CN208182893U - A kind of system for continuous esterification production ethyl cyanoacetate - Google Patents
A kind of system for continuous esterification production ethyl cyanoacetate Download PDFInfo
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- CN208182893U CN208182893U CN201820512446.6U CN201820512446U CN208182893U CN 208182893 U CN208182893 U CN 208182893U CN 201820512446 U CN201820512446 U CN 201820512446U CN 208182893 U CN208182893 U CN 208182893U
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Abstract
The utility model discloses a kind of system for continuous esterification production ethyl cyanoacetate, which includes: feeding device: being provided with inlet port and outlet port；Multi-stage reacting device: every further device of the multi-stage reacting device all includes reaction kettle of the esterification and evaporator, and the feed inlet of the reaction kettle of the esterification and the discharge port of feeding device connect, and the discharge port of the reaction kettle of the esterification and the feed inlet of evaporator connect；It is connected by the liquid outlet opening of upper level evaporator with the feed inlet of next stage reaction kettle of the esterification between adjacent multistage reaction unit, whole grade base of evaporator discharging；Condensate recycling device: the gas feed of the condensate recycling device is connect with the gas vent of evaporators at different levels.System provided by the utility model carries out continuous esterification by continuous feed, continuous discharge, realizes the continuous production of ethyl cyanoacetate, and by multistage esterification device, carries out esterification step by step, conversion ratio is greatly improved.
Description
Technical field
The utility model relates to chemical production technical fields, more particularly to a kind of continuous esterification that is used for produce ethyl cyanoacetate
System.
Background technique
Ethyl cyanoacetate is a kind of important organic chemical industry's intermediate, is widely used in synthesizing ester, amides, acids
Equal compounds, production technology have preceding cyanidation technology and rear cyanidation technology and three kinds of ester exchange process.Preceding cyanidation technology refers to use
Monoxone obtains cyanoacetic acid by neutralization, cyaniding, acidification and obtains ethyl cyanoacetate with ethyl alcohol progress esterification again.Cyaniding work afterwards
Skill refers to that first carrying out esterification with ethyl alcohol with monoxone prepares ethyl chloroacetate, carries out cyanogenation with Cymag after refining, obtains
To ethyl cyanoacetate.Ester exchange process refer to methyl cyanoacetate and ethyl alcohol carry out transesterification synthesis ethyl cyanoacetate, but due to
Ester exchange catalyst effect is not ideal, and catalyst is recycled higher cost, the methanol recycled and ethyl alcohol it is mixed
It is more intractable to close object, so this preparation method is also difficult to realize industrialization.
Currently, the continuous production technology research of ethyl cyanoacetate is still few, for rear cyanidation technology, only one invention is special
Benefit: CN2012100738914 report it is a kind of using chloracetate and Cymag be raw material using tubular reactor continuously after cyanogen
The technique of chemical industry skill production cyanoacetate.But for preceding cyanidation technology, domestic overwhelming majority enterprise is still anti-using interval
Technique is answered, the continuous esterification system of ethyl cyanoacetate is there is not yet document report.
Utility model content
The technical problem to be solved by the present invention is to provide it is a kind of for continuous esterification production ethyl cyanoacetate system,
Aim to solve the problem that the problem of existing preceding cyanidation technology production ethyl cyanoacetate is unable to continuous production.
In order to solve the above technical problems, technical solution provided by the utility model is:
A kind of system for continuous esterification production ethyl cyanoacetate:
Feeding device: inlet port and outlet port are provided with；
Multi-stage reacting device: every further device of the multi-stage reacting device all includes reaction kettle of the esterification and evaporator, institute
The discharge port of the feed inlet and feeding device of stating reaction kettle of the esterification connects, the discharge port of the reaction kettle of the esterification and evaporator into
Material mouth connection；Pass through the liquid outlet opening of upper level evaporator and next stage reaction kettle of the esterification between adjacent multistage reaction unit
Feed inlet series connection, whole grade base of evaporator discharging；
Condensate recycling device: the gas feed of the condensate recycling device is connect with the gas vent of evaporators at different levels.
