CN106750072B - A kind of continuous production device and method of amino resins - Google Patents
A kind of continuous production device and method of amino resins Download PDFInfo
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- CN106750072B CN106750072B CN201710032768.0A CN201710032768A CN106750072B CN 106750072 B CN106750072 B CN 106750072B CN 201710032768 A CN201710032768 A CN 201710032768A CN 106750072 B CN106750072 B CN 106750072B
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Abstract
The present invention relates to a kind of continuous production device of amino resins and methods, it is continuous operation of the reaction mass under automatic temperature-controlled in described device that wherein described device, which includes the automatic continuous measurer of raw material being sequentially communicated, primary screw reactor and twin-screw cylinder bloom combined reactor, the method,.Raw material is added in the automatic continuous measurer front end of raw material, naval stores is continuously escaped from twin-screw cylinder bloom combined reactor end, it is the update of batch reactor production resin methods, meet the quality stability requirement that subsequent workshop section uses resin semi-finished product, prevent the discharge of chemical component in conventional apparatus macromolecular synthetic reaction, avoid the various deficiencies such as the resin viscosity difference that traditional reaction kettle intermittent mode produces is big, quality stability is poor, and molecular weight distribution is wide.
Description
Technical field
The present invention relates to amino resins production technical field, the continuous production device of especially a kind of amino resins and
Method.
Background technique
Amino resins is the general name as the compound containing amino and formaldehyde through resin made of polycondensation, important amino tree
Rouge has Lauxite, melamine resin and aniline-formaldehyde resin etc..The production of this resinoid continue to use always it is traditional between
Reaction kettle have a rest to complete, Batch Process makes the passage of the quality of every a collection of resin at any time changes, and molecular weight distribution is wide etc.
Various deficiencies, for melamine resin, the change of quality is constrained further is given birth to by melamine resin
At the quality stability of melamine foam；And batch reactor reaction condition is not easy to control, and waste water and gas is more, by
This proposes the requirement of serialization to the production of melamine resin.
Summary of the invention
The shortcomings that producing amino resins the present invention be directed to existing intermittent reaction method, provides a kind of the continuous of amino resins
Metaplasia produces device and method.
The continuous production device of a kind of amino resins of the invention, it is characterised in that the raw material including being sequentially communicated is automatic
Continuous batching device, primary screw reactor and twin-screw cylinder bloom combined reactor, the automatic continuous measurer packet of raw material
Include the automatic continuous measurer of solid material and the automatic continuous measurer of liquid charging stock, the automatic continuous measurer of solid material and
The automatic continuous measurer of liquid charging stock is connected to primary screw reactor respectively, and the primary screw reactor includes that the first heat is handed over
The primary screw rod for changing cavity and being enclosed in the first heat exchange cavity, the primary screw design is alternately arranged several conveyings
Section and several mixing sections, the conveying section setting have the conveyor screw slot of conveying effect, and the mixing section setting has mixed
The mixing auger slot of cooperation, several conveying sections and several mixing section phase of the first heat exchange cavity corresponding to primary screw rod
It is designed as several segments with answering, each section is provided with heat exchanger and carries out temperature control, the twin-screw cylinder bloom combined reactor packet
It includes the second heat exchange cavity and two cylindrical shafts being enclosed in the second heat exchange cavity, be mounted on two parallel cylindrical shafts
Cylinder bloom, several pieces of the cylinder bloom to be close to before and after cylinder bloom each in one group, each group, different hearts are mounted on
On cylindrical shaft, each group of cylinder bloom is alternately installed, so that driving on two cylindrical shafts when two cylindrical shaft rotating Vortexes
Opposite cylinder bloom group staggeredly rotates, and the second heat exchange cavity is designed as several segments, and each section is provided with heat exchanger
Carry out temperature control.
Preferably, the automatic continuous measurer of the solid material includes feed bin, the first helicoidal pump and the second helicoidal pump, weightlessness
Electronic scale, weighing sensor, PLC, frequency converter, the feed bin above, are connected the first helicoidal pump, then through material under material channel
Channel is connected with the weightless electronic scale of weighing sensor, then connects the second spiral shell helicoidal pump, the weighing and sensing through material channel
Device, frequency converter are connected with PLC；
The automatic continuous measurer of liquid charging stock include charging basket, flowmeter, plunger pump, weightless electronic scale, weighing sensor,
PLC, frequency converter, diaphragm pump, the charging basket above, connect through connecting flowmeter and plunger pump under material channel, then through material channel
Be equipped with the weightless electronic scale of weighing sensor, then connect diaphragm pump through material channel, the weighing sensor, frequency converter with
PLC is connected.
Preferably, the first heat exchange cavity is the first automatic control heat exchange cavity, and described first automatically controls heat
Exchange cavity corresponds to several conveying sections of primary screw rod and several mixing sections are correspondingly designed as several segments, and each section is provided with
The heat exchanger of one automatic control carries out temperature control, and the second heat exchange cavity is the second automatic control heat exchange cavity, institute
It states the second automatic control heat exchange cavity and is designed as several segments, each section of heat exchanger for being provided with an automatic control carries out temperature
Control.
