CN209555116U - A kind of cyanoacetate esterification pretreatment unit - Google Patents
A kind of cyanoacetate esterification pretreatment unit Download PDFInfo
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- CN209555116U CN209555116U CN201920171408.3U CN201920171408U CN209555116U CN 209555116 U CN209555116 U CN 209555116U CN 201920171408 U CN201920171408 U CN 201920171408U CN 209555116 U CN209555116 U CN 209555116U
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- kettle
- blade
- pretreatment unit
- autoclave body
- alcohol
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Abstract
The utility model discloses a kind of cyanoacetates to be esterified pretreatment unit, belong to chemical equipment technical field, pretreatment unit includes dehydration device, demineralizer and esterifying kettle, key is: the demineralizer includes a sequentially connected filter, concentration liquid storage tank, alcohol analysis kettle, aflter-fillter and processed concentrate holding vessel, it further include alcohol measuring tank, the outlet of alcohol measuring tank is connect with the import of alcohol analysis kettle, the import of filter and the discharge port of dehydration device connect, and the discharge port of processed concentrate holding vessel is connect with esterifying kettle.Raw material needed for the salt in cyanoacetate being removed and the organic solvent or subsequent reactions that use, environmental protection and saving, other auxiliary agents are not added, easy to operate, effect is good, and the removal rate of impurity sodium chloride can achieve 99% or more, prevent the generation of subsequent mixed salt, problem of environmental pollution caused by mixed salt is avoided, the consumption of sulfuric acid is reduced, it is therefore prevented that the generation of side reaction.
Description
Technical field
The utility model belongs to chemical equipment technical field, is related to a kind of pretreatment unit, especially a kind of cyanoacetic acid
Ester is esterified pretreatment unit.
Background technique
Cyanoacetate is a kind of important industrial chemicals and medicine intermediate, can be used for the synthesis of medicine, dyestuff, adhesive
Deng.Cyanoacetate is in process of production, it may appear that since raw material cyanoacetic acid brings sodium chloride into, leads to more consumption sulphur in production
Acid, generates side reaction, and esterification generates the problems such as mixed salt can not be handled.It is most of at present for the pretreatment of cyanoacetate esterification
Raw material cyanoacetic acid is only simply dehydrated desalination by technique, is still had partial oxidation sodium to be brought into esterification after this treatment, is influenced ester
Change reaction and subsequent processing.
Summary of the invention
The utility model in order to overcome the drawbacks of the prior art, devises a kind of cyanoacetate esterification pretreatment unit, can
With raw material needed for the organic solvent or subsequent reactions that remove the salt in cyanoacetate and use, environmental protection and saving does not add it
His auxiliary agent, easy to operate, effect is good, and the removal rate of impurity sodium chloride can achieve 99% or more, it is therefore prevented that the production of subsequent mixed salt
It is raw, problem of environmental pollution caused by mixed salt is avoided, the consumption of sulfuric acid is reduced, it is therefore prevented that the generation of side reaction.
The specific technical solution that the utility model is taken is: a kind of cyanoacetate esterification pretreatment unit, including dehydration
Device, demineralizer and esterifying kettle, key are: the demineralizer includes sequentially connected filter, a concentrate
Storage tank, alcohol analysis kettle, aflter-fillter and processed concentrate holding vessel, further include alcohol measuring tank, the outlet of alcohol measuring tank and alcohol
The import connection of kettle is analysed, the import of filter and the discharge port of dehydration device connect, and processed concentrate holding vessel goes out
Material mouth is connect with esterifying kettle.
The demineralizer further includes the first delivery pump being connected between dehydration device and a filter, is connected to
The second delivery pump between concentration liquid storage tank and alcohol analysis kettle, the third delivery pump being connected between alcohol analysis kettle and aflter-fillter,
The 4th delivery pump being connected between processed concentrate holding vessel and esterifying kettle.