The beneficial effect of the system of synthesis ethyl cyanoacetate provided by the utility model is:
1, the continuous production for realizing ethyl cyanoacetate, and saving more stable than traditional batch technology production operation
It is artificial, reduce production cost.
2, using multistage esterification device, esterification is carried out step by step, and esterification is more thorough, has broken traditional esterifications skill
The ester conversion rate that thermodynamical equilibrium limits in art, is greatly improved conversion ratio, and product quality is more stable.
3, in evaporation process, using the property of ethyl alcohol azeotrope with water, using feed ethanol itself as water entrainer, by ester
Change the water that reaction generates and constantly take system out of, is not necessarily to other additional water entrainers, avoids the introducing of impurity, ensure that product
Purity, and moisture steam make to react to be conducive to generate ester direction carry out, improve the conversion ratio of esterification.
Detailed description of the invention
In order to illustrate more clearly of the technical scheme in the embodiment of the utility model, will make below to required in embodiment
Attached drawing is briefly described, it should be apparent that, the drawings in the following description are merely some embodiments of the present invention,
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings
Other attached drawings.
Fig. 1 is the device structure schematic diagram that the utility model embodiment 1 carries out ethyl cyanoacetate continuous production；
1- ethanol storage tank 2- ethyl alcohol delivery pump 3- cyanoacetic acid storage tank
4- cyanoacetic acid delivery pump 5- level-one esterifying kettle 6- first-level transport pump
7- level-one evaporator 8- second level esterifying kettle 9- two-stage conveying pump
10- secondary evaporimeter 11- three-level esterifying kettle 12- three-level delivery pump
13- three-level evaporator 14- is esterified finished product storage tank 15- first-stage condenser
16- secondary condenser 17- ethyl alcohol recycling can 18- vacuum system
Specific embodiment
In order to make the purpose of the utility model, technical solutions and advantages more clearly understood, with reference to embodiments, to this
Utility model is further elaborated.It should be appreciated that specific embodiment described herein is only used to explain that this is practical
It is novel, it is not used to limit the utility model.
The utility model embodiment is described in detail below.
Referring to Fig. 1, existing say the system provided by the utility model for continuous esterification production ethyl cyanoacetate
It is bright.
Feeding device: inlet port and outlet port are provided with；
Multi-stage reacting device: every further device of the multi-stage reacting device all includes reaction kettle of the esterification and evaporator, institute
The discharge port of the feed inlet and feeding device of stating reaction kettle of the esterification connects, the discharge port of the reaction kettle of the esterification and evaporator into
Material mouth connection；Pass through the liquid outlet opening of upper level evaporator and next stage reaction kettle of the esterification between adjacent multistage reaction unit
Feed inlet series connection, whole grade base of evaporator discharging；
Condensate recycling device: the gas feed of the condensate recycling device is connect with the gas vent of evaporators at different levels.
In the present embodiment, reaction raw materials point multistage is esterified, and every level-one is all divided into two processes of esterification and evaporation, is passed through
Esterification step by step carries out esterification more abundant, and is constantly separated from system by that will be esterified the water generated, makes
It obtains esterification to carry out to the direction for being conducive to generate ester, has broken the conversion ratio of thermodynamical equilibrium restriction, conversion rate of esterification mentions
Up to 98% or more.And reaction raw materials ethyl alcohol itself is also used as water entrainer, and water entrainer is added without additional, ensure that production
The purity of product reduces production cost simultaneously.Entire esterification system uses continuous feed, and the mode continuously produced carries out continuous ester
Change reaction, realizes the continuous production of ethyl cyanoacetate.
Optionally, the series connection series of the multi-stage reacting device is no less than 3.
Optionally, the multi-stage reacting device is third-order reaction device, including level-one esterifying kettle 5, level-one evaporator 7, two
Grade esterifying kettle 8, secondary evaporimeter 10, three-level esterifying kettle 11 and three-level evaporator 13.
All one evaporator of mating setting, the distillation of side border ring fractionate out product in time, reduce and generate after every level-one esterifying kettle
The concentration of object may advantageously facilitate esterification to the direction movement for generating esterification products, improve the conversion ratio of cyanoacetic acid.
