CN106671416A - Distillation cooling device and method for nylon powder for SLS - Google Patents
Distillation cooling device and method for nylon powder for SLS Download PDFInfo
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- CN106671416A CN106671416A CN201611236188.5A CN201611236188A CN106671416A CN 106671416 A CN106671416 A CN 106671416A CN 201611236188 A CN201611236188 A CN 201611236188A CN 106671416 A CN106671416 A CN 106671416A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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Abstract
The invention discloses a distillation cooling device and method for preparing nylon powder for SLS through a solvent deposition method. The distillation cooling device comprises an autoclave body, a stirring device, an online temperature monitoring device, a control valve, an MFC, a condenser and a receiving device. According to the distillation cooling method, through the arrangement of the MFC, the evaporation gas flow control manner is adopted for controlling the cooling temperature of the system, crystallized enthalpy generated during nylon deposition can be brought away in time, the temperature rise range in the autoclave body is reduced, the system temperature uniformity is guaranteed, and the sphere-like nylon powder controllable in particle size, regular in shape and appearance and good in fluidity can be prepared.
Description
Technical field
The invention belongs to advanced manufacturing technology and field of material preparation, prepare more particularly, to a kind of solvent precipitation
Selective laser sintering (SLS) the distillation chiller and cool-down method of nylon powder.
Background technology
Selective laser sintering (Selective Laser Sintering, SLS) is current widely used 3D printing technique
One of, it is, with pressed powder as raw material, directly 3D solid zero to be produced from CAD model using Layered manufacturing principle of stacking
Part.At present, crystalline polymer nylon (polyamide, PA) can directly manufacture plastic functional piece by SLS, nylon and its multiple
The features such as condensation material product has excellent forming property, product strength high precision, good toughness, is selective laser sintering 3D printing skill
A most class materials, occupies more than the 95% of SLS material markets at this stage used in art.
Solvent precipitation is the main method for preparing selective laser sintering nylon powder at present, and it is to select certain solvent
(dissolubility of the nylon under the solvent high temperature is good, and almost insoluble at low temperature), by nylon raw material, various auxiliary agents and solvent
Add and heat up in reactor stirring to raw material to be completely dissolved, then gradually cooling down discharging, drying, ball milling, screening obtain Buddhist nun
Imperial dusty material.
Nylon powder is prepared by solvent precipitation, cooling method and speed have significantly to the crystalline deposit process of powder
Impact, and then affect powder quality.In temperature-fall period, crystallization enthalpy can be released during nylon Precipitation so that the temperature of system
Degree is raised, if crystallization enthalpy can not be taken away in time, solution system temperature rises obvious, the geometrical morphology and particle diameter to powder
Detrimental effect will be brought, the bulk density for being mainly reflected in powder is low, SLS drip molding poor mechanical properties.Traditional cooling
Mode includes:Natural cooling is lowered the temperature, cooling coil water flowing cooling in kettle, cooling jacket oil cooling, is cooled outside kettle.Although on
Stating method can well solve the problems, such as the cooling of little kettle, but for big reactor, due to thermal capacity it is too big, and by cryogenic liquid
Thermograde is easily formed with the heat transfer type of system directly contact in kettle, the uniformity of system temperature cannot be guaranteed, and cause powder
Last particle diameter distribution width, sphericity are poor, bulk density is low.Therefore, crystallization enthalpy, control system when nylon is precipitated how is taken away rapidly
Rate of cooling and the uniformity of guarantee system temperature become and prepare that particle diameter is suitable, pattern is regular, the nylon that bulk density is high
The crucial problem of powder.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of solvent precipitation prepares laser choosing
Area's sintering (SLS) the distillation chiller and cool-down method of nylon powder, its object is to by the drop using distillation cooling
Warm device and cool-down method, realize the cooling rate of control system by way of control boil-off gas flow, and Buddhist nun is taken away in time
Crystallization enthalpy during dragon precipitation, thus solving the heat sink and cool-down method of prior art can not take away in time when nylon is precipitated
Crystallization enthalpy, the lack of homogeneity of system temperature and the caused nylon powder particle diameter distribution width being prepared from, sphericity be poor, accumulation is close
The low technical problem of degree.