The dehydration device includes that sequentially connected cyanoacetic acid dehydrating kettle, condenser and condensation water storage tank, cyanoacetic acid are de-
Water kettle includes autoclave body and the collet that autoclave body periphery is arranged in, and the cavity between autoclave body and collet is heating chamber, is provided on collet
Steam (vapor) outlet for the steam inlet of the outlet connection with heat source and for being connect with the refluxing opening of heat source, steam inlet
It is all connected to heating chamber with steam (vapor) outlet, control valve is provided at steam inlet, is provided with temperature sensor and pressure in autoclave body
Sensor, dehydration device further include controller, and temperature sensor, controller, control valve, which are in turn connected to form to control for temperature, is
System, the import of filter and the discharge port of autoclave body bottom connect, and condense and are provided with vacuum outlet at the top of water storage tank.
The cyanoacetic acid dehydrating kettle further includes rabbling mechanism, rabbling mechanism include be arranged in agitating shaft inside autoclave body with
And the driving motor above autoclave body is set, the lower end of agitating shaft is fixed with stirrer paddle, the upper end of agitating shaft and driving motor
Output shaft be fixedly connected,
The stirrer paddle includes upper blade and lower layer's blade, all fixed at the center of upper blade and lower layer's blade
There is screw shell, external screw thread is provided on agitating shaft, upper blade and lower layer's blade are all by screw shell and agitating shaft spiral shell
Line connection, makes upper blade and lower layer's blade all have lifting freedom degree.
The beneficial effects of the utility model are: dilute cyanoacetic acid and sulfuric acid react and are concentrated in dehydration device,
Then it is once filtered by a filter, removes most of impurity sodium chloride, then analyse the analysis of kettle alcohol by alcohol, using
Aflter-fillter carries out secondary filter, further removes remaining a small amount of sodium chloride.The demineralizer process is simple, impurity-eliminating effect
It is good, the salt in cyanoacetate can be effectively removed, used sulfuric acid amount is esterified and is substantially reduced, cyanoacetate impurity peaks out
Seldom.
Organic solvent sulfuric acid used in concentration process is the raw material of subsequent reactions, will not bring new impurity or precipitating into
Agent, process safety are low in cost.The salt in cyanoacetic acid is completely removed in advance, it is therefore prevented that the generation of subsequent mixed salt avoids mixed
Problem of environmental pollution caused by salt reduces the consumption of sulfuric acid, it is therefore prevented that the generation of side reaction.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the utility model.
In attached drawing, 1 represents cyanoacetic acid dehydrating kettle, and 2 represent the first delivery pump, and 3 represent a filter, and 4 represent concentrate
Storage tank, 5 represent the second delivery pump, and 6 represent alcohol analysis kettle, and 7 represent alcohol measuring tank, and 8 represent third delivery pump, and 9 represent secondary filter
Device, 10 represent processed concentrate holding vessel, and 11 represent the 4th delivery pump, and 12 represent temperature sensor, and 13 represent esterifying kettle, and 14
Condenser is represented, 15 represent condensation water storage tank, and 16 represent agitating shaft, and 17 represent driving motor, and 18 represent stirrer paddle.
Specific embodiment
It elaborates in the following with reference to the drawings and specific embodiments to the utility model:
Specific embodiment, as shown in Figure 1, a kind of cyanoacetate is esterified pretreatment unit, including dehydration device, demineralizer
With esterifying kettle 13, the demineralizer includes a sequentially connected filter 3, concentration liquid storage tank 4, alcohol analysis kettle 6, secondary mistake
Filter 9 and processed concentrate holding vessel 10, further include alcohol measuring tank 7, and the outlet of alcohol measuring tank 7 and the import of alcohol analysis kettle 6 connect
It connects, the import of filter 3 and the discharge port of dehydration device connect, the discharge port of processed concentrate holding vessel 10 and esterification
Kettle 13 connects.
As to further improvement of the utility model, demineralizer further includes being connected to dehydration device and a filter
The first delivery pump 2 between 3, the second delivery pump 5 being connected between concentration liquid storage tank 4 and alcohol analysis kettle 6 are connected to alcohol analysis kettle 6
Third delivery pump 8 between aflter-fillter 9, the 4th be connected between processed concentrate holding vessel 10 and esterifying kettle 13
Delivery pump 11.Material can be made rapidly to be entered in next equipment by an equipment using delivery pump, production can be improved
Efficiency.