Optionally, the feeding device includes ethanol storage tank 1 and cyanoacetic acid storage tank 3；The discharge port of the ethanol storage tank 1 point
It is not connect with the feed inlet of esterifying kettles at different levels；The discharge port of the cyanoacetic acid storage tank 3 is connect with the feed inlet of level-one esterifying kettle 5.
Ethanol storage tank is connect by delivery pump with esterifying kettles at different levels, is used for continuous into esterifying kettles at different levels in the esterification reaction
It is passed through ethyl alcohol, ethyl alcohol excessively helps to improve the conversion ratio of cyanoacetic acid.
Optionally, the condensate recycling device includes first-stage condenser 15, secondary condenser 16 and ethyl alcohol recycling can 17；Institute
Gas of the gas feed of first-stage condenser 15 respectively with level-one evaporator 7, secondary evaporimeter 10 and three-level evaporator 13 is stated to go out
Mouth connection, the gas vent of the first-stage condenser 15 are connect with the gas feed of secondary condenser 16；The first-stage condenser
15 and the liquid outlet of secondary condenser 16 connect with ethyl alcohol recycling can 17 by connecting line, the lower end of the connecting line
Below 17 liquid level of ethyl alcohol recycling can.
Optionally, the evaporator at different levels is set at the position on 8~12 meters of esterifying kettle tops at different levels.
Difference in height between evaporators at different levels and the esterifying kettle of lower part is at 8~12 meters, it is ensured that each under vacuum conditions
Material in grade evaporator can flow automatically under the effect of gravity into esterifying kettles at different levels, save equipment and the energy.
Optionally, the evaporator liquid outlet openings at different levels are connected and is located at institute with the pipeline lower end of corresponding esterifying kettle feed inlet
State the liquid level of esterifying kettle or less；The end grade base of evaporator discharges into esterification finished product storage tank 14, and the pipeline lower end that discharges is located at
It is esterified the liquid level of finished product storage tank 14 or less.
It connects under the pipeline lower end of esterifying kettles at different levels and corresponding evaporator liquid outlet opening, the discharging pipeline of whole grade evaporator
The pipeline lower end of end and connection first-stage condenser 15 and 16 liquid outlet of secondary condenser and ethyl alcohol recycling can be located at liquid level with
Under, fluid-tight can be played the role of, guarantee the vacuum state of vaporising devices at different levels.
Optionally, the esterifying kettle at different levels is equipped with collet, is added for being passed through heat medium to material in esterifying kettle
Heat；It is additionally provided with rabbling mechanism in the reaction kettle of the esterification at different levels, for the material in esterifying kettle to be uniformly mixed.
Esterifying kettles at different levels are heated using collet, material in reactor can be made heated more evenly, temperature during simultaneous reactions
It is influenced by the external world smaller.
Optionally, vacuum system 18, the vacuum system 18 and secondary condenser are additionally provided on the secondary condenser 16
Gas vent connection.
Optionally, it is additionally provided with flowmeter on the feeding pipe of the reaction kettle of the esterification at different levels and evaporator at different levels, for controlling
System is delivered to the flow of reaction kettle of the esterification at different levels and the material in evaporator at different levels.
The conveying of materials at different levels controls certain flow by flowmeter, guarantees continuous feed and the reaction finished product of raw material
Continuous extraction and each device in liquid level stabilization.
