CN106671416B - A kind of the distillation cooling device and cool-down method of SLS nylon powders - Google Patents
A kind of the distillation cooling device and cool-down method of SLS nylon powders Download PDFInfo
- Publication number
- CN106671416B CN106671416B CN201611236188.5A CN201611236188A CN106671416B CN 106671416 B CN106671416 B CN 106671416B CN 201611236188 A CN201611236188 A CN 201611236188A CN 106671416 B CN106671416 B CN 106671416B
- Authority
- CN
- China
- Prior art keywords
- temperature
- gas
- distillation
- gas flow
- nylon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- B33Y30/00—Apparatus for additive manufacturing; Details thereof or accessories therefor
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Polyamides (AREA)
Abstract
The invention discloses distillation cooling devices and cool-down method that a kind of solvent precipitation prepares selective laser sintering (SLS) nylon powder, the distillation cooling device includes autoclave body, agitating device, temperature on-line monitoring device, control valve, gas mass flow controller (MFC), condenser, reception device, the distillation method of cooling is by the way that MFC is arranged, the cooling rate of control system in a manner of controlling boil-off gas flow, crystallization enthalpy when Buddhist nun's precipitation can be taken away in time, reduce the rise amplitude of temperature in the kettle, the uniformity of guarantee system temperature, it is controllable particle size can be prepared, pattern rule, the subsphaeroidal nylon powder of good fluidity.
Description
Technical field
The invention belongs to advanced manufacturing technologies and field of material preparation, are prepared more particularly, to a kind of solvent precipitation
The distillation cooling device and cool-down method of selective laser sintering (SLS) nylon powder.
Background technology
Selective laser sintering (Selective Laser Sintering, SLS) is current widely used 3D printing technique
One of, it is directly to produce 3D solid zero from CAD model using Layered manufacturing principle of stacking using solid powder as raw material
Part.Currently, crystalline polymer nylon (polyamide, PA) can directly manufacture plastic functional piece by SLS, nylon and its multiple
Condensation material product has the characteristics that forming property is excellent, product strength precision is high, good toughness, is selective laser sintering 3D printing skill
Most commonly used one kind material, occupies 95% or more of SLS material markets at this stage in art.
Solvent precipitation is the main method for preparing selective laser sintering nylon powder at present, 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
Heating stirring to raw material in reaction kettle is added to be completely dissolved, then gradual cooling down discharging, drying, ball milling, screening obtain Buddhist nun
Imperial dusty material.
Preparing nylon powder, cooling method and speed by solvent precipitation has significantly the crystalline deposit process of powder
Influence, and then influence powder quality.In temperature-fall period, when nylon Precipitation, can release the temperature that crystallization enthalpy makes system
Degree increases, if crystallization enthalpy cannot be taken away in time, solution system temperature rise is apparent, to the geometrical morphology and grain size of 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 cools down, cooling coil water flowing cooling in kettle, the cooling of cooling jacket oil, cools outside kettle.On although
The cooling problem that method can be well solved small kettle is stated, but for big reaction kettle, since thermal capacity is too big, and passes through cryogenic liquid
The heat transfer type being in direct contact with system in kettle easily forms temperature gradient, and the uniformity of system temperature cannot be guaranteed, and cause powder
Last particle diameter distribution is wide, sphericity is poor, bulk density is low.Therefore, how to take away rapidly nylon precipitation when crystallization enthalpy, control system
Cooling velocity and guarantee system temperature uniformity become prepare the nylon that grain size is suitable, pattern is regular, bulk density is high
The crucial problem of powder.
Invention content
For the disadvantages described above or Improvement requirement of the prior art, the present invention provides a kind of solvent precipitations to prepare laser choosing
Area is sintered the distillation cooling device and cool-down method that (SLS) uses nylon powder, and its object is to by using the cooling drop of distillation
Warm device and cool-down method realize the cooling rate of control system by way of controlling boil-off gas flow, take away Buddhist nun in time
Crystallization enthalpy when dragon precipitation, the heat sink and cool-down method for thus solving the prior art cannot be taken away in time when nylon precipitates
Crystallization enthalpy, system temperature lack of homogeneity caused by the nylon powder particle diameter distribution that is prepared is wide, sphericity is poor, accumulation is close
Spend low technical problem.
