CN110158161A - Uniform sticking/defoaming integrated device and method for ceramic precursor polymer spinning melt - Google Patents
Uniform sticking/defoaming integrated device and method for ceramic precursor polymer spinning melt Download PDFInfo
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- CN110158161A CN110158161A CN201910373877.8A CN201910373877A CN110158161A CN 110158161 A CN110158161 A CN 110158161A CN 201910373877 A CN201910373877 A CN 201910373877A CN 110158161 A CN110158161 A CN 110158161A
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- deaeration
- umbrella shape
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/06—Feeding liquid to the spinning head
- D01D1/065—Addition and mixing of substances to the spinning solution or to the melt; Homogenising
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/06—Feeding liquid to the spinning head
- D01D1/09—Control of pressure, temperature or feeding rate
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/10—Filtering or de-aerating the spinning solution or melt
- D01D1/103—De-aerating
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- Mechanical Engineering (AREA)
- Textile Engineering (AREA)
- Degasification And Air Bubble Elimination (AREA)
- Inorganic Fibers (AREA)
Abstract
An integrated device and a method for uniform sticking/defoaming of a ceramic precursor polymer spinning melt. The device comprises a defoaming kettle body, wherein a feeding metering pump is arranged on the upper part of the defoaming kettle body or on the upper cover of the kettle body, a spinning metering pump is arranged at the bottom of the defoaming kettle body, a first umbrella-shaped flow guide surface, a second anti-umbrella-shaped flow guide surface, a third umbrella-shaped flow guide surface and a fourth flow guide uniform-temperature arc surface are sequentially arranged in an inner cavity of the defoaming kettle from top to bottom, and a first overflow seam and a second overflow seam are arranged at the joints of the first umbrella-shaped flow guide surface and the second anti-umbrella-shaped flow guide surface and the inner wall of the defoaming kettle body respectively. The invention also comprises a method for homoclination/defoaming by using the homoclination/defoaming integrated device of the ceramic precursor polymer spinning melt. The invention separates the bubbles in the spinning melt completely, realizes uniform temperature and uniform viscosity of the melt, improves the defoaming efficiency and the viscosity uniformity of the melt, avoids the interruption, deformation and fiber fracture of the spinning trickle in the spinning process, reduces the protofilament dimension defect and improves the performance of the finished ceramic fiber.
Description
Technical field
The invention belongs to fiber preparation fields, and in particular to a kind of particular for Preceramic Polymers spinning melt
The device and method of viscous/deaeration one.
Background technique
Continuous SiC fiber, Si3N4The high performance continuous ceramic fibers such as fiber, SiBN (C) fiber due to its with high temperature resistant,
The features such as high-intensitive, high-modulus and special electromagnetic property is the key raw material of the fields such as aerospace military affairs application.Pioneer
Body conversion method is the common method for preparing high-performance continuous ceramic fiber, step be first synthesize Polycarbosilane, Polycarbosilane and
The Preceramic Polymers such as polysilazane, then through melt spinning, non-fusible and high temperature pyrolysis, it is fine that continuous ceramics can be prepared
Dimension.
The melt spinning of Preceramic Polymers is the committed step for preparing continuous ceramic fiber, because its fibrinogen
Quality is the key that determine finally continuous Properties of Ceramic Fiber.Under normal conditions, Preceramic Polymers are a kind of viscous temperature sensitives
The higher material of property, that is to say, that small temperature change is likely to vary widely its viscosity, so, when spinning
Wish that polymer melt temperature (back abbreviation samming) impartial as far as possible only in this way just can guarantee polymer melt at every place
Viscosity it is consistent, be conducive to fiberizing and improve the quality of precursor.