In conclusion the synthesis process of the ethyl cyanoacetate of the utility model embodiment are as follows:
Cyanoacetic acid and ethyl alcohol are passed through cyanoacetic acid delivery pump 4 and ethyl alcohol delivery pump 2 respectively continuously to send to level-one esterifying kettle 5
In, keep certain temperature to carry out level-one esterification, when the liquid level in level-one esterifying kettle reach a certain height, by level-one ester
The material changed in kettle is continuously introduced into level-one evaporator 7 by first-level transport pump 6, and the water of generation and excessive ethyl alcohol are steamed,
Continuous self-flowing enters in second level esterifying kettle 8 remaining material under the effect of gravity, while being esterified by ethyl alcohol delivery pump 2 to second level
It is continuously added to ethyl alcohol in kettle 8, keeps certain temperature to carry out second level esterification in second level esterifying kettle 8, when second level esterifying kettle
In liquid level reach a certain height, when liquid level did not had lower end of duct of the level-one evaporator to second level esterifying kettle, give level-one evaporator
Band vacuum to absolute pressure is less than 12kpa, and material is risen in level-one evaporator under vacuum by pipeline, when level-one is steamed
When hair device liquid level reach a certain height, the material in second level esterifying kettle is continuously introduced into secondary evaporimeter by two-stage conveying pump 9
In 10, the water generated in second level esterification and excessive ethyl alcohol are steamed, remaining material continuous self-flowing under the effect of gravity
It is continuously added to ethyl alcohol into three-level esterifying kettle 11 into three-level esterifying kettle 11, while through ethyl alcohol delivery pump 2, is esterified in three-level
Certain temperature is kept to carry out three-level esterification in kettle 11, when the liquid level in three-level esterifying kettle 11 reach a certain height, liquid level
When not crossing lower end of duct of the secondary evaporimeter to three-level esterifying kettle, it is less than 12kpa to secondary evaporimeter band vacuum to absolute pressure,
Material is risen in secondary evaporimeter under vacuum by pipeline, will when secondary evaporimeter liquid level reach a certain height
Material in three-level esterifying kettle is continuously introduced into three-level evaporator 13 by three-level delivery pump 12, by what is generated in three-level esterification
Water and excessive ethyl alcohol steam, and the ethyl cyanoacetate of synthesis flows into certainly under the effect of gravity in esterification finished product storage tank 14, when
Liquid level in esterification finished product storage tank 14 reach a certain height, when liquid level did not had lower end of duct of the three-level evaporator to finished product storage tank,
Be less than 12kpa to three-level evaporator band vacuum to absolute pressure, at the same start first-stage condenser 15 and secondary condenser 16 into
Return water, the mixing liquid of the second alcohol and water distilled from three evaporators form liquid after condenser condenses and enter second
Alcohol recycling can 17, the ethyl alcohol of recycling return to esterification system recycling after carrying out alcohol-water separation processing.
Difference in height between evaporating kettles at different levels and the esterifying kettles at different levels of lower part is at 12 meters, entire esterification system esterifying kettles at different levels
Keeping liquid level is 60%, 80~90 DEG C of temperature, and guarantee that lower end of duct from evaporator to esterifying kettle is located at the liquid of esterifying kettle
Below face；In evaporators at different levels keep liquid level be 60%, 50~60 DEG C of temperature, and keep absolute pressure be less than 12kpa；It is esterified into
It is 60% that liquid level is kept in product storage tank, and the lower end of duct from three-level evaporator to esterification finished product storage tank is located at esterification finished product storage tank
Liquid level is hereinafter, the lower end of duct of the outlet of connection condenser and ethyl alcohol recycling can is located at ethyl alcohol recycling jar liquid surface or less.To level-one ester
The flow-rate ratio for changing the cyanoacetic acid and ethyl alcohol that convey in kettle is 1:1.3~1.35；The material that is conveyed into secondary evaporimeter and to two
The flow-rate ratio that ethyl alcohol is conveyed in grade esterifying kettle is 1:0.85~0.9；Material is conveyed into three-level evaporator and to three-level esterifying kettle
The flow-rate ratio for conveying ethyl alcohol is 1:0.4~0.45.The conveying of materials at different levels controls certain flow by flowmeter, guarantees former
The stabilization of liquid level, material stop in esterifying kettles at different levels in the continuous feed of material and the continuous extraction of reaction finished product and each device
Staying the time is 1.5 hours, and residence time in evaporating kettles at different levels is 1.5 hours, required flow according to system volume into
Row adjustment, thereby realizes the successive reaction of ethyl cyanoacetate.
In order to better illustrate the utility model, illustrated below by embodiment is further.
Embodiment 1
Cyanoacetic acid (90%) feed rate is 2 ton/hours, and ethyl alcohol (99%) feed rate is respectively level-one esterifying kettle:
2.63 ton/hours, second level esterifying kettle: 1.7 ton/hours, three-level esterifying kettle: 0.8 ton/hour, esterifying kettles at different levels are to corresponding each
The feed rate of grade evaporator is 2 ton/hours.The extraction flow of ethyl cyanoacetate are as follows: 2.25 ton/hours of (ethyl cyanoacetates
Gas phase content: 95%, moisture: 2.5%), and conversion rate of esterification: 98.44%.Specific process parameter is referring to table 1.