To achieve the above object, according to one aspect of the present invention, a kind of distillation cooling of SLS nylon powders is provided
Heat sink, the cooling device include autoclave body 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 autoclave body 1 is equipped with agitating device 2 and temperature on-line monitoring device 3；
Control valve 4 is equipped at 1 top vent pipe of the autoclave body, the control valve 4 is connected with the gas flow controller 5
It connects, the control valve 4 and the gas flow controller 5 are used to control the gas flow in autoclave body 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 gas condensing recovery in body 1, the gas buffer 7 are recycled for gas buffer and portion gas.
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 close to the gas buffer
One end of device 7 is less than close to one end of the gas flow controller 5.
Other side according to the invention provides a kind of distillation of SLS nylon powders and cools method, including
Following steps：
(1) it keeps kettle body temperature between 140~180 DEG C, keeps the temperature 1~3h, nylon is made to be completely dissolved；
(2) opening controlling valve adjusts retort gas flow, so that retort gas is flowed out out of autoclave body, to reduce in autoclave body
Temperature, until temperature on-line monitoring device shows that temperature is reduced to nylon crystallization temperature for the first time in autoclave body；
(3) increase retort gas flow within the scope of 9.5~15.8L/min, until temperature on-line monitoring device shows kettle
Body temperature is reduced to nylon crystallization temperature for the second time；
(4) retort gas flow is adjusted within the scope of 3.2~12.6L/min, until temperature on-line monitoring device shows kettle
Body temperature is down to solvent boiling point or less；
(5) closing control valve, cooled to room temperature discharging.
Preferably, the adjusting of the retort gas flow is digital regulated by the flow control panel of gas flow controller
To realize.
Preferably, step (2) the adjusting retort gas flow makes cooling rate control within the scope of 3.2~9.5L/min
System is within the scope of 20~60 DEG C/h.
Preferably, step (3) the adjusting retort gas flow makes cooling rate within the scope of 60~100 DEG C/h.
Preferably, the moment observes temperature variations in step (3) temperature-fall period, makes temperature by adjusting retort gas flow
Degree gos up to be no more than 0.5 DEG C.
Preferably, step (4) the adjusting retort gas flow makes cooling rate within the scope of 20~80 DEG C/h.
Preferably, the nylon is PA12, PA11, PA6, PA66, PA610, PA612, PA1010, PA1012 and PA1212
In it is one or more.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can obtain down and show
Beneficial effect.
(1) present invention employs gas mass flow controller (MFC), distillation speed is can accurately measure and controls, to
The cooling rate of control system.On the one hand, in the nylon Precipitation stage, accelerate distillation speed, nylon precipitation can be taken away in time
Crystallization heat when precipitation, reduce temperature increases the adverse effect brought to powder geometrical morphology and grain size again, ensure that Buddhist nun
The regularity of imperial powder morphology and the controllability of grain size.On the other hand, controllable by controlling cooling velocity after nylon crystallization
The growth process of nucleus obtains the powder of required particle size with this；
(2) the distillation method that cools of the present invention is simple and practicable, and can guarantee the uniformity of system temperature；
(3) present invention uses receivers, can recycle and reuse, economize on resources to the condensed solvent of steam；
(4) distillation cooling device and cool-down method of the present invention, can prepare that particle 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 schematic diagram of present invention distillation cooling device.
In figure：1- autoclave bodies, 2- agitating devices, 21- stir driver, 22- blenders, 3- on-line temperature monitoring devices, 31- temperature
Degree sensor, 32- conducting wires, 33- digital display temperature meters, 4- control valves, 5- gas flow controllers, 6- condensers, 61- coolant liquids enter
Mouthful, 62- cooling liquid outlets, 7- gas buffers, 71- gas feeds, 72- gas vents, 73- safety valves, 74- pressure gauges,
75- leakage fluid drams, 8- gas reception devices, 81- tails are taken over, 82- receivers, 83- absorbing liquids.
