CN110975782B - Device and method for continuous flow synthesis of ethylene bis fatty acid amide - Google Patents
Device and method for continuous flow synthesis of ethylene bis fatty acid amide Download PDFInfo
- Publication number
- CN110975782B CN110975782B CN201911336650.2A CN201911336650A CN110975782B CN 110975782 B CN110975782 B CN 110975782B CN 201911336650 A CN201911336650 A CN 201911336650A CN 110975782 B CN110975782 B CN 110975782B
- Authority
- CN
- China
- Prior art keywords
- fatty acid
- reactor
- ethylenediamine
- film reactor
- control system
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/004—Multifunctional apparatus for automatic manufacturing of various chemical products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/10—Preparation of carboxylic acid amides from compounds not provided for in groups C07C231/02 - C07C231/08
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a device and a method for continuously synthesizing ethylene bis fatty acid amide, belonging to the technical field of synthesis of ethylene bis fatty acid amide. The device provided by the invention comprises a control system 12, and a raw material storage tank, a micro-channel mixing reactor 5, a vertical wiped film reactor 6, a receiving tank 8 and a horizontal rotary thin film reactor 10 which are sequentially communicated; the micro-channel mixing reactor 5, the vertical wiped film reactor 6 and the horizontal rotary film reactor 10 are in control connection with a control system 12, and the control system 12 controls and automatically adjusts the running states of the micro-channel mixing reactor 5, the vertical wiped film reactor 6 and the horizontal rotary film reactor 10. The device provided by the invention can realize continuous flow synthesis of ethylene bis fatty acid amide, and has good product quality consistency and stability.
Description
Technical Field
The invention relates to the technical field of synthesis of ethylene bis fatty acid amide, in particular to a device and a method for continuously synthesizing ethylene bis fatty acid amide.
Background
Ethylene bis-fatty acid amide belongs to aliphatic bis-amide compounds, the main varieties comprise ethylene bis-stearic acid amide (EBS), ethylene bis-oleic acid amide (EBO), ethylene bis-erucic acid amide (EBE), ethylene bis-behenic acid amide (EBB), ethylene bis-12-hydroxystearic acid amide (EBH) and the like, and the ethylene bis-fatty acid amide is an important industrial surfactant and is also an additive which is widely applied in the field of material processing. With the continuous expansion of the application field and the high-end development trend of material products, the market puts higher requirements on the quality of the additive auxiliaries, and high-quality products with good consistency and stability are urgently needed.
The traditional ethylene bis fatty acid amide industrial synthesis method generally adopts a reaction kettle with a stirrer to carry out single-kettle intermittent operation, so that the produced ammonium salt intermediate is easy to oxidize and color, the product chromaticity is deep, the consistency and the stability of the product are poor, the popularization and the application of the product in large petrochemical devices and high-end fields are limited, the market development and the high added value display of the product are influenced, and a large-scale and intelligent industrial technology is difficult to form.
Disclosure of Invention
The invention aims to provide a device and a method for continuously synthesizing ethylene bis fatty acid amide, which can realize continuous synthesis of ethylene bis fatty acid amide and have good product quality consistency and stability.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a device for synthesizing ethylene bis fatty acid amide by continuous flow, which comprises a control system 12, and a raw material storage tank, a micro-channel mixing reactor 5, a vertical wiped film reactor 6, a receiving tank 8 and a horizontal rotary thin film reactor 10 which are sequentially communicated;
the micro-channel mixing reactor 5, the vertical wiped film reactor 6 and the horizontal rotary film reactor 10 are in control connection with a control system 12, and the control system 12 controls and automatically adjusts the running states of the micro-channel mixing reactor 5, the vertical wiped film reactor 6 and the horizontal rotary film reactor 10.
Preferably, the raw material storage tanks comprise a fatty acid storage tank 1 and an ethylenediamine storage tank 3, and the discharge ports of the fatty acid storage tank 1 and the ethylenediamine storage tank 3 are communicated with the feed port of the microchannel mixing reactor 5.
Preferably, a fatty acid metering pump 2 is arranged between the fatty acid storage tank 1 and the micro-channel mixing reactor 5, and an ethylenediamine metering pump 4 is arranged between the ethylenediamine storage tank 3 and the micro-channel mixing reactor 5;
the fatty acid metering pump 2 and the ethylenediamine metering pump 4 are in control connection with a control system 12, and the control system 12 controls and automatically adjusts the running states of the fatty acid metering pump 2 and the ethylenediamine metering pump 4.
Preferably, the device also comprises a demister 7, and the demister 7 is communicated with an air outlet at the top end of the receiving tank 8; the demister 7 is in control connection with a control system 12, and the control system 12 controls and automatically adjusts the running state of the demister 7.
Preferably, a delivery pump 9 is further included, and the delivery pump 9 is arranged between the receiving tank 8 and the horizontal rotary membrane reactor 10; the delivery pump 9 is in control connection with a control system 12, and the control system 12 controls and automatically adjusts the running state of the delivery pump 9.
