CN106905176B - Continuous hydrolysis prepares the method and self-oscillation reactor of imido oxalic acid - Google Patents
Continuous hydrolysis prepares the method and self-oscillation reactor of imido oxalic acid Download PDFInfo
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- CN106905176B CN106905176B CN201710076675.8A CN201710076675A CN106905176B CN 106905176 B CN106905176 B CN 106905176B CN 201710076675 A CN201710076675 A CN 201710076675A CN 106905176 B CN106905176 B CN 106905176B
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- oxalic acid
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 30
- 235000006408 oxalic acid Nutrition 0.000 title claims abstract description 28
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 27
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 141
- 239000007788 liquid Substances 0.000 claims abstract description 59
- 238000003860 storage Methods 0.000 claims abstract description 31
- 230000000694 effects Effects 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- CSIFGMFVGDBOQC-UHFFFAOYSA-N 3-iminobutanenitrile Chemical compound CC(=N)CC#N CSIFGMFVGDBOQC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims description 64
- 239000002994 raw material Substances 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 2
- 238000010438 heat treatment Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 3
- 230000004308 accommodation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000001154 acute effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- -1 amido oxalic acid Chemical compound 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/26—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing carboxyl groups by reaction with HCN, or a salt thereof, and amines, or from aminonitriles
-
- 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
-
- 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
- B01J19/0013—Controlling the temperature of the process
-
- 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
-
- 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
- B01J19/18—Stationary reactors having moving elements inside
-
- 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
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/185—Stationary reactors having moving elements inside of the pulsating type
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00092—Tubes
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00162—Controlling or regulating processes controlling the pressure
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a kind of method that continuous hydrolysis prepares imido oxalic acid.Include the following steps: in proportion to mix reaction mass imido grpup diacetonitrile and water；Perfectly mixed reactor is provided, reaction mass is delivered in the perfectly mixed reactor, reaction is hydrolyzed；Tubular reactor is provided, the reaction solution in the perfectly mixed reactor is delivered in the tubular reactor under the effect of liquid level differential pressure；Product storage tank is provided, reaction mass is in periodical self-oscillation flowing between the tubular reactor and the product storage tank, and product drains into the product storage tank after reaction.The method that continuous hydrolysis provided by the invention prepares imido oxalic acid, improves reaction yield.The present invention also provides a kind of self-oscillation reactors.
Description
Technical field
The present invention relates to chemical equipment technical fields, and in particular to a kind of method that continuous hydrolysis prepares imido oxalic acid
And self-oscillation reactor.
Background technique
In chemical reaction, liquid-solid reaction is mostly used to carry out in tank reactor, and interphase mass transfer, mixing and heat transfer are to determine
The important technology index for determining reactor performance, directly influences response intensity, conversion ratio and product quality.By mode of operation, kettle
Formula reactor includes batch tank reactor and continuous tank reactor, and wherein interval tank reactor is adapted to small lot, more
Kind, reaction time longer production, but have the characteristics that unstable product quality, and reactant species are limited；Continuously
Tank reactor can avoid the shortcomings that batch tank reactor, but stirring action will cause the back-mixing of fluid in kettle, acute in stirring
Strong, liquid viscosity is lower or the longer occasion of mean residence time, and logistics flow pattern may be regarded as complete mixing flow in kettle.It is requiring to convert
Under conditions of rate, high income, the air-teturning mixed phenomenon in tank reactor is unfavorable factor.Generally use the concatenated side of multi-stage reacting kettle
Formula, to reduce the adverse effect of back-mixing.However, the concatenated mode of multistage tank reactor, keeps the residence time of material longer, instead
Low efficiency is answered, and conversion ratio can only be improved to a certain extent.
Therefore, it is necessary to provide a kind of new technique solution above-mentioned technical problem.
Summary of the invention
The purpose of the present invention is overcoming above-mentioned technical problem, it is good to provide a kind of mass transfer, heat-transfer effect, the continuous water of high income
The method that solution prepares imido oxalic acid.
The technical scheme is that
A kind of method that continuous hydrolysis prepares imido oxalic acid, includes the following steps:
Step S1: reaction mass imido grpup diacetonitrile and water are mixed in proportion；
Step S2: perfectly mixed reactor is provided, reaction mass is delivered in the perfectly mixed reactor, reaction is hydrolyzed；
Step S3: providing tubular reactor, and the reaction solution in the perfectly mixed reactor conveys under the effect of liquid level differential pressure
In to the tubular reactor；
Step S4: providing product storage tank, and reaction mass is in the period between the tubular reactor and the product storage tank
Property self-oscillation flowing, product drains into the product storage tank after reaction.