On the other hand, spinning melt can have a bubble in heating melting and (or) transmission process, in preceramic polymer
Existing small molecule part, can also generate part bubble during high-temperature fusion, and biggish bubble will cause by spinneret orifice
The interruption and deformation of dynamic analysis of spinning.Lesser bubble can remain in the fibre although it is possible to not make fibrous fracture, cause original
Silk dimension defect, the final defect can be inherited in ceramic fibre, the final intensity for influencing finished product ceramic fibre.So spinning is molten
Body is before entering spinning pack, it is necessary to the thoroughly bubble and nubbin small molecule in abjection melt.But since spinning is molten
The viscosity of body is big, and bubble abjection acquires a certain degree of difficulty.
Currently, general add the method suitably depressurized using raising temperature, the spinning melt for making to rest in molten-bath is slow
Deaeration.After temperature increases, melt viscosity decline is conducive to micro-molecular gas evolution.Decompression can be reduced liquid level and hydraulic internal difference, have
Conducive to small molecule and the extruding of bubble, diffusion abjection.Obviously, this method deaeration low efficiency, production capacity is not high, can not make
Melt realizes uniform thorough deaeration.On the other hand, since molten-bath volume is larger, heating is usually the heating agent outside kettle wall
Or electric heating body is completed, turn heat is to be transmitted to autoclave body center by kettle wall, is bound to cause internal and external temperature difference, the temperature of melt in this way
Homogeneity is poor, inadequate so as to cause the viscosity homogeneity of melt, adversely affects, makes under precursor quality to fibre spinning
Drop.
Summary of the invention
The technical problem to be solved by the present invention is to overcome drawbacks described above of the existing technology, provide a kind of deaeration and
The device and method of viscous/deaeration one of the good Preceramic Polymers spinning melt of temp effect.
The technical solution adopted by the present invention to solve the technical problems is:
Preceramic Polymers spinning melt glues/deaeration integrated device, including deaeration autoclave body, sets at the top of deaeration autoclave body
There is autoclave body upper cover, the closed cavity that the inner wall of deaeration autoclave body and the lower surface of autoclave body upper cover surround is deaeration kettle inner cavity, deaeration
The top of autoclave body or autoclave body upper cover are pumped equipped with fuel gauge, and the bottom of deaeration autoclave body is equipped with spinning pump, deaeration kettle inner cavity
In to be disposed with No.1 umbrella shape guide face, No. two anti-umbrella shape guide faces, No. three umbrella shape guide faces, No. four water conservancy diversion from top to bottom equal
Warm arcwall face, No.1 umbrella shape guide face, No. two anti-umbrella shape guide faces, No. three umbrella shape guide faces connect with the inner wall of deaeration autoclave body
It connects, the junction of No.1 umbrella shape guide face and deaeration inner wall of kettle is stitched equipped with the first overflow, the center of No. two anti-umbrella shape guide faces
Equipped with hole is collected, collection hole is through-hole, and the junction of No. three umbrella shape guide faces and deaeration inner wall of kettle is stitched equipped with the second overflow, four
Number water conservancy diversion samming arcwall face is the arc inner wall face of deaeration autoclave body lower part；No.1 umbrella shape guide face, No. two anti-umbrella shape guide faces, three
Number umbrella shape guide face and No. four water conservancy diversion samming arcwall faces are with the central axes bilateral symmetry of deaeration autoclave body.
Further, inert atmosphere is installed on lid on autoclave body and enters pipe and the first vacuum connection tube, inert atmosphere enters pipe and the
Valve is respectively arranged on one vacuum connection tube, inert atmosphere enters the external inert atmosphere storage tank in one end of pipe, and inert atmosphere enters the another of pipe
One end is connected to deaeration kettle inner cavity, and the other end of the external vacuum system in one end of the first vacuum connection tube, the first vacuum connection tube connects
Unconventional bubble kettle inner cavity.
Further, heating agent inner cavity between the inner wall of deaeration autoclave body and the outside wall surface of deaeration autoclave body, heating agent inner cavity is with deaeration
The central axes bilateral symmetry of autoclave body；The top of deaeration autoclave body is equipped with the heating agent entrance that is connected to heating agent inner cavity, under deaeration autoclave body
Portion is equipped with the heating agent outlet being connected to heating agent inner cavity, and the outside wall surface periphery of deaeration autoclave body is equipped with insulating layer, heating agent entrance and heating agent
Outlet runs through insulating layer.
