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Preparation method of paraben pentaerythritol based zinc alkoxide

A technology based on pentaerythritol ester-based zinc and p-hydroxybenzoic acid, which is applied to the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of difficult reaction, limited anti-mildew performance, and high melting point, so as to speed up PVC production. Processing speed, energy consumption reduction, green process effect

Active Publication Date: 2020-06-05
山东海螺型材有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN102153824A discloses a method for preparing polyalcohol metal alkoxide by reacting pentaerythritol and ZnO. In this method, zinc oxide and pentaerythritol are mixed and reacted at high temperature for 4-6 hours, and the obtained product is not easy to hydrolyze, stable, and has excellent thermal stability effect; but the disadvantages There are also many, such as difficult reaction, high melting point (>220 ° C, much higher than the PVC processing temperature of 180 ° C), etc., poor compatibility with PVC, which limits its application
Inorganic antifungal agents are safe to use, heat-resistant, durable, and have a wide antibacterial spectrum. However, in actual use, due to poor dispersion or compatibility, their antifungal performance is limited and cannot meet actual needs.
Traditional organic antibacterial and antifungal agents mainly include phenolic compounds (substituted aromatic hydrocarbons), sulfur-containing organic compounds, nitrogen-containing organic compounds, and halogen-containing organic compounds. , but some antifungal agents have poor heat resistance, short duration of antifungal effect, etc., and there is no antibacterial and antifungal agent for PVC

Method used

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  • Preparation method of paraben pentaerythritol based zinc alkoxide
  • Preparation method of paraben pentaerythritol based zinc alkoxide
  • Preparation method of paraben pentaerythritol based zinc alkoxide

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Mix 138g of p-hydroxybenzoic acid, 130g of pentaerythritol and 1.7g of p-toluenesulfonic acid in a high-speed pulverizer, then move it into a reaction kettle, add 190mL of ether, fully stir at 30°C for 30min, then distill out the ether at 80°C ; Add 40mL of toluene as a water-carrying agent, react at 120°C for 3 hours, and evaporate the toluene under reduced pressure to obtain pentaerythritol p-hydroxybenzoate.

[0045] Add 200mL of absolute ethanol to the reaction kettle, take 250g of pentaerythritol p-hydroxybenzoate and add it to the reaction kettle, heat to 50°C and fully stir until dissolved; add 65g of zinc ethylate, 6mL of acetic acid, and 3.5g of zinc powder into the reaction kettle respectively, at 130 ℃, reflux reaction for 3 hours, when the reaction has flocculent solids, remove the reflux device at this time, evaporate to dryness and use a vacuum pump to further distill off the solvent under reduced pressure, after the reaction is completed, take the product ...

Embodiment 2

[0047] Mix 138g of p-hydroxybenzoic acid, 135g of pentaerythritol and 2.5g of p-toluenesulfonic acid in a high-speed pulverizer, then move it into a reaction kettle, add 250mL of ether, fully stir at 35°C for 20min, then distill out the ether at 85°C ; Add 60mL of toluene as a water-carrying agent, react at 140°C for 4h, and evaporate the toluene to dryness under reduced pressure to obtain pentaerythritol p-hydroxybenzoate.

[0048] Add 200mL of absolute ethanol to the reaction kettle, take 250g of pentaerythritol p-hydroxybenzoate and add it to the reaction kettle, heat to 60°C and stir until dissolved; add 55g of zinc ethylate, 7mL of acetic acid, and 3.8g of zinc powder into the reaction kettle respectively, at 140 ℃, reflux reaction for 3 hours, when the reaction has flocculent solids, remove the reflux device at this time, evaporate to dryness and use a vacuum pump to further distill out the solvent under reduced pressure. After the reaction is completed, take the product ...

Embodiment 3

[0050] Mix 138g of p-hydroxybenzoic acid, 140g of pentaerythritol and 2.0g of p-toluenesulfonic acid in a high-speed pulverizer, then move it into a reaction kettle, add 220mL of ether, stir at 32°C for 25min, then distill out the ether at 82°C ; Add 50mL of toluene as a water-carrying agent, react at 130°C for 3.5h, and evaporate the toluene under reduced pressure to obtain pentaerythritol p-hydroxybenzoate.

[0051] Add 200mL of absolute ethanol to the reaction kettle, take 250g of pentaerythritol p-hydroxybenzoate and add to the reaction kettle, heat to 55°C and stir until dissolved; add 45g of zinc ethylate, 7mL of acetic acid, and 4g of zinc powder into the reaction kettle respectively, and heat at 120°C Under reflux reaction for 4 hours, when flocculent solids are produced in the reaction, remove the reflux device at this time, evaporate to dryness and use a vacuum pump to further distill out the solvent under reduced pressure. After the reaction is completed, take the pr...

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of paraben pentaerythritol based zinc alkoxide. The method comprises the following steps: uniformly mixing p-hydroxybenzoic acid, pentaerythritol and a catalyst, adding a solvent, stirring, distilling off the solvent, carrying out an esterification reaction to obtain paraben pentaerythritol; and carrying out a reflux reaction on paraben pentaerythritol, zinc ethylate, a solvent, a catalyst and a stabilizer to obtain paraben pentaerythritol based zinc alkoxide. The preparation process is simple, the prepared PVC heat stabilizer (paraben pentaerythritol based zinc alkoxide) has a good antibacterial effect, the initial whiteness of PVC can be improved, and the long-term heat stability of PVC is prolonged.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of pentaerythritol ester-based zinc metal p-hydroxybenzoate alkoxide. Background technique [0002] Polyvinyl chloride (PVC) is one of the most widely used plastic varieties. Because of its acid resistance, corrosion resistance, and electrical insulation properties, it is widely used in packaging products, household appliances, building materials, medical equipment and other fields. The inherent structural defects of PVC molecules make it poor in thermal stability. Long-term exposure to ultraviolet rays and high temperature environments will accelerate the degradation of PVC and release hydrogen chloride, which will cause discoloration of products, decrease in physical and mechanical properties and lose their use value. In 2006, Johan Steenwijk and others found that polyols can significantly improve the thermal stability of PVC, such as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/29C07C69/84C08K5/134C08L27/06
CPCC07C67/29C07C67/08C08K5/1345C08L2201/08C07C69/84C08L27/06
Inventor 李德刚张曼琦胡希敏石朋朱东坡路维东唐圣奎袁效东陈伟
Owner 山东海螺型材有限责任公司
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