Preferably, the device also comprises a filter 11, and the filter 11 is communicated with a discharge hole of the horizontal rotary membrane reactor 10.
The invention provides a method for continuous flow synthesis of ethylene bis fatty acid amide by adopting the device in the technical scheme, which comprises the following steps:
taking fatty acid and ethylenediamine as preparation raw materials, and carrying out a salt forming reaction in a micro-channel mixing reactor 5 to obtain an intermediate ammonium salt;
the intermediate ammonium salt enters a vertical wiped film reactor 6 for early amidation dehydration reaction, and then enters a horizontal rotary film reactor 10 through a receiving tank 8 for later amidation dehydration reaction to obtain the ethylene bis fatty acid amide.
Preferably, the fatty acid comprises one or more of lauric acid, palmitic acid, stearic acid, oleic acid, erucic acid, behenic acid, 12-hydroxystearic acid and isostearic acid.
Preferably, the fatty acid is pumped from the fatty acid storage tank 1 into the microchannel mixing reactor 5 via the fatty acid metering pump 2, and the ethylenediamine is pumped from the ethylenediamine storage tank 3 into the microchannel mixing reactor 5 via the ethylenediamine metering pump 4.
Preferably, in the process of continuously synthesizing the ethylene bis-fatty acid amide, the temperature in the micro-channel mixing reactor 5 is 80-150 ℃, the pressure at the discharge port of the micro-channel mixing reactor 5 is 0.05-0.60 MPa, and the retention time of the materials in the micro-channel mixing reactor 5 is 2-6 min;
the temperature in the vertical wiped film reactor 6 is 155-185 ℃, and the retention time of the materials in the vertical wiped film reactor 6 is 5-30 min;
the pressure at the air outlet of the demister 7 is-0.01-0.1 MPa;
the temperature in the horizontal rotary thin film reactor 10 is 175-220 ℃, the vacuum degree at the exhaust port of the horizontal rotary thin film reactor 10 is less than or equal to 100Pa, and the residence time of materials in the horizontal rotary thin film reactor 10 is 10-60 min.
The invention provides a device for synthesizing ethylene bis fatty acid amide by continuous flow, which comprises a control system 12, and a raw material storage tank, a micro-channel mixing reactor 5, a vertical wiped film reactor 6, a receiving tank 8 and a horizontal rotary thin film reactor 10 which are sequentially communicated; the micro-channel mixing reactor 5, the vertical wiped film reactor 6 and the horizontal rotary film reactor 10 are in control connection with a control system 12, and the control system 12 controls and automatically adjusts the running states of the micro-channel mixing reactor 5, the vertical wiped film reactor 6 and the horizontal rotary film reactor 10. The device provided by the invention can realize continuous flow synthesis of ethylene bis fatty acid amide, and the product quality consistency and stability are good; in addition, the device provided by the invention has reasonable design, can realize the intellectualization and automation of production operation, reduces the labor intensity, shortens the material retention and reaction time, saves the energy consumption, reduces the cost and is beneficial to large-scale fine production.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for continuous flow synthesis of ethylene bis fatty acid amide according to the present invention, in which a 1-fatty acid storage tank, a 2-fatty acid metering pump, a 3-ethylenediamine storage tank, a 4-ethylenediamine metering pump, a 5-microchannel mixing reactor, a 6-vertical wiped film reactor, a 7-demister, an 8-receiving tank, a 9-delivery pump, a 10-horizontal rotary thin film reactor, an 11-filter, and a 12-control system are provided.
Detailed Description
The invention provides a device for synthesizing ethylene bis fatty acid amide by continuous flow, which comprises a control system 12, and a raw material storage tank, a micro-channel mixing reactor 5, a vertical wiped film reactor 6, a receiving tank 8 and a horizontal rotary thin film reactor 10 which are sequentially communicated;
the micro-channel mixing reactor 5, the vertical wiped film reactor 6 and the horizontal rotary film reactor 10 are in control connection with a control system 12, and the control system 12 controls and automatically adjusts the running states of the micro-channel mixing reactor 5, the vertical wiped film reactor 6 and the horizontal rotary film reactor 10.
The device for continuously synthesizing the ethylene bis fatty acid amide comprises a control system 12, a data acquisition system and a data processing system, wherein the control system is used for controlling the overall operation state of the device; as an embodiment of the present invention, the control system 12 is specifically a DCS control system 12, and the connection relationship thereof will be described in detail later.
The device for continuously synthesizing the ethylene bis fatty acid amide comprises a raw material storage tank and a micro-channel mixing reactor 5 which are communicated, and the raw material storage tank and the micro-channel mixing reactor are respectively used for storing raw materials and carrying out salt forming reaction.
As an embodiment of the present invention, the raw material storage tanks include a fatty acid storage tank 1 and an ethylenediamine storage tank 3 for storing fatty acid and ethylenediamine, respectively, and discharge ports of the fatty acid storage tank 1 and the ethylenediamine storage tank 3 are both communicated with a feed port of the microchannel mixing reactor 5.
