CN216321891U

CN216321891U - Continuous production device of dodecyl alcohol ester

Info

Publication number: CN216321891U
Application number: CN202122570267.2U
Authority: CN
Inventors: 王恒秀; 陈纪忠; 张千; 陈维斌; 顾海平; 吕乘欣
Original assignee: Lianyungang Zhonggang Fine Chemical Co ltd; Shandong Hengxing New Material Technology Co ltd; Jiangsu Hengxing New Material Technology Co ltd
Current assignee: Lianyungang Zhonggang Fine Chemical Co ltd; Shandong Hengxing New Material Technology Co ltd; Jiangsu Hengxing New Material Technology Co ltd
Priority date: 2021-10-25
Filing date: 2021-10-25
Publication date: 2022-04-19
Anticipated expiration: 2031-10-25

Abstract

A continuous production device of dodecyl alcohol ester belongs to the technical field of organic synthesis reaction devices and comprises a stirring kettle, a coil reactor and a tubular heat exchanger, wherein the coil reactor is fixedly arranged in the stirring kettle, an inlet end of the coil reactor is fixedly communicated with a feeding pipe A, the feeding pipe A penetrates through the side wall of the stirring kettle and extends out of the kettle, and an outlet end of the coil reactor is directly communicated with the inside of the stirring kettle; the top of the stirring kettle is fixedly communicated with a charging pipe B, the top of the stirring kettle is provided with a stirrer, the lower part of the stirrer is connected with a stirring shaft extending into the stirring kettle, and the outer side wall of the stirring kettle is provided with a kettle wall heat exchanger; the outlet end of the stirring kettle is communicated with the inlet end pipeline of the tube array heat exchanger, the outlet end of the tube array heat exchanger is respectively communicated with the discharge pipe and the inlet end of the circulating pipeline, the outlet end of the circulating pipeline is communicated with an inlet pipe opening at the side wall of the upper part of the stirring kettle, and a valve is arranged in the middle of each section of pipeline. The temperature of the reaction process is respectively controlled to be matched with the reaction characteristics, so that the reaction heat is effectively utilized and the reaction result is optimized.

Description

Continuous production device of dodecyl alcohol ester

Technical Field

The utility model relates to the technical field of organic synthesis reaction devices, in particular to a continuous production device for dodecyl alcohol ester.

Background

The dodecyl alcohol ester (also called alcohol ester dodecyl or Texanol ester) with the scientific name of 2, 2, 4-trimethyl-1, 3-pentanediol monoisobutyrate is a transparent oily liquid with high boiling point, water insolubility, low freezing point, good stability, no toxicity and no harm. Mainly used as a film forming aid, a synthetic lubricant and a plasticizer of the latex paint, compared with a common film forming aid, the dodecyl alcohol ester has the advantages that: the resin has good phase solubility, small dosage, low film forming temperature, good film leveling property, good color development, low freezing point, good hydrolytic stability and low toxicity, and is a novel green additive.

In the prior art, in order to simplify the mixing of production equipment and liquid-liquid phase materials, a batch production process of the dodecanol ester synthesis reaction is mostly completed by adopting a stirring kettle. For example, CN1417195 is reacted for 0.5 to 8 hours at 48 to 150 ℃, and the target product of dodecyl alcohol ester is obtained by one-step synthesis. CN1380281 is made by controlling the reaction speed and material temperature by adding isobutyraldehyde dropwise, CN106699556A alternately adding raw material and catalyst, and reacting stepwise to reduce the reaction degree, thereby controlling the reaction heat and reaction temperature increase. In patent CN1325841, water and aqueous solution of sodium hydroxide are first put into a reaction kettle, and then isobutyraldehyde is slowly added under stirring, so as to avoid the reaction temperature from being difficult to control due to too violent reaction. Two reaction kettles are also adopted to carry out aldol condensation reaction and esterification reaction respectively, and different catalysts are also used in some cases. The method of CN01838197A comprises the steps of putting water and a sodium hydroxide aqueous solution into an aldol condensation reaction kettle, controlling the pH = 12-13 of a reaction solution, controlling the reaction temperature at 28-52 ℃, cooling the reaction solution to 20-25 ℃ after the material addition for 10 min-2H, standing for 30 min-6H, putting an upper layer (oil layer) into the esterification reaction kettle, starting stirring, heating the reaction solution to 45 ℃ by introducing steam into a jacket, and adding a catalyst Ba (OH) 2.8H 2O for reaction. However, the batch synthesis process and the device used by the process have the problems of complex operation process, difficult temperature control, increased side reactions and low production efficiency, and are difficult to realize clean production.