For achieving the above object, according to one aspect of the present invention, there is provided a kind of distillation cooling of SLS nylon powders
Heat sink, the cooling device includes kettle 1, agitating device 2, temperature on-line monitoring device 3, control valve 4, gas stream
Amount controller 5, condenser 6, gas buffer 7 and gas reception device 8;
The kettle 1 is provided with agitating device 2 and temperature on-line monitoring device 3;
Control valve 4 is provided with the top vent pipe of the kettle 1, the control valve 4 is connected with the gas flow controller 5
Connect, the control valve 4 and the gas flow controller 5 are used to control the gas flow in kettle 1;
The gas flow controller 5 connects the condenser 6, and the condenser 6 connects the gas buffer 7,
The gas buffer 7 connects the gas reception device 8, and the condenser 6 and the gas reception device 8 are used for kettle
Retort gass condensation in body 1 is reclaimed, and the gas buffer 7 is used for gas buffer and portion gas are reclaimed.
Preferably, the gas flow controller 5 is high temperature and high pressure gas mass flow controller MFC.
Preferably, the installation direction of the condenser 6 has certain angle with horizontal direction, and near the gas buffer
One end of device 7 is less than near one end of the gas flow controller 5.
According to another aspect of the present invention, there is provided a kind of distillation of SLS nylon powders cools method, including
Following steps:
(1) keep kettle body temperature between 140~180 DEG C, be incubated 1~3h, be completely dissolved nylon;
(2) opening controlling valve, adjusts retort gass flow, retort gass is flowed out from kettle, so as to reduce in kettle
Temperature, until temperature on-line monitoring device shows that kettle body temperature is reduced to nylon crystallization temperature for the first time;
(3) retort gass flow is increased in the range of 9.5~15.8L/min, until temperature on-line monitoring device shows kettle
Body temperature is reduced to for the second time nylon crystallization temperature;
(4) retort gass flow is adjusted in the range of 3.2~12.6L/min, until temperature on-line monitoring device shows kettle
Body temperature is down to below solvent boiling point;
(5) closing control valve, naturally cools to room temperature discharging.
Preferably, the regulation of the retort gass flow is digital regulated by the flow-control panel of gas flow controller
To realize.
Preferably, step (2) the retort gass flow that adjusts makes cooling rate control in the range of 3.2~9.5L/min
System is in the range of 20~60 DEG C/h.
Preferably, step (3) the regulation retort gass flow makes cooling rate in the range of 60~100 DEG C/h.
Preferably, moment observation temperature variations in step (3) temperature-fall period, by adjusting retort gass flow temperature is made
Degree gos up to be less than 0.5 DEG C.
Preferably, step (4) the regulation retort gass flow makes cooling rate in the range of 20~80 DEG C/h.
Preferably, the nylon is PA12, PA11, PA6, PA66, PA610, PA612, PA1010, PA1012 and PA1212
In one or more.
In general, by the contemplated above technical scheme of the present invention compared with prior art, can obtain down and show
Beneficial effect.
(1) gas mass flow controller (MFC) is present invention employs, distillation speed is can accurately measure and control, so as to
The cooling rate of control system.On the one hand, in the nylon Precipitation stage, accelerate distillation speed, can in time take away nylon precipitation
Crystallization heat during precipitation, reduce temperature raises again the adverse effect brought to powder geometrical morphology and particle diameter, it is ensured that Buddhist nun
The regularity of imperial powder morphology and the controllability of particle diameter.On the other hand, after nylon crystallization, can control by controlling rate of cooling
The growth process of nucleus, with this powder of required particle diameter size is obtained;
(2) the distillation method that cools of the present invention is simple, and can guarantee system temperature uniformity;
(3) present invention uses receptor, can recycle and reuse to the condensed solvent of steam, economize on resources;
(4) distillation cooling device and cool-down method of the present invention, can prepare that size is controllable, pattern rule
Then, the high subsphaeroidal nylon powder of good fluidity, bulk density.
Description of the drawings
Fig. 1 is the structural representation of present invention distillation chiller.
In figure:1- kettlies, 2- agitating devices, 21- stirring drivers, 22- agitators, 3- on-line temperature monitoring devices, 31- temperature
Degree sensor, 32- wires, 33- digital display temperature meters, 4- control valves, 5- gas flow controllers, 6- condensers, 61- coolants enter
Mouthful, 62- cooling liquid outlets, 7- gas buffers, 71- gas feeds, 72- gas outlets, 73- relief valve, 74- pressure gauges,
75- leakage fluid drams, 8- gas reception devices, the adapter of 81- tails, 82- receptors, 83- absorbing liquids.