Further, the first snorkel is housed, the upper end of the first snorkel extend out to No.1 umbrella shape on No.1 umbrella shape guide face
The top of guide face, the lower end of the first snorkel extend out to the top of No. two anti-umbrella shape guide faces；It is filled on No. three umbrella shape guide faces
There is the second snorkel, the upper end of the second snorkel extend out to the top of No. three umbrella shape guide faces, and the lower end of the second snorkel is protruded into
In the space that No. four water conservancy diversion samming arcwall faces surround；
Deaeration autoclave body is equipped with the second vacuum connection tube and third vacuum connection tube, the second vacuum connection tube and third bonding in vacuum
Pipe is symmetrically set in the central axes two sides of deaeration autoclave body, and the upper end of the second vacuum connection tube and the upper end of third vacuum connection tube are stretched
Three are extend out to the top of No.1 umbrella shape guide face, the upper end of the second vacuum connection tube and the lower end of third vacuum connection tube out
The top of number umbrella shape guide face.
Viscous/deaeration is carried out using viscous/deaeration integrated device of Preceramic Polymers spinning melt as previously described
Method, include the following steps:
Step 1, the heating agent entrance of viscous/deaeration integrated device and the heating agent of the heating agent circulatory system are exported and is connected, viscous/deaeration
The heating agent outlet of integrated device is connect with the heating agent entrance of the heating agent circulatory system, and the heating agent circulatory system is existing mature system, root
Heat medium temperature is set according to the softening point to spinning polymer, heat medium temperature is 80 DEG C higher than the softening point to spinning polymer~and 120 DEG C；It opens
The dynamic heating agent circulatory system keeps the temperature 1-4 hours, and heating agent flows into heating agent inner cavity through heating agent entrance, and holding temperature is equal to heat medium temperature；
By the external vacuum system of the first vacuum connection tube of viscous/deaeration integrated device, the valve on the first vacuum connection tube is opened
Door opens vacuum system, when the vacuum degree in the deaeration kettle inner cavity of viscous/deaeration integrated device is -70kPa~-85kPa
When, close the valve on the first vacuum connection tube；Inert atmosphere is entered into the external inert atmosphere storage tank of pipe, inert atmosphere is opened and enters pipe
On valve, be filled with inert gas into deaeration kettle inner cavity, the rate that is filled with of inert gas is 1-10L/min, according to deaeration kettle
The volume of inner cavity and the rate that is filled with of inert gas are acquired full of the time needed for inert gas in deaeration kettle inner cavity, when deaeration kettle
When being full of inert gas in inner cavity, the valve that is again turned on the first vacuum connection tube；Inert atmosphere, which enters pipe, to be continued to deaeration kettle
It is filled with inert gas in inner cavity, extra inert gas is flowed out from the first vacuum connection tube in deaeration kettle inner cavity；
Step 2, it feeds.Start fuel gauge pump, is pumped into deaeration kettle inner cavity to spinning polymer melt by fuel gauge；For
Expect that the revolving speed of metering pump is determined according to the revolving speed of spinning pump, the revolving speed of fuel gauge pump and the revolving speed of spinning pump
Match, the fast 3%-7% of revolving speed of the rotating ratio spinning pump of fuel gauge pump；
Step 3, first order deaeration.Spinning melt is that melting in deaeration kettle inner cavity to spinning polymer is pumped by fuel gauge
Body is uniformly spread under the effect of gravity on No.1 umbrella shape guide face, formed 0.5 mm -3.5mm(be preferably 1.5mm~
Film 2.0mm), melt is in the flowing booth membrane process on No.1 umbrella shape guide face, since polymer melt is thinning, melt
In micro-molecular gas and part bubbles burst and realize first order deaeration.
