Method for preparing vegetable oil-based plasticizer by micro-reaction continuous flow by using amido

A vegetable oil-based and amide-based technology, which is applied in the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problem that the miscibility of pure epoxy soybean oil and epoxy resin cannot exert plasticizing performance and instability Migration resistance and volatility of the three-membered ring, etc., to achieve the effects of avoiding intense heat release for a long time, optimizing the synthesis process, and improving mass and heat transfer efficiency

Active Publication Date: 2019-01-25
CHINA PETROLEUM & CHEM CORP
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Problems solved by technology

However, epoxy soybean oil also has many shortcomings. The unstable three-membered ring in the structure makes its migration resistance and volatility have certain problems, especially the miscibility between pure epoxy soybean oil and epoxy resin is not very good and cannot be used. It has the best plasticizing performance, but the epoxy group and flexible long chain of epoxy soybean oil make it have good modification conditions

Method used

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  • Method for preparing vegetable oil-based plasticizer by micro-reaction continuous flow by using amido
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  • Method for preparing vegetable oil-based plasticizer by micro-reaction continuous flow by using amido

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preparation example Construction

[0036] The preparation steps of the inventive method are:

[0037] Step 1: dissolving epoxidized soybean oil in an organic solvent to obtain a solution A, dissolving an amide ring-opening reagent and a ring-opening reaction catalyst in an organic solvent to obtain a solution B;

[0038] Step 2: The solution A and solution B obtained in step 1 are simultaneously pumped into the first mixer of the micro-reaction device to mix, and then enter the first micro-reactor of the micro-reaction device to react to obtain the ring-opened product of epoxidized soybean oil;

[0039] Step 3: Dissolve the acetylation reagent and acetylation reaction catalyst in an organic solvent to obtain solution C, and simultaneously pump the epoxidized soybean oil ring-opening product obtained in step 2 into the second mixer of the micro-reaction device for mixing, and then enter the micro-reaction The reaction is carried out in the second microreactor of the device, and the reaction product is obtained b...

Embodiment 1

[0043] Dilute epoxidized soybean oil with THF as one phase into the syringe pump, dissolve acetamide in THF, add sodium ethoxide as the other phase into the syringe pump, inject the two phases into the microreactor at the same time, and react at 50°C 15min, wherein the mol ratio of epoxy compound and acetamide in epoxy soybean oil is 1:5, two-phase flow velocity is respectively 0.146,0.054, and the mol ratio of the epoxy compound in catalyst sodium ethylate and epoxy soybean oil is 0.01: 1. The obtained epoxy soybean oil ring-opening product continues to pass into another section of microreactor, mixed with acetic anhydride and catalyst perchloric acid as another phase, passes through the microreactor, and reacts at 10°C for 15min, wherein the epoxy large The molar ratio of soybean oil ring-opening products to acetic anhydride was 1:5, and the molar ratio of perchloric acid to epoxidized soybean oil ring-opening products was 0.2:1. The pH of the product is adjusted to about 7 ...

Embodiment 2

[0045] Dilute epoxidized soybean oil with THF as one phase into the syringe pump, dissolve acetamide in THF, add sodium ethoxide as the other phase into the syringe pump, inject the two phases into the microreactor at the same time, and react at 100°C 10min, wherein the mol ratio of epoxy compound and acetamide in epoxy soybean oil is 1:10, two-phase flow velocity is respectively 0.176,0.074, the mol ratio of the epoxy compound in catalyst sodium ethylate and epoxy soybean oil is 0.08: 1. The obtained epoxy soybean oil ring-opening product continues to pass into another section of micro-reactor, mixed with acetic anhydride and catalyst perchloric acid as another phase, passes through the micro-reactor, and reacts at 25°C for 10 minutes, wherein the epoxy large The molar ratio of soybean oil ring-opening product to acetic anhydride was 1:10, and the molar ratio of perchloric acid to epoxidized soybean oil ring-opening product was 0.08:1. The pH of the product is adjusted to abo...

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Abstract

The invention discloses a method for preparing a vegetable oil-based plasticizer by micro-reaction continuous flow by using amido, which comprises the steps of dissolving epoxy soybean oil in an organic solvent to obtain a solution A, dissolving an amide ring-opening reagent and a ring-opening reaction catalyst in an organic solvent to obtain a solution B, pumping the solution A and the solution Bsimultaneously into a first mixer of a microreactor to mix, enabling the mixture to enter a first microreactor of the microreaction device and react to obtain an epoxy soybean oil ring-opening product, dissolving an acetylation reagent and an acetylation reaction catalyst in an organic solution to obtain a solution C, simultaneously pumping with the epoxy soybean oil ring-opening product into a second mixer of the microreaction device to mix, enabling the mixture to enter a second microreactor of the microreaction device to react, and performing rotary evaporation a reaction product to obtainthe vegetable oil-based plasticizer. Compared with a conventional preparation process, the method has the advantages that the specificity of an amide group is utilized and combined with the micro-reaction continuous flow device, and the new plasticizer with superior performance is prepared by the ring-opening reaction and the acetylation reaction in sequence,.

Description

technical field [0001] The invention relates to a method in which amide groups are applied to vegetable oil-based plasticizers for micro-reaction continuous flow preparation, and belongs to the field of chemical synthesis. Background technique [0002] Epoxy soybean oil (ESO) is a common plasticizer and stabilizer. Its main features are low price, green and environmental protection. In addition, it has better compatibility with PVC resin, which makes it more stable than other plasticizers. more prominent. However, epoxy soybean oil also has many shortcomings. The unstable three-membered ring in the structure makes its migration resistance and volatility have certain problems, especially the miscibility between pure epoxy soybean oil and epoxy resin is not very good and cannot be used. It has the best plasticizing performance, but the epoxy group and flexible long chain of epoxidized soybean oil make it have good modification conditions. [0003] Many amide compounds themse...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/12C07C233/83C07C233/47C07D209/48
CPCC07C231/12C07D209/48C07C233/83C07C233/47
Inventor 郭凯周宇方正刘成扣胡欣段金电邱江凯欧阳平凯
Owner CHINA PETROLEUM & CHEM CORP
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