Fig. 2 is that solvent precipitation prepares the distillation of SLS nylon powders and cools process schematic;
Fig. 3 is the electromicroscopic photograph of the nylon powder that embodiment 1 is prepared;
Fig. 4 is the grain size distribution of the nylon powder that embodiment 1 is prepared.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, and
It is not used in the restriction present invention.As long as additionally, technical characteristic involved in invention described below each embodiment
Not constituting conflict each other just can be mutually combined.
The distillation cooling device of the SLS nylon powders that the present invention is provided, including kettle 1, agitating device 2, temperature
On-Line Monitor Device 3, control valve 4, gas flow controller 5, condenser 6, gas buffer 7 and gas reception device 8;
Kettle 1 is provided with agitating device 2 and temperature on-line monitoring device 3.
Agitating device 2 includes stirring driver 21 and agitator 22, and stir speed (S.S.) can as needed in 0~1000r/min
Scope is adjusted.
Temperature on-line monitoring device 3 includes temperature sensor 31, wire 32, digital display temperature meter 33, and temperature sensor 31 sets
Inside kettle 1, it passes through wire 32 and is connected with the digital display temperature meter 33 located at the top of kettle 1.
Control valve 4 is provided with the top vent pipe of kettle 1, for controlling the switch of still-process, the aperture for controlling valve 4 also may be used
To adjust, control valve 4 is preferably connected by bridge piece with the gas flow controller 5 being transversely mounted, for controlling in kettle
Gas flow.
Gas flow controller 5 be preferably high temperature and high pressure gas mass flow controller MFC, it include flow transducer,
Flow control valve, amplification control circuit and diverter control passage, possess accurate measurement function and automatically control gas flow
Function.
Gas flow controller 5 connects condenser 6, and condenser 6 is provided with coolant inlet 61 and cooling liquid outlet 62, cools down
Liquid entrance 61 and cooling liquid outlet 62 are respectively provided with a valve.Condenser 6 connects gas buffer 7, and gas buffer 7 connects
Gas reception device 8 is connect, condenser 6 and reception device 8 are used to reclaim the retort gass condensation in kettle 1, gas buffer dress
7 are put for gas buffer and gas-liquid separation, can partially recycled solvent.The installation direction of condenser 6 has certain with horizontal direction
Angle, and be easy to steam less than near one end of the gas flow controller 5 near one end of the gas buffer 7
The condensed solvent recovery of vapour, coolant inlet 61 is arranged on low side, and cooling liquid outlet 62 is arranged on high-end.
Gas buffer 7 includes gas feed 71, gas outlet 72, relief valve 73, pressure gauge 74, leakage fluid dram 75.Gas
Body entrance 71 is arranged on low and middle-end, and gas outlet 72 is arranged on middle and high end, and fluid cross-section product increase, gas velocity reduces, it is ensured that
Outlet pressure will not produce mutation, serve effective cushioning effect;Surge flask 7 can be used as gas-liquid separator, and liquid can pass through
Bottom leakage fluid dram 75 is discharged, recovery section solvent;Relief valve 73 is provided with explosion diaphragm, it is ensured that the safety of surge flask.
Reception device 8 includes tail adapter 81, receptor 82 and absorbing liquid 83.The end of tail adapter 81 has larger horizontal stroke
Sectional area, is placed in absorbing liquid surface nearby, i.e., close absorbing liquid liquid level position, can improve uncooled vapor absorption molten
The response rate of agent.
The distillation of the SLS nylon powders that the present invention is provided cools method, including the following steps shown in Fig. 2:
(1) keep temperature in kettle 1 to be incubated 1~3h at 140~180 DEG C, be completely dissolved nylon;
(2) opening controlling valve 4, adjust retort gass flow, retort gass is flowed out from kettle 1, so as to reduce kettle 1
Interior temperature, shows that temperature is reduced to nylon crystallization temperature for the first time in kettle 1 to temperature on-line monitoring device 3;
(3) retort gass flow is increased in the range of 9.5~15.8L/min, temperature on-line monitoring device 3 shows kettle 1
Interior temperature is reduced to for the second time nylon crystallization temperature;
(4) retort gass flow is adjusted in the range of 3.2~12.6L/min, until temperature is down to below the boiling point of solvent;
(5) closing control valve 4, naturally cools to room temperature discharging.
