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Preparation method of high-plasticizing and anti-migration cardanol-based plasticizer

A cardanol-based polyoxyethylene ether and anti-migration technology, applied in the field of plasticizers, can solve the problems of low plasticization efficiency and migration risk in plasticizing properties, achieve excellent ductility, realize high-value utilization, and be practical sexual effect

Active Publication Date: 2022-07-29
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although cardanol has been reported in many literatures for the preparation of bio-based plasticizers, there are still two problems in the use of the reported cardanol-derived plasticizers: (1) small molecular weight cardanol-derived plasticizers Cardanol-derived plasticizers (<1200g / mol) have better plasticizing properties but have migration risks; (2) Cardanol-derived plasticizers have lower plasticizing efficiency than traditional toxic dioctyl phthalate (DOP), only Can be used as auxiliary plasticizer

Method used

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  • Preparation method of high-plasticizing and anti-migration cardanol-based plasticizer
  • Preparation method of high-plasticizing and anti-migration cardanol-based plasticizer
  • Preparation method of high-plasticizing and anti-migration cardanol-based plasticizer

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Embodiment 1

[0035] The preparation method of cardanol-based polyoxyethylene ether fatty acid ester, the steps are as follows:

[0036] 1) Synthesis of cardanol-based polyoxyethylene ether:

[0037] Add 328g cardanol, 3.8g KOH to the closed autoclave, use N 2 Replace 3 to 5 times, then under the condition of temperature of 90 to 100 ℃, vacuum dehydration for 20 to 60 minutes, add 3076g of ethylene oxide under the condition of temperature of 110 to 120 ℃ to start the reaction, and control by condensed water during the feeding process The reaction temperature is 120-125 ℃, the pressure in the kettle is 0.1 MPa-0.3 MPa, and the reaction is completed by aging for 60 min after feeding, cooling to 60 ℃, adding phosphoric acid for neutralization, then adding 5 g of activated clay, adsorbing at 60 ℃ for 1 hour, and filtering, To obtain cardanol polyoxyethylene ether with a molecular weight of 3129 g / mol, the hydrogen nuclear magnetic spectrum is as follows figure 1 shown.

[0038]2) Synthesis o...

Embodiment 2

[0041] Utilize the cardanol polyoxyethylene ether in embodiment 1, synthesize cardanol polyoxyethylene ether n-butyl ester, the process is as follows: 110g above-mentioned cardanol polyoxyethylene ether; 8.0g n-butyric acid, 3.3g p-toluenesulfonic acid, 33.0 g of cyclohexane was added to the four-necked flask, and the reaction was terminated after 8 h at 82-105 °C. Excess cyclohexane was removed by distillation under reduced pressure, followed by 10 wt% NaHCO 3 The solution washes the remaining liquid until the pH of the system becomes neutral; finally, it is dehydrated and dried by distillation under reduced pressure to obtain cardanol polyoxyethylene ether n-butyrate (CPEB). Figure 4 shown; GPC results are shown in Figure 5 As shown, the number average molecular weight Mn was 3813 g / mol.

Embodiment 3

[0043] Utilize the cardanol polyoxyethylene ether in Example 1 to synthesize cardanol polyoxyethylene ether oleate, and the process is as follows: 80 g of the above-mentioned cardanol polyoxyethylene ether; 20.2 g of oleic acid, 0.8 g of p-toluenesulfonic acid, 32.0 g of g-cyclohexane was added to the four-necked flask, and the reaction was terminated after 7 h at 93-105 °C. Excess cyclohexane was removed by distillation under reduced pressure, followed by 10 wt% NaHCO 3 The solution washes the remaining liquid until the pH of the system becomes neutral; finally, it is dehydrated and dried by distillation under reduced pressure to obtain cardanol polyoxyethylene ether oleate (CPEO). Image 6 shown; GPC results are shown in Figure 7 As shown, the number average molecular weight Mn was 4113 g / mol.

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Abstract

The invention discloses a preparation method of high-plasticization and anti-migration cardanol-based polyoxyethylene ether fatty acid ester, which is characterized in that cardanol, ethylene oxide and fatty acid are used as raw materials, and the cardanol-based polyoxyethylene ether fatty acid ester with the molecular weight of 3400-4200 is synthesized by means of epoxy ring-opening polymerization and direct esterification. The cardanol-based polyoxyethylene ether fatty acid ester prepared by the invention has a large number of ether bond groups with high polarity and good flexibility in the structure, can endow a PVC product with excellent extension, migration resistance and other properties, and can completely replace traditional petroleum-based dioctyl phthalate. The method not only realizes high-valued utilization of the agricultural and forestry byproduct cardanol, but also provides a new method for preparing the high-quality environment-friendly plasticizer, and has good practicability.

Description

technical field [0001] The invention belongs to the technical field of plasticizers, and in particular relates to a preparation method of a highly plasticized and anti-migration type cardanol-based plasticizer and its application in PVC resins. Background technique [0002] A plasticizer is a kind of agent that can weaken the secondary valence bonds between the molecules of the material, improve the processability, plasticity, flexibility, and stretchability of the material, and reduce the melt viscosity and glass transition temperature without changing the basic chemical properties of the plasticized material. Polymer additives have been widely used in medical equipment, automobile manufacturing, children's toys, food packaging, coatings and electrical insulation and other fields. At present, the global plasticizer consumption exceeds 8 million t / a, and the market size exceeds 19.5 billion US dollars, of which phthalate plasticizers account for more than 65% of the total pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08G65/332C08L27/06C08L71/02C08J5/18
CPCC08G65/2612C08G65/3322C08J5/18C08J2327/06C08J2471/02
Inventor 谈继淮余敏姚玉成王凡黄能坤齐维君韦丽芬王文耕王玘王学峰陈泽源
Owner NANJING FORESTRY UNIV
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