As an embodiment of the invention, the fatty acid storage tank 1 and the ethylenediamine storage tank 3 are in control connection with a control system 12, and the control system 12 controls and automatically adjusts the operating states of the fatty acid storage tank 1 and the ethylenediamine storage tank 3, for example, controls the temperatures of the fatty acid storage tank 1 and the ethylenediamine storage tank 3 to be constant-temperature storage tanks, so that the raw materials can be in a constant-temperature state, and the stable control of the feeding temperature is facilitated.
In the present invention, the microchannel mixing reactor 5 is in control connection with the control system 12, and the control system 12 controls and automatically adjusts the operation state of the microchannel mixing reactor 5, such as controlling and automatically adjusting the temperature, the material flow rate and the pressure at the discharge port in the microchannel mixing reactor 5. In the invention, fatty acid and ethylenediamine are subjected to salt forming reaction to generate intermediate ammonium salt, the ammonium salt is easy to oxidize and color, the method is used for performing salt forming reaction in a micro-channel mixing reactor 5, the salt forming reaction can be completed within a very short time (2-6 min) to generate the ammonium salt, the retention time is very short, and the oxidation and the color of the ammonium salt can be effectively prevented.
The specific structure, size and material of the fatty acid storage tank 1, the ethylenediamine storage tank 3 and the microchannel mixing reactor 5 are not specially required, and the fatty acid storage tank, the ethylenediamine storage tank and the microchannel mixing reactor can be selected according to actual needs.
As an embodiment of the invention, a fatty acid metering pump 2 is arranged between the fatty acid storage tank 1 and the microchannel mixing reactor 5, and an ethylenediamine metering pump 4 is arranged between the ethylenediamine storage tank 3 and the microchannel mixing reactor 5; the fatty acid metering pump 2 and the ethylenediamine metering pump 4 are in control connection with a control system 12, and the control system 12 controls and automatically adjusts the running states of the fatty acid metering pump 2 and the ethylenediamine metering pump 4. The fatty acid metering pump 2 and the ethylenediamine metering pump 4 are respectively used for controlling the flow of the fatty acid and the flow of the ethylenediamine, and salt forming reaction of the fatty acid and the ethylenediamine in the microchannel mixing reactor 5 is ensured under a proper proportion condition.
The device for synthesizing the ethylene bis fatty acid amide by the continuous flow comprises a vertical wiped film reactor 6, wherein the vertical wiped film reactor 6 is used for carrying out early amidation dehydration reaction on an intermediate ammonium salt obtained after salt forming reaction. As an embodiment of the invention, the top feed inlet of the vertical wiped film reactor 6 is communicated with the discharge outlet of the micro-channel mixing reactor 5, and the bottom discharge outlet of the vertical wiped film reactor 6 is communicated with the feed inlet of the receiving tank 8.
The invention does not have special requirements on the specific structure, size and material of the vertical wiped film reactor 6, and can be selected according to actual needs; specifically, the vertical wiped film reactor 6 includes a vertical cylinder with jacket heating, a distributor and a wiped film device.
In the invention, the vertical wiped film reactor 6 is in control connection with a control system 12, and the control system 12 controls and automatically adjusts the running state of the vertical wiped film reactor 6, such as controlling and automatically adjusting the temperature in the vertical wiped film reactor 6 and the rotating speed of the wiped film reactor.
The ammonium salt is subjected to early amidation dehydration reaction in a vertical wiped film reactor 6, the ammonium salt continuously enters the vertical wiped film reactor 6 from a top feeding hole, specifically, the ammonium salt is distributed to the inner wall of a vertical cylinder through a distributor positioned at the top feeding hole, then the ammonium salt is accelerated by a wiped film device and immediately forms a layer of reaction liquid film on a heating surface, the reaction liquid film is spirally pushed downwards, and the rotating wiped film device ensures the uniformity and continuity of the reaction liquid film, so that the reaction liquid film can form a good turbulent flow effect, and the mass transfer and heat transfer processes are optimized, thereby greatly improving the amidation dehydration reaction efficiency of the ammonium salt.
The device for synthesizing the ethylene bis fatty acid amide by continuous flow comprises a receiving tank 8, wherein a feed inlet of the receiving tank 8 is communicated with a discharge outlet at the bottom of the vertical wiped film reactor 6, and the receiving tank 8 is used for collecting materials output by the vertical wiped film reactor 6.
According to one embodiment of the present invention, the continuous flow ethylene bis fatty acid amide synthesis apparatus further comprises a demister 7, the demister 7 is communicated with an exhaust port at the top end of the receiving tank 8, the demister 7 is in control connection with a control system 12, and the control system 12 controls and automatically adjusts the operation state of the demister 7. In the invention, a demister 7 is used for discharging water in the form of water vapor generated by a vertical wiped film reactor 6, and the residual liquid material (comprising a product ethylene bis fatty acid amide and a small amount of ammonium salt) is conveyed to a subsequent horizontal rotary thin film reactor 10 through a receiving tank 8; wherein the pressure at the air outlet of the demister 7 can be controlled and automatically adjusted by means of the control system 12.
