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Vegetable oil polyol preparation method by using continuous method

A vegetable oil polyol, continuous method technology, applied in the field of preparation of vegetable oil polyol, can solve the problems of non-continuous production, low product quality, long reaction time, etc., and achieve the effect of short reaction time, less pollution, and simple production equipment

Active Publication Date: 2013-09-04
NANJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The technical problem to be solved by the present invention is, in order to overcome the long reaction time, high energy consumption, low product quality, and non-continuous production of vegetable oil polyols existing in the production of vegetable oil polyols based on the principle of epoxy ring opening. Continuous method and method for preparing vegetable oil polyol by combining epoxidation and ring-opening two-step reaction into one step

Method used

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  • Vegetable oil polyol preparation method by using continuous method

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Effect test

Embodiment 1

[0026] Mix 1360.4g of 30wt% hydrogen peroxide (12mol) with 563.63g of formic acid (12mol), add 20.02g (0.2mol) of sulfuric acid and 2.92g (0.01mol) of EDTA, then add 200g of soybean oil (containing 0.99mol of double bonds) and the above The mixed solution was pumped into the microchannel modular reaction device at the same time as the injection rate of 0.2mL / min and 2.1mL / min respectively, and the reaction residence time was kept for 16min, and the reaction was carried out in the sandwich reactor HC at normal pressure and 100°C. The product was allowed to stand for liquid separation, and the oil phase was collected with 5% Na 2 CO 3 The aqueous solution was washed until neutral, and then liquid separation and rotary evaporation were performed to obtain a vegetable oil polyol with a hydroxyl value of 334 mgKOH / g.

Embodiment 2

[0028] Mix 1133.67g of 30wt% hydrogen peroxide (10mol) with 603.52g of acetic acid (10mol), add 12.31g (0.123mol) of sulfuric acid and 11.69g (0.04mol) of EDTA, then mix 200g of cottonseed oil (containing 0.812mol of double bonds) with the above The mixed solution was pumped into the microchannel modular reaction device at the same time at the injection rate of 0.5mL / min and 4.5mL / min respectively, and the reaction residence time was kept for 8min. reaction, the reaction product was left to separate liquids, and the oil phase was collected with 5% Na 2 CO 3 The aqueous solution was washed until neutral, and then liquid separation and rotary evaporation were performed to obtain a vegetable oil polyol with a hydroxyl value of 246 mgKOH / g.

Embodiment 3

[0030] Mix 1700.5g of 30wt% hydrogen peroxide (15mol) with 905.28g of acetic acid (15mol), then add 19.83g of phosphoric acid (0.172mol) and 20.46g of EDTA (0.07mol), then add 200g of rapeseed oil (containing 0.785mol of double bonds) and The above mixed solution was pumped into the microchannel modular reaction device at the same time at the injection rate of 0.3mL / min and 3.4mL / min respectively, and the reaction residence time was kept for 10min. The product was allowed to stand for liquid separation, and the oil phase was collected with 5% Na 2 CO 3 The aqueous solution was washed until neutral, and then liquid separation and rotary evaporation were performed to obtain a vegetable oil polyol with a hydroxyl value of 265 mgKOH / g.

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Abstract

The invention discloses a vegetable oil polyol preparation method by using a continuous method. The vegetable oil polyol preparation method comprises the following steps: firstly mixing oxydol and organic acid, adding a catalyst and a stabilizing agent, simultaneously pumping vegetable oil and mixed solution into a micro-channel modular reactor, maintaining reaction residence time for 5-18 min, performing reaction at normal pressure with the temperature of 65-130 DEG C, still standing a reaction product for liquid separation, collecting oil phase to be washed to neutral by using a Na2CO3 solution, and then performing liquid separation and rotary evaporation to obtain the vegetable oil polyol. The vegetable oil polyol preparation method provided by the invention can be operated continuously, and in the process, two steps of epoxidation and ring-opening are integrated into one step, so that the preparation process is simple, easy to control, high in safety, short in reaction time, low in energy consumption and low in pollution, can weaken side reaction, further has the characteristics of simple production device, easiness in assembly and disassembly, and convenience in carrying and moving, can be adjusted by simply increasing or decreasing the number of micro-channels for regulation, and can avoid 'amplification effect' generated in similar industrial production.

Description

technical field [0001] The invention relates to a preparation method of vegetable oil polyol, in particular to a method for preparing vegetable oil polyol by using vegetable oil as a raw material, adopting a continuous method and combining two-step reactions of epoxidation and ring opening into one step. Background technique [0002] With the increase of petroleum consumption, the decrease of petrochemical resource reserves and the continuous rise of petrochemical product prices, people pay more and more attention to the use of renewable resources to produce materials and fuels, and the use of renewable resources as raw materials for chemical products has attracted people's attention. Vegetable oil polyols are substitutes for petroleum-based polyols with outstanding environmental protection value. According to biosphere analysis data, compared with petroleum-based polyols, the overall energy consumption of vegetable oil polyols is reduced by 23%, the consumption of non-renew...

Claims

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Application Information

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IPC IPC(8): C07C67/31C07C69/675C07C69/732
Inventor 郭凯方正季栋欧阳平凯
Owner NANJING UNIV OF TECH
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