Preparation method of polymerization type environment-friendly plasticizer diethylene glycol dicyclohexyl-1,3-diisobutyl dicarboxylate

A technology of diisooctyl dicarboxylate and diethylene glycol reduction, which is applied in the field of chemical engineering and can solve problems such as high prices, increased production costs of plasticizers, and large consumption

Inactive Publication Date: 2011-05-18
ZHEJIANG SHANGTONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, trioctyl trimellitate (TOTM) is the main plasticizer used in 105°C grade cable materials, but the consumption of raw material alcohol used in the domestic synthesis of TOTM is large (more than 715kg of 2-ethylhexanol is required for each ton of TOTM). The long-term domestic supply of this alcohol is tight, and the price remains high. It is the world's largest importer for a long time, which directly leads to an increase in the production cost of domestic plasticizers. Therefore, how to comprehensively utilize the existing domestic resources to reduce the production cost of plasticizers , is a major issue facing the majority of plasticizer manufacturers

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0009] The steps of the preparation method of polymeric environment-friendly plasticizer diethylene glycol dicyclohexane-1,3-dicarboxylic acid diisooctyl are as follows:

[0010] 1) Mix 1 mole of diethylene glycol, 4.25 moles of cyclohexane-1,3-dicarboxylic acid anhydride and catalyst, stir and heat for cross-linking reaction, control the reaction temperature at 150°C, and keep the reaction at 150°C After 2-3 hours, add 1.7-2.1 moles of 2-ethylhexanol and catalyst to the reaction system, continue to stir and heat up to 220°C, react for 3-4 hours, remove excess 2-ethylhexanol, and obtain a The crude product of diethylene glycol bicyclohexane-1,3-dicarboxylate diisooctyl;

[0011] 2) Cool the crude diethylene glycol dicyclohexane-1,3-dicarboxylic acid diisooctyl to 85°C and add 1% Na 2 CO 3 The aqueous solution neutralizes the trace monoester in the material system, the catalyst in the hydrolysis system, washes with deionized water at 90°C to remove the lye entrained in the cr...

Embodiment 1

[0015] Add diethylene glycol and cyclohexane-1,3-dicarboxylic anhydride with a molar ratio of 1 / 4.25 and a total mass of 1180kg of diethylene glycol and cyclohexane-1,3-dicarboxylic anhydride to react In the container, add relative cyclohexane-1, the zinc acetate catalyst of 0.5% of the quality of 3-dicarboxylic acid anhydride, stir and heat to 150 ℃, and add 1.7 mol total mass of 1490kg after the reaction at 150 ℃ for 2 hours 2-Ethylhexanol and 0.3% tetraisopropyl titanate catalyst relative to the mass of cyclohexane-1,3-dicarboxylic acid anhydride, continue to stir and heat up to 220°C for 3 hours, then dealcoholize, cool to 85°C and add 100kg1.0wt %Na 2 CO 3 Neutralize with aqueous solution, wash with ion-free water at 90°C, refine with direct steam stripping under reduced pressure for 3 hours, add 0.1% of the total amount of the kettle material to absorb and decolorize for 30 minutes, and obtain diethylene glycol bicyclohexane- 1,3-Diisooctyl dicarboxylate, its yield is ...

Embodiment 2

[0017] Add diethylene glycol and cyclohexane-1,3-dicarboxylic anhydride with a molar ratio of 1 / 4.25 and a total mass of 1180kg of diethylene glycol and cyclohexane-1,3-dicarboxylic anhydride to react In the container, add 0.5% zinc acetate catalyst relative to the mass of cyclohexane-1,3-dicarboxylic acid anhydride, stir and heat to 150°C, and keep warm at 150°C for 2.5 hours before adding 1.8 moles of 1580kg 2-Ethylhexanol and 0.3% tetraisopropyl titanate catalyst relative to the mass of cyclohexane-1,3-dicarboxylic acid anhydride, continue to stir and heat up to 220°C for 3 hours, then dealcoholize, cool to 85°C and add 100kg1.0wt %Na 2 CO 3 Neutralize with aqueous solution, wash with ion-free water at 90°C, refine with direct steam stripping under reduced pressure for 3 hours, add 0.1% of the total amount of the kettle material to absorb and decolorize for 30 minutes, and obtain diethylene glycol bicyclohexane- 1,3-Diisooctyl dicarboxylate has a yield of 99.13%, a purity...

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Abstract

The invention discloses a preparation method of polymerization type environment-friendly plasticizer diethylene glycol dicyclohexyl-1,3-diisobutyl dicarboxylate. The preparation method comprises the following steps of: putting 1 molar of diethylene glycol, 4.25 molar of cyclohexane-1,3-dicardoxylic acid anhydride and a catalyst into a reactor, and then stirring and heating the obtained mixture to 150 DEG C for cross-linking reaction; adding 1.7-2.1 molar of 2-ethylhexanol and a catalyst in the reaction system, and then stirring and heating the mixture to 220 DEG C for esterification reaction; removing the excessive alcohol to obtain the crude diethylene glycol dicyclohexyl-1,3-diisobutyl dicarboxylate; cooling the crude diethylene glycol dicyclohexyl-1,3-diisobutyl dicarboxylate to 85 DEG C, then adding 1% Na2CO3 aqueous solution for neutralization; washing the neutralized product with non-ion water at the temperature of 90 DEG C; and steaming stripping and refining for 3-4 hours under the condition of reduced pressure, adding activated carbon for absorption and decoloration, filterng and then obtaining the purified product. The heat-resisting environment-friendly plasticizer prepared by the method can be used for heat-resisting and perdurable articles, such as heat-resisting electric wire and cable materials, plank stuffs, sheets, sealing gaskets and the like.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a method for preparing a polymeric environment-friendly plasticizer diethylene glycol bicyclohexane-1,3-diisooctyl dicarboxylate. Background technique [0002] The development of polyvinyl chloride (PVC) industry is inseparable from plasticizers. 90% of all production of plasticizers is used in PVC industry, and special plasticizers account for about 1 / 5 of the market share. Due to its excellent cost performance, PVC is widely used in wire and cable insulation and sheathing. 105°C grade cable material is the highest temperature-resistant variety among wire and cable. It is mainly used for the wiring of high-temperature-resistant machinery and equipment required to increase the current carrying capacity of wire and cable, and the lead and wiring of high-temperature machinery and equipment, such as steel plants, The wiring of steam boilers and stoves in thermal power ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/75C07C67/08C08L27/06C08K5/12
Inventor 商集平周少杰方猷泉
Owner ZHEJIANG SHANGTONG TECH
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