SUMMERY OF THE UTILITY MODEL

The utility model provides a continuous production device of dodecyl alcohol ester, which aims to overcome the defects that in a tubular reactor, isobutyraldehyde condensation reaction with high reaction speed and the disproportionation reaction of generated 2, 2, 4-trimethyl-3-hydroxypentanal and isobutyraldehyde are carried out at low temperature so as to inhibit the trimerization of isobutyraldehyde to generate byproducts; carrying out esterification reaction with slower reaction speed by using a reaction kettle with cooling and stirring to generate a target product of dodecyl alcohol ester, and cooling and reducing the temperature by a tube heat exchanger after discharging materials of the stirring kettle to improve the conversion rate of the esterification reaction; the temperature in the reaction process is respectively controlled to be matched with the reaction characteristics, so that the reaction heat is effectively utilized and the reaction result is optimized.

In order to achieve the purpose, the utility model provides the following technical scheme: a continuous production device of dodecyl alcohol ester comprises a stirring kettle, a coil reactor and a tubular heat exchanger, wherein the coil reactor is fixedly arranged in the stirring kettle, an inlet end of the coil reactor is fixedly communicated with a feeding pipe A, the feeding pipe A penetrates through the side wall of the stirring kettle and extends out of the kettle, and an outlet end of the coil reactor is directly communicated with the inside of the stirring kettle; the top of the stirring kettle is fixedly communicated with a charging pipe B, the top of the stirring kettle is provided with a stirrer, the lower part of the stirrer is connected with a stirring shaft extending into the stirring kettle, and the outer side wall of the stirring kettle is provided with a kettle wall heat exchanger; the stirred tank outlet end is communicated with a tube heat exchanger inlet end pipeline, the tube heat exchanger outlet end is respectively communicated with a discharge pipe and a circulation pipeline inlet end, the circulation pipeline outlet end is communicated with an inlet pipe opening at the side wall of the upper part of the stirred tank, and a valve is arranged in the middle of each section of pipeline. The working principle is as follows: firstly: introducing the pre-mixed isobutyraldehyde and the catalyst into a coil reactor arranged in a stirred tank through a feeding pipe A to perform isobutyraldehyde condensation reaction with a higher reaction speed and disproportionation reaction of a generated product, directly feeding the material discharged by the coil reactor into the stirred tank to perform esterification reaction with a lower reaction speed to generate a target product of dodecyl alcohol ester, and controlling the reaction temperature and the reaction speed in the stirred tank by using a tank wall heat exchanger and a stirrer; secondly, the stirred tank material is discharged and is cooled by a tubular heat exchanger to improve the conversion rate of the esterification reaction, meanwhile, partial material discharged by the tubular heat exchanger can enter the stirred tank through a circulating pipeline under the control of a valve to adjust the reaction temperature in the stirred tank, so that the reaction efficiency is improved, and other partial material discharged by the tubular heat exchanger is discharged through a discharging pipe, so that the continuous reaction and production of the dodecanol ester are finally realized.

Further preferred scheme: the coil reactor is formed by stacking a plurality of U-shaped tubes up and down, the inlet and outlet ends of two adjacent U-shaped tubes are sequentially communicated in order, and a cooling sleeve is arranged outside the coil reactor. The U-shaped pipes are stacked to form the coil reactor, so that the space is saved, the reaction time of reactants in the pipes can be prolonged, and the reaction sufficiency is guaranteed.

Further preferred scheme: and a pipeline delivery pump is fixedly arranged on a pipeline between the outlet end of the stirring kettle and the inlet end of the tube heat exchanger. The pipeline delivery pump is arranged, so that substances generated by the reaction of the stirring kettle can be timely sent into the tube still heat exchanger for cooling by using external force, and the improvement of the conversion rate of the esterification reaction is facilitated.

Further preferred scheme: the stirring shaft penetrates through the coil reactor from top to bottom without contacting, and the bottom end of the stirring shaft is connected with two annular stirring rings. The stirring shaft with enough length is arranged, and the stirring ring is arranged at the bottom of the stirring shaft, so that the contact area between the stirring shaft and the reactant can be increased, and the stirring effect can be promoted.

Further preferred scheme: and cooling water inlets and outlets are respectively arranged at diagonal positions of the wall of the shell and tube heat exchanger. The cooling water inlet and the cooling water outlet are arranged at the diagonal positions of the heat exchanger, so that the circulation path of the cooling water can be prolonged to the maximum degree, and the cooling water can be fully utilized to cool.

Further preferred scheme: the kettle wall heat exchanger consists of a plurality of bent heat exchange tubes and is wound on the outer side wall of the stirring kettle. The heat exchanger formed by the bent heat exchange tubes is arranged, so that the wall of the stirring kettle can be wrapped, and the heat exchange effect is favorably improved.

The utility model provides a continuous production device of dodecanol ester, which has the following beneficial effects:

1. according to the method, isobutyraldehyde condensation reaction with high reaction speed and disproportionation reaction of generated 2, 2, 4-trimethyl-3-hydroxypentanal and isobutyraldehyde are carried out at low temperature in a tubular reactor, so that the generation of byproducts by trimerization of isobutyraldehyde is inhibited; carrying out esterification reaction with slower reaction speed by using a reaction kettle with cooling and stirring to generate a target product of dodecyl alcohol ester, and cooling and reducing the temperature by a tube heat exchanger after discharging materials of the stirring kettle to improve the conversion rate of the esterification reaction; the temperature in the reaction process is respectively controlled to be matched with the reaction characteristics, so that the reaction heat is effectively utilized and the reaction result is optimized.

2. The utility model has the advantages that the U-shaped pipes are stacked to form the coil pipe reactor, so that the space is saved, the reaction time of reactants in the pipe can be prolonged, and the reaction sufficiency is favorably ensured; the stirring shaft with enough length is arranged, and the stirring ring is arranged at the bottom of the stirring shaft, so that the contact area between the stirring shaft and the reactant can be increased, and the stirring effect can be promoted.

Drawings

Fig. 1 is a schematic view of the connection structure of the whole system of the present invention.

FIG. 2 is a schematic structural diagram of a coil reactor according to the present invention.

FIG. 3 is a schematic view of the configuration of the stirring shaft of the present invention.

FIG. 4 is a schematic view of the distribution of the heat exchangers in the still wall according to the present invention.

In FIGS. 1-4: 1. a feeding pipe A; 2. a coil reactor; 3. stirring the mixture in a kettle; 4. a kettle wall heat exchanger; 5. a pipeline delivery pump; 6. a valve; 7. a shell and tube heat exchanger; 8. a cooling water inlet and outlet; 9. a circulation line; 10. a discharge pipe; 11. feed tubes B, 12 and a stirrer; 13. a stirring shaft; 1301. and (4) stirring a ring.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 to 4 in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example (b):

please refer to fig. 1 to 4:

a twelve carbon alcohol ester continuous production device, the coil reactor 2 is fixedly arranged in a stirred tank 3, the inlet end of the coil reactor 2 is fixedly communicated with a feed pipe A1, the feed pipe A1 penetrates through the side wall of the stirred tank 3 and extends out of the stirred tank, and the outlet end of the coil reactor 2 is directly communicated with the inside of the stirred tank 3; the top of the stirring kettle 3 is fixedly communicated with a charging pipe B11, the top of the stirring kettle 3 is provided with a stirrer 12, the lower part of the stirrer 12 is connected with a stirring shaft 13 extending into the stirring kettle 3, the outer side wall of the stirring kettle 3 is provided with a kettle wall heat exchanger 4, and the kettle wall heat exchanger 4 consists of a plurality of bent heat exchange pipes and is wound and connected on the outer side wall of the stirring kettle 3; the outlet end of the stirring kettle 3 is communicated with the inlet end pipeline of the tube heat exchanger 7, a pipeline delivery pump 5 is fixedly arranged on the pipeline between the outlet end of the stirring kettle 3 and the inlet end of the tube heat exchanger 7, a cooling water inlet and outlet 8 is respectively arranged at the diagonal positions of the wall of the tube heat exchanger 7, the outlet end of the tube heat exchanger 7 is respectively communicated with a material discharging tube 10 and the inlet end of a circulating pipeline 9, the outlet end of the circulating pipeline 9 is communicated with an inlet tube opening at the upper side wall of the stirring kettle 3, and a valve 6 is arranged in the middle of each section of pipeline.