Step 4, second level deaeration.The melt flowed down from No.1 umbrella shape guide face, through No.1 umbrella shape guide face and deaeration
The first overflow seam of inner wall of kettle junction flows down, and after flowing through kettle wall, flows directly into No. 2 reversed umbrella shape water conservancy diversion and faces the wall and meditates, forms 0.5
Mm -3.5mm(is preferably 1.5mm~2.0mm) thick film, flowing of the melt on No. two anti-umbrella shape guide faces spread out film mistake
Cheng Zhong, remaining micro-molecular gas and part bubbles burst in melt, realizes deaeration again, this is second level deaeration.
Step 5, third level deaeration.The melt flowed down from No. two anti-umbrella shape guide faces, through in No. two anti-umbrella shape guide faces
The collection hole of the heart flows down, and flows directly into No. three umbrella shape guide faces, and forming 0.5 mm -3.5mm(is preferably 1.5mm~2.0mm)
Thick film, melt is in the flowing booth membrane process on No. three umbrella shape guide faces, remaining micro-molecular gas and part in melt
Bubbles burst realizes deaeration again, this is third level deaeration.
No.1 umbrella shape guide face, No. two anti-umbrella shape guide faces and No. three umbrella shape guide faces are mainly used for deaeration, subsidiary simultaneously
Samming effect.In first order deaeration, second level deaeration and third level de-aeration, melt flows separately through No.1 umbrella shape water conservancy diversion
When face, No. two anti-umbrella shape guide faces and No. three umbrella shape guide faces, since the symmetry of autoclave body (specifically refers to No.1 umbrella shape water conservancy diversion
Face, No. two anti-umbrella shape guide faces and No. three umbrella shape guide faces with the central axes of deaeration autoclave body bilateral symmetry and heating agent inner cavity with
The central axes bilateral symmetry of deaeration autoclave body), it is led hence for No.1 umbrella shape guide face, No. two anti-umbrella shape guide faces and No. three umbrella shapes
Stream interface, it is consistent with the heat transfer distances between the heating agent in heating agent inner cavity in each point on same level section, thus No.1 umbrella shape
The temperature of each point on the same level section of guide face is consistent, each point on the same level section of No. two anti-umbrella shape guide faces
Temperature, No. three umbrella shape guide faces same level section on each point temperature it is consistent, so, melt is in No.1 umbrella shape water conservancy diversion
In the flowing booth membrane process in face, No. two anti-umbrella shape guide faces and No. three umbrella shape guide faces, the heated scoring path of solution is identical, same water
The heating temperature of solution on plane section is also identical, to realize during first order deaeration to the third level is steeped
Temperature.
Step 6, samming+fourth stage deaeration.It is same that No. four water conservancy diversion samming arcwall faces increase the volume of deaeration kettle inner cavity
When, heat build-up area is increased, thus No. four water conservancy diversion samming arcwall faces are mainly used for samming and glue, while subsidiary deaeration effect.From
The melt flowed down on No. three umbrella shape guide faces, the second overflow through No. three umbrella shape guide faces and deaeration inner wall of kettle junction, which is stitched, flows
Under, No. four water conservancy diversion samming arcwall faces are flowed directly into, when solution flows through No. four big water conservancy diversion samming arcwall faces of heat build-up area, due to kettle
The symmetry of body (specifically refers to No. four water conservancy diversion samming arcwall faces with the central axes bilateral symmetry of deaeration autoclave body and heating agent inner cavity
With the central axes bilateral symmetry of deaeration autoclave body) so that each point of No. four water conservancy diversion samming arcwall faces on same level section and heat
The heat transfer distances between heating agent in matchmaker inner cavity are consistent, thus each point on the same level section of No. four water conservancy diversion samming arcwall faces
Temperature it is also consistent, so, melt is in the flowing booth membrane process of No. four water conservancy diversion samming arcwall faces, No. four water conservancy diversion samming arcwall faces
On solution heated scoring path it is identical, the heating temperature of the solution on same level section is also identical, and since No. four water conservancy diversion are equal
The heat build-up area of warm arcwall face is big, so melt is able to achieve in the flowing booth membrane process of No. four water conservancy diversion samming arcwall faces than first
The grade deaeration even temperature effect good to third level de-aeration；
The solution for flowing into No. four water conservancy diversion samming arcwall faces, it is preferred on No. four water conservancy diversion samming arcwall faces to form 0.5 mm -3.5mm(
For the film of 1.5mm~2.0mm) thickness, melt is in the flowing booth membrane process on No. four water conservancy diversion samming arcwall faces, in melt
Remaining micro-molecular gas and part bubble rupture again, realize deaeration again, this is fourth stage deaeration.
