The function of the here and now development is precisely to the limitation of raw materials as well as processes existing in the prior art, suggests a chemical synthesis process of Alpha-Hexylcinnamaldehyde with affordable procedure, moderate response problems, and pure product scent, as well as offers 30% low-level n-octylaldehyde for oneself, made use of in the synthesis of Alpha-Hexylcinnamaldehyde, considerably minimizing the yield of organic solvents in the process of supplying n-octaldehyde for itself, attaining the objective of energy saving and cost reduction, as well as decreasing the by-product hexyl nonyl created by the self-condensation of n-octaldehyde at high web content Alkenal overcomes the shortcoming of the foul hexyl nonenal that limits the flower scent of the item, and makes the scent of the product pure and soft.
The technological issue to be fixed by the present development is accomplished with the following technical options:
The low-content n-octylaldehyde is straight made use of in the technique for manufacturing the initial Alpha-Hexylcinnamaldehyde, the condensation reaction of 30% n-octaldehyde as well as benzaldehyde is used to manufacture the initial hexyl cinnamaldehyde by one-step method. The response conditions are moderate as well as the item is easy to cleanse. Handling, the item fragrance is pure, the steps consist of:
a) Benzaldehyde, adding about 30% of n-octylaldehyde in the reactor in a molar ratio of 1:1 to 0.5, and afterwards adding a condensation stimulant in a proportion of 1 to 10% by weight of benzaldehyde;
b) open up the home heating and mixing reaction pot, heat up to 35 ～ 40 ℃, after the pot temperature level is steady, start to trickle the n-octaldehyde of 30% web content, control the reaction temperature level to 38 ℃ ～ 42 ℃, react under normal stress, 30% n-octaldehyde The dropwise addition amount is 1:1 ~ 0.5 (100% in n-octylaldehyde) by benzaldehyde mol proportion, and the including time is regulated at 4 ~ 6 hrs;
c) tasting and also testing after the dropwise enhancement is finished, when the n-octaldehyde web content is less than 0.5%, it is judged that the reaction is completed, as well as antarctic acetic acid is contributed to end the response, neutralized to pH 6.5 to 7.0 of the response system, split, and also the reduced layer water is divided;
d) move the item after water separation in step c) to the autoclave flash column, the temperature level on top of the column is 60 ～ 90 ℃, under the condition of vacuum pressure 1000 ～ 3000Pa, unreacted benzaldehyde and also n-octanol in the flash Total recovery and distillation, when the temperature level at the top of the tower goes down or does not release, the flash recovery of n-octanol ends;
e) move the unrefined product symphonious d) into the autoclave fixing tower, manage the tower top temperature 120 ～ 150 ℃, vacuum stress 133 ～ 1000Pa, reflux ratio 1:1 ～ 1:10 fractional distillation, get qualified item content 99.0 wt%.
The condensation driver added in the action a) is 1-10% potassium hydroxide or 1-10% sodium hydroxide.
The activator in the action a) is an enamel reactor.
When the material of n-octaldehyde detected in c) tasting described in step c) is above 0.5%, the response is continued with heat preservation as well as mixing until the web content of n-octaldehyde reaches below 0.5%.
The optimal reflux proportion in the step e) is 1:2 ~ 1:3.
The autoclave flash column and also the autoclave rectification column are specifically filled with BX500 and also cy700 stainless-steel cord corrugated cable mesh packings.
One more object of today development is to give a tool for directly synthesizing the very first Alpha-Hexylcinnamaldehyde with a reduced material of n-octylaldehyde, including a mixing container as well as a n-octylcinnamaldehyde gathering storage tank, and the mixing container is connected with the lye to a header tank and a benzaldehyde The total tank is gone through the very first chemical pump, and also the bottom of the lye top-level storage tank as well as the benzaldehyde total amount container is connected with the enamel response pot with the pipeline, and also the n-octaldehyde total tank is gotten in touch with the enamel reaction pot via the pipe  Drop volume pump, The enamel response kettle is also connected with the antarctic acetic acid accumulating tank, the discharge port of the enamel response kettle is gotten in touch with the upright accumulating tank through the second chemical pump, and the upright gathering container is gotten in touch with the autoclave via the 3rd chemical pump The flash tower is connected, and the top of the autoclave flash tower is gotten in touch with the first gas-liquid separator via the very first spiral plate heat exchanger, and the first gas-liquid separator is all-time low of the autoclave flash tower and also the very first gas-liquid separator. The initial receiving tank is linked, the 4th chemical pump is connected with the autoclave rectification tower, the top of the autoclave rectification tower is gotten in touch with the 2nd gas-liquid separator with an additional spiral plate warm exchanger, the 2nd The gas-liquid separator is gotten in touch with the second receiving container. The top of the autoclave flash tower is connected with the initial gas-liquid separator with the initial spiral plate warmth exchanger, the very first gas-liquid separator is connected with the initial receiving tank, and the autoclave flashes The 4th chemical pump at the end of the steaming tower is connected with the autoclave correction tower, and also the top of the autoclave rectification tower is connected with the 2nd gas-liquid separator with the second spiral plate warm exchanger, as well as the 2nd gas-liquid separation The gadget is linked to the second receiving tank. The top of the autoclave flash tower is connected with the very first gas-liquid separator through the very first spiral plate warmth exchanger, the first gas-liquid separator is connected with the very first finding container, as well as the autoclave flashes The fourth chemical pump at the bottom of the steaming tower is connected with the autoclave correction tower, as well as the top of the autoclave rectification tower is gotten in touch with the 2nd gas-liquid separator through the secondary spiral plate warm exchanger, and the 2nd gas-liquid separation The gadget is linked to the 2nd finding storage tank. The top of the autoclave correction tower is connected with the 2nd gas-liquid separator via the secondary spiral plate heat exchanger, and the second gas-liquid separator is connected with the second receiving storage tank. The top of the autoclave correction tower is connected with the second gas-liquid separator with the additional spiral plate heat exchanger, as well as the 2nd gas-liquid separator is connected with the second receiving tank.
The advantageous results of the here and now development are as follows: the technical system of today development adopts benzaldehyde and also 30% n-octyl aldehyde as resources, and in the visibility of a catalyst, Alpha-Hexylcinnamaldehyde is synthesized under normal stress to obtain Alpha-Hexylcinnamaldehyde, and also after the n-octanol is recuperated by flash evaporation, the Rectification obtains a qualified item with a material of 99.0 wt%. For that reason, the technique of the development addresses the spin-off hexylnonenal generated by the self-condensation of n-octylaldehyde when the material is high, overcomes the imperfection that the smell of hexylnonenal prevents the scent of floral products, and has the advantages of reduced production cost, high purity of ended up products, and also fragrance. Pure personality.