Preparation method and product of adipate epoxy plasticizer

Abstract

The invention discloses a preparation method of adipate epoxy plasticizer, which comprises the following steps: (1) extracting fatty acid in vegetable oil leftovers; (2) performing reduction reaction on the obtained long-chain fatty acid under the catalytic reduction action of lithium aluminum hydride, thus obtaining long-chain fatty alcohol; (3) mixing the long-chain fatty alcohol and adipic acid, and adding a reverse micelle nano aluminum oxide catalyst, thus obtaining a system solution containing adipic acid di(long-chain fatty ester); (4) performing epoxy reaction, thus obtaining a finished product solution; and (5) introducing chlorine gas into the epoxy finished product solution, simultaneously performing ultraviolet irradiation until the chlorination reaction is completed, and then treating to obtain the modified epoxy plasticizer. The invention also discloses the epoxy plasticizer prepared by the method. According to the invention, the long-chain alcohol group is introduced into the molecular structure of the adipic acid, so that the plasticizing efficiency of the product is greatly improved, the raw material cost is low, and the comprehensive recovery of the vegetable oil leftovers is realized; and meanwhile, the epoxy group in the plasticizer enhances the heat resistance, stability and compatibility of the product.

Description

technical field

[0001] The invention belongs to the field of fine chemicals, and particularly relates to a preparation method of an adipate epoxy plasticizer and the prepared plasticizer. Background technique

[0002] Dioctyl adipate plasticizer is widely recognized due to its good cold resistance, but due to its poor compatibility and long-term storage will produce oil, so it can only be used as an auxiliary plasticizer . Traditional cold-resistant plasticizers are based on octanol, which is derived from petroleum products. With the increasing depletion of petroleum resources, it is the general trend to find alternative bio-renewable resources.

[0003] Epoxy plasticizer is a new type of environmentally friendly plasticizer that has emerged in recent years, and it is becoming more and more popular. Because epoxy grease has good heat resistance, stability and compatibility, it can play a role in The dual function of stabilizer and plasticizer, the synthesis of epoxy plast...

Examples

Embodiment 1

[0043] Dissolve azobenzene in 100ml of n-heptane / n-butanol mixed solvent, the volume ratio of mixed solvent n-heptane / n-butanol is 10:1, and the concentration is 1×10 -6 mol / L solution, and then sonicated for 30 min.

[0044] At room temperature, add the prepared sodium aluminate aqueous solution with a mass percentage concentration of 5% dropwise with a dropper, add it to saturation and end when it is not turbid (about 9g), and continue to ultrasonically vibrate for 30min after adding to accelerate. The micelles are formed, and the micelle structure is stabilized, and then the ultrasonic reaction is continued for 1 hour while carbon dioxide is introduced into it.

[0045] Add concentrated sulfuric acid (the amount of added sulfuric acid is 16% of the soapstock weight) dropwise to the raw vegetable oil residue, control the pH of the solution in the range of about 2-3, stir for 3h, use ethanol as an extractant to extract the fatty acid, and the amount of ethanol About 500 mL, ...

Embodiment 2

[0050] Dissolve azobenzene in 100ml of n-heptane / n-butanol mixed solvent, the volume ratio of mixed solvent n-heptane / n-butanol is 10:1, and the concentration is 2×10 -5 mol / L solution, and then sonicated for 30 min.

[0051] At room temperature, add the prepared sodium aluminate aqueous solution with a mass percentage concentration of 7% dropwise with a dropper, add it to saturation and end when it is not turbid (about 6g), and continue to ultrasonically vibrate for 45min after the addition to accelerate. The micelles are formed and the micelle structure is stabilized, and then the ultrasonic reaction is continued for 2 hours while carbon dioxide is introduced into it.

[0052] Add concentrated sulfuric acid (the amount of added sulfuric acid is 16% of the soapstock weight) dropwise to the raw vegetable oil residue, control the pH of the solution in the range of about 2-3, stir for 3h, use ethanol as an extractant to extract the fatty acid, and the amount of ethanol About 50...