Preferably, circulation path of the reaction mass between the tubular reactor and the product storage tank is inverted u-shaped, institute
The discharge port position for stating tubular reactor is higher than the feed inlet position of the tubular reactor and lower than the tubular type
The highest liquid level of reactor.
Preferably, the difference in height between the discharge port of the tubular reactor and the feed inlet of the pipe reaction is described
The 1/3-1/2 of tubular reactor highest level value.
Preferably, the discharge port position of the complete mixed reaction kettle is higher than the tubular reactor topmost.
Preferably, in step S1, reaction mass is mixed and is delivered to using feed system and is mixed in reaction kettle entirely,
The feed system includes metering screw, the solid-liquid mixer connecting with the output end of the metering screw and for that will mix
Close the delivery pump that material is delivered to the perfectly mixed reactor.
Preferably, in step S2, further include the steps that preheating reaction mass, the reaction mass after preheating is delivered to
It is reacted in the entirely mixed reaction kettle.
Preferably, in reaction raw materials imido grpup diacetonitrile and water mixing molar ratio 1:5-20.
Preferably, the entirely mixed material in reactor reaction temperature is 190-200 DEG C, reaction pressure 9-11MPa.
Preferably, material reaction temperature is 190-220 DEG C in the tubular reactor.
The present invention also provides a kind of self-oscillation reactor, including set gradually by Flow of Goods and Materials direction complete mixed reaction kettle,
Tubular reactor, communicating pipe and product storage tank, the communicating pipe both ends are separately connected the tubular reactor and the product is store
Slot keeps circulation path of the material between the tubular reactor and the product storage tank inverted u-shaped, the complete mixed reaction kettle
Discharge port position is higher than the tubular reactor topmost, sets the terminal of the communicating pipe as the tubular reactor
Discharge port, the discharge port position of the tubular reactor are higher than the feed inlet position of the tubular reactor and are lower than
The highest liquid level of the tubular reactor.
Compared with prior art, the method that continuous hydrolysis provided by the invention prepares imido oxalic acid, have has as follows
Beneficial effect:
One, the method that continuous hydrolysis provided by the invention prepares imido oxalic acid, using imido grpup diacetonitrile and water as
Reaction raw materials answer in the self-oscillation and reaction are hydrolyzed in device, wherein the self-oscillation reverse answers device by mixing reaction kettle and pipe entirely
Formula combination of reactors makes wherein the discharge port of the complete mixed reaction kettle is higher than the tubular reactor topmost in complete mixed reaction
The reaction mass reached a certain level in kettle is flowed under the action of pressure difference in the tubular reactor；The tubular reactor with
It is connected between the product storage tank by the communicating pipe for keeping the circulation path of material inverted u-shaped, the terminal of the communicating pipe is made
For the discharge port of the tubular reactor, and the discharge port position of the tubular reactor is higher than the tubular reactor
Feed inlet position and the highest liquid level for being lower than the tubular reactor, the liquid level in the tubular reactor reach certain height
After degree, material overcomes the resistance of the tubular reactor to flow into the product storage tank from the discharge port of the tubular reactor；?
During Flow of Goods and Materials, the material liquid level in the tubular reactor is higher, and flowing velocity is fast, when its flowing velocity increases up to
After certain flow velocity, the material liquid level in the tubular reactor is reduced, and as its liquid level reduces to a certain extent, material is in institute
The flow velocity stated in tubular reactor reduces, since siphonage makes the material liquid level in the tubular reactor lower than its highest liquid
Position but the liquid level for being higher than its discharge port.When liquid level cannot overcome the resistance of the tubular reactor, the tubular reactor
The outflow of discharge port no liquid or flow very little；Material liquid level in the subsequent tubular reactor increases again, so as to form stream
The fast-slow circulation of speed.
Therefore, reaction mass enhances the pipe reaction in periodical self-oscillation flowing in the tubular reactor
The mass transfer and biography heat transfer effect of device, equally have preferable reaction and temperature control effect under lower flow velocity, it is anti-to improve material
The yield answered.