Embodiment 2
Cyanoacetic acid (92%) feed rate is 3 ton/hours, and ethyl alcohol (99%) feed rate is respectively level-one esterifying kettle:
4.02 ton/hours, second level esterifying kettle: 2.61 ton/hours, three-level esterifying kettle: 1.29 ton/hours, esterifying kettles at different levels are to corresponding
The feed rate of evaporators at different levels is 2.9 ton/hours.The extraction flow of ethyl cyanoacetate are as follows: 3.88 ton/hours of (cyanoacetic acids
Ethyl ester gas phase content: 96%, moisture: 3%), and conversion rate of esterification: 98.45%.Specific process parameter is referring to table 1.
Embodiment 3
Cyanoacetic acid (89%) feed rate is 4 ton/hours, and ethyl alcohol (99%) feed rate is respectively level-one esterifying kettle: 5.4
Ton/hour, second level esterifying kettle: 3.52 ton/hours, three-level esterifying kettle: 1.69 ton/hours, esterifying kettles at different levels are to corresponding at different levels
The feed rate of evaporator is 3.8 ton/hours.The extraction flow of ethyl cyanoacetate are as follows: 4.95 ton/hours of (ethyl cyanoacetates
Gas phase content: 96.5%, moisture: 2.3%), and conversion rate of esterification: 98.66%.Specific process parameter is referring to table 1.
Embodiment 4
Cyanoacetic acid (85%) feed rate is 3 ton/hours, and ethyl alcohol (99%) feed rate is respectively level-one esterifying kettle:
3.96 ton/hours, second level esterifying kettle: 2.66 ton/hours, three-level esterifying kettle: 1.25 ton/hours, esterifying kettles at different levels are to corresponding
The feed rate of evaporators at different levels is 3.1 ton/hours.The extraction flow of ethyl cyanoacetate are as follows: 3.54 ton/hours of (cyanoacetic acids
Ethyl ester gas phase content: 97%, moisture: 3%), and conversion rate of esterification: 98.25%.Specific process parameter is referring to table 1.
The technological parameter of 1 each device of embodiment 1-4 of table
| Reaction unit | Embodiment one | Embodiment two | Embodiment three | Example IV |
| Level-one is esterified kettle temperature (DEG C) | 80 | 88 | 87 | 90 |
| Second level is esterified kettle temperature (DEG C) | 80 | 85 | 88 | 90 |
| Three-level is esterified kettle temperature (DEG C) | 80 | 85 | 85 | 90 |
| Level-one evaporator temperature (DEG C) | 50 | 57 | 54 | 60 |
| Level-one evaporator pressure (Mpa) | -0.089 | -0.091 | -0.092 | -0.088 |
| Secondary evaporimeter temperature (DEG C) | 50 | 52 | 58 | 60 |
| Secondary evaporimeter pressure (Mpa) | -0.088 | -0.089 | -0.093 | -0.092 |
| Three-level evaporator pressure (DEG C) | 50 | 53 | 55 | 60 |
| Three-level evaporator pressure (Mpa) | -0.088 | -0.094 | -0.093 | -0.095 |
The synthesizer of ethyl cyanoacetate provided by the utility model, equipment is few, and process route is succinct, ensure that technique
Safety and continuous production, stability, the conversion ratio for improving product and purity reduce energy consumption, have saved production cost.
Esterification device and vaporising device in embodiment 1-4 can also be esterification device and steaming more than 3 grades
Transmitting apparatus, the conversion ratio of esterification can reach 98% or more.
The above is only the preferred embodiment of the utility model only, is not intended to limit the utility model, all at this
Made any modification, equivalent replacement or improvement etc., should be included in the utility model within the spirit and principle of utility model
Protection scope within.
