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Method for continuously synthesizing tetradecyl acrylate through microwave-micro reactor catalysis

A technology of tetradecyl acrylate and micro-reactor, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve problems such as unsafe production process, sulfuric acid corrosion equipment, inaccurate temperature control, etc. Achieve the effect of reducing difficulty, improving purity and penetrating

Inactive Publication Date: 2019-04-12
XIAN UNITED PRESSURE VESSEL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the most common and convenient method for preparing tetradecyl acrylate is the direct esterification method. For a long time, concentrated sulfuric acid has been used as a catalyst in the synthesis of esters. The existing problems are: low yield; inaccurate temperature control, prone to "flying temperature" Phenomenon, the production process is unsafe, the cycle is long and discontinuous, and the operation is troublesome; there are many side reactions, the post-processing is difficult, and sulfuric acid seriously corrodes the equipment

Method used

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  • Method for continuously synthesizing tetradecyl acrylate through microwave-micro reactor catalysis
  • Method for continuously synthesizing tetradecyl acrylate through microwave-micro reactor catalysis
  • Method for continuously synthesizing tetradecyl acrylate through microwave-micro reactor catalysis

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Embodiment 1

[0038] The method of the present embodiment comprises the following steps:

[0039] Step 1. Put 50 g of tetradecyl alcohol in a water bath to heat and melt into a liquid, and then transfer it to the raw material mixed liquid beaker 1; the tetradecyl alcohol is a commercially available analytical reagent; the temperature of the water bath is 70° C.;

[0040] Step 2: Add 0.421g of hydroquinone and 0.561g of p-toluenesulfonic acid into the raw material mixed liquid beaker 1 filled with myristyl alcohol liquid in step 1, and then place the raw material mixed liquid beaker 1 in an ultrasonic oscillator for vibration and stirring , so that the solid particles are completely dissolved to obtain a mixed solution; the temperature of the shaking and stirring is 35° C., and the time is 4 minutes;

[0041] Step 3, adding 20.17g of acrylic acid and 45g of p-xylene to the mixed solution obtained in step 2, and then stirring evenly to obtain a raw material mixed solution; the stirring time i...

Embodiment 2

[0048] The method of the present embodiment comprises the following steps:

[0049] Step 1. Put 50 g of tetradecyl alcohol in a water bath to heat and melt into a liquid, and then transfer it to the raw material mixed liquid beaker 1; the tetradecyl alcohol is a commercially available analytical reagent; the temperature of the water bath is 70° C.;

[0050] Step 2: Add 0.431g of hydroquinone and 0.575g of p-toluenesulfonic acid into the raw material mixed liquid beaker 1 filled with myristyl alcohol liquid in step 1, and then place the raw material mixed liquid beaker 1 in an ultrasonic oscillator for vibration and stirring , so that the solid particles are completely dissolved to obtain a mixed solution; the temperature of the shaking and stirring is 35° C., and the time is 4 minutes;

[0051] Step 3, adding 21.85g of acrylic acid and 45g of p-xylene to the mixed solution obtained in step 2, and then stirring evenly to obtain a raw material mixed solution; the stirring time i...

Embodiment 3

[0056] The method of the present embodiment comprises the following steps:

[0057] Step 1. Put 50 g of tetradecyl alcohol in a water bath to heat and melt into a liquid, and then transfer it to the raw material mixed liquid beaker 1; the tetradecyl alcohol is a commercially available analytical reagent; the temperature of the water bath is 70° C.;

[0058] Step 2: Add 0.426g of hydroquinone and 0.568g of p-toluenesulfonic acid into the raw material mixed liquid beaker 1 filled with myristyl alcohol liquid in step 1, and then place the raw material mixed liquid beaker 1 in an ultrasonic oscillator for vibration and stirring , so that the solid particles are completely dissolved to obtain a mixed solution; the temperature of the shaking and stirring is 35° C., and the time is 4 minutes;

[0059] Step 3, adding 21.01g of acrylic acid and 45g of p-xylene to the mixed solution obtained in step 2, and then stirring evenly to obtain a raw material mixed solution; the stirring time i...

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Abstract

The invention discloses a method for continuously synthesizing tetradecyl acrylate through microwave-micro reactor catalysis, which comprises the following steps of: 1, heating and melting tetradecanol into liquid; 2, adding hydroquinone and p-toluenesulfonic acid into the tetradecanol liquid, and shaking and stirring to obtain a mixed solution; 3, adding acrylic acid and paraxylene into the mixedsolution, and uniformly stirring to obtain a raw material mixed liquid; 4. turning on microwave-micro reactor equipment, and then conveying the raw material mixed liquid into a capillary tube for esterification reaction to obtain a product; 5, distilling the product under reduced pressure to remove the paraxylene, and sequentially washing, neutralizing and drying the obtained crude product to obtain tetradecyl acrylate. According to the method, the raw material mixed liquid for synthesizing the tetradecyl acrylate generates a vortex effect through microwave synergistic heating, so that the heat transfer and mass transfer performances are improved, the reaction temperature is effectively and accurately controlled, the selectivity of esterification reaction is improved, the difficulty of post-treatment procedures is reduced, the purity of the product tetradecyl acrylate is improved and continuous production can be achieved.

Description

technical field [0001] The invention belongs to the technical field of chemical organic synthesis, and in particular relates to a method for continuously synthesizing myristyl acrylate by using a microwave-microreactor to catalyze. Background technique [0002] The reaction of acrylic acid and higher-carbon alkyl esters under specific conditions to synthesize higher-carbon alkyl acrylates is a very important class of chemical industrial reactions in the acrylic acid industry, and the synthesis of tetradecyl acrylate from acrylic acid and myristyl alcohol is one of the important ones. Myristyl acrylate, as one of the excellent functional macromolecular monomers in the field of acrylic acid industrial application, has a wide range of applications in the field of fine chemicals: a) as a modified monomer for coatings, adhesives, paper corrosion agents, suspension dispersants , building sealant, etc. to modify it to have lower shrinkage and higher flexibility; b) The copolymer ob...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/54
CPCC07C67/08C07C69/54
Inventor 杨哲叶建林郗大来李宁袁敏哲
Owner XIAN UNITED PRESSURE VESSEL CO LTD
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