As to further improvement of the utility model, dehydration device includes sequentially connected cyanoacetic acid dehydrating kettle 1, condensation
Device 14 and condensation water storage tank 15, cyanoacetic acid dehydrating kettle 1 includes autoclave body and the collet that autoclave body periphery is arranged in, between autoclave body and collet
Cavity be heating chamber, be provided on collet for the steam inlet of outlet connection with heat source and for being returned with heat source
The steam (vapor) outlet of head piece connection, steam inlet and steam (vapor) outlet are all connected to heating chamber, and control valve, kettle are provided at steam inlet
Be provided with temperature sensor 12 and pressure sensor in vivo, dehydration device further includes controller, temperature sensor 12, controller,
Control valve is in turn connected to form as temperature control system, and the import of filter 3 and the discharge port of autoclave body bottom connect, condensation
The top of water storage tank 15 is provided with vacuum outlet.The vacuum outlet for condensing 15 top of water storage tank is connect with negative pressure system, is utilized
Heat source conveys hot gas into heating chamber, carries out heating concentration to the intracorporal solution of kettle, the effect of the steam of generation in negative pressure system
Under enter in condenser 14 and be condensed into liquid, then flow into inside condensation water storage tank 15, make in autoclave body in vacuum state.Temperature
Spend sensor 12, controller and control valve cooperate, can make the temperature range that setting is maintained inside autoclave body, automation control,
It is more time saving and energy saving.
As to further improvement of the utility model, cyanoacetic acid dehydrating kettle 1 further includes rabbling mechanism, and rabbling mechanism includes
The driving motor 17 that the agitating shaft 16 inside autoclave body is arranged in and is arranged in above autoclave body, the lower end of agitating shaft 16, which is fixed with, to be stirred
Blade 18 is mixed, the upper end of agitating shaft 16 is fixedly connected with the output shaft of driving motor 17.Agitating shaft is driven using driving motor 17
16 and stirrer paddle 18 rotate, the intracorporal solution of kettle is stirred, both makes to be sufficiently mixed reaction, mixing can be improved and imitate
Fruit.
As to further improvement of the utility model, stirrer paddle 18 includes upper blade and lower layer's blade, upper-layer paddle
It is all fixed with screw shell at the center of leaf and lower layer's blade, external screw thread, upper blade and lower layer's blade are provided on agitating shaft
All it is to be threadedly coupled by screw shell with agitating shaft 16, makes upper blade and lower layer's blade that all there is lifting freedom degree.Pass through
Rotate screw shell, thus it is possible to vary between the upper and lower position and upper blade and lower layer's blade of upper blade and lower layer's blade
Away to obtain better mixed effect.
A certain amount of dilute cyanoacetic acid and sulfuric acid are first added into cyanoacetic acid dehydrating kettle 1 when specifically used for the utility model,
Start stirring simultaneously, vacuum and steam automatic control carry out concentration, and the concentration for the sodium sulfocyanate for producing reaction is controlled in 85-
90%, it is then turned on the dispensing valve of 1 bottom of cyanoacetic acid dehydrating kettle, opens the inlet valve of the first delivery pump 2 and concentration liquid storage tank 4
Door makes material enter concentrate storage tank 4 after a filter 3, removes most of impurity sodium chloride, closes after blowing
The dispensing valve of 1 bottom of cyanoacetic acid dehydrating kettle.The agitating device for opening alcohol analysis kettle 6, is then turned on the outlet valve of concentration liquid storage tank 4
Door opens the outlet valve of the second delivery pump 5 and 7 bottom of alcohol measuring tank.When liquid level is higher than the high report liquid of setting in alcohol analysis 6 kettle of kettle
When position, the outlet valve of the second delivery pump 5 and 7 bottom of alcohol measuring tank is closed, third delivery pump 8 is opened, material is sent into secondary
It is filtered in filter 9, further removes remaining a small amount of sodium chloride, filtrate enters in processed concentrate holding vessel 10.
When esterification needs, processed 10 bottom valve of concentrate holding vessel is opened, opens the 4th delivery pump 11 to 13 feeding of esterifying kettle.
