Method for preparing diethylene glycol dibenzoate plasticizer

A polyol benzoate and polyol technology, applied in the field of rubber additives, can solve the problems of slow reaction temperature, high raw material price, poor compatibility and durability, etc., and achieve good compatibility and durability , Shorten the reaction time, reduce the effect of production cost

Inactive Publication Date: 2011-03-23
成都亚恩科技实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 2. Persistent Bioaccumulative and Toxic (PBT);
[0006] 3. High persistent cumulative toxicity (very Persistent, very Bioaccumulative, vPvB)
[0016] From production practice, we find that among the plasticizers prepared by prior art methods, the compatibility and durability of diethylene glycol dibenzoate (DEDB) and PVC are slightly poor, and when the addition amount is large, the surface The precipitation is obvious, and it cannot completely replace DOP in PVC soft products; and although dipropylene glycol dibenzoate (DPGDB) has good compatibility and durability with PVC, it can completely replace DOP in PVC soft products, but due to The price of raw materials is too expensive, resulting in high cost, and the product is highly volatile and has an unpleasant smell, which brings difficulties to use and poor market acceptance
[0017] There are also products on the market that are simply mixed with diethylene glycol dibenzoate and dipropylene glycol dibenzoate at a ratio of 1:1, but this is just a simple mixture of the two single components produced separately, which has no effect on product performance. The change of the product is not obvious, and the volatility of the product increases instead, the resistance to water extraction increases, and the durability does not improve, and it does not change the current situation of the high production cost of dipropylene glycol dibenzoate, and the production process of various components. High reaction temperature or slow reaction speed, long reaction time, etc.

Method used

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  • Method for preparing diethylene glycol dibenzoate plasticizer
  • Method for preparing diethylene glycol dibenzoate plasticizer
  • Method for preparing diethylene glycol dibenzoate plasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0098] Add 0.55mol of diethylene glycol, 0.45mol of dipropylene glycol, and 0.02mol of glycerol into a reactor with a reflux condensation water separator, and stir evenly; add 0.05mol of sulfuric acid as a catalyst, and 40ml of petroleum ether as a water-carrying agent; add 2.06 mol benzoic acid; heat under stirring, adjust the temperature to 90-110°C for 7 hours, separate the water produced by the reaction, and make the reaction complete; when the temperature drops to 70-80°C, add sodium carbonate to remove the acidic catalyst; vacuum separation Recovery of water and water-carrying agents; filtration, that is.

[0099] In this example, the product conversion rate was 96.5%.

Embodiment 2

[0101] Add 0.5mol diethylene glycol, 0.5mol dipropylene glycol, and 0.15mol glycerol into a reactor with a reflux condensation water separator and stir evenly; add 0.04mol p-toluenesulfonic acid as a catalyst, and 50ml heptane as a water-carrying agent; Add 2.45mol benzoic acid; heat under stirring, adjust the temperature to 100-120°C and keep it warm for 6 hours, separate the water produced by the reaction to complete the reaction; when the temperature drops to 70-80°C, add sodium hydroxide to remove the acidic catalyst ; Vacuum separation and recovery of water and water-carrying agents; filtration, that is.

[0102] In this example, the product conversion rate was 97.2%.

Embodiment 3

[0104] Add 0.45mol of diethylene glycol, 0.55mol of dipropylene glycol, and 0.2mol of glycerol into a reactor with a reflux condensation water separator and stir well; add 0.03mol of phosphoric acid and 0.02mol of phosphotungstic acid as a catalyst, and 52ml of n-hexane as a belt Water agent; add 2.6mol benzoic acid; heat under stirring, adjust the temperature to 110-130°C for 9 hours, separate the water produced by the reaction, and make the reaction complete; when the temperature drops to 70-80°C, add calcium hydroxide Remove the acidic catalyst; vacuum separation and recovery of water and water-carrying agent; filter, that is.

[0105] In this example, the product conversion rate was 97.0%.

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Abstract

The invention discloses a method for preparing a diethylene glycol dibenzoate plasticizer. The method comprises the following steps of: mixing multiple kinds of polyalcohol raw materials and reacting with benzoic acid, wherein the polyalcohol raw materials comprise diglycol, dipropylene glycol, glycol and/or glycerol; adding the polyalcohol raw materials into a reactor and uniformly stirring; adding benzoic acid, a catalyst and a water-carrying agent; heating to 90 to 130 DEG C and reacting for 6 to 10 hours; and neutralizing after the reaction is finished, separating and recovering water and the water-carrying agent, and filtering. In the method, the multiple kinds of polyalcohol raw materials are mixed and then subjected to esterification reaction together with the benzoic acid, so that the esterification reaction can be smoothly carried out, the reaction temperature can be reduced, the reaction speed can be increased, the reaction time can be shortened, the industrial mass production is facilitated, and the production cost can be reduced; the plasticizer prepared by the method has equivalent plasticizing performance as that of dioctyl phthalate (DOP) and superior oil resistance, solvent resistance and the like to those of DOP; in addition, both each raw material and the reaction product are nontoxic or low-toxicity components which meet the environmental protection requirement.

Description

technical field [0001] The invention belongs to the technical field of rubber additives in material science and technology fine chemical industry, in particular to a preparation method of polyol benzoate plasticizer. Background technique [0002] Plasticizers are the most widely used additives in the processing and production of PVC and other plastics. If plasticizers are not used, PVC will become very hard and brittle, which cannot meet the softness or flexibility requirements of plastic products in production and life. Plasticizers can be widely used in the manufacture of wire and cable sheaths, artificial leather, agricultural films, calendered films, foam products, flooring and laminated products, shoe soles, sheets, floor coverings, plastic flooring and asbestos flooring, records and film bases , pipes, foams, molded products such as castings and injections, etc., can also be used as plasticizers in coatings, adhesives, pigments and spices. [0003] The "EU Regulations...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/78C07C67/08C08K5/103
Inventor 杜林海陈德东
Owner 成都亚恩科技实业有限公司
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