The digital regulated realization of flow-control panel that the regulation of retort gass flow passes through gas flow controller 5, step
(2) the regulation retort gass flow preferably adjusts retort gass flow in the range of 3.2~9.5L/min, makes cooling rate control
System is in the range of 20~60 DEG C/h.Step (2) purpose is, in order to control distillation speed, to make system rate of cooling drop as required
Temperature, controls nucleation process;When heterogeneous nucleation agent is added without, there is homogenous nucleation process, the nucleus of the slower formation of rate of cooling
More, then powder is thinner, therefore can suitably slow down distillation speed;It is nucleus growth control process when there is heterogeneous nuclei, it is cold
But there is nuclei growth process when temperature is higher if speed is slower, then powder diameter is bigger, therefore distillation speed can be increased
Degree, while ensure that process efficiency.
Step (3) regulation retort gass flow makes cooling rate in the range of 60~100 DEG C/h.In step (3), by gas
Body flow controller, increases gas mass flow, accelerates distillation speed, can in time take away crystallization during nylon Precipitation
Heat, reduce temperature raises again the adverse effect brought to powder geometrical morphology, it is ensured that the regularity of nylon powder pattern
With the controllability of particle diameter.Moment observation temperature variations in step (3) temperature-fall period, by adjusting retort gass flow temperature is made
Degree gos up to be less than 0.5 DEG C.
Step (4) regulation retort gass flow makes cooling rate in the range of 20~80 DEG C/h.According to specific distillation speed
Degree cooling is, in order to control the growth process of nucleus, with this size of product powder to be controlled.
Nylon be PA12, PA11, PA6, PA66, PA610, PA612, PA1010, PA1012 and PA1212 in one kind and
It is various.
The present invention uses nylon powder by preparing selective laser sintering (SLS) using solvent precipitation, especially by one kind
The method that cools is distilled, crystallization enthalpy when nylon is precipitated, the rate of cooling of control system temperature, it is ensured that system temperature are taken away rapidly
The uniformity of degree, prepares particle diameter is suitable, pattern is regular, bulk density is high nylon powder to meet the need of 3D printing technique
Ask.
The solvent of the solvent precipitation distillation crystallisation by cooling method selection of the present invention is ethanol, due to mole gasification of ethanol
Enthalpy very big (being 4.26KJ/mol under 78 DEG C of equilibrium conditions), can absorb substantial amounts of heat during evaporation, the present invention is with vigorous stirring
Distillation is not in the phenomenon of topical hypothermia, and can maintain the relative stable and uniform of kettle temperature, and by controlling boil-off gas
The method of body flow realizes the cooling rate of control system, can in time take away crystallization enthalpy when Buddhist nun is precipitated, and reduces temperature in the kettle
Go up.
Heat sink of the present invention, employs high temperature and high pressure gas mass flow controller (MFC), can be for gas
Mass flow carry out accurate measurement and control, so as to control distillation speed, reach control kettle in system cooling rate purpose,
And ensure that system temperature uniformity;In temperature-fall period, when the crystallization temperature of fast close nylon, distillation can be suitably increased
Speed, takes away in time crystallization heat, so as to reduce the rise amplitude of temperature.Heat sink of the present invention, employs reception dress
Put, the solvent recovery distilled can be recycled, so as to save resource and will not be to environment.By of the present invention
Heat sink and cool-down method can prepare that size is controllable, pattern is regular, good fluidity, bulk density are high subsphaeroidal Buddhist nun
Imperial powder, is especially suitable for powdering and the shaping of SLS.
It is below embodiment:
As shown in figure 1, a kind of solvent precipitation prepares the distillation cooling device of SLS nylon powders, including kettle
1st, agitating device 2, temperature on-line monitoring device 3, control valve 4, gas flow controller 5, condenser 6, the and of gas buffer 7
Gas reception device 8;
Kettle 1 is provided with agitating device 2 and temperature on-line monitoring device 3.Agitating device 2 includes stirring driver 21 and stirring
Device 22, stir speed (S.S.) can be adjusted as needed in 0~1000r/min scopes.
Temperature on-line monitoring device 3 includes temperature sensor 31, wire 32, digital display temperature meter 33, and temperature sensor 31 sets
Inside kettle 1, it passes through wire 32 and is connected with the digital display temperature meter 33 located at the top of kettle 1.
Control valve 4 is provided with the top vent pipe of kettle 1, for controlling the switch of still-process, control valve 4 is preferably by connecting
Connect bend pipe and be connected with the gas flow controller 5 being transversely mounted, for controlling the gas flow in kettle.
