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Preparation method of n-butyl benzoate

A technology of n-butyl benzoate and a manufacturing method, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as difficulty in heating, potential safety hazards, prolonged reaction time, etc., and achieves simple and convenient operation process. The effect of stability, safe transportation and storage, and less pollution of the three wastes

Inactive Publication Date: 2013-04-03
WUHAN YOUJI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] 1, because the unreacted benzoic acid content in the material after the reaction affects the acid value of the finished product after rectification, so the literature adopts the method for washing the organic layer after the reaction with water, dilute sodium carbonate solution and water to remove the unreacted benzoic acid. Benzoic acid, which will generate a large amount of wastewater, and n-butanol in the organic layer will also be washed into the wastewater, resulting in increased consumption of n-butanol and difficulties in wastewater treatment
According to the actual production situation, every 1 ton of finished products will produce 4 tons of waste water, and the COD value of the waste water is about 40,000, which brings huge pressure on environmental protection.
[0006] 2. N-butanol is put into the reaction kettle at one time for reflux and water separation reaction, resulting in too fast reaction speed and excessive reflux in the early stage; it is difficult to heat up in the later stage reaction and the reaction time is prolonged
The amount of n-butanol used in the literature is much more than the theoretically required amount of the reaction. The excess n-butanol increases the concentration of the reactants, and at the same time acts as a solvent and takes out the water generated by the reaction, so the early stage of the reaction is very fast , the return flow is very large, so there are potential safety hazards in industrial production, and safety accidents such as flushing are prone to occur
And when the benzoic acid concentration in the late stage of the reaction decreases and causes the reaction speed to decline, there is still a large amount of n-butanol in the reaction system, which makes it difficult to increase the reaction speed, thereby prolonging the reaction time
In addition, investing too much n-butanol will reduce the utilization rate of equipment, increase energy consumption, and etherification reaction will easily occur to increase the consumption of n-butanol

Method used

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  • Preparation method of n-butyl benzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 450g of benzoic acid, 170g of n-butanol, and 25.4g of sodium bisulfate into a 1000ml four-necked bottle, install a water separator, a reflux condenser and a thermometer, stir and heat to reflux to separate water. After the reaction temperature rises to 135°C, add 170g of n-butanol dropwise. When the temperature rises to 150°C and no water comes out of the water separator, stop the reaction. The reaction time is 1.5h. After the reaction, the temperature was lowered to below 40°C to recover the catalyst by suction filtration and 722g of the filtrate was obtained. Sample analysis showed that the content of n-butyl benzoate was 88.75% (GC), the content of benzoic acid was 0.37% (GC), and the content of n-butanol was 10.1% (GC). . The filtrate was neutralized by adding 20g of solid alkali at 60°C for 20 minutes, and then suction filtered again. The crude product was sampled and analyzed, and the content of benzoic acid (GC) was 0.016%. After rectification, 610 g of n-bu...

Embodiment 2

[0030] Feeding amount and reaction operation are the same as in Example 1. After the reaction is completed, the catalyst is recovered by cooling and suction filtration and 724g of filtrate is obtained. Sampling analysis shows that the content of n-butyl benzoate is 89.29% (GC), the content of benzoic acid is 0.46% (GC), and n-butanol Content 9.55% (GC). The filtrate was neutralized by adding 10 g of solid alkali at 60°C for 60 minutes, and then suction filtered again. The crude product was sampled and analyzed, and the content of benzoic acid (GC) was 0.17%. After rectification, 614g of n-butyl benzoate was obtained. Sample analysis showed that the content was 99.4% (GC), the acid value was 1.48 (mgKOH / g), and the total yield was 93.4%.

Embodiment 3

[0032] Feeding amount and reaction operation are the same as in Example 1. After the reaction is over, the material is distilled under reduced pressure to recover n-butanol, and the remaining material is 670g. Sampling analysis shows that the content of n-butyl benzoate is 96.42% (GC), and the content of benzoic acid is 0.47% (GC). The n-butanol content is 2.61% (GC). Then add 20g of solid alkali to neutralize at 60°C for 20 minutes, and then filter again. The crude product is sampled and analyzed. The content of n-butyl benzoate is 97% (GC), the content of benzoic acid is 0.33% (GC), and the content of n-butanol is 2.18% (GC). .

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Abstract

The invention discloses a preparation method of n-butyl benzoate. The preparation method mainly comprises the following steps of: taking benzoic acid as a raw material, enabling the benzoic acid to react with n-butyl alcohol under the existence of a solid acid catalyst to obtain a crude product, then neutralizing the crude product by using solid alkali, and then rectifying and purifying to obtain the finished product, namely the n-butyl benzoate. The preparation method disclosed by the invention is simple, convenient and stable in operation process, little in three-waste pollution and suitable for industrial production.

Description

technical field [0001] The present invention relates to the manufacture method of chemical product, particularly a kind of manufacture method of n-butyl benzoate. Background technique [0002] N-butyl benzoate is a colorless, transparent liquid with a fruity aroma. It is mainly used as a solvent for resins, paints, etc., and as a raw material for spices. It has a wide range of uses. [0003] At present, n-butyl benzoate is produced by the esterification reaction of benzoic acid and n-butanol with concentrated sulfuric acid as a catalyzer. This method has disadvantages such as large consumption of sulfuric acid, many side reactions, serious corrosion, troublesome post-processing and environmental pollution. In recent years, people have used various solid superacids, heteropolyacids, activated carbon immobilized heteropolyacids, some Lewis acids or immobilized Lewis acids as esterification catalysts and achieved good results. Among them, p-toluenesulfonic acid (Fujian Chemic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/78C07C67/08
CPCY02P20/584
Inventor 毛利民邹晓虹王丽华周宇李毅
Owner WUHAN YOUJI IND
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