In the step 3, it is further excellent that spinning melt forms 1.5mm~2.0mm(on No.1 umbrella shape guide face (3)
It is selected as 1.8mm) thick film；In the step 4, melt forms 1.5mm~2.0mm on No. 2 reversed umbrella shape guide faces (4)
The film of (further preferably 1.8mm) thickness；In the step 5, melt forms 1.5mm on No. three umbrella shape guide faces (5)
~2.0mm(is more preferably 1.8mm) thick film；In the step 6, solution is on No. four water conservancy diversion samming arcwall faces (6)
Forming 1.5mm~2.0mm(is more preferably 1.8mm) thick film, in favor of obtaining preferable deaeration effect and
Preferable deaeration efficiency (the spinning solution amount of deaeration is completed in the unit time) is had both while temp effect.
By the rate of control fuel gauge pump, spinning melt can control in each umbrella shape guide face, anti-umbrella shape water conservancy diversion
Fluid thickness on face and water conservancy diversion samming arcwall face.
Melt is during first order deaeration, second level deaeration, third level deaeration and fourth stage deaeration, due to No.1 umbrella
Shape guide face, No. two anti-umbrella shape guide faces, No. three umbrella shape guide faces and No. four water conservancy diversion samming arcwall faces are in deaeration autoclave body
Axis bilateral symmetry and heating agent inner cavity are with the central axes of deaeration autoclave body bilateral symmetry, so course that melt flows through and heated
Course it is consistent, thus the shear history of melt is identical；And the viscosity of melt is determined by temperature and shear history, so, melt
Samming through No.1 umbrella shape guide face, No. two anti-umbrella shape guide faces, No. three umbrella shape guide faces and No. four water conservancy diversion samming arcwall faces with
And after identical shear history, melt is when No. four water conservancy diversion samming arcwall faces flow out into spinning pump, the temperature of melt
With viscosity be it is impartial (it is be into the temperature of the solution of spinning pump identical, into spinning pump solution it is viscous
Degree is also identical).That is, while realizing deaeration, also having synchronously completed melt after the flowing of step 3- step 6
Viscous process.So far, melt is after the process of above first order deaeration to fourth stage deaeration, while realizing polymerization
The viscous and deaeration of object melt.
Step 7, start spinning pump, melt enters the spinning pump of deaeration autoclave body bottom, then through spinning pump
It is pumped into filament spinning component, starts spinning.
The junction of No.1 umbrella shape guide face and deaeration inner wall of kettle is equipped with the first overflow and stitches, No. three umbrella shape guide faces with take off
The junction for steeping inner wall of kettle is stitched equipped with the second overflow, is specifically shown in attached drawing 2, it is ensured that autoclave body heat is transmitted to the same of corresponding guide face
When, melt can flow into next guide face in the form of a film.
First snorkel, the second snorkel, the second vacuum connection tube and third vacuum connection tube purpose be to ensure that
It can be connected everywhere with vacuum in kettle, and ensure that inert gas can be filled in kettle everywhere, it is ensured that small molecule and bubble can have
Effect discharge.