Gas flow controller 5 is high temperature and high pressure gas mass flow controller MFC, and it includes flow transducer, flow
Regulating valve, amplification control circuit and diverter control passage, possess accurate measurement function and automatically control the function of gas flow.
Gas flow controller 5 connects condenser 6, and condenser 6 is provided with coolant inlet 61 and cooling liquid outlet 62, cools down
Liquid entrance 61 and cooling liquid outlet 62 are respectively provided with a valve.Condenser 6 connects gas buffer 7, and gas buffer 7 connects
Gas reception device 8 is connect, condenser 6 and reception device 8 are used to reclaim the retort gass condensation in kettle 1, gas buffer dress
7 are put for gas buffer and gas-liquid separation, can partially recycled solvent.The installation direction of condenser 6 has certain with horizontal direction
Angle, and be easy to steam less than near one end of the gas flow controller 5 near one end of the gas buffer 7
The condensed solvent recovery of vapour, coolant inlet 61 is arranged on low side, and cooling liquid outlet 62 is arranged on high-end.
Gas buffer 7 includes gas feed 71, gas outlet 72, relief valve 73, pressure gauge 74, leakage fluid dram 75.Gas
Body entrance 71 is arranged on low and middle-end, and gas outlet 72 is arranged on middle and high end, and fluid cross-section product increase, gas velocity reduces, it is ensured that
Outlet pressure will not produce mutation, serve effective cushioning effect;Surge flask can be used as gas-liquid separator, and liquid can pass through bottom
Portion's leakage fluid dram 75 is discharged;Relief valve 73 is provided with explosion diaphragm, it is ensured that the safety of surge flask.
Reception device 8 includes tail adapter 81, receptor 82 and absorbing liquid 83.Inside the immersion of tail adapter 81 absorbing liquid,
Uncooled vapor absorption can be improve the response rate of solvent.
A kind of solvent precipitation prepares SLS nylon powders, first by nylon 12, ethanol and other additives according to certain
Proportioning be placed in kettle 1, under certain heating rate, 140 DEG C are warming up to, then according to the following distillation side of cooling
Method carries out cooling operation:
(1) after nylon 12 is incubated 1 hour in 140 DEG C, before the process of cooling starts, gas is arranged by MFC
Mass flow be 9.5L/min, make cooling rate control in 60 DEG C/h;
(2) opening controlling valve 4, start distillation and cool process;
(3) when temperature drops to 106 DEG C of 12 crystallization temperature of close nylon, setting MFC is 15.8L/min, plus atmospheric matter
Amount flow, accelerates distillation speed, makes cooling rate control observe temperature variations in 100 DEG C/h, and moment, makes temperature recovery
Less than 0.5 DEG C;
(4) when temperature uniform descent again, setting MFC is 12.6L/min, makes cooling rate be 80 DEG C/h, works as temperature
Closing control valve when being down to less than 78 DEG C.
(5) room temperature discharging is naturally cooled to.
The pattern of the powder of nylon 12 that the present embodiment is prepared and particle diameter distribution respectively as shown in Figure 3 and Figure 4, can be seen
It is 54.8 μm and narrow distribution to go out nylon powder pattern rule, higher sphericity, good fluidity, mean diameter, is especially suitable for swashing
Light constituency sinters.
Embodiment 2
Distillation cooling device is with embodiment 1.
A kind of solvent precipitation prepares SLS nylon powders, first by nylon 11, ethanol and other additives according to certain
Proportioning be placed in kettle 1, under certain heating rate, 150 DEG C are warming up to, then according to the following distillation side of cooling
Method carries out cooling operation:
(1) after nylon 11 is incubated 2.5 hours in 150 DEG C, before the process of cooling starts, gas is arranged by MFC
The mass flow of body is 6.3L/min, cooling rate is controlled in 40 DEG C/h;
(2) opening controlling valve 4, start distillation and cool process;
(3) when temperature drops to 110 DEG C of close nylon 11 crystallization temperature, setting MFC is 12.6L/min, plus atmospheric matter
Amount flow, accelerates distillation speed, makes cooling rate control observe temperature variations in 80 DEG C/h, and moment, makes temperature recovery
Less than 0.5 DEG C.
(4) when temperature uniform descent again, setting MFC is 9.5L/min, makes cooling rate be 60 DEG C/h, when temperature drop
To closing control valve when less than 78 DEG C.
(5) room temperature discharging is naturally cooled to.
Embodiment 3
Distillation cooling device is with embodiment 1.
