, carries out following steps successively:

[0051] 1) Mix 34.8g (0.2mol) of 1,10-decanediol with 48g (0.8mol, 4eq) of acetic acid and place it in a 250mL reaction bottle as a reaction solution, raise the temperature to 115°C for esterification reaction, esterification reaction The steamed water is discharged in real time; after 4 hours of the esterification reaction, no water is produced, and at this time, the temperature is raised to 200°C to steam the acetic acid and recover the acetic acid;

[0052] When the acetic acid is no longer distilled out, the temperature is lowered to room temperature to obtain an esterification intermediate product;

[0053] 2), the esterification intermediate product is put into the dripping device 1, and the esterification intermediate product is dripped into the fixed bed reactor 3 through the connecting pipe 2 in the form of dripping (about 10g / h droppi...

Embodiment 2

[0061] Embodiment 2, a kind of method utilizing fixed bed reactor to prepare 1,9-decadiene, carries out following steps successively:

[0062] 1), with embodiment 1 step 1);

[0063] 2), the temperature in the fixed-bed reactor 3 remains unchanged at 450°C, and the drop rate of the esterification intermediate product is changed, so that the reaction space velocity is changed from 16.7h -1 changed to 8.3h -1 ; All the other are equal to the same embodiment 1 step 2);

[0064] 3), the same as step 3) of Example 1; 25.0 g of 1,9-decadiene product (purity 99.1%) was obtained, and the yield was 90.7%;

[0065] 4), the same as step 4) of Example 1; 24.8 g of 1,9-decadiene product (purity: 98.8%) was obtained, and the yield was 90.0%.

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Abstract

The invention discloses a method for preparing 1,9-decadiene using a fixed-bed reactor, which comprises the following steps in sequence: mixing 1,10-decanediol and acetic acid to form a reaction solution for esterification; The esterification intermediate product enters the fixed-bed reactor in the form of dropping to carry out the ester pyrolysis reaction, and the reaction product is collected by the collection container; the collected reaction product is left to stand for layering, and the upper layer is taken for vacuum distillation to obtain 1, 9-Decadiene; lower layer is recovered acetic acid. Adopting the method of the present invention to prepare 1,9-decadiene has high raw material utilization rate, good reaction yield and selectivity, avoids the use of expensive catalysts, not only reduces the discharge of three wastes, reduces production costs, but also has high product purity, The yield is high, the energy consumption is small, and the method has good industrial application value.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a preparation method of organic compound 1,9-decadiene. Background technique [0002] 1,9-Decadiene is an important fine chemical intermediate, its structural formula is as follows: [0003] At present, the synthesis process of 1,9-decadiene mainly includes the following types: [0004] 1. Patent US20140155666 report: using unsaturated fatty acid 10-undecylenic acid as raw material, PdCl 2 (PPh 3 ) 2 As a catalyst, a decarboxylation reaction occurs, and the yield of 1,9-decadiene is only 59%, and the catalyst is expensive and the production conditions are complicated. [0005] 2. Literature (Synthesis, 2012, 44(19): 3003-3005) reports: using dodecanedioic acid as raw material, PdCl 2 (PPh 3 ) 2 As a catalyst, the decarboxylation reaction occurs above 190°C, and the yield of 1,9-decadiene is only 55%. Like the above method, the production cost is high and the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C11/12C07C1/20C07C7/04C07C69/16C07C67/08
CPCC07C1/20C07C7/04C07C67/08C07C69/16C07C11/12
Inventor 韦隆武毛崇智张小莲陈新发
Owner 宁波永顺精细化工有限公司
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