Claims (10)
1. a kind of system for continuous esterification production ethyl cyanoacetate, which is characterized in that the system includes:
Feeding device: inlet port and outlet port are provided with；
Multi-stage reacting device: every further device of the multi-stage reacting device all includes reaction kettle of the esterification and evaporator, the ester
The discharge port of the feed inlet and feeding device of changing reaction kettle connects, the discharge port of the reaction kettle of the esterification and the feed inlet of evaporator
Connection；Pass through the charging of the liquid outlet opening of upper level evaporator and next stage reaction kettle of the esterification between adjacent multistage reaction unit
Mouth series connection, whole grade base of evaporator discharging；
Condensate recycling device: the gas feed of the condensate recycling device is connect with the gas vent of evaporators at different levels.
2. the system for continuous esterification production ethyl cyanoacetate as described in claim 1, which is characterized in that described multistage anti-
The series connection series of device is answered to be no less than 3.
3. the system for continuous esterification production ethyl cyanoacetate as claimed in claim 2, which is characterized in that described multistage anti-
Answering device is third-order reaction device, including level-one esterifying kettle (5), level-one evaporator (7), second level esterifying kettle (8), secondary evaporimeter
(10), three-level esterifying kettle (11) and three-level evaporator (13).
4. the system for continuous esterification production ethyl cyanoacetate as claimed in claim 3, which is characterized in that the charging dress
It sets including ethanol storage tank (1) and cyanoacetic acid storage tank (3)；The discharge port of the ethanol storage tank (1) respectively with esterifying kettles at different levels into
Material mouth connection；The discharge port of the cyanoacetic acid storage tank (3) is connect with the feed inlet of level-one esterifying kettle (5).
5. the system for continuous esterification production ethyl cyanoacetate as claimed in claim 3, which is characterized in that described to be condensed back to
Receiving apparatus includes first-stage condenser (15), secondary condenser (16) and ethyl alcohol recycling can (17)；The first-stage condenser (15)
Gas feed is connect with the gas vent of level-one evaporator (7), secondary evaporimeter (10) and three-level evaporator (13) respectively, described
The gas vent of first-stage condenser (15) is connect with the gas feed of secondary condenser (16)；The first-stage condenser (15) and two
The liquid outlet of grade condenser (16) is connect by connecting line with ethyl alcohol recycling can (17), and the lower end of the connecting line is located at
Below ethyl alcohol recycling can (17) liquid level.
6. the system for continuous esterification production ethyl cyanoacetate as described in claim 1, which is characterized in that the steamings at different levels
Hair device is set at the position on 8~12 meters of esterifying kettle tops at different levels.
7. the system for continuous esterification production ethyl cyanoacetate as claimed in claim 6, which is characterized in that connection is described each
Grade evaporator liquid outlet opening is located at the liquid level of the esterifying kettle or less with the pipeline lower end of corresponding esterifying kettle feed inlet；The end
Grade base of evaporator discharge into esterification finished product storage tank (14), and discharge pipeline lower end be located at esterification finished product storage tank (14) liquid level with
Under.
8. the system for continuous esterification production ethyl cyanoacetate as described in claim 1, which is characterized in that the esters at different levels
Change kettle and be equipped with collet, is heated for being passed through heat medium to the material in esterifying kettle；It is also set in the esterifying kettle at different levels
There is rabbling mechanism, for the material in esterifying kettle to be uniformly mixed.
9. the system for continuous esterification production ethyl cyanoacetate as claimed in claim 5, which is characterized in that the second level is cold
It is additionally provided on condenser (16) vacuum system (18), the vacuum system (18) connect with the gas vent of secondary condenser.
10. the system for continuous esterification production ethyl cyanoacetate as described in claim 1, which is characterized in that described at different levels
Be additionally provided with flowmeter on the feeding pipe of reaction kettle of the esterification and evaporator at different levels, for control be delivered to reaction kettle of the esterification at different levels and
The flow of material in evaporators at different levels.
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| CN110496575A (en) * | 2019-07-17 | 2019-11-26 | 江苏新东风化工科技有限公司 | A kind of esterification production after-treatment system and its treatment process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110496575A (en) * | 2019-07-17 | 2019-11-26 | 江苏新东风化工科技有限公司 | A kind of esterification production after-treatment system and its treatment process |
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