Fig. 2 is that solvent precipitation prepares the distillations of SLS nylon powders and cools process schematic；
Fig. 3 is the electromicroscopic photograph for the nylon powder that embodiment 1 is prepared；
Fig. 4 is the grain size distribution for the nylon powder that embodiment 1 is prepared.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
It does not constitute a conflict with each other and can be combined with each other.
The distillation cooling device of SLS nylon powders provided by the invention, including autoclave body 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；
Autoclave body 1 is equipped with agitating device 2 and temperature on-line monitoring device 3.
Agitating device 2 includes stirring driver 21 and blender 22, stir speed (S.S.) can be as needed in 0~1000r/min
Range is adjusted.
Temperature on-line monitoring device 3 includes temperature sensor 31, conducting wire 32, digital display temperature meter 33, and temperature sensor 31 is set
Inside autoclave body 1, it is connect with the digital display temperature meter 33 set on 1 top of autoclave body by conducting wire 32.
Control valve 4 is equipped at 1 top vent pipe of autoclave body, for controlling the switch of distillation process, the aperture of control valve 4 also may be used
To adjust, control valve 4 is preferably connect by bridge piece with the gas flow controller 5 being transversely mounted, for controlling in autoclave body
Gas flow.
Gas flow controller 5 is preferably high temperature and high pressure gas mass flow controller MFC comprising flow sensor,
Flow control valve, amplification control circuit and current divider control channel have accurate measurement function and automatically control gas flow
Function.
Gas flow controller 5 connects condenser 6, and condenser 6 is equipped with coolant inlet 61 and cooling liquid outlet 62, cooling
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 for the retort gas condensing recovery in autoclave body 1, gas buffer dress
It sets 7 and is used for gas buffer and gas-liquid separation, it can partially recycled solvent.The installation direction of condenser 6 has certain with horizontal direction
Angle, and be less than close to one end of the gas flow controller 5 close to one end of the gas buffer 7, convenient for that will steam
The condensed solvent recovery of vapour, the setting of coolant inlet 61 are arranged in low side, cooling liquid outlet 62 high-end.
Gas buffer 7 includes gas feed 71, gas vent 72, safety valve 73, pressure gauge 74, leakage fluid dram 75.Gas
The setting of body entrance 71 increases in low and middle-end, the setting of gas vent 72 in middle and high end, fluid cross-section product, and gas velocity reduces, and ensures
Outlet pressure not will produce mutation, play 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；Safety valve 73 is equipped with explosion diaphragm, ensure that the safety of surge flask.
Reception device 8 includes tail take over 81, receiver 82 and absorbing liquid 83.81 end of tail take over has larger cross
Sectional area is placed in absorbing liquid surface nearby, i.e., close to absorbing liquid liquid level position, can improve uncooled vapor absorption molten
The rate of recovery of agent.
The distillation of SLS provided by the invention nylon powders cools method, including following steps shown in Fig. 2：
(1) it keeps temperature in autoclave body 1 to keep the temperature 1~3h at 140~180 DEG C, nylon is made to be completely dissolved；
(2) opening controlling valve 4 adjust retort gas flow, make retort gas outflow out of autoclave body 1, to reduce autoclave body 1
Interior temperature, until temperature on-line monitoring device 3 shows that temperature is reduced to nylon crystallization temperature for the first time in autoclave body 1；
(3) increase retort gas flow within the scope of 9.5~15.8L/min, temperature on-line monitoring device 3 shows autoclave body 1
Interior temperature is reduced to nylon crystallization temperature for the second time；
(4) retort gas flow is adjusted within the scope of 3.2~12.6L/min, until temperature is down to the boiling point of solvent or less；
(5) closing control valve 4, cooled to room temperature discharging.