This demineralizer process is simple, and good impurity removing effect, the removal rate of impurity sodium chloride can achieve 99% or more, ester
Sulfuric acid amount used in changing is substantially reduced, and cyanoacetate impurity peaks out are few.Organic solvent sulphur used in concentration process
Acid is the raw material of subsequent reactions, will not bring new impurity or precipitating reagent into, and process safety is low in cost.In advance by cyanoacetic acid
In salt completely remove, it is therefore prevented that the generation of subsequent mixed salt avoids problem of environmental pollution caused by mixed salt, reduces sulfuric acid
Consumption, it is therefore prevented that the generation of side reaction.
Claims (5)
1. a kind of cyanoacetate is esterified pretreatment unit, including dehydration device, demineralizer and esterifying kettle (13), feature exists
In: the demineralizer includes a sequentially connected filter (3), concentration liquid storage tank (4), alcohol analysis kettle (6), secondary filter
Device (9) and processed concentrate holding vessel (10) further include alcohol measuring tank (7), the outlet of alcohol measuring tank (7) and alcohol analysis kettle (6)
Import connection, the import of filter (3) and the discharge port of dehydration device connect, processed concentrate holding vessel (10)
Discharge port is connect with esterifying kettle (13).
2. a kind of cyanoacetate according to claim 1 is esterified pretreatment unit, it is characterised in that: the demineralizer
Further include the first delivery pump (2) being connected between dehydration device and a filter (3), be connected to concentration liquid storage tank (4) with
Alcohol analyses the second delivery pump (5) between kettle (6), the third delivery pump being connected between alcohol analysis kettle (6) and aflter-fillter (9)
(8), the 4th delivery pump (11) being connected between processed concentrate holding vessel (10) and esterifying kettle (13).
3. a kind of cyanoacetate according to claim 1 is esterified pretreatment unit, it is characterised in that: the dehydration device
Include including sequentially connected cyanoacetic acid dehydrating kettle (1), condenser (14) and condensation water storage tank (15), cyanoacetic acid dehydrating kettle (1)
Autoclave body and the collet that autoclave body periphery is arranged in, cavity between autoclave body and collet are heating chamber, be provided on collet for heat
The steam inlet that the outlet in source connects and the steam (vapor) outlet for connecting with the refluxing opening of heat source, steam inlet and steam go out
Mouth is all connected to heating chamber, and control valve is provided at steam inlet, temperature sensor (12) and pressure sensing are provided in autoclave body
Device, dehydration device further include controller, and temperature sensor (12), controller, control valve, which are in turn connected to form to control for temperature, is
System, the import of filter (3) and the discharge port of autoclave body bottom connect, and are provided with negative pressure at the top of condensation water storage tank (15) and go out
Mouthful.
4. a kind of cyanoacetate according to claim 1 is esterified pretreatment unit, it is characterised in that: the cyanoacetic acid is de-
Water kettle further includes rabbling mechanism, and rabbling mechanism includes the agitating shaft (16) being arranged in inside autoclave body and is arranged in above autoclave body
Driving motor (17), the lower end of agitating shaft (16) are fixed with stirrer paddle (18), the upper end of agitating shaft (16) and driving motor
(17) output shaft is fixedly connected.
5. a kind of cyanoacetate according to claim 4 is esterified pretreatment unit, it is characterised in that: the stirrer paddle
(18) include upper blade and lower layer's blade, be all fixed with screw shell, agitating shaft at the center of upper blade and lower layer's blade
On be provided with external screw thread, upper blade and lower layer's blade are all to be threadedly coupled by screw shell with agitating shaft (16), make upper layer
Blade and lower layer's blade all have lifting freedom degree.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920171408.3U CN209555116U (en) | 2019-01-31 | 2019-01-31 | A kind of cyanoacetate esterification pretreatment unit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920171408.3U CN209555116U (en) | 2019-01-31 | 2019-01-31 | A kind of cyanoacetate esterification pretreatment unit |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN209555116U true CN209555116U (en) | 2019-10-29 |
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ID=68310232
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201920171408.3U Active CN209555116U (en) | 2019-01-31 | 2019-01-31 | A kind of cyanoacetate esterification pretreatment unit |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN209555116U (en) |
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2019
- 2019-01-31 CN CN201920171408.3U patent/CN209555116U/en active Active
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