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Epoxy anacardol acetic acid ester plasticizer and preparation method thereof

A cardanol-based acetate and plasticizer technology, which is applied in the field of epoxy plasticizer preparation, can solve the problems of low temperature resistance, poor compatibility and the like, and achieves high epoxy value and excellent plasticizing performance. , the effect of reducing the reaction time

Inactive Publication Date: 2013-10-09
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the performance defects of traditional epoxy fatty acid methyl esters such as poor compatibility and low temperature resistance, the invention discloses an epoxy cardanyl acetate plasticizer and a preparation method thereof, which is composed of a magnetic heteropoly acid solid catalyst Catalyzed preparation of cardanol, the raw material is cashew oil, a wide range of sources, the catalyst has the advantages of environmental protection, easy to recycle, etc.

Method used

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  • Epoxy anacardol acetic acid ester plasticizer and preparation method thereof
  • Epoxy anacardol acetic acid ester plasticizer and preparation method thereof
  • Epoxy anacardol acetic acid ester plasticizer and preparation method thereof

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Embodiment 1

[0053] Step 1, the preparation of the magnetic core: FeCl with a mass ratio of 1:3.3 3 with FeCl 2 Dissolve in distilled water, blow nitrogen, at 500r·min -1 Under the rotating speed, add ammonia water drop by drop until the pH is 12, raise the temperature to 60°C, stir and mature for 1 hour, let it stand, and separate Fe with a strong magnet 3 o 4 Particles were washed repeatedly with distilled water until neutral to obtain the magnetic core Fe 3 o 4 .

[0054] Step 2, SiO 2 Preparation of modified magnetic core: 1g magnetic core Fe 3 o 4 Add 50mL of isopropanol, stir vigorously for 30min, then ultrasonically disperse for 15min, add 150mL of isopropanol, 10mL of deionized water, and stir for 15 minutes. Add 1-6 mL tetraethyl orthosilicate dropwise at 25°C, and at the same time adjust the pH to 10.5 with ammonia water. After the dropwise addition was complete, stirring was continued at 40°C for 12 hours. Then, settle naturally and wash with deionized water and ethano...

Embodiment 2

[0060] Step 1, the preparation of magnetic core: FeCl with a mass ratio of 1:3.3 3 with FeCl 2 Dissolve in distilled water, blow nitrogen, at 500r·min -1 Under the rotating speed, add ammonia water drop by drop until the pH is 12, raise the temperature to 60°C, stir and mature for 1 hour, let it stand, and separate Fe with a strong magnet 3 o 4 Particles were washed repeatedly with distilled water until neutral to obtain the magnetic core Fe 3 o 4 .

[0061] Step 2, SiO 2 Preparation of modified magnetic core: 1g magnetic core Fe 3 o 4Add 50mL of isopropanol, stir vigorously for 30min, then ultrasonically disperse for 15min, add 150mL of isopropanol, 10mL of deionized water, and stir for 15 minutes. Add 1-6 mL tetraethyl orthosilicate dropwise at 25°C, and at the same time adjust the pH to 10.5 with ammonia water. After the dropwise addition was complete, stirring was continued at 40°C for 12 hours. Then, settle naturally and wash with deionized water and ethanol unt...

Embodiment 3

[0067] Step 1, preparation of magnetic core: weigh 1.874g FeCl 2 4H 2 O and 4.7 g FeCl 3 ·6H 2 O, dissolved in 150ml of water, put into a four-neck bottle. in N 2 Under protection, heat to 60°C, dissolve 3.0g NaOH in 80ml water, add quickly, stir at high speed, and add 6.0g oleic acid at the same time. After 30 minutes of heat preservation, the temperature was raised to 90°C and aged for 45 minutes. Cool to room temperature and disperse the precipitate with cyclohexane to obtain a stable dispersed magnetic core Fe3O4 suspension.

[0068] Step 2, SiO 2 Preparation of Modified Magnetic Cores: Fe Dispersed into Cyclohexane 3 o 4 Add 20ml tetraethyl orthosilicate solution to the suspension, and ultrasonically disperse for 15min. Transfer the mixture to a four-necked bottle, stir well, and N 2 Under the atmosphere, add 22ml of ammonia water dropwise, stir for 6 hours to ensure complete hydrolysis of orthosilicate, filter with suction, and dry the particles in a vacuum ove...

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Abstract

The invention discloses an epoxy anacardol acetic acid ester plasticizer and a preparation method thereof. The method comprises the following steps of: with anacardol and acetic anhydride as raw materials, performing a reaction under catalysis of solid alkali to generate anacardol acetic acid ester; then, under catalysis of a magnetic heteropolyacid solid catalyst, dropwise adding an organic oxide liquor for reaction to obtain a reactant; separating and recovering the catalyst by a magnetic field; and processing a coarse product to obtain the epoxy anacardol acetic acid ester plasticizer. The magnetic heteropolyacid solid catalyst has a nuclear shell structure, wherein a magnetic core is nanoscale SiO2-Fe3O4, and the active component is phosphotungstic heteropoly acid which is structured as HPWA / SiO2-Fe3O4, and the magnetic particle size distribution is 50-100nm, so that the plasticizer is of superparamagnetism. The method is wide in source of raw materials which are regenerative. The catalyst is high in activity and easy to separate. Double bonds in the anacardol are epoxidized and acetylated by phenolic hydroxyl group, so that the epoxy anacardol acetic acid ester plasticizer is prevented from generating color change in the storage process, and the epoxy anacardol acetic acid ester plasticizer is high in epoxide number, shallow in luster and excellent in plasticizing performance.

Description

technical field [0001] The invention belongs to the field of preparation of epoxy plasticizers, and in particular relates to a method for preparing epoxy cardanol-based acetate plasticizers by using cardanol as a raw material and applying a magnetic solid acid catalyst. Background technique [0002] Phthalic plasticizers are the most used additives in plastic processing, accounting for about 90% of plasticizers. However, during the application process, it was found that phthalic acid plasticizers have persistent reproductive toxicity. In October 2008, the European Chemicals Agency explicitly banned the use in industries such as electronics, food, daily necessities and toys. How to develop green, environmentally friendly and non-toxic plasticizers that can replace phthalic acid is now a hot spot of global concern. [0003] The world has accelerated the research and development of non-toxic plasticizer products, especially the basic application research of plastic products wit...

Claims

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Application Information

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IPC IPC(8): C08K5/1515C07D303/16C07D301/14C08L63/00B01J31/28
CPCY02P20/584
Inventor 聂小安刘振兴米桢陈洁常侠
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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