The adjusting of retort gas flow passes through the digital regulated realization of flow control panel of gas flow controller 5, step
(2) the adjusting retort gas flow preferably adjusts retort gas flow within the scope of 3.2~9.5L/min, makes cooling rate control
System is within the scope of 20~60 DEG C/h.Step (2) purpose is to make the cooling velocity drop of system as required to control distillation speed
Temperature controls nucleation process；When being added without heterogeneous nucleation agent, homogenous nucleation process, the nucleus of the slower formation of cooling velocity occurs
More, then powder is thinner, therefore can suitably slow down distillation speed；Process is controlled for nucleus growth when there are heterogeneous nuclei, it is cold
But nuclei growth process occurs if speed is slower when temperature is higher, then powder diameter is bigger, therefore can increase distillation speed
Degree, while ensure that process efficiency.
Step (3), which adjusts retort gas flow, makes cooling rate within the scope of 60~100 DEG C/h.In step (3), pass through gas
Body flow controller increases gas mass flow, accelerates distillation speed, can take away crystallization when nylon Precipitation in time
Heat, reduce temperature increases the adverse effect brought to powder geometrical morphology again, ensure that the regularity of nylon powder pattern
With the controllability of grain size.The moment observes temperature variations in step (3) temperature-fall period, makes temperature by adjusting retort gas flow
Degree gos up to be no more than 0.5 DEG C.
Step (4), which adjusts retort gas flow, makes cooling rate within the scope of 20~80 DEG C/h.According to specific distillation speed
Degree cooling is that the particle size of product powder is controlled with this in order to control the growth process of nucleus.
Nylon be PA12, PA11, PA6, PA66, PA610, PA612, PA1010, PA1012 and PA1212 in one kind and
It is a variety of.
The present invention prepares selective laser sintering (SLS) nylon powder by using solvent precipitation, especially by one kind
The method that cools is distilled, takes away crystallization enthalpy when nylon precipitation, the cooling velocity of control system temperature, guarantee system temperature rapidly
The uniformity of degree prepares the nylon powder that grain size is suitable, pattern is regular, bulk density is high to meet the need of 3D printing technique
It asks.
The solvent of the solvent precipitation distillation crystallisation by cooling method selection of the present invention is ethyl alcohol, due to mole gasification of ethyl alcohol
Enthalpy is very big (being 4.26KJ/mol under 78 DEG C of equilibrium conditions), and when evaporation can absorb a large amount of heat, and the present invention is with vigorous stirring
The phenomenon that distillation is not in topical hypothermia, and the opposite stable and uniform of autoclave body temperature can be maintained, and by controlling boil-off gas
The method of body flow realizes the cooling rate of control system, can take away crystallization enthalpy when Buddhist nun's precipitation in time, reduce temperature in the kettle
Go up.
Heat sink of the present invention uses high temperature and high pressure gas mass flow controller (MFC), can be for gas
Mass flow carry out accurate measurement and control, to control distillation speed, achieve the purpose that control system cooling rate in kettle,
And it ensure that system temperature uniformity；In temperature-fall period, when soon close to the crystallization temperature of nylon, distillation can be suitably increased
Speed takes away crystallization heat in time, to reduce the rise amplitude of temperature.Heat sink of the present invention uses reception dress
It sets, the solvent recovery of distillation can be recycled, to save resource and not can cause environmental pollution.It is described through the invention
Heat sink and cool-down method can prepare the subsphaeroidal Buddhist nun that particle size is controllable, pattern is regular, good fluidity, bulk density are high
Imperial powder is very suitable for powdering and the forming of SLS.
It is embodiment below：
As shown in Figure 1, a kind of solvent precipitation prepares the distillation cooling device of SLS nylon powders, including autoclave body
1, agitating device 2, temperature on-line monitoring device 3, control valve 4, gas flow controller 5, condenser 6,7 and of gas buffer
Gas reception device 8；
Autoclave body 1 is equipped 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 in 0~1000r/min ranges as needed.
Temperature on-line monitoring device 3 includes temperature sensor 31, conducting wire 32, digital display temperature meter 33, and temperature sensor 31 is set
Inside autoclave body 1, it is connect with the digital display temperature meter 33 set on 1 top of autoclave body by conducting wire 32.
Control valve 4 is equipped at 1 top vent pipe of autoclave body, for controlling the switch of distillation process, control valve 4 preferably passes through company
It connects bend pipe to connect with the gas flow controller 5 being transversely mounted, for controlling the gas flow in autoclave body.