The beneficial effects of the present invention are: the present invention substitutes existing stirring vacuum foam removing method, (i.e. by 4 grades of deaerations
First order deaeration, second level deaeration, third level deaeration, fourth stage deaeration) and level Four samming (i.e. first order deaeration is de- to the fourth stage
Samming during bubble), while the bubble in Preceramic Polymers spinning melt being detached from clean, realize melt
Samming is viscous, improves deaeration efficiency and melt viscosity homogeneity, can effectively avoid the dynamic analysis of spinning in subsequent spinning process
Interruption, deformation and fibrous fracture reduce precursor dimension defect, effectively improve the performance of finished product ceramic fibre.It is filled in deaeration autoclave body
Enter inert gas to be conducive to that melt is avoided to chemically react with the oxygen in air.
Detailed description of the invention
Fig. 1 is the section structure signal of viscous/deaeration integrated device of Preceramic Polymers spinning melt of the present invention
Figure.
Fig. 2 is the equal top view of the No.1 umbrella shape guide face of viscous/deaeration integrated device and autoclave body connecting place shown in Fig. 1.
In figure: 1, deaeration autoclave body；10, heating agent entrance；11, heating agent exports；2, autoclave body upper cover；21, inert atmosphere enters pipe；
22, the first vacuum tube；23, fuel gauge pumps；3, No.1 umbrella shape guide face；31, the first snorkel；4, No. two anti-umbrella shape water conservancy diversion
Face；5, No. three umbrella shape guide faces；51, the second snorkel；6, No. four water conservancy diversion samming arcwall faces；61, the second vacuum connection tube；62,
Third vacuum connection tube；63, spinning pump；100, deaeration kettle inner cavity；200, heating agent inner cavity；7, insulating layer.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, with reference to the accompanying drawing and specific embodiment party
Present invention is further described in detail for formula.
Embodiment 1:
Referring to Fig.1, viscous/deaeration integrated device, including deaeration autoclave body 1 of Preceramic Polymers spinning melt, deaeration kettle
The top of body 1 is equipped with autoclave body upper cover 2, and the closed cavity that the inner wall of deaeration autoclave body 1 and the lower surface of autoclave body upper cover 2 surround is de-
Kettle inner cavity 100 is steeped, the top of deaeration autoclave body 1 or autoclave body upper cover 2 are equipped with fuel gauge pump 23, and the bottom of deaeration autoclave body 1 is equipped with
Spinning pump 63 is disposed with 3, No. two anti-umbrella shape water conservancy diversion of No.1 umbrella shape guide face in deaeration kettle inner cavity 100 from top to bottom
5, No. four water conservancy diversion samming arcwall faces 6 of umbrella shape guide face of face 4, three, No.1 umbrella shape guide face 3, two anti-umbrella shape guide faces 4, three
Number umbrella shape guide face 5 is connect with the inner wall of deaeration autoclave body 1, and No.1 umbrella shape guide face 3 and the junction of 1 inner wall of deaeration autoclave body are set
There is the first overflow to stitch 8, the center of No. two anti-umbrella shape guide faces 4, which is equipped with, collects hole, and collection hole is through-hole, No. three umbrella shape guide faces 5
The second overflow is equipped with the junction of 1 inner wall of deaeration autoclave body and stitches (not shown), and No. four water conservancy diversion samming arcwall faces 6 are deaeration kettle
The arc inner wall face of 1 lower part of body；4, No. three umbrella shape guide faces 5 of No.1 umbrella shape guide face 3, two anti-umbrella shape guide faces and No. four are led
Samming arcwall face 6 is flowed with the central axes bilateral symmetry of deaeration autoclave body 1.
In the present embodiment, inert atmosphere is installed in autoclave body upper cover 2 and enters pipe 21 and the first vacuum connection tube 22, inert atmosphere
Enter and be respectively arranged with valve on pipe 21 and the first vacuum connection tube 22, inert atmosphere enters the external inert atmosphere storage tank in one end of pipe 21, lazy
Property atmosphere enter pipe 21 the other end connection deaeration kettle inner cavity 100, the external vacuum system in one end of the first vacuum connection tube 22, first
The other end of vacuum connection tube 22 is connected to deaeration kettle inner cavity 100.