Embodiment 3

[0057] Dissolve azobenzene in 100ml of n-heptane / n-butanol mixed solvent, the molar ratio of mixed solvent n-heptane / n-butanol is 10:1, and the mass percentage concentration is 6×10 -4 mol / L solution, and then sonicated for 30 min. At room temperature, add the prepared sodium aluminate aqueous solution with a concentration of 10% dropwise with a dropper, add it to saturation and end when it is not turbid (about 6g), and continue to ultrasonically shake for 60min after the addition to accelerate the micelles. The micelle structure is formed and stabilized, and then the ultrasonic reaction is continued for 3 hours while carbon dioxide is introduced into it, and the reaction temperature is 60° C. The desired catalyst-reverse micelle nano-alumina catalyst can be obtained.

[0058] Add concentrated sulfuric acid (the amount of added sulfuric acid is 16% of the soapstock weight) dropwise to the raw vegetable oil residue, control the pH of the solution in the range of about 2-3, stir...

technical field

[0001] The invention belongs to the field of fine chemicals, and particularly relates to a preparation method of an adipate epoxy plasticizer and the prepared plasticizer. Background technique

[0002] Dioctyl adipate plasticizer is widely recognized due to its good cold resistance, but due to its poor compatibility and long-term storage will produce oil, so it can only be used as an auxiliary plasticizer . Traditional cold-resistant plasticizers are based on octanol, which is derived from petroleum products. With the increasing depletion of petroleum resources, it is the general trend to find alternative bio-renewable resources.

[0003] Epoxy plasticizer is a new type of environmentally friendly plasticizer that has emerged in recent years, and it is becoming more and more popular. Because epoxy grease has good heat resistance, stability and compatibility, it can play a role in The dual function of stabilizer and plasticizer, the synthesis of epoxy plast...

Examples

Embodiment 1

[0043] Dissolve azobenzene in 100ml of n-heptane / n-butanol mixed solvent, the volume ratio of mixed solvent n-heptane / n-butanol is 10:1, and the concentration is 1×10 -6 mol / L solution, and then sonicated for 30 min.

[0044] At room temperature, add the prepared sodium aluminate aqueous solution with a mass percentage concentration of 5% dropwise with a dropper, add it to saturation and end when it is not turbid (about 9g), and continue to ultrasonically vibrate for 30min after adding to accelerate. The micelles are formed, and the micelle structure is stabilized, and then the ultrasonic reaction is continued for 1 hour while carbon dioxide is introduced into it.

[0045] Add concentrated sulfuric acid (the amount of added sulfuric acid is 16% of the soapstock weight) dropwise to the raw vegetable oil residue, control the pH of the solution in the range of about 2-3, stir for 3h, use ethanol as an extractant to extract the fatty acid, and the amount of ethanol About 500 mL, ...

Embodiment 2

[0050] Dissolve azobenzene in 100ml of n-heptane / n-butanol mixed solvent, the volume ratio of mixed solvent n-heptane / n-butanol is 10:1, and the concentration is 2×10 -5 mol / L solution, and then sonicated for 30 min.

[0051] At room temperature, add the prepared sodium aluminate aqueous solution with a mass percentage concentration of 7% dropwise with a dropper, add it to saturation and end when it is not turbid (about 6g), and continue to ultrasonically vibrate for 45min after the addition to accelerate. The micelles are formed and the micelle structure is stabilized, and then the ultrasonic reaction is continued for 2 hours while carbon dioxide is introduced into it.

[0052] Add concentrated sulfuric acid (the amount of added sulfuric acid is 16% of the soapstock weight) dropwise to the raw vegetable oil residue, control the pH of the solution in the range of about 2-3, stir for 3h, use ethanol as an extractant to extract the fatty acid, and the amount of ethanol About 50...

Embodiment 3

[0057] Dissolve azobenzene in 100ml of n-heptane / n-butanol mixed solvent, the molar ratio of mixed solvent n-heptane / n-butanol is 10:1, and the mass percentage concentration is 6×10 -4 mol / L solution, and then sonicated for 30 min. At room temperature, add the prepared sodium aluminate aqueous solution with a concentration of 10% dropwise with a dropper, add it to saturation and end when it is not turbid (about 6g), and continue to ultrasonically shake for 60min after the addition to accelerate the micelles. The micelle structure is formed and stabilized, and then the ultrasonic reaction is continued for 3 hours while carbon dioxide is introduced into it, and the reaction temperature is 60° C. The desired catalyst-reverse micelle nano-alumina catalyst can be obtained.

[0058] Add concentrated sulfuric acid (the amount of added sulfuric acid is 16% of the soapstock weight) dropwise to the raw vegetable oil residue, control the pH of the solution in the range of about 2-3, stir...

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