Gas flow controller 5 is high temperature and high pressure gas mass flow controller MFC comprising flow sensor, flow
Regulating valve, amplification control circuit and current divider control channel have accurate measurement function and automatically control the function of gas flow.
Gas flow controller 5 connects condenser 6, and condenser 6 is equipped with coolant inlet 61 and cooling liquid outlet 62, cooling
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 for the retort gas condensing recovery in autoclave body 1, gas buffer dress
It sets 7 and is used for gas buffer and gas-liquid separation, it can partially recycled solvent.The installation direction of condenser 6 has certain with horizontal direction
Angle, and be less than close to one end of the gas flow controller 5 close to one end of the gas buffer 7, convenient for that will steam
The condensed solvent recovery of vapour, the setting of coolant inlet 61 are arranged in low side, cooling liquid outlet 62 high-end.
Gas buffer 7 includes gas feed 71, gas vent 72, safety valve 73, pressure gauge 74, leakage fluid dram 75.Gas
The setting of body entrance 71 increases in low and middle-end, the setting of gas vent 72 in middle and high end, fluid cross-section product, and gas velocity reduces, and ensures
Outlet pressure not will produce mutation, play 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；Safety valve 73 is equipped with explosion diaphragm, ensure that the safety of surge flask.
Reception device 8 includes tail take over 81, receiver 82 and absorbing liquid 83.Inside 81 immersion absorbing liquid of the tail take over,
Uncooled vapor absorption can be improved the rate of recovery of solvent.
A kind of solvent precipitation preparation SLS nylon powders, first by nylon 12, ethyl alcohol and other additives according to certain
Proportioning be placed in autoclave body 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) before the process of cooling starts, gas is arranged by MFC after 140 DEG C keep the temperature 1 hour after nylon 12
Mass flow be 9.5L/min, make cooling rate control in 60 DEG C/h；
(2) opening controlling valve 4 start to distill the process that cools；
(3) when temperature is dropped to close to 106 DEG C of 12 crystallization temperature of nylon, setting MFC is 15.8L/min, increases gas matter
Flow is measured, distillation speed is accelerated, so that cooling rate control is observed temperature variations in 100 DEG C/h, and moment, makes temperature recovery
No more than 0.5 DEG C；
(4) when temperature uniform descent again, setting MFC is 12.6L/min, and it is 80 DEG C/h to make cooling rate, works as temperature
Closing control valve when being down to 78 DEG C or less.
(5) cooled to room temperature discharges.
Pattern and the particle diameter distribution difference for 12 powder of nylon that the present embodiment is prepared are as shown in Figure 3 and Figure 4, can see
Go out higher nylon powder pattern rule, sphericity, good fluidity, average grain diameter are 54.8 μm and narrow distribution, be very suitable for swashing
Light constituency is sintered.
Embodiment 2
Cooling device is distilled with embodiment 1.
A kind of solvent precipitation preparation SLS nylon powders, first by nylon 11, ethyl alcohol and other additives according to certain
Proportioning be placed in autoclave body 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) before the process of cooling starts, gas is arranged by MFC after 150 DEG C keep the temperature 2.5 hours after nylon 11
The mass flow of body is 6.3L/min, makes cooling rate control in 40 DEG C/h；
(2) opening controlling valve 4 start to distill the process that cools；
(3) when temperature is dropped to close to 110 DEG C of nylon 11 crystallization temperature, setting MFC is 12.6L/min, increases gas matter
Flow is measured, distillation speed is accelerated, so that cooling rate control is observed temperature variations in 80 DEG C/h, and moment, makes temperature recovery
No more than 0.5 DEG C.
(4) when temperature uniform descent again, setting MFC is 9.5L/min, and it is 60 DEG C/h to make cooling rate, when temperature drops
To closing control valve at 78 DEG C or less.
(5) cooled to room temperature discharges.
Embodiment 3
Cooling device is distilled with embodiment 1.