As an embodiment of the present invention, the continuous flow apparatus for synthesizing ethylene bis fatty acid amide further comprises a transfer pump 9, wherein the transfer pump 9 is arranged between the receiving tank 8 and the horizontal rotary thin film reactor 10; the delivery pump 9 is in control connection with a control system 12, and the control system 12 controls and automatically adjusts the running state of the delivery pump 9. The invention utilizes a delivery pump 9 to deliver the liquid material in a receiving tank 8 to a horizontal rotary membrane reactor 10.
The device for continuous flow synthesis of ethylene bis fatty acid amide provided by the invention comprises a horizontal rotary thin film reactor 10, which is used for carrying out later amidation dehydration reaction on intermediate ammonium salt, in particular further dehydrating ammonium salt contained in liquid material in a receiving tank 8.
The invention does not make special requirements on the specific structure, size and material of the horizontal rotary thin film reactor 10, and can be selected according to actual needs; specifically, the horizontal rotary thin film reactor 10 includes a horizontal cylinder with jacket heating and a rotary thin film reactor.
In the present invention, the horizontal rotary membrane reactor 10 is in control connection with a control system 12, and the control system 12 controls and automatically adjusts the operation state of the horizontal rotary membrane reactor 10, such as controlling and automatically adjusting the temperature in the horizontal rotary membrane reactor 10.
As an embodiment of the invention, the exhaust port of the horizontal rotary thin film reactor 10 is communicated with a vacuum pump for pumping out and discharging trace moisture in the form of water vapor generated in the later amidation dehydration reaction.
As an embodiment of the present invention, the vacuum pump is in control connection with the control system 12, and the control system 12 controls and automatically adjusts the operation state of the vacuum pump, so that the exhaust port of the horizontal rotary thin film reactor 10 maintains a proper vacuum degree under the action of the vacuum pump.
The later dehydration reaction rate of the ammonium salt is relatively slow, the ammonium salt is subjected to the later dehydration reaction in the horizontal rotary thin film reactor 10, the flow of reaction materials (namely, liquid materials output from the receiving tank 8) is not influenced by gravity, the residence time of the reaction materials can be regulated, and a better dehydration effect is ensured; specifically, the reaction materials continuously enter the horizontal rotary film reactor 10, are accelerated and distributed by the rotary film reactor and immediately form a layer of flowing film on the heating surface, the flowing film can keep a turbulent flow state, the reaction materials are subjected to continuous dehydration reaction, and the residence time of the reaction materials can be adjusted through the rotating speed of the rotary film reactor; and pumping out a small amount of moisture in the form of water vapor generated by the dehydration reaction by a vacuum pump and discharging.
The device for continuous flow synthesis of ethylene bis fatty acid amide provided by the invention also comprises a filter 11, wherein the filter 11 is communicated with a discharge hole of the horizontal rotary thin film reactor 10; the filter 11 is used for filtering materials output from the horizontal rotary thin film reactor 10 and filtering mechanical impurities.
The invention provides a method for continuous flow synthesis of ethylene bis fatty acid amide by adopting the device in the technical scheme, which comprises the following steps:
taking fatty acid and ethylenediamine as preparation raw materials, and carrying out a salt forming reaction in a micro-channel mixing reactor 5 to obtain an intermediate ammonium salt;
the intermediate ammonium salt enters a vertical wiped film reactor 6 for early amidation dehydration reaction, and then enters a horizontal rotary film reactor 10 through a receiving tank 8 for later amidation dehydration reaction to obtain the ethylene bis fatty acid amide.
The method takes fatty acid and ethylenediamine as preparation raw materials, and performs salt forming reaction in a micro-channel mixing reactor 5 to obtain an intermediate ammonium salt. In the present invention, the fatty acid preferably includes one or more of lauric acid, palmitic acid, stearic acid, oleic acid, erucic acid, behenic acid, 12-hydroxystearic acid and isostearic acid, and more preferably lauric acid, palmitic acid, stearic acid, oleic acid, erucic acid, behenic acid, 12-hydroxystearic acid or isostearic acid. In the present invention, the fatty acid and the ethylenediamine are preferably stored in the fatty acid storage tank 1 and the ethylenediamine storage tank 3, respectively, and the temperatures in the fatty acid storage tank 1 and the ethylenediamine storage tank 3 are kept constant, wherein the temperature in the ethylenediamine storage tank 3 is preferably kept constant at 65 to 80 ℃, the temperature in the fatty acid storage tank 1 can be specifically selected according to the type of the fatty acid, for example, when the fatty acid is stearic acid, the temperature in the fatty acid storage tank 1 is preferably 110 ± 2 ℃, and when the fatty acid is oleic acid, the temperature in the fatty acid storage tank 1 is preferably 80 ± 2 ℃. The temperature in the fatty acid storage tank 1 and the temperature in the ethylenediamine storage tank 3 are controlled to be the set values, so that the viscosity of the feeding material is reduced, and the fluidity is improved.
