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Citric ester plasticizer and preparation method thereof

A citric acid ester and plasticizer technology, which is applied in the fields of environmentally friendly and non-toxic citric acid ester plasticizers, additives or auxiliary agents, food packaging plastics, medical equipment and children's toys, can solve the problem of high volatility and the impact of citric acid Problems such as the range of use of ester plasticizers, easy precipitation and migration, etc., to achieve the effect of improving processing performance and product performance, facilitating industrial production, and expanding the scope of application

Active Publication Date: 2014-05-21
HENAN ZHENGTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although tributyl citrate (TBC), acetyl tributyl citrate (ATBC), and triethyl citrate (TEC) have excellent plasticizing effects and good cold resistance, light resistance, water resistance, and enzyme resistance , but compared with phthalate plasticizers, there are problems such as easy precipitation and migration, and its volatility is relatively large, which affects the scope of use of citrate plasticizers

Method used

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  • Citric ester plasticizer and preparation method thereof
  • Citric ester plasticizer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 250Kg of citric acid, 455Kg of glyceryl monostearate and 370Kg of n-butanol into the reaction kettle, add 8.5Kg of p-toluenesulfonic acid, heat to 110-130°C under normal pressure, and carry out reflux esterification reaction through the water separator , 5-6 hours measured acid value less than 5.0 can stop the reaction. Then raise the temperature to 160-170°C under vacuum, and distill off about 180Kg of excess n-butanol (which can be recycled). After cooling down to 50-60°C, add 270Kg of acetic anhydride, and carry out the acetylation reaction at 100-125°C. After 2-3 hours, the reaction is complete and the by-product acetic acid is distilled out under vacuum. After neutralization, washing, drying and other refining processes, the reaction end point is controlled by measuring the acid value, saponification value, and hydroxyl value. After meeting the requirements, it can be filtered and packaged to become the finished product of acetylated glyceryl citrate monosteara...

Embodiment 2

[0021] In the reaction kettle, react 195Kg of measured citric acid with 350 Kg of glyceryl monostearate to generate glyceryl monostearate of citric acid, add 180Kg of ethanol, add 5Kg of sulfuric acid dropwise under stirring, and heat to 110-120°C , carry out the reflux esterification reaction, and the acid value measured in 8-9 hours is less than 3.0 to stop the reaction. Then raise the temperature to 170-180°C, and distill off about 90Kg of excess ethanol (which can be recycled). After cooling down to 50-60°C, add 210Kg of acetic anhydride, and carry out acetylation reaction at 100-125°C. After 2-3 hours of complete reaction, turn on vacuum to distill out the by-product acetic acid. After neutralization, washing, drying and other refining processes, the reaction end point is controlled by measuring the acid value, saponification value, and hydroxyl value. After meeting the requirements, it can be filtered and packaged to become the finished product of acetylated glyceryl cit...

Embodiment 3

[0023] Add 230Kg of citric acid, 330Kg of glyceryl monolaurate and 310Kg of n-hexanol into the reaction kettle, add 8Kg of p-toluenesulfonic acid, heat to 140-150°C under vacuum, and carry out reflux esterification reaction through the water separator, 6 The reaction can be stopped if the acid value measured in -7 hours is less than 5.0. Then raise the temperature to 140-150°C under vacuum, and distill off about 120Kg of excess n-hexanol (which can be recycled). After cooling down to 50-60°C, add 250Kg of acetic anhydride, and carry out acetylation reaction at 120-130°C. After 2-3 hours, turn on the vacuum to distill out the by-product acetic acid. After neutralization, washing, drying and other refining processes, the reaction end point is controlled by measuring the acid value, saponification value, and hydroxyl value. After meeting the requirements, it can be filtered and packaged to become the finished product of acetylated monolaurin citrate. The conversion rate is 94.6%...

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Abstract

The invention discloses a citric ester plasticizer and a preparation method thereof, belonging to the fields of plastic aids. The citric ester plasticizer is acetyl monoglyceride citrate and has the structure as shown in specifications, wherein n is 1 to 7 and m is 6 to 16. A glycerin fatty acid ester long-chain structure is inserted into the acetyl monoglyceride citrate of the plasticizer, so compared with the traditional citric ester plasticizers (TBC, ATBC and TEC), the citric ester plasticizer has the advantages that the problems that the citric ester plasticizer is easy to separate out and large in migration are solved; the processability and the product performance are greatly improved; and the application range of the products is enlarged.

Description

technical field [0001] The invention relates to an additive or auxiliary agent for the plastic industry, in particular to an environmentally friendly and nontoxic citrate plasticizer, which is mainly used in food packaging plastics, medical equipment and children's toys, and belongs to the field of plastic auxiliary agents. Background technique [0002] Citrate plasticizers are safe and non-toxic, and are one of the first-choice environmentally friendly plasticizers in the plastics industry at home and abroad. At present, the main varieties are tributyl citrate (TBC), acetyl tributyl citrate (ATBC) , Triethyl citrate (TEC). Although tributyl citrate (TBC), acetyl tributyl citrate (ATBC), and triethyl citrate (TEC) have excellent plasticizing effects and good cold resistance, light resistance, water resistance, and enzyme resistance , but compared with phthalate plasticizers, there are problems such as easy precipitation and large migration, and its volatility is relatively ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/11C07C69/67C07C67/08
Inventor 楚喆王青楚军政
Owner HENAN ZHENGTONG CHEM
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