The reaction yield of the method for continuous hydrolysis imido oxalic acid provided by the invention is 95% or more.
Two, the method that continuous hydrolysis provided by the invention prepares imido oxalic acid, in the self-oscillation reactor into
Row, the self-oscillation reactor are flow reactor, by control reaction temperature and reaction pressure, improve reaction rate, into
And water consumption needed for the reaction can be reduced, reduce energy consumption.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of self-oscillation reactor provided by the invention.
Specific embodiment
Below in conjunction with drawings and embodiments, the invention will be further described.
Fig. 1 is please referred to, is the structural schematic diagram of self-oscillation reactor provided by the invention.The self-oscillation reactor
100 include feed system 1, heat exchanger 2, entirely mixed reaction kettle 3, tubular reactor 4, communicating pipe 5 and product storage tank 6, and it is described into
Material system 1, heat exchanger 2, mixed reaction kettle 3, tubular reactor 4, communicating pipe 5 and product storage tank 6 are sequentially connected entirely.
The feed system 1 includes metering screw 11, solid-liquid mixer 12 and material-handling pump 13, and the metering spiral shell
The output end of rotation 11 is connect with the solid-liquid mixer 12.Wherein the metering screw 11 is used for conveying solid material, and root
According to material proportion accurate measurement, the material for being delivered to the solid-liquid mixer 12 is made to meet ratio requirement.The fixed mixing
Device 12 is connect with liquid material feeding mechanism (not shown), and fixed material and liquid material are mixed in the solid-liquid mixer 12
The heat exchanger 2 is delivered to by the material-handling pump 13 after conjunction and carries out reaction mass preheating.The solid-liquid mixer 12
It can be solid-liquid mixing pump, structure can refer to solid-liquid mixing pump in the prior art.
The heat exchanger 2 is for heating reaction mass comprising the first noumenon 21, first charging aperture 22 and the first discharge port
23, the first charging aperture 22 is set to the bottom of the first noumenon 21, and first discharge port 23 is set to second ontology
21 top.
In the present invention, the heat exchanger 2 is inessential component, because may be used also other than using heat exchanger heating reaction mass
It is realized in a manner of using collet is arranged outside the entirely mixed reaction kettle 3.
The entirely mixed reaction kettle 3 includes the second ontology 31, the second charging aperture 32 set on the autoclave body 31, the second discharge port
33, discharge gate 34, blender 35, the first temperature measurement-control instrument 36 for detecting material reaction temperature in kettle and for detecting in kettle
The pressure testing and controlling instrument 37 of reaction pressure.
Second ontology 31 is hollow structure, the interior accommodation space for forming a receiving material, the blender 35
It is mounted on 31 top of the second ontology, stirring blade is set in the accommodation space.The second charging aperture 32 is set
In the top of second ontology 31, second discharge port 33 is set to the bottom of second ontology 31, the discharge gate 34
It is equally set to the bottom of second ontology 31, and it is arranged position and is lower than 33 position of the second discharge port, for clear
Material in kettle is drained when washing.
Certainly, other than above embodiment, the setting position of the second charging aperture 32 can also be located at described second
The bottom of ontology 31, position are lower than 33 position of the second discharge port.
First temperature measurement-control instrument 36 is used to detect the material reaction temperature in the complete mixed reaction kettle 3, and can will survey
Amount data are sent to the material-handling pump 13, for controlling the output quantity of the material-handling pump 13.The pressure testing and controlling instrument
37 for detecting the reaction pressure in the complete mixed reaction kettle 3, and adjusts reaction pressure according to testing result, accords with pressure in kettle
It closes and requires.
The tubular reactor 4 includes third ontology 41, third feed inlet 42, third discharge port 43 and second temperature observing and controlling
Instrument 44.
Wherein, set the terminal of the communicating pipe 5 as the third discharge port 43, the terminal of the communicating pipe 5 refer to its with
One end that the product storage tank 6 connects.
Second discharge port, 33 position is higher than the third feed inlet 42 and 43 institute of the third discharge port is in place
It sets；Preferably, 33 position of the second discharge port is higher than the top position of the tubular reactor 4, i.e., described
Second discharge port 33 is higher than the highest liquid level of the tubular reactor 4.The highest liquid level of the tubular reactor 4, which refers in it, to be contained
Liquid level when greatest limit material, as shown in Figure 1, its highest liquid level is the top of the tubular reactor.
43 position of third discharge port is higher than 42 position of third feed inlet, and anti-lower than the tubular type
The highest liquid level for answering device 4, the circulation path for making material flow into the product storage tank 6 from the tubular reactor 4 are inverted u-shaped.It is excellent
Choosing, the difference in height between the third discharge port 43 and the third feed inlet 42 is the tubular reactor highest level value
1/3-1/2.
The second temperature measurement and control instrument 44 is used to detect the temperature of charge in the tubular reactor 4, makes material certain
Temperature under the conditions of complete reaction.
Self-oscillation reactor provided by the invention, working principle are as follows:
The discharge port position of the complete mixed reaction kettle 3 is higher than the tubular reactor 4 topmost, makes in complete mixed reaction
The reaction mass reached a certain level in kettle 3 is flowed under the action of pressure difference in the tubular reactor 4；The tubular reactor
It is connected between 4 and the product storage tank 6 by the communicating pipe 5 for keeping the circulation path of material inverted u-shaped, by the communicating pipe 5
Discharge port of the terminal as the tubular reactor 4, and the discharge port position of the tubular reactor 4 is higher than the tubular type
The feed inlet position of reactor 4 and the highest liquid level for being lower than the tubular reactor 4, when in the tubular reactor 4
After liquid level reach a certain height, material overcomes the resistance of the tubular reactor 4 to flow into from the discharge port of the tubular reactor 4
The product storage tank 6；During Flow of Goods and Materials, the material liquid level in the tubular reactor 4 is higher, and flowing velocity is fast, when
After its flowing velocity increases up to certain flow velocity, the material liquid level in the tubular reactor 4 is reduced, as its liquid level reduces
To a certain extent, flow velocity of the material in the tubular reactor 4 reduces, since siphonage makes in the tubular reactor 4
Material liquid level lower than its highest liquid level but be higher than its discharge port liquid level.When liquid level cannot overcome the tubular reactor 4
When resistance, the discharge port no liquid outflow of the tubular reactor 4 or flow very little；Object in the subsequent tubular reactor 4
Feed liquid position increases again, so as to form the fast-slow circulation of flow velocity.
Therefore, material enhances the tubular reactor 4 in periodical self-oscillation flowing in the tubular reactor 4
Mass transfer and pass heat transfer effect, equally there is preferable reaction and temperature control effect under lower flow velocity, improve material reaction
Yield.
It is elaborated below by way of specific embodiment and the self-oscillation reactor is applied to continuous hydrolysis preparation Asia
The technique of amido oxalic acid.
Embodiment 1
A kind of method that continuous hydrolysis prepares imido oxalic acid, includes the following steps:
Step S1: reaction mass imido grpup diacetonitrile and water are mixed according to molar ratio 1:5；
Specifically, raw material imido grpup diacetonitrile is delivered to the solid-liquid mixer 12 by the metering screw 11；
Raw water is equally delivered to the solid-liquid mixer 12, mixes the two in proportion；
Step S2: mixed material is delivered in the entirely mixed reaction kettle 3, reaction is hydrolyzed；
Specifically, mixed material is delivered in the heat exchanger 2 by the material-handling pump 13, carries out reaction mass and add
Heat, reaction mass enters in the entirely mixed reaction kettle 3 through the second charging aperture 32 after heating；And control the entirely mixed reaction kettle
Reaction temperature in 3 is 190 DEG C, reaction pressure 9MPa；
Step S3: the reaction solution in the complete mixed reaction kettle 3 flows into the tubular reactor 4 under the effect of liquid level differential pressure
It is interior；
Specifically, when the material reaction in the complete mixed reaction kettle 3 to a certain extent after, under the action of pressure difference material by
Second discharge port 33 flows out, and enters in the tubular reactor 4 through the third feed inlet 42；And it is anti-to control the tubular type
Answering device interior reaction temperature is 220 DEG C.
Step S4: reaction mass is between the tubular reactor 4 and the product storage tank 6 in periodical self-oscillation stream
Dynamic, product drains into the product storage tank 6 after reaction；
Specifically, material overcomes the tubular reactor after liquid level in the tubular reactor 4 reach a certain height
4 resistance flows into the product storage tank from third discharge port 43；Material during Flow of Goods and Materials, in the tubular reactor
Liquid level is higher, and flowing velocity is fast, material after its flowing velocity increases up to certain flow velocity, in the tubular reactor 4
Liquid level reduces, and as its liquid level reduces to a certain extent, flow velocity of the material in the tubular reactor is reduced, since siphon is existing
As making the material liquid level in the tubular reactor lower than its highest liquid level but higher than the liquid level of its discharge port；
When liquid level cannot overcome the resistance of the tubular reactor 4,43 no liquid of the third discharge port outflow or stream
Measure very little；Material liquid level in the subsequent tubular reactor 4 increases again, so as to form the fast-slow circulation of flow velocity, makes to react
Material flows in the tubular reactor 4 in periodic self-oscillation.
Embodiment 2
A kind of method that continuous hydrolysis prepares imido oxalic acid, includes the following steps:
Step S1: reaction mass imido grpup diacetonitrile and water are mixed according to molar ratio 1:10；
Step S2: mixed material is delivered in the entirely mixed reaction kettle 3, reaction is hydrolyzed；
Specifically, mixed material is delivered in the heat exchanger 2 by the material-handling pump 13, carries out reaction mass and add
Heat, reaction mass enters in the entirely mixed reaction kettle 3 through the second charging aperture 32 after heating；Controlling reaction temperature is 195 DEG C,
Reaction pressure is 10MPa；
Step S3: the reaction solution in the complete mixed reaction kettle 3 flows into the tubular reactor 4 under the effect of liquid level differential pressure
It is interior；
Specifically, when the material reaction in the complete mixed reaction kettle 3 to a certain extent after, under the action of pressure difference material by
Second discharge port 33 flows out, and enters in the tubular reactor 4 through the third feed inlet 42；And it is anti-to control the tubular type
Answering 4 interior reaction temperature of device is 200 DEG C.
Step S4: step S4: reaction mass is between the tubular reactor 4 and the product storage tank 6 in periodically certainly
Oscillation Flows, product drains into the product storage tank 6 after reaction；
The principle that material is periodically flowed in self-oscillation in the tubular reactor 4 is referring to embodiment 1.
Embodiment 3
A kind of method that continuous hydrolysis prepares imido oxalic acid, includes the following steps:
Step S1: reaction raw materials imido grpup diacetonitrile and water are mixed according to molar ratio 1:20；
Step S2: mixed material is delivered in the entirely mixed reaction kettle 3, reaction is hydrolyzed；
Specifically, mixed material is delivered in the heat exchanger 2 by the material-handling pump 13, carries out reaction mass and add
Heat, reaction mass enters in the entirely mixed reaction kettle 3 through the second charging aperture 32 after heating；Controlling reaction temperature is 200 DEG C,
Reaction pressure is 11MPa；
Step S3: the reaction solution in the complete mixed reaction kettle 3 flows into the tubular reactor 4 under the effect of liquid level differential pressure
It is interior；
Specifically, when the material reaction in the complete mixed reaction kettle 3 to a certain extent after, under the action of pressure difference material by
Second discharge port 33 flows out, and enters in the tubular reactor 4 through the third feed inlet 42；And it is anti-to control the tubular type
Answering 4 interior reaction temperature of device is 190 DEG C.
Step S4: reaction mass is between the tubular reactor 4 and the product storage tank 6 in periodical self-oscillation stream
Dynamic, product drains into the product storage tank 6 after reaction；
The principle that material is periodically flowed in self-oscillation in the tubular reactor 4 is referring to embodiment 1.
The method for preparing imido oxalic acid by continuous hydrolysis described in embodiment 1-3 respectively, in the self-oscillation reactor
Continuous operation 1 month in 100 carries out yield statistics, and yield statistical result is as follows:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Yield (%) | 95.4 | 96.7 | 95.9 |
It can be seen that by above-mentioned data and continuous hydrolysis preparation carried out using self-oscillation reactor 100 provided by the invention
The method of imido oxalic acid, reaction yield are greater than 95%.
Compared with prior art, the method that continuous hydrolysis provided by the invention prepares imido oxalic acid, have has as follows
Beneficial effect:
One, the method that continuous hydrolysis provided by the invention prepares imido oxalic acid, using imido grpup diacetonitrile and water as
Reaction raw materials answer in the self-oscillation and reaction are hydrolyzed in device, and the self-oscillation reactor is anti-by mixed reaction kettle and tubular type entirely
Device is answered to combine, material, in periodical self-oscillation flowing, enhances the mass transfer of the tubular reactor in the tubular reactor
With biography heat transfer effect, equally there is preferable reaction and temperature control effect under lower flow velocity, improve the yield of material reaction.
The reaction yield of the method for continuous hydrolysis imido oxalic acid provided by the invention is 95% or more.
Two, the method that continuous hydrolysis provided by the invention prepares imido oxalic acid, in the self-oscillation reactor into
Row, the self-oscillation reactor are flow reactor, by control reaction temperature and reaction pressure, improve reaction rate, into
And water consumption needed for the reaction can be reduced, reduce energy consumption.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification and accompanying drawing content is applied directly or indirectly in other relevant skills
Art field, is included within the scope of the present invention.
Claims (8)
1. a kind of method that continuous hydrolysis prepares imido oxalic acid, which comprises the steps of:
Step S1: reaction mass imido grpup diacetonitrile and water are mixed in proportion；
Step S2: perfectly mixed reactor is provided, reaction mass is delivered in the perfectly mixed reactor, reaction is hydrolyzed；
Step S3: providing tubular reactor, and the reaction solution in the perfectly mixed reactor is delivered to institute under the effect of liquid level differential pressure
It states in tubular reactor；
Step S4: product storage tank is provided, reaction mass is between the tubular reactor and the product storage tank in periodically certainly
Oscillation Flows, product drains into the product storage tank after reaction；
Wherein the discharge port position of the complete mixed reaction kettle is higher than the tubular reactor topmost, and reaction mass is described
Circulation path between tubular reactor and the product storage tank is inverted u-shaped, the discharge port position of the tubular reactor
Feed inlet position higher than the tubular reactor and the highest liquid level lower than the tubular reactor.
2. the method that continuous hydrolysis according to claim 1 prepares imido oxalic acid, which is characterized in that the tubular type is anti-
Answering the difference in height between the discharge port of device and the feed inlet of the tubular reactor is the tubular reactor highest level value
1/3-1/2。
3. the method that continuous hydrolysis according to claim 1 prepares imido oxalic acid, which is characterized in that in step S1,
Reaction mass is mixed and is delivered to using feed system and is mixed in reaction kettle entirely, the feed system includes metering spiral shell
Rotation, the solid-liquid mixer that connect with the output end of the metering screw and for mixed material to be delivered to described mix entirely instead
Answer the delivery pump of device.
4. the method that continuous hydrolysis according to claim 1 prepares imido oxalic acid, which is characterized in that in step S2,
Further include the steps that preheating reaction mass, the reaction mass after preheating is delivered in the entirely mixed reaction kettle and carries out instead
It answers.
5. the method that continuous hydrolysis according to any one of claim 1 to 4 prepares imido oxalic acid, feature exist
In the mixing molar ratio 1:5-20 of imido grpup diacetonitrile and water in reaction raw materials.
6. the method that continuous hydrolysis described in any one of -4 prepares imido oxalic acid according to claim 1, which is characterized in that
The entirely mixed material in reactor reaction temperature is 190-200 DEG C, reaction pressure 9-11MPa.
7. the method that continuous hydrolysis described in any one of -4 prepares imido oxalic acid according to claim 1, which is characterized in that
Material reaction temperature is 190-220 DEG C in the tubular reactor.
8. a kind of self-oscillation reactor, which is characterized in that including the complete mixed reaction kettle, tubular type set gradually by Flow of Goods and Materials direction
Reactor, communicating pipe and product storage tank, the communicating pipe both ends, which are separately connected the tubular reactor and the product storage tank, to be made
Circulation path of the material between the tubular reactor and the product storage tank is inverted u-shaped, the discharging of the complete mixed reaction kettle
Mouth position is higher than the tubular reactor topmost, sets the terminal of the communicating pipe as the discharging of the tubular reactor
Mouthful, the discharge port position of the tubular reactor is higher than the feed inlet position of the tubular reactor and lower than described
The highest liquid level of tubular reactor, and between the discharge port of the tubular reactor and the feed inlet of the tubular reactor
Difference in height is the 1/3-1/2 of the tubular reactor highest level value.
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| CN101676292A (en) * | 2008-09-15 | 2010-03-24 | 李坚 | Method for preparing N-(phosphonomethyl) iminodiacetic acid and glyphosate by using non-alkali metal |
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