In the present invention, the fatty acid is preferably pumped from a fatty acid storage tank 1 into a microchannel mixing reactor 5 via a fatty acid metering pump 2, and the ethylenediamine is preferably pumped from an ethylenediamine storage tank 3 into the microchannel mixing reactor 5 via an ethylenediamine metering pump 4. The flow ratio of the fatty acid to the ethylenediamine is preferably determined according to the actual acid value of the fatty acid and the amine value of the ethylenediamine, and specifically, may be calculated according to the following formula: the acid value of the fatty acid × the flow rate of the fatty acid ═ the amine value of ethylenediamine × the flow rate of ethylenediamine.
In the invention, fatty acid and ethylenediamine are subjected to salt forming reaction in a micro-channel mixing reactor 5 to obtain an intermediate ammonium salt; the intermediate ammonium salt enters a vertical wiped film reactor 6 for early amidation dehydration reaction, and then enters a horizontal rotary film reactor 10 through a receiving tank 8 for later amidation dehydration reaction to obtain the ethylene bis fatty acid amide. In the process of continuously synthesizing the ethylene bis-fatty acid amide, the temperature in the micro-channel mixing reactor 5 is preferably 80-150 ℃, the pressure at the discharge port of the micro-channel mixing reactor 5 is preferably 0.05-0.60 MPa, and the residence time of materials in the micro-channel mixing reactor 5 is preferably 2-6 min; the temperature in the vertical wiped film reactor 6 is preferably 155-185 ℃, and the retention time of the materials in the vertical wiped film reactor 6 is 5-30 min; the pressure at the air outlet of the demister 7 is preferably-0.01-0.1 MPa; the temperature in the horizontal rotary thin film reactor 10 is preferably 175-220 ℃, the vacuum degree at the exhaust port of the horizontal rotary thin film reactor 10 is preferably less than or equal to 100Pa, and the residence time of the materials in the horizontal rotary thin film reactor 10 is preferably 10-60 min.
After the final amidation dehydration reaction is completed, the invention preferably filters the material discharged from the horizontal rotary film reactor 10 through a filter 11, and then carries out the subsequent molding granulation process to obtain the granular (or powder) product.
In the invention, the reaction process for preparing ethylene bis fatty acid amide from fatty acid and ethylenediamine is as follows:
wherein, the fatty acid preferably comprises one or more of lauric acid, palmitic acid, stearic acid, oleic acid, erucic acid, behenic acid, 12-hydroxystearic acid and isostearic acid.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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 1
Specifically, the method for continuously synthesizing Ethylene Bis Stearamide (EBS) by using stearic acid and ethylenediamine as raw materials and the device shown in FIG. 1 comprises the following steps:
storing stearic acid in a fatty acid storage tank 1, controlling the temperature of the fatty acid storage tank 1 to be 110 +/-2 ℃, and continuously pumping the stearic acid into a micro-channel mixing reactor 5 by a fatty acid metering pump 2, wherein the flow rate of the stearic acid is 300 kg/h; storing ethylenediamine in an ethylenediamine storage tank 3, controlling the temperature of the ethylenediamine storage tank 3 to be 75 +/-2 ℃, and continuously pumping the ethylenediamine into a micro-channel mixing reactor 5 by an ethylenediamine metering pump 4, wherein the flow rate of the ethylenediamine is 33.2 kg/h;
controlling the temperature (T1) in the micro-channel mixing reactor 5 to be 140 +/-2 ℃, the pressure (P1) at the discharge port to be 0.46-0.53 MPa, and controlling the residence time of stearic acid and ethylenediamine in the micro-channel mixing reactor 5 to be 4 min; controlling the temperature (T2) in the vertical wiped film reactor 6 to 178 +/-2 ℃, continuously feeding intermediate ammonium salt formed by the reaction of stearic acid and ethylenediamine into the vertical wiped film reactor 6 for early amidation dehydration reaction, controlling the retention time of materials in the vertical wiped film reactor 6 to be 20min, continuously feeding a product system obtained by the early amidation dehydration reaction into a receiving tank 8, controlling the pressure (P2) at the air outlet of a demister 7 to be 0.05-0.08 MPa, discharging water existing in the product system in the form of water vapor by using the demister 7, conveying the residual liquid materials into a horizontal rotary thin film reactor 10 through a conveying pump 9 for later amidation dehydration reaction, and pumping the generated trace water existing in the form of water vapor out of the air outlet of the horizontal rotary thin film reactor 10 through a vacuum pump, wherein the temperature (T3) in the horizontal rotary thin film reactor 10 is controlled to be 186 +/-2 ℃, the vacuum degree (P3) at the gas outlet is 60-80 Pa, and the retention time of the materials in the horizontal rotary film reactor 10 is 30 min; and filtering a liquid product discharged from the horizontal rotary thin film reactor 10 through a filter 11, and then performing a subsequent molding granulation process to obtain a granular product.
