Flavors Of New Synthetic Ethyl - Flavors And Fragrances, Food Additives - Food Industry

Summary : Synthesis of a polyvinyl chloride resin

, a pyridine, and by elemental analysis and infrared spectra were characterized. At the same time with PVC - pyridine resin (PVC-Pyridine) Synthesis of spices Benzoic acid Ester, the amount of catalyst, Raw material Ratio and reaction time on esterification reaction, test results show that PVC resin is the esterification reaction of a pyridine good catalyst, yield was 97%.

Keywords : PVC resin, a pyridine; synthesis; spices

Also known as benzoin ethyl ethyl benzoate, is a colorless or pale yellow liquid, a little like aroma of ylang ylang oil, was a strong aroma of wintergreen oil and fruit, sweet incense to reconcile Incidentally, China to the provisions of allows the use of Flavors Can be used for preparation of synthetic ylang ylang oil, and the next month Sesame oil , A small amount of soap used for the Flavor and tobacco flavors, often used in Soft drinks , Pudding, ice cream, baked foods, cigarettes and alcohol and other flavoring products [1].

Ethyl Ester Synthesis of carboxylic acids such as commonly used in concentrated sulfuric acid as the catalyst for direct esterification [2 3], in concentrated sulfuric acid as catalyst, although low cost, high rate of esterification, but sulfuric acid selectivity, there is the role of oxidation and carbonization, which many side reactions, the product purity is not high, serious corrosion of equipment and the environment. Xiao-Jun Peng [4] and other strong acid cation exchange resin used to do to replace the sulfuric acid esterification catalyst, with people rising environmental awareness, green catalyst instead of sulfuric acid catalyzed esterification of more and more attention. In this paper, polyvinyl chloride and a pyridine pyridine PVC resin, and use it as catalyst of the favorable conditions for synthesis of ethyl benzoate.

1 Reagents and Instruments Polyvinyl chloride (PVC): The average degree of polymerization of 200-2000, Cl50.57%, pyridine, and other reagents for the pure commercial chemical products. PE-2400CHN elemental analyzer, 5107P Fourier transform infrared spectrometer, the other for the common glassware.

2 N ethylene an adjoining lakes Poly Resin

With stirrer and reflux condenser in the three-neck flask were added 40mL of pyridine, sodium hydroxide, water, stir, heat, then add a certain amount of 20gPVC, temperature 80 , stirring 8h, placed certain period of time, temperature halfway to 100 , stir it. Then pour into a large number of water, standing and filtered, washed with water to neutral no chloride, then 95% ethanol wash to no pyridine odor, put Soxhlet extractor using ethanol extraction 8h 10h, the vacuum drying to constant weight.

With PE-2400CHN elemental analyzer for elemental analysis, oxygen flask combustion method [5] Determination of chlorine content, use 5107P Fourier transform infrared spectroscopy to measure the infrared spectrum.

3 Synthesis of Ethyl In with divider, thermometer and reflux Condenser The flask, by adding a certain amount of PVC resin, pyridine, benzoic acid, ethanol and acid, micro-heat to make the dissolution of benzoic acid and p-toluenesulfonic acid, shake to start heating oil bath after returning, with the response to the continued separation of the water produced to separate the water when the reaction is almost the end.

Not start in the refluxed reaction before and after the reaction of acid value were determined by the following formula esterification rate [6]:

Esterification rate% = [(initial reaction when the acid value? Response to the end of the acid value) / initial reaction when the acid value] %.

Esterification end, filtering out the catalyst separation, excessive alcohol distillation, the reaction solution by washing, Caustic (10% sodium carbonate aqueous solution), then washed with anhydrous calcium chloride drying, the final vacuum distillation, collecting 102 103 of the fractions for the product, measuring refractive index.

4 Results and Discussion 4.1 a poly vinyl pyridine-N Synthesis and Characterization

And pyridine by the PVC resin black granular solid, insoluble in the solvent can dissolve the PVC, its reaction time and elemental analysis results in Table 1.

Table 1 Seen from Table 1, PVC with pyridine, the increase of reaction time, decrease the weight of the product, chlorine content also decreased, likely to occur off hydrogen halide reactions.

Synthetic resin measured by infrared spectra in Figure 1.

Figure 1 Can be seen by the infrared spectrum, absorption of the resin after the reaction were altered significantly, 326.01cm-1 appears in the strong OH absorption peak, 1633.91cm-1 occurred C = C and C = N absorption peak, 3028 .50 cm-1 = CH absorption peak appears, indicating the pyridine has been combined with the PVC and the emergence of isolated and polyene C = C and C = N stretching vibration band; PVC on the 610cm-1, and 690cm-1, in the vicinity of the C-Cl stretching vibration bands greatly reduced, 1427cm-1 in a CHCl-CH2-CHCl a bending vibration bands and 1255cm-1 in a CHCl-CHC a bending vibration bands are greatly reduced, also shows that PVC HCl removal reaction occurs, the above facts fully prove that the reaction of PVC and the formation of pyridine occurred long polyene chain structure of pyridine bases, the structure is as follows:

Structure of pyridine bases This structure is set out in the quarter solid polymer base, similar to the alkaline ion exchange resin is polymer-salt as a phase transfer catalyst, for some reaction has a certain phase transfer catalytic activity.

To Figure 1, resin, PVC and PVC pyridine absorption peak compared in Table 2.

4.2 catalyst to synthesize 4.2.1 of catalyst 0.5mo acid, 0.8mol ethanol in a poly vinyl pyridine resin catalyst nitrogen under reflux 3h, investigates the amount of catalyst on the esterification rate, the results shown in Table 3.

Table 3 From the Table 3 shows the amount of catalyst there is a big influence on the reaction, the dosage of 2.5g when the esterification rate was the highest amount of catalyst esterification rate is too high or too low will drop.

4.2.2 ratio of raw materials

With 0.5mol of benzoic acid, 2.5g of the catalyst, the reaction 3h, effects of different acid ratio on the esterification rate, the results shown in Table 4

by: gaga

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