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Preparation method of triethylene glycol dibenzoate

A technology of triethylene glycol dibenzoate and benzoate, applied in the field of preparation of triethylene glycol dibenzoate, can solve problems such as unfavorable large-scale production, sewage treatment and the like, and is suitable for large-scale industrial The effect of production, easy separation, environmental protection or safe production

Active Publication Date: 2014-01-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the patented method requires neutralization and water washing steps after the reaction, which brings about the problem of sewage treatment, and the crude product needs to be added with an adsorbent and filtered to obtain the desired refined product after dehydration under reduced pressure.
These are not conducive to mass production

Method used

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  • Preparation method of triethylene glycol dibenzoate
  • Preparation method of triethylene glycol dibenzoate
  • Preparation method of triethylene glycol dibenzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] This embodiment is used to illustrate the preparation method of triethylene glycol dibenzoate provided by the invention.

[0030]Add 30g (0.2mol) triethylene glycol (gas chromatography content 99.2%; containing 0.8% diethylene glycol) and 108.9g (0.8mol) benzoic acid into a 250mL round bottom flask with condenser, liquid separator and stirrer Methyl ester, 5.5g (0.04mol) anhydrous potassium carbonate, heat the oil bath in contact with the round bottom flask to 155°C, react at 0.1MPa, and distill the generated alcohol to the separator and remove it by distillation during the reaction , after reacting for 6 hours, add toluene in the round bottom flask, add 6 times in total, the time interval between two adjacent additions is 2.1 hours, add 12mL each time, react for 2 hours after each addition of toluene and simultaneously add toluene and The azeotrope was distilled out of the round bottom flask, and the next toluene was added after the reaction liquid was cooled for about...

Embodiment 2

[0035] This embodiment is used to illustrate the preparation method of triethylene glycol dibenzoate provided by the invention.

[0036] Add 22.53g (0.15mol) triethylene glycol (gas chromatography content 99.2%; containing 0.8% diethylene glycol) and 81.69g (0.6mol) benzoic acid into a 150mL single-necked flask with a condenser, separator, and stirrer Methyl ester, 2.07g (0.015mol) anhydrous potassium carbonate, heat the oil bath in contact with the single-necked flask to 155°C, react at 0.1MPa, and distill the generated alcohol to the liquid separator by distillation during the reaction and remove it, After reacting for 6 hours, add xylene to the single-necked flask, add 6 times in total, the time interval between two adjacent additions is 2.1 hours, add 12mL each time, heat the oil bath that contacts the single-necked flask after adding xylene each time To 170°C, react for 2 hours and distill xylene and azeotrope out of the single-necked flask at the same time, wait for the ...

Embodiment 3

[0038] This example is used to illustrate the preparation of triethylene glycol dibenzoate by using anhydrous potassium carbonate supported on a carrier alumina as a catalyst provided by the present invention.

[0039] (1) Preparation of catalyst loaded with anhydrous potassium carbonate onto alumina

[0040] The neutral alumina was calcined at 550°C for 4 hours before use. Dry anhydrous potassium carbonate in a blast drying oven at 105°C for 3 hours, take 6g of dried anhydrous potassium carbonate and dissolve it in 40mL of deionized water, add 24g of neutral alumina after fully dissolved, and let it stand for 24 hours after fully stirring. The mixture was put into an evaporating dish to evaporate the water to dryness, and then put into a blast drying oven to dry at 105° C. for 24 hours. The obtained solid was calcined in a muffle furnace at 600° C. for 5 hours to obtain 28.89 g of a catalyst powder in which anhydrous potassium carbonate was supported on alumina.

[0041] (2...

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Abstract

The invention provides a preparation method of triethylene glycol dibenzoate represented by the structural formula (I). The method includes the steps: in the presence of a catalyst containing anhydrous potassium carbonate, a reaction of triethylene glycol represented by the structural formula (II) and benzoic acid ester PhCOOR is carried out, and a product including triethylene glycol dibenzoate represented by the structural formula (I) and a corresponding alcohol HOR is generated, wherein R is methyl or ethyl. The method of the invention is conducive to environmental protection; and the product has high yield and good purity.

Description

technical field [0001] The invention relates to a method for preparing plasticizer component triethylene glycol ester compounds, in particular to a method for preparing triethylene glycol dibenzoate. Background technique [0002] Plasticizers refer to plastic additives used in the molding process of polyvinyl chloride and other plastics. Adding them to the polymer system can reduce the glass transition temperature of the polymer and increase its plasticity, making it easy to process. The output of plasticizer accounts for about 60% of the total amount of plastic additives, mainly used in PVC products, and the consumption accounts for 80%. There are many types of plasticizers, most of which are esters, of which phthalates (including DOP, DBP, BBP, DINP, DIDP, DnOP, etc.) account for about 85% of the output. However, the use of phthalate plasticizers has been restricted in Europe and the United States. In the context of Taiwan's "plasticizer" incident, calls for the use of no...

Claims

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Application Information

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IPC IPC(8): C07C69/78C07C67/03
CPCC07C67/03C07C69/78
Inventor 谢伦嘉张雄辉赵思源田宇孙竹芳冯再兴
Owner CHINA PETROLEUM & CHEM CORP
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