CN210506155U

CN210506155U - Process system for producing citronellyl formate

Info

Publication number: CN210506155U
Application number: CN201920860789.6U
Authority: CN
Inventors: 姚婉平
Original assignee: Shanghai Pu Jie Fragrance Co ltd
Current assignee: Shanghai Pu Jie Fragrance Co ltd
Priority date: 2019-06-06
Filing date: 2019-06-06
Publication date: 2020-05-12
Anticipated expiration: 2029-06-06

Abstract

The utility model provides a process system for producing citronellyl formate, which comprises a mixing kettle (2) for mixing formic acid and citronellol and further carrying out esterification reaction, a liquid separating kettle (4) and a distillation kettle (5); the mixing kettle (2) is connected with the liquid separating kettle (4), the liquid separating kettle (4) is provided with a liquid outlet (10), and the liquid outlet (10) is connected with the distillation kettle (5); and a discharge port is arranged at the middle upper part of the distillation kettle (5) and used for returning the extracted front fraction to the mixing kettle (2) to participate in esterification reaction and extracting citronellyl formate. The utility model provides a process systems of production citronellyl formate can make to add the measurement accurate, easy operation, and equipment investment is few, has practiced thrift area, and economic nature is high.

Description

Process system for producing citronellyl formate

Technical Field

The utility model relates to a process systems of production chemical products, in particular to process systems of production citronellyl formate.

Background

Esterification is a type of organic chemical reaction, which is the reaction of alcohol with carboxylic acid or oxygen-containing inorganic acid to produce ester and water. The method is divided into three types of reactions, namely a reaction of carboxylic acid and alcohol, a reaction of inorganic oxyacid and alcohol and a reaction of inorganic strong acid and alcohol. Esterification of carboxylic acids with alcohols is reversible and generally very slow, so catalysts are often required. The esterification reaction is widely applied to the fields of organic synthesis and the like.

The traditional esterification process is limited by the equilibrium of esterification reaction, generally the equilibrium conversion rate is lower, so in order to accelerate the reaction, in addition to adding a catalyst in the reaction process, the product can be distilled in time to promote the reaction and improve the conversion rate, which requires a distillation device to be added besides a necessary reaction kettle in the production process, thereby increasing the equipment cost.

The citronellyl formate is widely applied to chemical products such as coating, essential oil, food and the like and daily chemical products. The production of citronellyl formate is a common basic process, and few documents and patents are available for researching the process system for producing citronellyl formate. The preparation of citronellyl formate in the prior art is reported in A Convenient Stereospecific Reduction of epoxides and thiohydrans to aldehydes, Philip E.Sonnet, Synthesis [1980, (10),828-830] that the corresponding citronellyl formate is prepared catalytically with an epoxy compound of citronellal, which is not suitable for large-scale production due to the low availability of the starting materials used in the process and the use of a relatively expensive catalyst. The reaction of formic acid with citronellol in the absence of a catalyst to form citronellyl formate is reported in chemistry of voltalide Compounds from parachloroac glans of the american crocodile (crocodius acutus), Silvina garca-Rubio et al. journal of chemical ecology [2002,28(04), 769-. The reaction of citronellyl formate with formic acid with citronellol with heating is reported in Ueber d-und-Configurationen inder citronellal reihe, Chemische Berichte [1898,30,33-38 ].

Production equipment in the prior art comprises a reaction kettle, the reaction kettle occupies a large area, the subsequent maintenance work on the reaction kettle consumes time and labor, and the fixed investment of the equipment is increased. The utility model discloses combine actual production state, invent a production technology system of citronellyl formate, make add measurement accurate, easy operation, equipment investment is few.

SUMMERY OF THE UTILITY MODEL

The to-be-solved technical problem of the utility model is to overcome the problem that equipment is more among the prior art, equipment investment is great, the operation is complicated, production efficiency is not high, provide a process systems of production citronellyl formate.

The utility model discloses an above-mentioned technical problem is solved through following technical scheme: a process system for producing citronellyl formate is characterized by comprising a mixing kettle, a liquid separating kettle and a distilling kettle, wherein the mixing kettle is used for mixing formic acid and citronellol and further carrying out esterification reaction; the mixing kettle is connected with the liquid separating kettle, the liquid separating kettle is provided with a liquid outlet, and the liquid outlet is connected with the distillation kettle; and a discharge port is arranged at the middle upper part of the distillation kettle and used for returning the extracted front fraction to the mixing kettle to participate in esterification reaction and extracting citronellyl formate.

Preferably, the front cut comprises water with a small amount of unreacted formic acid.

Preferably, the process system for producing the citronellyl formate comprises a metering system, and the metering system is connected with the other feed inlet of the mixing kettle.

Preferably, the process system for producing citronellyl formate further comprises a storage tank, wherein a feed inlet of the storage tank is connected with a discharge outlet of the mixing kettle, a discharge outlet of the storage tank is connected with a feed inlet of the liquid separating kettle, and the storage tank is used for storing excessive reaction products.

Preferably, the bottom of the liquid separation kettle is also provided with a water outlet, and the water outlet is connected with a waste water collection tank.

Preferably, be equipped with the trip valve between the outlet with the waste water collection tank, the setting of trip valve can adjust the liquid level of aqueous phase in the oil-water separator more accurately.

Preferably, the second discharge port is communicated with a product tank.

Preferably, the liquid outlet is positioned at the upper part of the cavity of the liquid separating kettle.