The coil reactor 2 is formed by stacking a plurality of U-shaped tubes up and down, the inlet and outlet ends of two adjacent U-shaped tubes are sequentially communicated in order, and a cooling sleeve is arranged outside the coil reactor 2.

The stirring shaft 13 penetrates through the coil reactor 2 from top to bottom without contacting, and the bottom end of the stirring shaft 13 is connected with two annular stirring rings 1301.

The working principle is as follows: firstly: introducing the pre-mixed isobutyraldehyde and the catalyst into a coil reactor 2 arranged in a stirred tank 3 through a feeding pipe A1 to perform isobutyraldehyde condensation reaction with a higher reaction speed and disproportionation reaction of a generated product, directly feeding the material discharged by the coil reactor 2 into the stirred tank 3 to perform esterification reaction with a lower reaction speed to generate a target product, namely dodecyl alcohol ester, and controlling the reaction temperature and the reaction speed in the stirred tank 3 by using a tank wall heat exchanger 4 and a stirrer 12; secondly, stirred tank 3 material is discharged and is cooled down through tubular heat exchanger 7 to improve esterification reaction's conversion rate, and the partial material of tubular heat exchanger 7 exhaust simultaneously can get into stirred tank 3 through circulation line 9 under the control of valve 6 and adjust the reaction temperature in the cauldron, and then promotes reaction efficiency, and other partial materials of tubular heat exchanger 7 exhaust are then discharged through arranging material pipe 10, finally realize continuous reaction, the production of dodecanol fat.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the utility model, the scope of which is defined in the appended claims and their equivalents.

Claims

1. The utility model provides a continuous production device of twelve carbon alcohol fat, includes stirred tank (3), coil reactor (2), shell and tube heat exchanger (7), its characterized in that: the coil reactor (2) is fixedly arranged in the stirring kettle (3), an inlet end of the coil reactor (2) is fixedly communicated with a feeding pipe A (1), the feeding pipe A (1) penetrates through the side wall of the stirring kettle (3) and extends out of the kettle, and an outlet end of the coil reactor (2) is directly communicated with the inside of the stirring kettle (3); the top of the stirring kettle (3) is fixedly communicated with a charging pipe B (11), the top of the stirring kettle (3) is provided with a stirrer (12), the lower part of the stirrer (12) is connected with a stirring shaft (13) extending into the stirring kettle (3), and the outer side wall of the stirring kettle (3) is provided with a kettle wall heat exchanger (4); stirred tank (3) exit end and tube heat exchanger (7) entrance point pipeline intercommunication, tube heat exchanger (7) exit end communicates row material pipe (10) and circulation pipeline (9) entrance point respectively, circulation pipeline (9) exit end intercommunication stirred tank (3) upper portion lateral wall department advances the mouth of pipe, all sets up valve (6) in the middle of each section pipeline.

2. The continuous production apparatus of dodecanol ester according to claim 1, wherein: the coil reactor (2) is formed by stacking a plurality of U-shaped pipes up and down, the inlet and outlet ends of two adjacent U-shaped pipes up and down are sequentially communicated, and a cooling sleeve is arranged outside the coil reactor (2).

3. The continuous production apparatus of dodecanol ester according to claim 1, wherein: and a pipeline conveying pump (5) is fixedly arranged on a pipeline between the outlet end of the stirring kettle (3) and the inlet end of the tubular heat exchanger (7).

4. The continuous production apparatus of dodecanol ester according to claim 1, wherein: the stirring shaft (13) penetrates through the coil reactor (2) from top to bottom without contacting, and the bottom end of the stirring shaft (13) is connected with two annular stirring rings (1301).

5. The continuous production apparatus of dodecanol ester according to claim 1, wherein: and a cooling water inlet and a cooling water outlet (8) are respectively arranged at diagonal positions of the wall of the tubular heat exchanger (7).

6. The continuous production apparatus of dodecanol ester according to claim 1, wherein: the kettle wall heat exchanger (4) is composed of a plurality of bent heat exchange tubes and is wound on the outer side wall of the stirring kettle (3).