Preferably, the automatic continuous measurer of raw material being sequentially communicated, primary screw reactor and twin-screw cylindrical steel
It is closed connection between block combined reactor, fills it up with inhibitor solution in the second heat exchange cavity.
Preferably, four pieces of the cylinder bloom are one group, and the cylinder bloom is nitriding bloom.
A kind of a kind of continuous production method of amino resins of continuous production device based on amino resins, feature
It is that the production method is realized as follows:
Step 1, the automatic continuous ingredient of solid material, solid material pass through the automatic continuous measurer ingredient of the solid material
And process units is added；
Step 2, the automatic continuous ingredient of liquid charging stock, liquid charging stock pass through the automatic continuous measurer ingredient of the liquid charging stock
And process units is added；
Step 3, the solid material and liquid charging stock of process units is added in primary spiro rod reaction, into the primary screw rod
Reactor adjusts reaction condition by control, automatically controls each section of heat exchange cavity of temperature, turn of primary screw rod including first
Speed and reaction time, make the primary transparent material of spiro rod reaction products therefrom；
Step 4, twin-screw cylinder bloom composite reaction enters twin-screw circle through the transparent material that primary spiro rod reaction flows out
Column bloom combined reactor, by control adjust reaction condition, including second automatically control each section of heat exchange cavity temperature, two
The revolving speed of root cylindrical shaft rotating Vortex and reaction time make twin-screw cylinder bloom composite reaction obtain product and meet subsequent workshop section
Use；
Step 1 and step 2 can carry out simultaneously.
Preferably, the step 1 specifically: the feed bin is added in solid material, passes through material channel through the first helicoidal pump
It is delivered to weightless electronic scale, the weighing sensor conduct data is compared calculating and reset frequency converter frequency to PLC, adjustment
The revolving speed of first helicoidal pump and the second helicoidal pump, the solid material are conveyed downwards by the second helicoidal pump through material channel；
The step 2 specifically: the charging basket is added in liquid charging stock, is conveyed through flowmeter and plunger pump by material channel
To weightless electronic scale, when liquid charging stock reaches the quality of setting, the weighing sensor conduct data in the weightlessness electronic scale is given
PLC is compared calculating and resets frequency converter frequency, adjusts the revolving speed of plunger pump and diaphragm pump, and the liquid charging stock passes through diaphragm
Pump is conveyed through material channel to primary screw reactor.
Preferably, in the step 3, control adjustment reaction temperature automatically controls each section of heat exchange cavity by control first
Temperature realize that in the step 4, control adjustment reaction temperature automatically controls each section of heat exchange cavity by control second
Temperature is realized.
Preferably, in the step 4, transparent material enters before twin-screw cylinder bloom combined reactor, and described second
It automatically controls in heat exchange cavity and is pre-filled with inhibitor solution.
The continuous production device and method of a kind of amino resins of the invention, continuous production device include successively closed
The automatic continuous measurer of the raw material of connection, primary screw reactor and twin-screw cylinder bloom combined reactor, by solid material
Primary screw reactor is added to by the automatic continuous measurer of raw material with liquid charging stock, ensure that in the unit time to primary spiral shell
The raw material quantity of input set amount in bar reactor；
The primary screw design being enclosed in the first heat exchange cavity in primary screw reactor is alternately arranged several
Conveying section and several mixing sections, several conveying sections that the first heat exchange cavity corresponds to primary screw rod and several mixing sections are correspondingly
Several segments are designed as, each section is provided with heat exchanger and carries out temperature control, can control temperature, primary screw speed and mixing in this way
And the reaction time (the primary screw rod transmission helicla flute that conveying section can design different lead according to specific requirement) makes solid, liquid
Each component is sufficiently mixed, and then mixed material enters high temperature section, and side reaction is mixed when promoting, makes reaction mixture in primary spiral shell
First stage polymerization reaction is completed before bar reactor outlet, generates transparent short chain amino resins；
Two cylindrical shafts being enclosed in the second heat exchange cavity in twin-screw cylinder bloom combined reactor are mounted on two
Cylinder bloom on the parallel cylindrical shaft of root, several pieces of cylinder bloom are to be close to not before and after each cylinder bloom in one group, each group
It is concentrically attached on cylindrical shaft, each group of cylinder bloom is alternately installed, so that driving two when two cylindrical shaft rotating Vortexes
Opposite cylinder bloom group staggeredly rotates on cylindrical shaft, and the second heat exchange cavity is designed as several segments, and each section is provided with hot friendship
It changes planes and carries out temperature control, and fill it up with inhibitor solution in the second heat exchange cavity, can be held in this way by the second heat exchange of control
Temperature, cylindrical shaft revolving speed, inhibitor concentration and the reaction time of chamber difference section, so that reaching the combination of twin-screw cylinder bloom in advance
Material in reactor must be promoted through speed side appropriate border ring, and effect equivalent not reflux, subsequent material follow closely, effect etc.
With not crossing the border forward, guarantee that the material being introduced into first is discharged after sufficiently reacting in this way, the material entered afterwards is after sufficiently reacting
After be discharged, all liq material effect is equal to not unordered crossfire, guarantees material in twin-screw cylinder bloom combined reactor
The extent of reaction is identical, so that reaction product is consistent and degree is abundant, it is to enter the combination of twin-screw cylinder bloom at first instead
The material (resin) of device is answered to be distributed in inhibitor solution, inhibitor concentration is relatively high, and polymerization reaction is inhibited, with material
The entrance of (resin), inhibitor concentration reduce, and polymerization rate increases, material (resin) after inhibitor solution is completely exhausted out
Polymerization reaction, which has reached, to be balanced and is adjusted to reaction end, and hereafter reaction speed balances, and product can be supplied continuously
Next workshop section uses；
The automatic continuous measurer of the raw material being sequentially communicated, primary screw reactor and twin-screw cylinder bloom combined reactor
Between be closed connection, optimize environment protection emission index, basically reach industrial chemicals and semi-finished product zero-emission, improve quality
Stability.
Detailed description of the invention
Fig. 1 is a kind of continuous production device structural schematic diagram of amino resins of the invention；
Fig. 2 is raw material (solid material and liquid charging stock) of the invention automatically continuously measurer structural schematic diagram；
Fig. 3 is the primary screw-rod structure schematic diagram of primary screw reactor of the invention；
Fig. 4 is two cylindrical shafts of twin-screw cylinder bloom combined reactor of the invention, is mounted on two parallel circles
The structural schematic diagram of cylinder bloom on axis of a cylinder；
Fig. 5 is a kind of continuous production method flow diagram of amino resins of the invention.
Wherein, the automatic continuous measurer of 1- raw material, 11- feed bin (or charging basket), the first helicoidal pump of 12- (or plunger pump), 13-
Second helicoidal pump (or diaphragm pump), 14- weightlessness electronic scale, 15- weighing sensor, 16-PLC, 17- frequency converter, 18- flowmeter,
2- primary screw reactor, 21- primary screw rod, 211- conveyor screw slot (211a- large pitch conveyor screw slot, the small lead of 211b-
Conveyor screw slot), 212- mixing auger slot, 22- the first heat exchange cavity, 3- twin-screw cylinder bloom combined reactor, 31- circle
Axis of a cylinder, 32- cylinder bloom, 33- the second heat exchange cavity, 4- material channel, 5- inhibitor solution, 6- observe visor, arrow in figure
The direction of head is the direction that raw material or product flow.
M is motor mark in Fig. 1, and EX-101 is the label number of primary screw reactor, and EX-102 is twin-screw cylindrical steel
The label number of block combined reactor.
Specific embodiment
The invention will be further described with reference to embodiments:
Embodiment 1: as shown in figures 1-4, a kind of continuous production device of amino resins, including the raw material being sequentially communicated
Automatic continuous measurer 1, primary screw reactor 2 and twin-screw cylinder bloom combined reactor 3, the automatic continuous measurer of raw material
1 includes the automatic continuous measurer of solid material and the automatic continuous measurer of liquid charging stock, is accordingly set according to the type of solid material
It is equipped with the automatic continuous measurer of multiple solid materials, the present embodiment has 3 kinds of melamine, paraformaldehyde, sodium carbonate solid materials,
It is correspondingly provided with the automatic continuous measurer of multiple liquid charging stocks according to the type of liquid charging stock, the present embodiment has desalted water, second two
2 kinds of liquid charging stocks of alcohol；The automatic continuous measurer of solid material includes feed bin 11, the first helicoidal pump 12 and the second helicoidal pump 13, loses
Weight electronic balancer 14, weighing sensor 15, PLC16, frequency converter 17, feed bin 11 above, through connecting the first helicoidal pump under material channel 4
12, then it is connected with through material channel 4 the weightless electronic scale 14 of weighing sensor 15, then connect the second spiral through material channel 4
Pump 13, weighing sensor 15, frequency converter 17 are connected with PLC16；The automatic continuous measurer of liquid charging stock includes charging basket 11, flow
Meter 18, plunger pump 12, weightless electronic scale 14, weighing sensor 15, PLC16, frequency converter 17, diaphragm pump 13, charging basket 11 above,
Connected flowmeter 18 and plunger pump 12 under material channel 4, then is connected with the weightless electronics of weighing sensor 15 through material channel 4
Scale 14, then diaphragm pump 13 is connected through material channel 4, weighing sensor 15, frequency converter 17 are connected with PLC16；
The automatic continuous measurer of 3 solid materials and 2 automatic continuous measurers of liquid charging stock respectively with primary spiral shell
Bar reactor 2 is connected to, and primary screw reactor 2 includes the first heat exchange cavity 22 and is enclosed in the first heat exchange cavity 22
Primary screw rod 21, primary screw rod 21 are designed as alternately arranged several conveying sections and several mixing sections, and conveying section setting has defeated
The conveyor screw slot 211 for sending effect designs large pitch conveyor screw slot 211a, needs small lead defeated when large pitch being needed to convey
Small lead conveyor screw slot 211b is designed when sending, and to control time of delivery, small lead conveyor screw is designed as in the present embodiment
Slot 211b, mixing section setting have the mixing auger slot 212 of immixture, and with the mixed effect reached, the first heat exchange is held
Chamber 22 corresponds to several conveying sections of primary screw rod 21 and several mixing sections are correspondingly designed as several segments, and each section is provided with heat
Interchanger carries out temperature control, to guarantee to efficiently control reaction temperature, the primary collection conveying of screw reactor 2 (propulsion), mixing spiral shell
Spin slot is staggered on Yu Yigen screw rod, and temperature section controls, and reaches good reaction effect, guarantees first stage of reaction
Generation short chain amino resins uniform quality；
Twin-screw cylinder bloom combined reactor 3 includes the second heat exchange cavity 33 and is enclosed within the second heat exchange cavity 33
Interior two cylindrical shafts 31, the cylinder bloom 32 being mounted on two parallel cylindrical shafts 31,32 several pieces of cylinder bloom are one
Group is mounted on cylindrical shaft 31 for three pieces in the present embodiment to be close to different hearts before and after each cylinder bloom 32 in one group, each group,
Each group of cylinder bloom 32 is alternately installed, so that driving circle opposite on two cylindrical shafts 31 when two 31 rotating Vortexes of cylindrical shaft
32 groups of column bloom staggeredly rotate, and the second heat exchange cavity 33 is designed as several segments, and each section is provided with heat exchanger and carries out temperature control,
To guarantee to efficiently control reaction temperature, it is short that twin-screw cylinder bloom combined reactor 3 generates first stage of reaction
Residence time is long wherein for chain amino resins, and slow to promote, capacity is big, gathered that plastics machinery is continuous and batch reactor it is big
Capacity feature can be promoted continuously in large volumes.
Embodiment 2: as shown in figures 1-4, a kind of continuous production device of amino resins,
Compared with Example 1 the difference is that:
There are 4 automatic continuous ingredients of solid material for being equipped with melamine, paraformaldehyde, sodium formate, phthalic anhydride
Device and 2 automatic continuous measurers of liquid charging stock for being equipped with desalted water, phosphoric acid；
Conveyor screw slot 211 is designed as large pitch conveyor screw slot 211a in the present embodiment；
First heat exchange cavity 22 is the first automatic control heat exchange cavity, and the first automatic control heat exchange cavity corresponds to
Several conveying sections of primary screw rod 21 and several mixing sections are correspondingly designed as several segments, and each section is provided with an automatic control
Heat exchanger carry out temperature control, with guarantee reaction temperature is accurately automatically controlled；
Second heat exchange cavity 33 is the second automatic control heat exchange cavity, and the second automatic control heat exchange cavity is designed as
Several segments, each section of heat exchanger for being provided with an automatic control carries out temperature control, to guarantee to reaction temperature accurately automatically
Control；
Remaining is the same as embodiment 1.
Embodiment 3: as shown in figures 1-4, a kind of continuous production device of amino resins,
Compared with Example 2 the difference is that:
Have and is equipped with melamine, paraformaldehyde, the automatic continuous measurer of 3 solid materials of sodium carbonate and outfit desalination
Water, sulfuric acid, hypophosphorous acid 3 automatic continuous measurers of liquid charging stock；
Conveyor screw slot 211 is designed as large pitch conveyor screw slot 211a, maximum lead in the present embodiment in the present embodiment
It is 50mm (flow and revolving speed also have relationship, and current revolving speed is 110 revs/min, and the value of flow is the resin of 3 kg/minutes)；
In the present embodiment, the automatic continuous measurer 1 of raw material, primary screw reactor 2 and the double spiral shells that are successively connected to pipeline
It is closed connection between bar cylinder bloom combined reactor 3, reaction carries out inside closed continuous production device, does not have
Any chemical component outlet, optimizes environment protection emission index, basically reaches zero-emission, this is that have relative to batch reactor outward
For discharge waste；Be pre-filled with inhibitor solution 5 in second heat exchange cavity 33, inhibitor solution 5 can for 1,4-benzoquinone,
The mixture of stannous chloride, weight percent each 0.1%, or with the mixture of m-dinitrobenzene and iron chloride, weight percent
Than each 0.1%；It is pre-filled with inertia inhibitor solution 5,5 ratio of inhibitor solution enters the combination of twin-screw cylinder bloom when big anti-
Answer product (abbreviation material) concentration of first stage of reaction of device 3 with regard to small, reaction speed is with regard to slow, with inhibitor solution 5
Outlet, material concentration is gradually increased, and reaction speed also rises；When inhibitor solution 5 empties completely, material passes in and out and reaction
Reach balance and gradually continuous-stable outlet, reaches continuous production purpose, practical is exactly that the concentration variation of inhibitor solution 5 makes elder generation
The material reaction speed that phase enters slows down, and the material reaction speed that the later period enters is relatively fast, can reach end reaction balance.In advance
It is first full of inertia inhibitor solution 5, attainable actual effect is: reaching twin-screw cylinder bloom combined reactor 3 in advance
Material must through speed side appropriate border ring promote be unable to reflux, subsequent material is followed closely but cannot be crossed the border forward, in this way guarantor
Advanced material is demonstrate,proved first to be discharged after sufficiently reacting, laggard material after sufficiently reacting after be discharged, all liq material is not
Unordered crossfire is obtained, guarantees that residence time of the material in twin-screw cylinder bloom combined reactor 3 is fixed, thus the extent of reaction one
It causes and abundant；
Observation visor 6 is set in primary 2 end of screw reactor, makes to complete the first stage in primary screw reactor 2
The short chain amino resins that polymerization reaction generates enters the reaction mixture before twin-screw cylinder bloom combined reactor 3, can be with
See whether its extent of reaction is appropriate through observation visor 6, it is then qualified that usual material is transparent, through high temperature dwell after adjustment is appropriate
Temperature is transported in twin-screw cylinder bloom combined reactor 3 by pipeline connection and carries out polymerization reaction；
Remaining content is the same as embodiment 2.
Embodiment 4: as shown in figure 5, corresponding to a kind of serialization of amino resins of the continuous production device of embodiment 2
Production method is realized as follows:
Step 1, the automatic continuous ingredient of solid material, solid material are matched by the automatic continuous measurer 1 of the solid material
Expect and be added process units, that is, enters primary screw reactor 2, specifically: the feed bin 11 is added in solid material, through the first spiral shell
Rotation pump 12 is delivered to weightless electronic scale 14 by material channel 4, and 15 conduct data of weighing sensor is to PLC16, through comparing
The frequency for resetting frequency converter 17 is calculated, the revolving speed of the first helicoidal pump 12 and the second helicoidal pump 13 is adjusted, the solid material is logical
It crosses the second helicoidal pump 13 and is conveyed through material channel 4 to primary screw reactor 2, such input and output material reaches balance forever, ensure that
To the solid material quantity of primary screw reactor 2 input set amount in unit time；
Step 2, the automatic continuous ingredient of liquid charging stock, liquid charging stock pass through the automatic continuous measurer ingredient of the liquid charging stock
And process units is added, that is, enter primary screw reactor 2, specifically: the charging basket 11 is added in liquid charging stock, through flowmeter 18
Weightless electronic scale 14 is delivered to by material channel 4 with plunger pump 12, when liquid charging stock reaches the quality of setting, the weightless electricity
Son claims 15 conduct data of weighing sensor in 14 to PLC16, calculates the frequency for resetting frequency converter 17 through comparing, adjusts plunger
The revolving speed of pump 12 and diaphragm pump 13, liquid charging stock carry out unit to primary screw reactor 2 through material channel 4 by diaphragm pump 13
The conveying of the fixed amount liquid charging stock of time, balances input and output material, guarantees the accurate stable of metering；
Step 3, the solid material and liquid charging stock of process units is added in primary spiro rod reaction, into the primary screw rod
Reactor 2 adjusts reaction condition by control, temperature, the primary screw rod 21 for automatically controlling each section of heat exchange cavity including first
Revolving speed and reaction time, each section of heat exchanger for being provided with an automatic control carry out temperature control, keep the polymerization of primary screw rod anti-
Answering the short chain amino resins of gained is transparent material；The heat exchanger of provisioned automatic control is led in addition to being provided with circulation conveying
Outside the oil pump of hot nurse, it is important to be additionally provided with the temperature accuracy to heat-conducting oil heating and cooling heat exchanger, controlled through PLC16
Height, control is flexibly convenient, so that technology controlling and process has guarantee；
Step 4, twin-screw cylinder bloom composite reaction enters twin-screw circle through the transparent material that primary spiro rod reaction flows out
Column bloom combined reactor 3, by control adjust reaction condition, including second automatically control each section of heat exchange cavity temperature,
The revolving speed of two 31 rotating Vortexes of cylindrical shaft and reaction time, each section of heat exchanger for being provided with an automatic control carry out temperature
Control makes twin-screw cylinder bloom composite reaction obtain product after 3 end of twin-screw cylinder bloom combined reactor evolution satisfaction
The use of continuous workshop section；
The sequence of step 1 and step 2 can exchange, and can also carry out simultaneously, two steps carry out simultaneously in the present embodiment.
Specific steps content is as follows in chronological order:
Starting the automatic continuous measurer 1~4 of solid material, (it is No. 1 that first measurer, which is compiled, and second measurer volume is
No. 2, it is No. 3 that third measurer, which is compiled, and it is No. 4 that the 4th measurer, which is compiled), the automatic continuous measurer of liquid charging stock 1~2 (the
It is No. 1 that one measurer, which is compiled, and it is No. 2 that second measurer, which is compiled), the weight of unit time charging for calculation in the molar ratio, simultaneously
Material is added to primary screw reactor 2, and 21 motor of primary screw rod for starting primary screw reactor is carried out to material is added
Conveying and mixing start the first stage polymerization reaction of resin.
Heat exchanger the 1st~the 6th of starting automatic control, it is 50 DEG C that the 1st~2 temperature, which is arranged, is the 1st~20 defeated
Square auger slot 211 preheats, and the heat exchanger temperature that the 3rd~6 automatic control is arranged is 80 DEG C, for primary screw reactor 2
Remaining conveyor screw slot 211 and mixing auger slot 212 preheat, and the heat exchanger temperature that the 7th~15 automatic control is arranged is 90
DEG C, it is preheated for twin-screw cylinder bloom combined reactor 3.To oil temperature and conveyor screw slot 211, mixing auger slot 212 and double spiral shells
3 displays temperature of bar cylinder bloom combined reactor starts the work of next step after stablizing.
After about 25 minutes, transparency stream mistake can be observed in primary 21 end of screw rod observation visor 6, illustrates that primary screw rod is anti-
It answers device 2 to convey mixing velocity and set reacting dose to coincide, continues to observe subsequent process.
Transparent material keeps about 85 DEG C of twin-screw cylinder bloom combined reactors 3 for entering horizontal placement, because polymerization is anti-
Initial stage is answered to absorb heat, mid-term heat release, later period autoreactivity is able to maintain thermal balance substantially, so the heating of the heat exchanger automatically controlled
End and colling end must meet the temperature condition of system requirements, automatically adjusted by system to be heated or cooled, it is anti-to meet polymerization
The needs answered.
3 end of twin-screw cylinder bloom combined reactor starts the naval stores of evolution heat after about 30 minutes, takes appropriate sample
Product are cooled to 25 DEG C of detection viscosity, density, tolerance etc., and the product to conform to quality requirements can be used for subsequent workshop section, if
Testing index needs to adjust, then can the heat exchanger control temperature that automatically controls of appropriate adjustment, two 31 revolving speeds of cylindrical shaft adjust
The whole extent of reaction.
Embodiment 5: as shown in figure 5, corresponding to a kind of serialization of amino resins of the continuous production device of embodiment 3
Production method is realized as follows:
Step 1, content is the same as embodiment 4；
Step 2, content is the same as embodiment 4；
Step 3, the solid material and liquid charging stock of process units is added in primary spiro rod reaction, into the primary screw rod
Reactor 2 adjusts reaction condition by control, temperature, the primary screw rod 21 for automatically controlling each section of heat exchange cavity including first
Revolving speed and reaction time, each section of heat exchanger for being provided with an automatic control carry out temperature control, table 1 is listed into primary
Three groups of matching numerical value of the inventory of screw reactor and revolving speed, temperature；
Table 1
| First group | Second group | Third group | |
| Solid, liquid material total amount | 2.5 kg/minute | 3 kg/minutes | 4 kg/minutes |
| Revolving speed | 80-100 revs/min | 100-120 revs/min | 120-130 revs/min |
| Temperature | 80-85℃ | 103-105℃ | 99-101℃ |
Short chain amino resins obtained by primary screw rod polymerization reaction is transparent material；The heat exchange of provisioned automatic control
Machine, other than being provided with the oil pump of circulation conveying Dowtherm, it is important to be additionally provided with to heat-conducting oil heating and cooling heat exchange
Device, the temperature accuracy through PLC16 control is high, and control is flexibly convenient, so that technology controlling and process has guarantee；
Step 4, twin-screw cylinder bloom composite reaction, the short chain amino resins (transparency flowed out through primary spiro rod reaction
Material) enter twin-screw cylinder bloom combined reactor 3, before this, filled in advance in the second automatic control heat exchange cavity
Full inhibitor solution 5, inhibitor solution 5 are the mixture of 1,4-benzoquinone, stannous chloride, and weight percent each 0.1% passes through control
Reaction condition is adjusted, automatically controls each section of heat exchange cavity of temperature, the revolving speed of two 31 rotating Vortexes of cylindrical shaft including second
And reaction time, each section of heat exchanger for being provided with an automatic control carry out temperature control, revolving speed is certain, and residence time of material is
Reaction time, the variation of the extent of reaction and the concentration of the transparent material flowed out through primary spiro rod reaction was adapted, with regard to certain to reach
To the pre-filled purpose of inertia inhibitor solution 5, table 2 lists the transparent inventory flowed out through primary spiro rod reaction and turns
Three groups of matching numerical value of speed, temperature obtain product through twin-screw cylinder bloom composite reaction and combine instead from twin-screw cylinder bloom
The evolution of 3 end of device is answered to meet the use of subsequent workshop section；
Table 2
The sequence of step 1 and step 2 can exchange, and can also carry out simultaneously, two steps carry out simultaneously in the present embodiment.
Specific steps content is as follows in chronological order:
Starting the automatic continuous measurer 1~3 of solid material, (it is No. 1 that first measurer, which is compiled, and second measurer volume is
No. 2, it is No. 3 that third measurer, which is compiled), and the automatic continuous measurer of liquid charging stock 1~3 (it is No. 1 that first measurer, which is compiled, second
It is No. 2 that a measurer, which is compiled, and it is No. 3 that third measurer, which is compiled) number, the weight of unit time charging for calculation in the molar ratio, simultaneously
Material is added to primary screw reactor 2, and 21 motor of primary screw rod for starting primary screw reactor is carried out to material is added
Conveying and mixing start the first stage polymerization reaction of resin.
Heat exchanger the 1st~the 6th of starting automatic control, it is 50 DEG C that the 1st~2 temperature, which is arranged, is the 1st~20 defeated
Square auger slot 211 preheats, and the heat exchanger temperature that the 3rd~6 automatic control is arranged is 80 DEG C, for primary screw reactor 2
Remaining conveyor screw slot 211 and mixing auger slot 212 preheat, and the heat exchanger temperature that the 7th~15 automatic control is arranged is 100
DEG C, it is preheated for twin-screw cylinder bloom combined reactor 3.To oil temperature and conveyor screw slot 211, mixing auger slot 212 and double spiral shells
3 displays temperature of bar cylinder bloom combined reactor starts the work of next step after stablizing.
After about 25 minutes, transparency stream mistake can be observed in primary 21 end of screw rod observation visor 6, illustrates that primary screw rod is anti-
It answers device 2 to convey mixing velocity and set reacting dose to coincide, continues to observe subsequent process.
Transparent material keeps about 85 DEG C of twin-screw cylinder bloom combined reactors 3 for entering horizontal placement, because polymerization is anti-
Initial stage is answered to absorb heat, mid-term heat release, later period autoreactivity is able to maintain thermal balance substantially, so the heating of the heat exchanger automatically controlled
End and colling end must meet the temperature condition of system requirements, automatically adjusted by system to be heated or cooled, it is anti-to meet polymerization
The needs answered.
3 end of twin-screw cylinder bloom combined reactor starts the naval stores of evolution heat after about 30 minutes, takes appropriate sample
Product are cooled to 25 DEG C of detection viscosity, density, tolerance etc., and the product to conform to quality requirements can be used for subsequent workshop section, if
Testing index needs to adjust, then can the heat exchanger control temperature that automatically controls of appropriate adjustment, two 31 revolving speeds of cylindrical shaft adjust
The whole extent of reaction.
Continuous production device self-cleaning effect is good, and continuous production does not need to clean, and Programmed Stop must stop feeding in advance,
Primary screw reactor 2 and the sufficiently conveying emptying of twin-screw cylinder bloom combined reactor 3, then feed and discharge port aluminium foil
Sealing keeps equipment inner wall not oxidation corrosion and drying；
The finished product amino resins index produced by the method for the present embodiment is: viscosity 7000mpas, and density 1.34 is public
Jin/liter, tolerance 7 is suitble to rear end process to use；It is by the resulting finished product amino resins index of former batch reactor: viscosity
6000-7500mpas, 1.3-1.35 kilograms/liter of density, tolerance 5-9, viscosity 7000-12000mpas after 7 hours, quality is not
Surely, back segment process is not available, and will cause frequent blindness adjusting process.
Claims (6)
1. a kind of continuous production device of amino resins, it is characterised in that the automatic continuous ingredient of raw material including being sequentially communicated
Device, primary screw reactor and twin-screw cylinder bloom combined reactor, the automatic continuous measurer of raw material include solid original
Expect automatic continuous measurer and the automatic continuous measurer of liquid charging stock, the automatic continuous measurer of the solid material and liquid charging stock
Automatic continuous measurer be connected to primary screw reactor respectively, the primary screw reactor include the first heat exchange cavity with
The primary screw rod being enclosed in the first heat exchange cavity, the primary screw design is alternately arranged several conveying sections and several
Mixing section, the conveying section setting have the conveyor screw slot of conveying effect, and the mixing section setting has immixture
Mixing auger slot, the first heat exchange cavity corresponds to several conveying sections of primary screw rod and several mixing sections correspondingly design
For several segments, each section is provided with heat exchanger and carries out temperature control, and the twin-screw cylinder bloom combined reactor includes the second heat
Exchange cavity and two cylindrical shafts being enclosed in the second heat exchange cavity, the cylindrical steel being mounted on two parallel cylindrical shafts
Block, several pieces of the cylinder bloom are to be close to before and after each cylinder bloom in one group, each group, and different hearts are mounted on cylindrical shaft
On, each group of cylinder bloom is alternately installed, so that driving when two cylindrical shaft rotating Vortexes opposite on two cylindrical shafts
Cylinder bloom group staggeredly rotates, and the second heat exchange cavity is designed as several segments, and each section is provided with heat exchanger and carries out temperature
Control；
The automatic continuous measurer of solid material includes feed bin, helicoidal pump, weightless electronic scale, weighing sensor, PLC, frequency conversion
Device, the feed bin above, is connected helicoidal pump under material channel, then the weightlessness electricity of weighing sensor is connected with through material channel
Sub- scale, then helicoidal pump is connected through material channel, the weighing sensor, frequency converter are connected with PLC；
The automatic continuous measurer of liquid charging stock includes charging basket, flowmeter, plunger pump, weightless electronic scale, weighing sensor, PLC, change
Frequency device, diaphragm pump, the charging basket above, are connected with through connecting flowmeter and plunger pump under material channel, then through material channel
The weightless electronic scale of weighing sensor, then connect diaphragm pump through material channel, the weighing sensor, frequency converter with PLC phase
Even；
The first heat exchange cavity is the first automatic control heat exchange cavity, and described first, which automatically controls heat exchange cavity, corresponds to
Several segments are correspondingly designed as in several conveying sections of primary screw rod and several mixing sections, each section is provided with an automatic control
Heat exchanger carry out temperature control, the second heat exchange cavity is second to automatically control heat exchange cavity, the described second automatic control
Heating exchange cavity is designed as several segments, and each section of heat exchanger for being provided with an automatic control carries out temperature control；
The automatic continuous measurer of raw material being sequentially communicated, primary screw reactor and twin-screw cylinder bloom combined reactor
Between be closed connection, fill it up with inhibitor solution in the second heat exchange cavity.
2. a kind of continuous production device of amino resins according to claim 1, it is characterised in that the cylinder bloom
Four pieces are one group, and the cylinder bloom is nitriding bloom.
3. based on a kind of company of a kind of amino resins of the continuous production device of amino resins as claimed in claim 1 or 2
Continuousization production method, it is characterised in that the production method is realized as follows:
Step 1, the automatic continuous ingredient of solid material, solid material pass through the automatic continuous measurer ingredient of the solid material and add
Enter process units；
Step 2, the automatic continuous ingredient of liquid charging stock, liquid charging stock pass through the automatic continuous measurer ingredient of the liquid charging stock and add
Enter process units；
Step 3, the solid material and liquid charging stock of process units is added in primary spiro rod reaction, into the primary spiro rod reaction
Device adjusts reaction condition by control, including first automatically control each section of heat exchange cavity temperature, primary screw rod revolving speed and
Reaction time makes the primary transparent material of spiro rod reaction products therefrom；
Step 4, twin-screw cylinder bloom composite reaction enters twin-screw cylindrical steel through the transparent material that primary spiro rod reaction flows out
Block combined reactor adjusts reaction condition by control, temperature, two circles including the second each section of heat exchange cavity of automatic control
The revolving speed of axis of a cylinder rotating Vortex and reaction time make twin-screw cylinder bloom composite reaction obtain product and meet making for subsequent workshop section
With.
4. a kind of a kind of amino resins of the continuous production device according to claim 3 based on amino resins is continuous
Change production method, which is characterized in that
The step 1 specifically: the feed bin is added in solid material, is delivered to weightless electricity by material channel through the first helicoidal pump
Sub- scale, the weighing sensor conduct data are compared calculating and reset frequency converter frequency to PLC, the first helicoidal pump of adjustment and
The revolving speed of second helicoidal pump, the solid material are conveyed downwards by the second helicoidal pump through material channel；
The step 2 specifically: the charging basket is added in liquid charging stock, is delivered to mistake by material channel through flowmeter and plunger pump
Barytron claims, when liquid charging stock reaches the quality of setting, the weighing sensor conduct data in the weightlessness electronic scale to PLC,
Compared calculating and reset frequency converter frequency, adjust the revolving speed of plunger pump and diaphragm pump, the liquid charging stock is passed through by diaphragm pump
Material channel is conveyed to primary screw reactor.
5. a kind of a kind of amino resins of the continuous production device according to claim 4 based on amino resins is continuous
Change production method, it is characterised in that in the step 3, control adjustment reaction temperature automatically controls heat exchange by control first and holds
The temperature that each section of chamber is realized, in the step 4, control adjustment reaction temperature automatically controls heat exchange cavity by control second
Each section of temperature is realized.
6. a kind of a kind of ammonia of the continuous production device based on amino resins according to any one of claim 3~5
The continuous production method of base resin, it is characterised in that in the step 4, it is anti-that transparent material enters the combination of twin-screw cylinder bloom
Before answering device, inhibitor solution is pre-filled in the second automatic control heat exchange cavity.
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| CN109012528B (en) * | 2018-08-14 | 2024-03-08 | 无锡创彩光学材料有限公司 | Tubular reactor and method for preparing monodisperse polyamic acid solution by using same |
| CN111269372B (en) * | 2020-01-17 | 2021-01-12 | 江苏长能节能新材料科技有限公司 | Method for preparing hexamethylol melamine with continuous and stable quality |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204237729U (en) * | 2014-10-22 | 2015-04-01 | 贵州省化工研究院 | A kind of urea formaldehyde continuous polymerization unit |
| CN105170065A (en) * | 2015-09-30 | 2015-12-23 | 宋晓轩 | Improved chemical reactor realizing continuous feeding and fast heat removing |
| CN106215842A (en) * | 2016-08-02 | 2016-12-14 | 郑州峰泰纳米材料有限公司 | A kind of device preparing melamine resin |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204237729U (en) * | 2014-10-22 | 2015-04-01 | 贵州省化工研究院 | A kind of urea formaldehyde continuous polymerization unit |
| CN105170065A (en) * | 2015-09-30 | 2015-12-23 | 宋晓轩 | Improved chemical reactor realizing continuous feeding and fast heat removing |
| CN106215842A (en) * | 2016-08-02 | 2016-12-14 | 郑州峰泰纳米材料有限公司 | A kind of device preparing melamine resin |
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