In the production process, the quality index of the synthesized product is analyzed by sampling at the discharge hole of the filter 11 every 20min, and the specific result is shown in table 1.
TABLE 1 method for continuous flow synthesis of ethylene bis stearamide operating parameters and detection results of the product
Example 2
The method for continuously synthesizing the ethylene bis-oleamide (EBO) by using oleic acid and ethylenediamine as raw materials and the device shown in figure 1 by using oleic acid as a fatty acid specifically comprises the following steps:
storing oleic acid in a fatty acid storage tank 1, controlling the temperature of the fatty acid storage tank 1 to be 80 +/-2 ℃, and continuously pumping the oleic acid into a micro-channel mixing reactor 5 by a fatty acid metering pump 2, wherein the flow rate of the oleic acid is 200 kg/h; storing ethylenediamine in an ethylenediamine storage tank 3, controlling the temperature of the ethylenediamine storage tank 3 to be 70 +/-2 ℃, and continuously pumping the ethylenediamine into a micro-channel mixing reactor 5 by an ethylenediamine metering pump 4, wherein the flow rate of the ethylenediamine is 21.2 kg/h;
controlling the temperature (T1) in the micro-channel mixing reactor 5 to be 95 +/-2 ℃, the pressure (P1) at the discharge port to be 0.20-0.40 MPa, and controlling the residence time of oleic acid and ethylenediamine in the micro-channel mixing reactor 5 to be 6 min; controlling the temperature (T2) in the vertical wiped film reactor 6 to be 165 +/-2 ℃, continuously feeding intermediate ammonium salt formed by the reaction of oleic acid and ethylenediamine into the vertical wiped film reactor 6 for early amidation dehydration reaction, controlling the retention time of materials in the vertical wiped film reactor 6 to be 30min, continuously feeding a product system obtained by the early amidation dehydration reaction into a receiving tank 8, controlling the pressure (P2) at the air outlet of a demister 7 to be 0.01-0.05 MPa, discharging water existing in the product system in the form of water vapor by using the demister 7, conveying the residual liquid materials into a horizontal rotary thin film reactor 10 through a conveying pump 9 for later amidation dehydration reaction, pumping the generated water existing in the form of water vapor from the air outlet of the horizontal rotary thin film reactor 10 through a vacuum pump, wherein the temperature (T3) in the horizontal rotary thin film reactor 10 is controlled to be 180 +/-2 ℃, the vacuum degree (P3) at the gas outlet is 40-60 Pa, and the retention time of the materials in the horizontal rotary film reactor 10 is 40 min; and filtering a liquid product discharged from the horizontal rotary thin film reactor 10 through a filter 11, and then performing a subsequent molding granulation process to obtain a powdery product.
In the production process, the quality index of the synthesized product is sampled and analyzed at the discharge hole of the filter 11 every 20min, and the specific result is shown in table 2.
TABLE 2 method for continuous flow synthesis of ethylenebisoleamide operating parameters and detection results of the product
Comparative example 1
Adding 300kg of stearic acid into a 500L batch kettle type reactor, heating to 100 ℃, then dropwise adding 33.2kg of ethylenediamine under the protection of ammonia gas for 30min, reacting at 100-115 ℃ for 40min after dropwise adding, heating, manually evacuating for reaction for 2h at 178-188 ℃, heating again, manually vacuumizing for reaction for 3h at 196-206 ℃, and sampling and analyzing the obtained product; 5 batches of products were synthesized according to the above method, and the results of the detection of each batch are shown in Table 3.
TABLE 3 detection results of Ethylene Bis Stearamide (EBS) synthesis in batch tank reactor
| Batches of | Acid value mgKOH/g | Amine value mgKOH/g | Chromaticity Gandner | Melting Point C |
| 1 | 7.82 | 2.11 | 3.5 | 144.6 |
| 2 | 8.31 | 1.98 | 3.0 | 143.9 |
| 3 | 6.98 | 2.23 | 4.0 | 142.3 |
| 4 | 7.14 | 1.89 | 3.5 | 143.1 |
| 5 | 8.79 | 2.59 | 4.0 | 142.9 |
Comparative example 2
Adding 200kg of oleic acid into a 500L batch kettle type reactor, heating to 95 ℃, then dropwise adding 21.2kg of ethylenediamine under the protection of ammonia gas for 20min, reacting at 95-110 ℃ for 60min after dropwise adding, heating, manually evacuating for reaction for 2h at 165-175 ℃, heating again, manually vacuumizing for reaction for 3h at 180-190 ℃, and sampling and analyzing the obtained product; 5 batches of products were synthesized according to the above method, and the results of the measurements of the respective batches are shown in Table 4.