A kind of solvent precipitation preparation SLS nylon powders, first by nylon 6, ethyl alcohol and other additives according to certain
Proportioning be placed in autoclave body 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 after 180 DEG C keep the temperature 3 hours, before the process of cooling starts, pass through MFC and gas is set
Mass flow is 3.2L/min, and control cooling rate is in 20 DEG C/h；
(2) opening controlling valve 4 start to distill the process that cools；
(3) when temperature is dropped to close to 120 DEG C of 6 crystallization temperature of nylon, setting MFC is 9.5L/min, increases gaseous mass
Flow, accelerates distillation speed, and control cooling rate observes temperature variations in 60 DEG C/h, and moment, temperature recovery is made not surpass
Cross 0.5 DEG C.
(4) when temperature uniform descent again, setting MFC is 3.2L/min, and it is 20 DEG C/h to make cooling rate, when temperature drops
To closing control valve at 78 DEG C or less.
(5) cooled to room temperature discharges.
Specific embodiment list:
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement etc., should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of distillation cooling device of SLS nylon powders, which is characterized in that the cooling device includes autoclave body
(1), control valve (4), gas flow controller (5), condenser (6), gas buffer (7) and gas reception device (8)；
The autoclave body (1) is equipped with agitating device (2) and temperature on-line monitoring device (3)；
Control valve (4), the control valve (4) and the gas flow controller (5) are equipped at autoclave body (1) the top vent pipe
It is connected, the control valve (4) and the gas flow controller (5) are used to control the gas flow in autoclave body (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 set for by the retort gas condensing recovery in autoclave body (1), the gas buffer (7) to be used for gas buffer and part
Gas recycles.
2. distillation cooling device as described in claim 1, which is characterized in that the gas flow controller (5) is height
Warm high pressure gas mass flow controller (MFC).
3. as described in claim 1 distillation cooling device, which is characterized in that the installation direction of the condenser (6) with
Horizontal direction has certain angle, and is less than close to one end of the gas buffer (7) and is controlled close to the gas flow
One end of device (5).
The method 4. a kind of distillation of SLS nylon powders cools, which is characterized in that include the following steps：
(1) it keeps kettle body temperature between 140~180 DEG C, keeps the temperature 1~3h, nylon is made to be completely dissolved；
(2) opening controlling valve adjusts retort gas flow, retort gas is made to be flowed out out of autoclave body, to reduce kettle body temperature,
Until temperature on-line monitoring device shows that temperature is reduced to nylon crystallization temperature for the first time in autoclave body；
(3) increase retort gas flow within the scope of 9.5~15.8L/min, until temperature on-line monitoring device is shown in autoclave body
Temperature is reduced to nylon crystallization temperature for the second time；
(4) retort gas flow is adjusted within the scope of 3.2~12.6L/min, until temperature on-line monitoring device is shown in autoclave body
Temperature is down to solvent boiling point or less；
(5) closing control valve, cooled to room temperature discharging.
The method 5. distillation as claimed in claim 4 cools, which is characterized in that the adjusting of the retort gas flow passes through
The flow control panel of gas flow controller is digital regulated to be realized.
The method 6. distillation as claimed in claim 5 cools, which is characterized in that step (2) adjusts retort gas flow and exists
Within the scope of 3.2~9.5L/min, make cooling rate control within the scope of 20~60 DEG C/h.
The method 7. distillation as claimed in claim 4 cools, which is characterized in that step (3) the adjusting retort gas stream
Amount makes cooling rate within the scope of 60~100 DEG C/h.
The method 8. distillation as claimed in claim 4 cools, which is characterized in that the moment is observed in step (3) temperature-fall period
Temperature variations make temperature recovery be no more than 0.5 DEG C by adjusting retort gas flow.
The method 9. distillation as claimed in claim 4 cools, which is characterized in that step (4) the adjusting retort gas stream
Amount makes cooling rate within the scope of 20~80 DEG C/h.
