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Method for producing environmentally friendly plasticizer diethylene glycol dibenzoate

A technology of diethylene glycol dibenzoate and an environmentally friendly plasticizer, which is applied in the preparation of carboxylate esters, chemical instruments and methods, and the separation/purification of carboxylic acid compounds, etc., and can solve the problem of unreachable and greatly affected by water content , long reaction time and other issues, to achieve the effect of reducing production energy consumption

Inactive Publication Date: 2019-05-21
杭州多向流化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN201110407912.7 discloses a process using tetrabutyl titanate as a catalyst and reactive distillation to produce DEDB, but no water agent is added in the process, the reaction time is long and the water content has a great influence on the reaction, Only relying on the separation tank on the top of the tower to divide the water may not achieve the expected yield

Method used

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  • Method for producing environmentally friendly plasticizer diethylene glycol dibenzoate
  • Method for producing environmentally friendly plasticizer diethylene glycol dibenzoate
  • Method for producing environmentally friendly plasticizer diethylene glycol dibenzoate

Examples

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Embodiment 1

[0036] The present embodiment is the laboratory experiment of esterification of benzoic acid and diethylene glycol. Put 96.0 g of benzoic acid, 39.72 g of diethylene glycol, 17.28 g of toluene and two zeolites into a three-necked flask, and heat slowly. Heat to about 120°C. After the benzoic acid is basically dissolved, add 1.0 g of tetrabutyl titanate as a catalyst, start stirring and condensing, and carry out esterification under heating and reflux. When the first drop of water was formed, the reaction start time was recorded. When the temperature reached 180°C, the toluene began to reflux to separate the water. The toluene was refluxed into the three-necked flask, and the water generated by the reaction was released in batches. Reflux and dehydrate at about 180°C for about 5 hours. When no water is separated, the esterification is complete, and then cool down to room temperature. Wash the above-mentioned materials with alkaline water, then stand still, separate the liquid,...

Embodiment 2

[0039] This example is similar to Example 1, except that the temperature is changed to 200° C. for the esterification reaction, and the remaining steps and amounts are the same.

[0040] The yield of diethylene glycol dibenzoate product is 35.2 wt%. Due to the high temperature, a large amount of toluene is evaporated, and the reflux of condensation is not enough, so that the water produced by the esterification reaction cannot be taken out of the reaction system in time, so that the conversion rate is not high.

Embodiment 3

[0042] This example is similar to Example 1, except that the amount of the catalyst is changed to 0.5 wt% of the total mass of the reactants, and the other steps and amounts are the same.

[0043] The yield of the diethylene glycol dibenzoate product determined by high performance liquid chromatography was 90.1 wt%.

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Abstract

The invention discloses a method for producing an environmentally friendly plasticizer diethylene glycol dibenzoate. The method includes the steps of 1) firstly feeding an oil phase in which benzoic acid is dissolved and diethylene glycol to an esterification reactor at a certain ratio, and gradually converting a benzoic acid component and the diethylene glycol into a diethylene glycol diethyleneglycol alcohol ester (DEDB); 2) taking generated water out of the esterification reactor by the vaporized oil phase, and recycling a recovered extractant back to an extraction unit; 3) making a crudeester DEDB be subjected to alkali washing, water washing and drying to obtain the environmentally friendly plasticizer diethylene glycol dibenzoate (DEDB). The method can efficiently produce a DEDB product from impure benzoic acid raw materials, and can greatly reduce the energy consumption of DEDB production.

Description

technical field [0001] The present invention relates to a kind of production method of high-efficiency environment-friendly plasticizer diethylene glycol dibenzoate (DEDB), realizes multi-stage esterification reaction steam stripping by the logistics that dissolves benzoic acid and diethylene glycol in multi-stage reactor Balanced and efficient preparation of diethylene glycol dibenzoate (DEDB) products. Background technique [0002] Compared with phthalate plasticizers, diethylene glycol dibenzoate (DEDB) with low toxicity is an environmentally friendly plasticizer. Moreover, DEDB has better compatibility, cold resistance, antistatic properties, thermal stability, etc., and is expected to replace the existing phthalate plasticizers on a large scale, and has a good market prospect. [0003] At present, the preparation of environmentally friendly plasticizer diethylene glycol dibenzoate (DEDB) in the industry mostly uses concentrated sulfuric acid, toluenesulfonic acid or al...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/58C07C69/78C07C51/42C07C51/48C07C51/44C07C63/06
Inventor 卢晓飞成有为祝炎雷李希
Owner 杭州多向流化学科技有限公司
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