TABLE 4 detection results of ethylene bis-oleamide (EBO) synthesis in batch tank reactor
| Batches of | Acid value mgKOH/g | Amine value mgKOH/g | Chromaticity Gandner | Melting Point C |
| 1 | 9.38 | 2.48 | 8.5 | 115.3 |
| 2 | 7.52 | 1.92 | 7.5 | 116.2 |
| 3 | 8.59 | 2.11 | 8.0 | 114.9 |
| 4 | 6.93 | 2.01 | 7.0 | 117.1 |
| 5 | 7.21 | 1.71 | 8.5 | 116.9 |
As can be seen from tables 1-2, the device provided by the invention can realize continuous synthesis of ethylene bis-fatty acid amide, and the main quality indexes of the synthesized product, such as acid value, amine value, melting point, color and luster, are stable, small in fluctuation range, good in consistency and stability, and obviously improved and stable in quality. As can be seen from tables 3-4, the traditional process adopts single-kettle intermittent operation, the reaction and retention time is long (5-8 h), and the oxidation and coloring of the intermediate ammonium salt are easily caused, so that the product chromaticity is deep; and the operating conditions are wide and inaccurate, resulting in poor product consistency and stability.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A device for continuous flow synthesis of ethylene bis fatty acid amide is characterized by comprising a control system (12), and a raw material storage tank, a micro-channel mixing reactor (5), a vertical wiped film reactor (6), a receiving tank (8) and a horizontal rotary thin film reactor (10) which are sequentially communicated;
the device is characterized in that the micro-channel mixing reactor (5), the vertical wiped film reactor (6) and the horizontal rotary film reactor (10) are in control connection with a control system (12), and the control system (12) controls and automatically adjusts the running states of the micro-channel mixing reactor (5), the vertical wiped film reactor (6) and the horizontal rotary film reactor (10).
2. The apparatus of claim 1, wherein the raw material storage tanks comprise a fatty acid storage tank (1) and an ethylenediamine storage tank (3), and the discharge ports of the fatty acid storage tank (1) and the ethylenediamine storage tank (3) are communicated with the feed port of the microchannel mixing reactor (5).
3. The apparatus according to claim 2, wherein a fatty acid metering pump (2) is arranged between the fatty acid storage tank (1) and the microchannel mixing reactor (5), and an ethylenediamine metering pump (4) is arranged between the ethylenediamine storage tank (3) and the microchannel mixing reactor (5);
the fatty acid metering pump (2) and the ethylenediamine metering pump (4) are in control connection with a control system (12), and the control system (12) controls and automatically adjusts the running states of the fatty acid metering pump (2) and the ethylenediamine metering pump (4).
4. The device according to claim 1, further comprising a demister (7), the demister (7) being in communication with the gas outlet at the top end of the receiving tank (8); the demister (7) is in control connection with a control system (12), and the control system (12) controls and automatically adjusts the running state of the demister (7).
5. The apparatus according to claim 1, further comprising a delivery pump (9), the delivery pump (9) being arranged between the receiving tank (8) and the horizontal rotary membrane reactor (10); the conveying pump (9) is in control connection with a control system (12), and the control system (12) controls and automatically adjusts the running state of the conveying pump (9).
6. The apparatus according to claim 1, further comprising a filter (11), the filter (11) being in communication with the outlet of the horizontal rotary membrane reactor (10).
7. A method for continuous flow synthesis of ethylene bis fatty acid amide by using the apparatus of any one of claims 1 to 6, comprising the steps of:
taking fatty acid and ethylenediamine as preparation raw materials, and carrying out salt forming reaction in a micro-channel mixing reactor (5) to obtain an intermediate ammonium salt;
the intermediate ammonium salt enters a vertical wiped film reactor (6) for early amidation dehydration reaction, and then enters a horizontal rotary film reactor (10) through a receiving tank (8) for later amidation dehydration reaction to obtain the ethylene bis fatty acid amide.
8. The method of claim 7, wherein the fatty acid comprises one or more of lauric acid, palmitic acid, stearic acid, oleic acid, erucic acid, behenic acid, 12-hydroxystearic acid, and isostearic acid.
9. The process according to claim 7, wherein the fatty acid is pumped from a fatty acid storage tank (1) into the microchannel mixing reactor (5) via a fatty acid metering pump (2), and the ethylenediamine is pumped from an ethylenediamine storage tank (3) into the microchannel mixing reactor (5) via an ethylenediamine metering pump (4).