A kind of solvent precipitation prepares SLS nylon powders, first by nylon 6, ethanol and other additives according to certain
Proportioning be placed in kettle 1, under certain heating rate, 180 DEG C are warming up to, then according to the following distillation side of cooling
Method carries out cooling operation:
(1) after nylon 6 is incubated 3 hours in 180 DEG C, before the process of cooling starts, gas is arranged by MFC
Mass flow is 3.2L/min, and control cooling rate is in 20 DEG C/h;
(2) opening controlling valve 4, start distillation and cool process;
(3) when temperature drops to 120 DEG C of 6 crystallization temperature of close nylon, setting MFC is 9.5L/min, increases gaseous mass
Flow, accelerates distillation speed, and control cooling rate is observed temperature variations, temperature recovery is not surpassed in 60 DEG C/h, and moment
Cross 0.5 DEG C.
(4) when temperature uniform descent again, setting MFC is 3.2L/min, makes cooling rate be 20 DEG C/h, when temperature drop
To closing control valve when less than 78 DEG C.
(5) room temperature discharging is naturally cooled to.
Specific embodiment list:
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, not to
The present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc. are limited, all should be included
Within protection scope of the present invention.
Claims (9)
1. a kind of distillation cooling device of SLS nylon powders, it is characterised in that the cooling device includes kettle
(1), valve (4), gas flow controller (5), condenser (6), gas buffer (7) and gas reception device (8) are controlled;
The kettle (1) is provided with agitating device (2) and temperature on-line monitoring device (3);
Control valve (4), control valve (4) and the gas flow controller (5) are provided with kettle (1) the top vent pipe
It is connected, the gas flow of control valve (4) and the gas flow controller (5) for controlling in kettle (1);
The gas flow controller (5) connects the condenser (6), and the condenser (6) connects the gas buffer
(7), the gas buffer (7) connects the gas reception device (8), and the condenser (6) and the gas receive dress
(8) are put for the retort gass condensation in kettle (1) to be reclaimed, the gas buffer (7) is for gas buffer and part
Gas is reclaimed.
2. it is as claimed in claim 1 to distill cooling device, it is characterised in that the gas flow controller (5) is height
Warm gases at high pressure mass flow controller MFC.
3. distillation cooling device as claimed in claim 1, it is characterised in that the installation direction of the condenser (6) with
Horizontal direction has certain angle, and near one end of the gas buffer (7) less than near gas flow control
One end of device (5).
4. a kind of distillation of SLS nylon powders cools method, it is characterised in that comprise the steps:
(1) keep kettle body temperature between 140~180 DEG C, be incubated 1~3h, be completely dissolved nylon;
(2) opening controlling valve, adjusts retort gass flow, retort gass is flowed out from kettle, so as to reduce kettle body temperature,
Until temperature on-line monitoring device shows that kettle body temperature is reduced to nylon crystallization temperature for the first time;
(3) retort gass flow is increased in the range of 9.5~15.8L/min, until temperature on-line monitoring device is shown in kettle
Temperature is reduced to for the second time nylon crystallization temperature;
(4) retort gass flow is adjusted in the range of 3.2~12.6L/min, until temperature on-line monitoring device is shown in kettle
Temperature is down to below solvent boiling point;
(5) closing control valve, naturally cools to room temperature discharging.
5. it is as claimed in claim 4 to distill the method that cools, it is characterised in that the regulation of the retort gass flow passes through
The flow-control panel of gas flow controller is digital regulated realizing, step (2) is described to adjust retort gass flow, preferred to adjust
Section retort gass flow makes cooling rate control in the range of 20~60 DEG C/h in the range of 3.2~9.5L/min.
6. it is as claimed in claim 4 to distill the method that cools, it is characterised in that step (3) is described to adjust retort gass stream
Amount makes cooling rate in the range of 60~100 DEG C/h.
7. it is as claimed in claim 4 to distill the method that cools, it is characterised in that moment observation in step (3) temperature-fall period
Temperature variations, make temperature recovery be less than 0.5 DEG C by adjusting retort gass flow.
8. it is as claimed in claim 4 to distill the method that cools, it is characterised in that step (4) is described to adjust retort gass stream
Amount makes cooling rate in the range of 20~80 DEG C/h.
9. distillation as claimed in claim 4 cools method, it is characterised in that the nylon be PA12, PA11, PA6,
One or more in PA66, PA610, PA612, PA1010, PA1012 and PA1212.
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