In a preferred embodiment of the present invention, the discharge port of the distillation still further comprises a first discharge port and a second discharge port, the first discharge port is connected to a feed port of the mixing still for returning the extracted front fraction to the mixing still to participate in the esterification reaction; and the second discharge hole is used for extracting citronellyl formate.

According to the technical scheme, formic acid, citronellol and an acid catalyst are added into a mixing kettle according to a certain proportion to react to obtain a product, the product enters a liquid separation kettle, the oil phase density is lower than the water phase density, the mixture is placed for a period of time and then layered, the upper layer is the oil phase, the lower layer is the water phase, the water phase enters a wastewater collection tank through a water outlet, the oil phase enters a distillation kettle through a liquid outlet to be further purified, and a citronellyl formate product is collected in a product tank through a second discharge outlet. The front distillate product after distillation can enter the mixing kettle through the first discharge hole to react again. The method used in the utility model breaks the thought of using excessive formic acid in the traditional process, adopts the expensive method of citronellol excess which is easy to be recovered, makes the formic acid react completely, reduces the pollution to the water phase caused by the excessive retention in the water phase.

The utility model has the advantages that:

1. the utility model provides a production citronellyl formate's process systems adopts mixed cauldron to replace reation kettle, has reduced area, has practiced thrift the maintenance cost to reation kettle, and economic nature is high.

2. The utility model provides a production citronellyl formate's process systems, the system is simple, convenient operation.

Drawings

FIG. 1 is a schematic flow chart of a process system for producing citronellyl formate according to the present invention.

In the attached drawings, 1, a metering system, 2, a mixing kettle, 3, a storage tank, 4, a liquid separating kettle, 5, a distillation kettle, 6, a product tank, 7, a waste water collecting tank, 8, a first discharge port, 9, a second discharge port, 10, a liquid outlet, 11 and a water outlet.

Detailed Description

The present invention is further illustrated by way of the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.

The process system for producing citronellyl formate shown in fig. 1 comprises 1 metering system 1, 1 mixing kettle 2, 1 storage tank 3, 1 liquid separation kettle 4 and 1 distillation kettle 5. Metering system 1, mixing kettle 2, basin 3, divide liquid cauldron 4 to connect gradually, wherein divide liquid cauldron 4's liquid outlet 10 and be connected with the stills, divide liquid cauldron 4's outlet 11 and waste water collection tank 7 to be connected, and stills 5's first discharge gate 8 is connected with a feed inlet of mixing kettle, and stills 5's second discharge gate 9 is linked together with product jar 6.

Measuring 30kg of formic acid, 120kg of citronellol and 3kg of p-toluenesulfonic acid by using a measuring system 1, introducing into a mixing kettle 2 for reaction to obtain a product, introducing into a storage tank 3 for temporary storage, then introducing into a liquid separation kettle 4, and standing for 72 hours because the density of an oil phase is lower than that of a water phase, wherein the upper layer is the oil phase and the lower layer is the water phase. Taking the upper oil phase for analysis, when the ester content in the oil phase is more than 82%, separating the oil phase, enabling the water phase to enter a wastewater collection tank 7 through a water outlet 11, enabling the upper oil phase to enter a distillation kettle 5 through a liquid outlet 10 for further purification, collecting the citronellyl formate product in a product tank 6 through a second discharge port 9, and enabling the distilled front fraction to enter a mixing kettle 2 through a first discharge port 8 for re-reaction. The utility model discloses a practice thrift and take up an area of, increase efficiency, effect such as device is simple.

Claims

1. A process system for producing citronellyl formate is characterized by comprising a mixing kettle (2) for mixing formic acid and citronellol and further carrying out esterification reaction, a liquid separating kettle (4) and a distillation kettle (5); the mixing kettle (2) is connected with the liquid separating kettle (4), the liquid separating kettle (4) is provided with a liquid outlet (10), and the liquid outlet (10) is connected with the distillation kettle (5); and a discharge port is arranged at the middle upper part of the distillation kettle (5) and used for returning the extracted front fraction to the mixing kettle (2) to participate in esterification reaction and extracting citronellyl formate.

2. The process system for producing citronellyl formate according to claim 1, wherein: the device also comprises a metering system (1), wherein the metering system (1) is connected with the mixing kettle (2).

3. The process system for producing citronellyl formate according to claim 1, wherein: the liquid separating device is characterized by further comprising a storage tank (3), wherein a feed inlet of the storage tank (3) is connected with the mixing kettle (2), and a discharge outlet of the storage tank is connected with a feed inlet of the liquid separating kettle (4).

4. The process system for producing citronellyl formate according to claim 1, wherein: the bottom of the liquid separation kettle (4) is also provided with a water outlet (11), and the water outlet (11) is connected with a waste water collection tank (7).

5. The process system for producing citronellyl formate according to claim 4, wherein: a stop valve is arranged between the water outlet (11) and the waste water collecting tank (7).

6. The process system for producing citronellyl formate according to claim 1, wherein: the liquid outlet (10) is positioned at the middle upper part of the cavity of the liquid separating kettle (4).

7. The process system for producing citronellyl formate according to claim 1, wherein: the discharge holes of the distillation kettle (5) comprise a first discharge hole (8) and a second discharge hole (9), the first discharge hole (8) is connected with a feed hole of the mixing kettle (2) and is used for returning the extracted front fraction to the mixing kettle (2) to participate in esterification reaction; the second discharge hole (9) is used for extracting citronellyl formate.

8. The process system for producing citronellyl formate according to claim 7, wherein: the second discharge hole (9) is communicated with a product tank (6).