The method 10. distillation as claimed in claim 4 cools, which is characterized in that the nylon is PA12, PA11, P A6,
It is one or more in PA66, PA610, PA612, PA1010, PA1012 and PA1212.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611236188.5A CN106671416B (en) | 2016-12-28 | 2016-12-28 | A kind of the distillation cooling device and cool-down method of SLS nylon powders |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611236188.5A CN106671416B (en) | 2016-12-28 | 2016-12-28 | A kind of the distillation cooling device and cool-down method of SLS nylon powders |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106671416A CN106671416A (en) | 2017-05-17 |
| CN106671416B true CN106671416B (en) | 2018-08-21 |
Family
ID=58871851
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611236188.5A Active CN106671416B (en) | 2016-12-28 | 2016-12-28 | A kind of the distillation cooling device and cool-down method of SLS nylon powders |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106671416B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111231308A (en) * | 2020-03-02 | 2020-06-05 | 温州医科大学附属第二医院、温州医科大学附属育英儿童医院 | Novel 3D printer |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102563984A (en) * | 2012-01-16 | 2012-07-11 | 张家港市金腾化工机械制造有限公司 | Cooling controlling device for condenser |
| CN104163929B (en) * | 2014-07-11 | 2017-07-18 | 东莞方易达三维科技有限公司 | A kind of 3D printing preparation method of macromolecule nylon dusty material |
| CN104497323B (en) * | 2014-12-17 | 2017-02-22 | 湖南华曙高科技有限责任公司 | Preparation method of nylon powder for selective laser sintering |
| EP3302937A1 (en) * | 2015-05-27 | 2018-04-11 | Stratasys, Inc. | Semi-crystalline build materials and methods of manufacturing three dimensional part |
| CN105694068B (en) * | 2016-04-22 | 2017-07-21 | 广东银禧科技股份有限公司 | A kind of polyamide powder and preparation method thereof |
-
2016
- 2016-12-28 CN CN201611236188.5A patent/CN106671416B/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111231308A (en) * | 2020-03-02 | 2020-06-05 | 温州医科大学附属第二医院、温州医科大学附属育英儿童医院 | Novel 3D printer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106671416A (en) | 2017-05-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101226732B1 (en) | Method for producing optical fiber | |
| CN106671416B (en) | A kind of the distillation cooling device and cool-down method of SLS nylon powders | |
| US20190194070A1 (en) | Method for expansion of sand grain-shaped raw material | |
| CN103387235B (en) | Polycrystalline silicon rod and process for production thereof | |
| US9878945B2 (en) | Method for expanding raw material in the form of sand grains | |
| CN104897358B (en) | A kind of experimental provision occurred applied to moisture film with measuring | |
| CN112517918A (en) | Preparation method and production equipment of high-sphericity gas atomized powder | |
| TW201446729A (en) | Nylon salt solution preparation processes with trim diamine | |
| US11511488B2 (en) | Device for producing three-dimensional objects layer by layer | |
| CN104793650A (en) | Method for reducing reject rate in oil furnace method charcoal black production | |
| CN105659359A (en) | Continuous-distillation-type trichlorosilane vaporization supply device and continuous-distillation-type trichlorosilane gas vaporization method | |
| CN104120407A (en) | Liquid raw material vaporization supply device for chemical vapor phase deposition and use method thereof | |
| CN105668999A (en) | Technology of directly producing low-hydroxyl quartz tube | |
| CN203833855U (en) | VK tube type reactor for polymerizing polyamide | |
| CN110666126B (en) | Method for stabilizing convection heat exchange coefficient of crystallizer copper plate cooling water | |
| KR20160051845A (en) | Granulation of molten material | |
| CN115509266A (en) | Control device and control method for adjusting melt flow through rapid reaction and application of control device and control method | |
| US8465680B2 (en) | Method for pelleting spherical fine particle of sodium nitrate | |
| CN104607642A (en) | Atomizing chamber cooling circulation system and method adopting system to cool atomizing chamber | |
| CN105129740B (en) | A kind of wet-method sulfur forming equipment and its moulding process | |
| CN211101488U (en) | System for stabilizing convection heat exchange coefficient of crystallizer copper plate cooling water | |
| CN208879672U (en) | A kind of Real-time Water cold flow amount control system | |
| CN106820989B (en) | Milk maker | |
| CN104526837A (en) | Device for preparing ceramic microspheres | |
| CN214193015U (en) | Feeding device suitable for basalt fiber production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |