阅读说明：本技术 一种香料青草醛的合成方法 (Synthetic method of perfume green grass aldehyde ) 是由 陶一竑 汤佳音 汤佳迎 于 2019-11-26 设计创作，主要内容包括：本发明公开了一种香料青草醛的的合成方法,将异戊二烯投入反应釜,降温至0～10℃,加入氯化钠,缓慢滴加盐酸,控制温度0～10℃,加完,合成中间体氯代异戊烯；将中间体氯代异戊烯称重,异丁醛用量,合并混溶,抽入高位槽,待用；在反应釜中配置1200kg碱液,加入5kg四丁基溴化铵；升温至68℃,滴入高位槽中物料,温度控制在68～70℃,滴加时间2～2.5小时；再保温2小时,取样检测,控制控制青草醛含量≥70％；将青草醛粗品投入蒸馏釜减压蒸馏。本发明工艺简单可控,青草醛的收率较高。(The invention discloses a synthesis method of aromatic aldehyde, which comprises the steps of putting isoprene into a reaction kettle, cooling to 0-10 ℃, adding sodium chloride, slowly dropwise adding hydrochloric acid, controlling the temperature to 0-10 ℃, and synthesizing an intermediate chloro isoamylene after the addition; weighing intermediate chloroisopentene, mixing and dissolving isobutyraldehyde, and pumping into an overhead tank for later use; preparing 1200kg of alkali liquor in a reaction kettle, and adding 5kg of tetrabutylammonium bromide; heating to 68 ℃, and dripping the materials in the elevated tank for 2-2.5 hours at 68-70 ℃; preserving the heat for 2 hours, sampling and detecting, and controlling the content of the turfgrass aldehyde to be more than or equal to 70 percent; and putting the crude product of the green grass aldehyde into a distillation still for reduced pressure distillation. The method has the advantages of simple and controllable process and higher yield of the green grass aldehyde.)

1. A synthetic method of perfume turfgraldehyde is characterized by comprising the following steps:

the method comprises the following steps: synthesis of intermediate chloroisopentene: putting isoprene into a reaction kettle, cooling to 0-10 ℃, adding sodium chloride, slowly dropwise adding hydrochloric acid, controlling the temperature to 0-10 ℃, after the addition is finished, carrying out suction filtration and layering after the detection is qualified, using salt for application, using hydrochloric acid at the lower layer for application, adding a sodium carbonate solution to wash the organic layer to be neutral for later use;

step two: weighing intermediate chloroisopentene, using the amount of isobutyraldehyde, mixing and dissolving, and pumping into an overhead tank. Standby; preparing 1200kg of alkali liquor in a reaction kettle, and adding 5kg of tetrabutylammonium bromide; heating to 68 ℃, and dripping the materials in the elevated tank for 2-2.5 hours at 68-70 ℃; preserving the heat for 2 hours, sampling and detecting, and controlling the content of the turfgrass aldehyde to be more than or equal to 70 percent; putting the crude product of the green grass aldehyde into a distillation still, recovering isoprene at normal pressure, after the recovery of the isoprene is finished, distilling under reduced pressure until the content of the green grass aldehyde is more than 80.0%, detecting, packaging and warehousing.

2. The method for synthesizing aromatic vanillin of claim 1, wherein: in the first step, 500L of isoprene is put into a reaction kettle, the temperature is reduced to 0-10 ℃, 90kg of sodium chloride is added, 1400kg of 30% hydrochloric acid is slowly dripped, the temperature is controlled to 0-10 ℃, and the addition is finished; the dripping time is controlled to be about 4 hours, the temperature is kept for 2 hours, and sampling and detection are carried out. Isoprene is less than or equal to about 2 percent, the reaction is finished, the content of the intermediate chloroisoamylene is about 70 percent, and 15-20 kg of sodium chloride is added when the content is not reached.

3. The method for synthesizing aromatic vanillin of claim 1, wherein: in the second step, according to the reaction condition of the raw materials, the chloroisoamylene is reacted completely, if the reaction is not completed, the isobutyraldehyde is supplemented until the reaction is completed, and the reaction product is washed to be neutral by using brine.

4. The method for synthesizing aromatic vanillin of claim 1, wherein: the alkali liquor is 330kg of sodium hydroxide and 870kg of water.

Technical Field

The invention belongs to the field of organic compound synthesis, and particularly relates to a synthesis method of aromatic aldehyde.

Background

The green grass aldehyde is a common spice and has wide application, but the prior art lacks a mature synthesis method.

Disclosure of Invention

The invention aims to provide a synthesis method of aromatic aldehyde, which has simple and controllable process and higher yield of the aldehyde.

In order to achieve the purpose, the invention adopts the following technical scheme: a synthetic method of aromatic aldehyde comprises the following steps:

the method comprises the following steps: synthesis of intermediate chloroisopentene: putting isoprene into a reaction kettle, cooling to 0-10 ℃, adding sodium chloride, slowly dropwise adding hydrochloric acid, controlling the temperature to 0-10 ℃, after the addition is finished, carrying out suction filtration and layering after the detection is qualified, using salt for application, using hydrochloric acid at the lower layer for application, adding a sodium carbonate solution to wash the organic layer to be neutral for later use;

step two: weighing intermediate chloroisopentene, using the amount of isobutyraldehyde, mixing and dissolving, and pumping into an overhead tank. Standby; preparing 1200kg of alkali liquor in a reaction kettle, and adding 5kg of tetrabutylammonium bromide; heating to 68 ℃, and dripping the materials in the elevated tank for 2-2.5 hours at 68-70 ℃; preserving the heat for 2 hours, sampling and detecting, and controlling the content of the turfgrass aldehyde to be more than or equal to 70 percent; putting the crude product of the green grass aldehyde into a distillation still, recovering isoprene at normal pressure, after the recovery of the isoprene is finished, distilling under reduced pressure until the content of the green grass aldehyde is more than 80.0%, detecting, packaging and warehousing.

Further preferably, in the first step, 500L of isoprene is put into a reaction kettle, the temperature is reduced to 0-10 ℃, 90kg of sodium chloride is added, 1400kg of 30% hydrochloric acid is slowly dripped, the temperature is controlled to 0-10 ℃, and the addition is finished; the dripping time is controlled to be about 4 hours, the temperature is kept for 2 hours, and sampling and detection are carried out. Isoprene is less than or equal to about 2 percent, the reaction is finished, the content of the intermediate chloroisoamylene is about 70 percent, and 15-20 kg of sodium chloride is added when the content is not reached.

Preferably, in the second step, according to the reaction condition of the raw materials, the chloroisoamylene is completely reacted, if the reaction is not completely finished, the isobutyraldehyde is supplemented until the reaction is completely finished, and the chloroisoamylene is washed to be neutral by the brine.

The invention has the technical effects that: the method has the advantages that the process is simple and controllable, the yield of the green grass aldehyde is high, and the green grass aldehyde is widely used in the perfume.

Detailed Description

The present invention will be explained in further detail below with reference to examples for the purpose of facilitating understanding.

A method for synthesizing aromatic aldehyde,

the chemical reaction formula is as follows: c₅H₈+HCl→C₅H₉Cl+C₄H₈O→C₉H₁₆O+HCl

The method comprises the following steps: synthesis of intermediate chloroisopentene: putting 500L of isoprene into a reaction kettle, cooling to 0-10 ℃, adding 90kg of sodium chloride, slowly dropwise adding 1400kg of 30% hydrochloric acid, controlling the temperature to 0-10 ℃, and finishing the addition; the dripping time is controlled to be about 4 hours, the temperature is kept for 2 hours, and sampling and detection are carried out. Isoprene is less than or equal to about 2 percent, the reaction is finished, the content of the intermediate chloroisoamylene is about 70 percent, and 15-20 kg of sodium chloride is added when the content is not reached. Sampling and detecting after 20 min. And after the detection is qualified, carrying out suction filtration and layering, using sodium chloride, using hydrochloric acid at the lower layer (matched with 30% hydrochloric acid), using an organic layer at the upper layer, and adding a sodium carbonate solution to wash the organic layer until the organic layer is neutral for later use.

Step two: weighing intermediate chloroisopentene, using isobutyraldehyde (chloroisopentene net weight 70% 1.18), mixing, pumping into a head tank for standby. 1200kg of an alkali solution (330kg of sodium hydroxide +870kg of water) was prepared in a reaction vessel, and 5kg of tetrabutylammonium bromide was added. And heating to 68 ℃, and dripping the materials in the elevated tank for 2-2.5 hours at 68-70 ℃. And preserving the heat for 2 hours, and sampling and detecting. The content of the green grass aldehyde is controlled to be more than or equal to 70 percent. The raw material reaction condition is observed, the chloroisoamylene is completely reacted, and if the chloroisoamylene is not completely reacted, the isobutyraldehyde is added until the reaction is completely finished. Washed with brine to neutral. Putting the crude product of the turfgrass aldehyde into a distillation still, recovering isoprene (which can be used after the content is detected) at normal pressure, and after the recovery of the isoprene is finished, carrying out reduced pressure distillation (the internal temperature is 130 ℃) until the turfgrass aldehyde content is more than 80.0%. And (6) detecting, packaging and warehousing.