10. The process according to any one of claims 7 to 9, wherein in the continuous flow synthesis of the ethylene bis fatty acid amide, the temperature in the microchannel mixing reactor (5) is 80 to 150 ℃, the pressure at the discharge port of the microchannel mixing reactor (5) is 0.05 to 0.60MPa, and the residence time of the material in the microchannel mixing reactor (5) is 2 to 6 min;
the temperature in the vertical wiped film reactor (6) is 155-185 ℃, and the retention time of the materials in the vertical wiped film reactor (6) is 5-30 min;
the pressure at the air outlet of the demister (7) is-0.01-0.1 MPa;
the temperature in the horizontal rotary film reactor (10) is 175-220 ℃, the vacuum degree at the exhaust port of the horizontal rotary film reactor (10) is less than or equal to 100Pa, and the retention time of materials in the horizontal rotary film reactor (10) is 10-60 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911336650.2A CN110975782B (en) | 2019-12-23 | 2019-12-23 | Device and method for continuous flow synthesis of ethylene bis fatty acid amide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911336650.2A CN110975782B (en) | 2019-12-23 | 2019-12-23 | Device and method for continuous flow synthesis of ethylene bis fatty acid amide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110975782A CN110975782A (en) | 2020-04-10 |
| CN110975782B true CN110975782B (en) | 2021-07-23 |
Family
ID=70074199
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911336650.2A Active CN110975782B (en) | 2019-12-23 | 2019-12-23 | Device and method for continuous flow synthesis of ethylene bis fatty acid amide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110975782B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704556B (en) * | 2020-06-29 | 2023-05-30 | 石家庄华复化工科技有限公司 | System and method for continuously preparing N, N' -ethylene bis (stearamide) through micro-channels |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101205194B (en) * | 2007-12-10 | 2010-06-23 | 江西威科油脂化学有限公司 | Three-stage continuous separation and purification technique of fatty primary amide |
| DE102008017216B4 (en) * | 2008-04-04 | 2013-08-14 | Clariant International Ltd. | Continuous process for the preparation of fatty acid amides |
| KR101328841B1 (en) * | 2011-05-09 | 2013-11-13 | 동국대학교 산학협력단 | Preparation Method of Tetraacetylethylenediamine(TEAD) Using Continuous Process |
| CN206654874U (en) * | 2017-01-20 | 2017-11-21 | 广州市海珥玛植物油脂有限公司 | A kind of reaction unit for producing environment-friendly plasticizer |
| CN109422635A (en) * | 2017-09-05 | 2019-03-05 | 东营市海科新源化工有限责任公司 | A kind of preparation method of 1,3 butylene glycol |
| CN207493235U (en) * | 2017-11-16 | 2018-06-15 | 上海一飒环保工程科技有限公司 | A kind of efficient combined-type MVR luwa evaporators |
| CN109096328A (en) * | 2018-07-17 | 2018-12-28 | 常州大学 | A kind of method of the continuous synthesizing phosphorous acid diethylester of micro passage reaction |
| CN109265361B (en) * | 2018-10-08 | 2020-07-10 | 南京工业大学 | Method for carrying out micro-reaction continuous flow preparation by applying acylamino to vegetable oil-based plasticizer |
-
2019
- 2019-12-23 CN CN201911336650.2A patent/CN110975782B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN110975782A (en) | 2020-04-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105601652B (en) | A kind of method for preparing metal-organic framework materials | |
| CN110975782B (en) | Device and method for continuous flow synthesis of ethylene bis fatty acid amide | |
| CN104072755B (en) | Polyamide fibre 6 three still polymerization new technologies | |
| CN105622639A (en) | Method for preparing nanoscale Cu-based metal organic framework material | |
| CN109438295B (en) | Method for preparing CLT acid sulfonate by continuous reaction | |
| CN107814395A (en) | A kind of cyanamide production technology | |
| CN113200862B (en) | Synthetic process of sodium p-nitrophenolate | |
| CN106335932B (en) | A kind of production technology of ruthenium trichloride | |
| CN104560707A (en) | Technological method and system for enzymatically synthesizing L-ascorbic acid 2-glucoside | |
| CN104439266A (en) | Preparation method of molybdenum powder large in particle size | |
| CN105111090B (en) | A kind of continuous preparation method of the dinitro ethene of 1,1 diaminourea 2,2 | |
| CN104128128B (en) | A kind of diamond synthesizing split stem stem and preparation method thereof | |
| CN214457723U (en) | Amino resin serialization apparatus for producing | |
| CN104725281A (en) | Method for producing urea peroxide | |
| CN213253867U (en) | Preparation facilities of covalence organic frame complex film | |
| CN112062720B (en) | Continuous preparation method of 1-methyl-3-hydroxypyrazole-4-carboxylic acid ethyl ester | |
| CN115043734A (en) | Continuous production process of 2,4,4 '-trichloro-2' -nitrodiphenyl ether | |
| CN211141542U (en) | Production device of food-grade and feed-grade anhydrous magnesium sulfate | |
| CN107245027A (en) | A kind of preparation method of D mannitol alpha crystal formations | |
| CN211800862U (en) | Continuous esterification reaction device | |
| CN113061076A (en) | Preparation method of chloro-tert-pentane | |
| CN207243467U (en) | A kind of production equipment of PHOSPHORIC ACID TECH.GRADE potassium dihydrogen coproduction Water soluble fertilizer | |
| CN203393074U (en) | Production system for continuous production of antistatic polyester melts and continuous film-drawing | |
| CN112968164A (en) | Experimental method for preparing lithium battery positive electrode material precursor | |
| CN111675607A (en) | Method for producing trimethyl orthoacetate through differential circulation and continuous production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |