A kind of parallel polymerization kettle
Technical field
The utility model discloses a kind of polymeric kettle, more particularly to a kind of parallel polymerization kettle.
Background technology
Polymeric kettle is the capital equipment for preparing high-molecular compound, is usually vertical type cylinder shape autoclave.In the prior art,
Polymeric kettle is generally made of autoclave body, chuck, blender, transmission device, gland seal device, supporting etc..Chuck is normally at polymeric kettle
Kettle body outer wall on, be heated or cooled for being passed through steam or cooling water.In order to polymerize needs, can also generally polymerize
Blender is set in kettle, blender is driven by motor and transmission device, implements stirring in the course of the polymerization process.Polymeric kettle gathers
Conjunction can be produced with one-pot gap, can also make multi-floating bodies continuous production.Polymerization reactant is entered next by the lower part of a kettle
The top of a kettle, equipped with instrument and feed inlet and outlet etc. such as temperature, pressure on kettle.
Existing polymeric kettle is to include a kettle body, and polymerization technique is completed in kettle body, to carry out parallel test, is then needed
To carry out, devote a tremendous amount of time in batches, and the precision of experiment cannot be held completely, cause scientific research personnel in reality
During testing, it has to repeat experiment even tens of times for several times, extend experimental period, influence research and development progress, increase experimentation cost.
It can be seen that:Existing polymeric kettle is not particularly suited for optimizing using parallel test the operation of reaction condition.The problems demand solves.
Utility model content
The utility model cannot adjust polymerization parameter to solve polymeric kettle in the prior art under an aggregation test, make
Obtaining parallel test cannot be smoothed out, so that the defects of wasting a large amount of repetition times and increasing experimentation cost, there is provided a kind of parallel
Polymeric kettle.The parallel polymerization kettle of the utility model can carry out the parallel test of different condition in same batch, reduce significantly
Test period, improve experiment precision.
The utility model provides a kind of parallel polymerization kettle, and the parallel polymerization kettle includes:Autoclave body and chuck, the chuck are set
It is placed on the outer wall of the autoclave body;The parallel polymerization kettle further includes a reactor frame, and the reactor frame is located at the kettle
In vivo.
One preferable technical solution of the utility model, the autoclave body include kettle cover and kettle body.
One preferable technical solution of the utility model, the shape of the inner wall of the autoclave body is any, can be same up and down
Wide cylinder, or truncated cone-shaped, the internal diameter of the truncated cone-shaped gradually decrease from top to bottom.
One preferable technical solution of the utility model, the kettle cover are equipped with gas feed and gas vent.
One preferable technical solution of the utility model, the reactor set up the bottom for being placed in the autoclave body.
One preferable technical solution of the utility model, the reactor frame is fixed on the bottom of the autoclave body, described
Fixed mode, can be this area usual manner, such as:It can be integrally formed with the autoclave body, alternatively, institute can be welded in
State the bottom of autoclave body.
One preferable technical solution of the utility model, the reactor frame can also be arranged to it is movable, it is and described
The bottom of autoclave body be not fixed, can be separated with the bottom of the autoclave body, i.e.,:Polymeric kettle is placed in the bottom of reaction kettle when reacting, instead
After answering, it can remove, easy to clean.One of them preferable technical solution, the reactor frame can be placed directly
In the bottom.Alternatively, one of them preferable technical solution, the reactor frame is connected with an elevating lever;The elevating lever
It is connected with the transmission device being arranged on the kettle cover, the transmission device controls the reactor frame by the elevating lever
Lifting.The elevating lever is used to taking out or placing the reactor frame.The connection mode of the reactor frame and the elevating lever
Preferably weld, riveting or bolt and nut connect.Wherein, it is furthermore preferred that the elevating lever passes through bolt with the reactor frame
Nut connects, and the connection mode is:A vertical through hole is equipped with the reactor frame, for penetrating for the elevating lever,
The bolt and nut is located at the bottom of the elevating lever, the fixation for the elevating lever and the reactor frame.The lifting
The length of bar is:Ensure the reactor frame move downward contacted with the bottom it is steady after, under the elevating lever can also continue
Certain distance drops, alternatively, when needing to take out reactor frame, the elevating lever rises a distance first, then drives described anti-
Device is answered to rise, the distance is preferably 1-10cm;In this way, ensureing between elevating lever and reactor frame, there is certain connection flexible
Property, it is not complete stuck contact, the serious forgiveness in whole parallel polymerization kettle preparation process can be improved.
The length of the elevating lever is:1.001-1.15 times of elevating lever full-length;The full-length is the liter
Drop bar is connected required length with the reactor seat according to this area routine connection mode.
One preferable technical solution of the utility model, the reactor frame is interior to be equipped with reactor seat.The reactor
Seat is used to place experimental facilities, such as beaker, flask or test tube etc..The reactor seat can be arranged to arbitrary shape, in order to
Ensure that experimental facilities is fixed in reaction seat, the reaction seat can carry out corresponding according to the shape of beaker, flask or test tube
Set, as long as experimental facilities can be fixed.
One preferable technical solution of the utility model, the quantity of the reactor seat are more than one, preferably 2-200
It is a, more preferably 6-100, most preferably 10-60.Diameter preferred 0.1-40cm, the more preferably 1-25cm of the reactor seat, most
It is preferred that 1-15cm.The highly preferred 5-30cm of the reactor seat, more preferably 8-20cm.
One preferable technical solution of the utility model, the size and dimension of the reactor frame do not limit particularly
It is fixed, if the progress of reaction is not influenced, and the reactor frame can be fixed on the bottom.It is in general, described
Reactor frame can be configured according to the size and dimension of the kettle body, be preferably the size of the scaled down of the kettle body
And shape.
The utility model people of the utility model has found, multiple reactor seats are contained by adding one in polymeric kettle
Reactor frame, can carry out parallel test in polymeric kettle.For example, it is carried out at the same time addition different additive or Different adding amount
Additive parallel test, or the parallel test etc. of differential responses raw material or reaction raw materials proportioning.
In further research, utility model people has found:The condition control of these parallel tests is not accurate enough, such as:
In polymerisation, since high temperature may cause the evaporation of raw material, the gas raw material of evaporation is pooled at the kettle cover of polymeric kettle, then is passed through
Condensation may may proceed to it is random return in reactor, cause the amount of raw material in reactor to have fluctuation, it is practical new on this basis
Type people is further improved again, has obtained superior technique scheme, realizes superior technique effect.
One preferable technical solution of the utility model, the parallel polymerization kettle of the utility model further include reactor cap.
The reactor cap is arranged at the top of the reactor frame.
The contact surface of the reactor cap and the reactor frame, positioned at the upper surface of the reactor frame, alternatively, being located at
In the reactor seat;As long as the effect for keeping each reactor independence can be played.The reactor cap is used for
It is placed in during reaction on the reactor of the reactor seat, prevents evaporation/distillation of raw material or reactant in reactor etc., so as to
The independence of the reactor in each reactor seat is kept, makes to influence each other between reactor.The number of the reactor cap
Amount can be more than one, preferably smaller than the quantity equal to the reactor seat, the more preferably quantity equal to the reactor seat.
The reactor cap is corresponded with the reactor seat.
The shape of the reactor cap is any, as long as can shroud residence states reactor in reactor seat.This reality
With a new preferable technical solution, the reactor cap is the unidirectional blocking pipe of test tube shape.
One preferable technical solution of the utility model, the reactor cap are equipped with some ventholes;The outlet
The position in hole is any, can be located at the top of the reactor cap, can also be located at the side wall of the reactor cap, be preferably placed at
The side wall of the reactor cap;The aperture is used for the gas exchanges in reactor during the reaction.The venthole
Quantity is preferably more than 1, more preferably 5-40, most preferably 10-30.The preferred 0.05-0.5cm of diameter of the venthole,
More preferably 0.1-0.2cm.The venthole can prevent the fluctuation of pressure in reactor.
The parallel polymerization kettle of the utility model can carry out the parallel test of different condition in same batch, reduce significantly
Test period, while the precision tested greatly improves.
Brief description of the drawings
Fig. 1 is the structure diagram of the parallel polymerization kettle of one embodiment of the utility model;
Fig. 2 is the structure diagram of the parallel polymerization kettle of one embodiment of the utility model;
Fig. 3 is the structure diagram of the reactor frame of one embodiment of the utility model;
Fig. 4 is the structure diagram of the reactor cap of one embodiment of the utility model;
Fig. 5 is the structure diagram of the parallel polymerization kettle of one embodiment of the utility model;
Fig. 6 is the enlarged drawing of a parts of the parallel polymerization kettle of Fig. 5;
Fig. 7 is that the viscosity number for the polyamide polymerizeing in the parallel polymerization kettle of one embodiment of the utility model and Amino End Group contain
The result figure of amount;
Fig. 8 is that the viscosity number for the polyamide polymerizeing in the parallel polymerization kettle of one embodiment of the utility model and Amino End Group contain
The result figure of amount;
Fig. 9 is the viscosity number of polyamide and the result figure of terminal amino group content polymerizeing in existing polymeric kettle.
Embodiment
Embodying the exemplary embodiment of the utility model features and advantages will describe in detail in the following description.It should be understood that
Be that the utility model can have various changes in different embodiments, it does not all depart from the model of the utility model
Enclose, and the descriptions and illustrations are essentially for illustration purposes, and it is not used to limitation the utility model.
Embodiment 1
A kind of parallel polymerization kettle, as shown in Figure 1, including:Autoclave body 1, the chuck 5 being arranged on the outer wall of autoclave body 1 and setting
Reactor frame 6 in the bottom of autoclave body 1;
Autoclave body 1:The inner wall of autoclave body 1 is cylinder, including kettle cover 2 and kettle body 3, it is gentle that kettle cover 2 is equipped with gas feed 41
Body outlet 42;
Reactor frame 6:As shown in figure 3, it is equipped with reactor seat 62 in reactor frame 6;Reactor seat 62, which is used to place, tests
Equipment, such as beaker, flask or test tube etc., can also place temp probe, by being connected in temperature sensor, detect reactant
The temperature of system, its shape can be set accordingly according to the shape of beaker, flask or test tube;In the present embodiment, reactor seat
62 a diameter of 1cm, is highly 15cm;Reactor frame 6 is fixed on the bottom of autoclave body 1;
The parallel polymerization kettle of the utility model, can carry out parallel test.For example, be carried out at the same time addition different additive or
The additive of person's Different adding amount, or be carried out at the same time the experiment of differential responses raw material or reaction raw materials proportioning etc., reduce significantly
Test period, the precision of experiment greatly improve.
Using the parallel polymerization kettle of the present embodiment, the parallel test of polymerizing polyamide is carried out, test method is as follows:Take
Pentanediamine 20.38g, adipic acid 29.20g and pure water 49.68g, configure 50% polyamide salt aqueous solution, are measured at 30 DEG C
Its pH value is 8.62.Take 4g polyamide salt solutions to be put into 15cm teat glasses respectively, be put into the reaction of above-mentioned parallel polymerization kettle
In device frame, temperature 275, polymerize under the conditions of vacuum -0.7atm, obtains polyamide 56 inside.
According to the method for SOP, the viscosity number and terminal amino group content of the polyamide 56 detected, are calculated the variance of viscosity number
For:12.9, the variance of terminal amino group content is:12.42.
The results are shown in Figure 7 for viscosity number and terminal amino group content.
Embodiment 2
A kind of parallel polymerization kettle, as shown in Fig. 2, including:Autoclave body 1, the chuck 5 being arranged on the outer wall of autoclave body 1, set
Reactor frame 6 and reactor cap 60 in the bottom of autoclave body 1;
Autoclave body 1:The inner wall of autoclave body 1 is cylinder, including kettle cover 2 and kettle body 3, it is gentle that kettle cover 2 is equipped with gas feed 41
Body outlet 42;
Reactor frame 6:As shown in figure 3, it is equipped with 20 reactor seats 62 in reactor frame 6;Reactor seat 62 is used to place
Experimental facilities, such as beaker, flask or test tube etc., its shape can be set accordingly according to the shape of beaker, flask or test tube
Put;In the present embodiment, a diameter of 1cm of reactor seat 62, is highly 15cm;
Reactor cap 60:For the unidirectional blocking pipe of test tube shape, for being placed in the test tube of reactor seat 62 in reaction, prevent
Only evaporation/the distillation of invisible spectro raw material or reactant etc., to keep the independence of the reactor in each reactor seat, makes
It will not influence each other between reactor;The quantity of reactor cap 60 is the same as the quantity of reactor seat 62, reactor cap and the reaction
Device seat corresponds;
Reactor cap 60 is arranged at the top of reactor frame 6, its contact surface with reactor frame 6, positioned at reactor frame 60
Upper surface, alternatively, in the reactor seat 62, as long as the effect for keeping each reactor independence can be played.
The parallel polymerization kettle of the utility model, can carry out parallel test.For example, be carried out at the same time addition different additive or
The additive of person's Different adding amount, or be carried out at the same time experiment etc. of differential responses raw material or reaction raw materials proportioning, and can be with
External interference factor is greatly excluded, the test period is greatly reduced, the precision of experiment greatly improves.
Embodiment 3
A kind of parallel polymerization kettle, as shown in Fig. 2, including:Autoclave body 1, the chuck 5 being arranged on the outer wall of autoclave body 1, set
Reactor frame 6 and reactor cap 60 in the bottom of autoclave body 1;
Autoclave body 1:The inner wall of autoclave body 1 is cylinder, including kettle cover 2 and kettle body 3, it is gentle that kettle cover 2 is equipped with gas feed 41
Body outlet 42;
Reactor frame 6:As shown in figure 3, it is equipped with 20 reactor seats 62 in reactor frame 6;Reactor seat 62 is used to place
Experimental facilities, such as beaker, flask or test tube etc., its shape can be set accordingly according to the shape of beaker, flask or test tube
Put;In the present embodiment, a diameter of 1.5cm of reactor seat 62, is highly 12cm;Reactor frame 6 is fixed on the bottom of autoclave body 1;
Reactor cap 60:As shown in figure 4, it is the unidirectional blocking pipe of test tube shape, for being placed in reactor seat 62 in reaction
Test tube on, evaporation/distillation of invisible spectro raw material or reactant etc. is prevented, to keep the reactor in each reactor seat
Independence, make to influence each other between reactor;The quantity of reactor cap 60 is the same as the quantity of reactor seat 62, reactor cap
Corresponded with the reactor seat;The side wall of reactor cap 60 is equipped with the venthole 601 of 22 diameter 0.1cm, for
Gas exchanges in reaction process in reactor.
Reactor cap 60 is arranged at the top of reactor frame 6, its contact surface with reactor frame 6, positioned at reactor frame 60
Upper surface, alternatively, in the reactor seat 62, as long as the effect for keeping each reactor independence can be played.
The parallel polymerization kettle of the utility model, can carry out parallel test.For example, be carried out at the same time addition different additive or
The additive of person's Different adding amount, or be carried out at the same time experiment etc. of differential responses raw material or reaction raw materials proportioning, and can be with
External interference factor is greatly excluded, the test period is greatly reduced, the precision of experiment greatly improves.
Embodiment 4
A kind of parallel polymerization kettle, as shown in figure 5, including:Autoclave body 1, the chuck 5 being arranged on the outer wall of autoclave body 1, set
Reactor frame 6 and reactor cap 60 in the bottom of autoclave body 1;
Autoclave body 1:The inner wall of autoclave body 1 is cylinder, including kettle cover 2 and kettle body 3, it is gentle that kettle cover 2 is equipped with gas feed 41
Body outlet 42;
Reactor frame 6:As shown in figure 3, it is equipped with 20 reactor seats 62 in reactor frame 6;Reactor seat 62 is used to place
Experimental facilities, such as beaker, flask or test tube etc., its shape can be set accordingly according to the shape of beaker, flask or test tube
Put;In the present embodiment, a diameter of 2cm of reactor seat 62, is highly 18cm;
Reactor cap 60:As shown in figure 4, it is the unidirectional blocking pipe of test tube shape, for being placed in reactor seat 62 in reaction
Test tube on, evaporation/distillation of invisible spectro raw material or reactant etc. is prevented, to keep the reactor in each reactor seat
Independence, make to influence each other between reactor;The quantity of reactor cap 60 is the same as the quantity of reactor seat 62, reactor cap
Corresponded with reactor seat;The side wall of reactor cap 60 is equipped with the venthole 601 of 22 diameter 0.1cm, for reacting
During gas exchanges in reactor.
Reactor frame 6 be arranged to it is movable, i.e.,:Reactor frame 6 is placed in the bottom of reaction kettle, reaction knot when polymeric kettle reacts
Shu Hou, can remove, easy to clean;Reactor frame 6 is connected with an elevating lever 8, and elevating lever 8 is with being arranged on the kettle cover 2
Transmission device connects, and transmission device controls the lifting of reactor frame 6 by elevating lever 8, for taking-up or placing response device frame 6;
Reactor frame 6 is connected with elevating lever 8 by bolt and nut, and connection mode is:It is vertical that one is equipped with reactor frame 6
Through hole, for penetrating for elevating lever 8, bolt and nut is located at the bottom of elevating lever 8, for consolidating for elevating lever 8 and reactor frame 6
It is fixed, as shown in fig. 6, Fig. 6 is the enlarged drawing of a parts of Fig. 5:The length of elevating lever is:Guarantee reactor frame 6 moves downward and kettle
After bottom contact is steady, elevating lever 8 can also continue to decline certain distance (distance herein is indicated by an arrow in figure 6), alternatively, working as
When needing to take out reactor frame 6, elevating lever 8 rises a distance (distance herein is indicated by an arrow in figure 6) first, then
Reactor frame 6 is driven to rise, 8 length of elevating lever is:1.05 times of elevating lever full-length;Full-length is for elevating lever and instead
Device seat is answered to connect required length according to conventional connection mode;In this way, ensureing between elevating lever and reactor frame, have certain
Connection flexibility, is not complete stuck contact, can improve the serious forgiveness in whole parallel polymerization kettle preparation process.
The parallel polymerization kettle of the utility model, can carry out parallel test.For example, be carried out at the same time addition different additive or
The additive of person's Different adding amount, or be carried out at the same time experiment etc. of differential responses raw material or reaction raw materials proportioning, and can be with
External interference factor is greatly excluded, the test period is greatly reduced, the precision of experiment greatly improves.
Using the parallel polymerization kettle of the present embodiment, the parallel test of polymerizing polyamide is carried out, test method is as follows:Take
Pentanediamine 20.38g, adipic acid 29.20g and pure water 49.68g, configure 50% polyamide salt aqueous solution, are measured at 30 DEG C
Its pH value is 8.62.Take 4g polyamide salt solutions to be put into 15cm teat glasses respectively, be put into the reaction of above-mentioned parallel polymerization kettle
In device frame, temperature 275, polymerize under the conditions of vacuum -0.7atm, obtains polyamide 56 inside.
According to the method for SOP, the viscosity number and terminal amino group content of the polyamide 56 detected, are calculated the variance of viscosity number
For:6.70, the variance of terminal amino group content is:6.36.
The results are shown in Figure 8 for viscosity number and terminal amino group content.
Comparative example 1
A kind of polymeric kettle, including the autoclave body with inlet port and outlet port, the chuck for being arranged on autoclave body periphery, blender,
The components such as axle envelope, transmission device, in the polymeric kettle, carry out the experiment with the polymerizing polyamide of embodiment same polymeric condition,
Carry out 16 times altogether, and according to the method for SOP, the viscosity number and terminal amino group content of the polyamide 56 detected, are calculated viscosity number
Variance be:27.45, the variance of terminal amino group content is:37.99.
The results are shown in Figure 9 for viscosity number and terminal amino group content.