In the present embodiment, heating agent inner cavity 200 between the inner wall of deaeration autoclave body 1 and the outside wall surface of deaeration autoclave body 1, in heating agent
Chamber 200 is with the central axes bilateral symmetry of deaeration autoclave body 1；The top of deaeration autoclave body 1 is equipped with the heating agent being connected to heating agent inner cavity 200 and enters
Mouth 10, the lower part of deaeration autoclave body 1 are equipped with the heating agent outlet 11 being connected to heating agent inner cavity 200, and the outside wall surface periphery of deaeration autoclave body 1 is set
There is insulating layer 7, heating agent entrance 10 and heating agent outlet 11 run through insulating layer 7.
In the present embodiment, the first snorkel 31 is housed, the upper end of the first snorkel 31 is extend out on No.1 umbrella shape guide face 3
The top of No.1 umbrella shape guide face 3, the lower end of the first snorkel 31 extend out to the top of No. two anti-umbrella shape guide faces 4；No. three umbrellas
Second snorkel 32 is housed on shape guide face 5, the upper end of the second snorkel 32 extend out to the top of No. three umbrella shape guide faces 5, the
The lower end of two snorkels 32 is protruded into the space that No. four water conservancy diversion samming arcwall faces 6 surround；
Deaeration autoclave body 1 is equipped with the second vacuum connection tube 61 and third vacuum connection tube 62, the second vacuum connection tube 61 and third
Vacuum connection tube 62 is symmetrically set in the central axes two sides of deaeration autoclave body 1, and the upper end of the second vacuum connection tube 61 and third vacuum connect
The upper end of adapter tube 62 extend out to the top of No.1 umbrella shape guide face 3, and the upper end of the second vacuum connection tube 61 and third vacuum connect
The lower end of adapter tube 62 extend out to the top of No. three umbrella shape guide faces 5.
Viscous/deaeration is carried out using viscous/deaeration integrated device of Preceramic Polymers spinning melt as previously described
Method, include the following steps:
In the present embodiment, the melt to deaeration is the preceramic polymer Polycarbosilane (PCS) of silicon carbide fibre, and softening point is
230℃。
Step 1, the heating agent entrance 10 of viscous/deaeration integrated device and the heating agent of the heating agent circulatory system are exported and is connected,
The heating agent outlet 11 of viscous/deaeration integrated device is connect with the heating agent entrance of the heating agent circulatory system, according to the softening to spinning polymer
Point setting heat medium temperature, sets heat medium temperature as 330 DEG C；Start the heating agent circulatory system and keep the temperature 2 hours, heating agent is through heating agent entrance stream
Enter in heating agent inner cavity, holding temperature is equal to heat medium temperature；
The external vacuum system of the first vacuum connection tube 22 of viscous/deaeration integrated device is opened on the first vacuum connection tube 22
Valve, open vacuum system, when the vacuum degree in the deaeration kettle inner cavity 100 of viscous/deaeration integrated device is -75kPa, close
Close the valve on the first vacuum connection tube 22；Inert atmosphere is entered into the external inert atmosphere storage tank of pipe 21, inert atmosphere is opened and enters pipe
Valve on 21 is filled with inert gas into deaeration kettle inner cavity 100, and it is nitrogen that inert gas, which is specifically selected, in the present embodiment, lazy
Property gas be filled with rate be 5L/min, acquired in deaeration kettle according to the rate that is filled with of the volume of deaeration kettle inner cavity and inert gas
Full of the time needed for inert gas in chamber 100, when being full of inert gas in deaeration kettle inner cavity 100, it is true to be again turned on first
Valve in empty connecting tube 22；Inert atmosphere, which enters pipe, to be continued to be filled with inert gas, deaeration kettle inner cavity into deaeration kettle inner cavity 100
Extra inert gas is flowed out from the first vacuum connection tube 22 in 100；
Step 2, starting fuel gauge pump 23, the speed of fuel gauge pump 23 are 25rpm, pass through feed meter to spinning polymer melt
Amount pump 23 is pumped into deaeration kettle inner cavity 100；
Step 3, spinning melt be pumped by fuel gauge pump 23 in deaeration kettle inner cavity 100 to spinning polymer melt, in weight
It is uniformly spread on No.1 umbrella shape guide face 3 under power effect, forms the film of 1.8mm thickness, melt is on No.1 umbrella shape guide face 3
Flowing booth membrane process in, since polymer melt is thinning, remaining micro-molecular gas and part bubbles burst in melt, realize
First order deaeration；
Step 4, the melt flowed down from No.1 umbrella shape guide face, through No.1 umbrella shape guide face 3 and 1 inner wall junction of deaeration autoclave body
First overflow seam 8 flows down, and after flowing through kettle wall, flows directly into No. 2 reversed umbrella shape guide faces 4, forms the film of 1.8mm thickness, melt
In the flowing booth membrane process on No. two anti-umbrella shape guide faces, remaining micro-molecular gas and part bubbles burst in melt are real
Existing second level deaeration；
Step 5, the melt flowed down from No. two anti-umbrella shape guide faces 4, the collection hole through No. two anti-4 centers of umbrella shape guide face are flowed
Under, No. three umbrella shape guide faces 5 are flowed directly into, the film of 1.8mm thickness, flowing booth of the melt on No. three umbrella shape guide faces 5 are formed
In membrane process, remaining micro-molecular gas and part bubbles burst in melt realize third level deaeration；
No.1 umbrella shape guide face 3, two anti-umbrella shape guide faces 4 and No. three umbrella shape guide faces 5 are mainly used for deaeration, while subsidiary equal
Temperature effect.In first order deaeration, second level deaeration and third level de-aeration, melt flow separately through No.1 umbrella shape guide face 3,
When No. two anti-umbrella shape guide faces 4 and No. three umbrella shape guide faces 5, since the symmetry of autoclave body (specifically refers to No.1 umbrella shape guide face
3, No. two anti-umbrella shape guide faces 4 and No. three umbrella shape guide faces 5 are with the central axes bilateral symmetry of deaeration autoclave body 1 and heating agent inner cavity
200 with the central axes bilateral symmetry of deaeration autoclave body 1), hence for No.1 umbrella shape guide face 3, two anti-umbrella shape guide faces 4 and three
Number umbrella shape guide face 5, it is consistent with the heat transfer distances between the heating agent in heating agent inner cavity in each point on same level section, thus
The temperature of each point on the same level section of No.1 umbrella shape guide face 3 is consistent, No. two anti-umbrella shape guide faces 4 same levels are cut
The temperature of each point on face, No. three umbrella shape guide faces 5 same level section on each point temperature it is consistent, so, melt exists
In the flowing booth membrane process of No.1 umbrella shape guide face 3, two anti-umbrella shape guide faces 4 and No. three umbrella shape guide faces 5, solution is heated
Path is identical, and the heating temperature of the solution on same level section is also identical, thus steeped in first order deaeration to the third level
Samming is realized in the process.
Step 6, while No. four water conservancy diversion samming arcwall faces 6 increase the volume of deaeration kettle inner cavity 100, heat build-up is increased
Area, thus No. four water conservancy diversion samming arcwall faces 6 are mainly used for samming and glue, while subsidiary deaeration effect.From No. three umbrella shape water conservancy diversion
The melt flowed down on face 5 (does not show through No. three umbrella shape guide faces 5 and the second overflow seam of 1 inner wall junction of deaeration autoclave body in figure
It flows down out), flows directly into No. four water conservancy diversion samming arcwall faces 6, solution flows through No. four big water conservancy diversion samming arcwall faces 6 of heat build-up area
When, due to autoclave body symmetry (specifically refer to No. four water conservancy diversion samming arcwall faces 6 with the central axes of deaeration autoclave body 1 bilateral symmetry, with
And heating agent inner cavity 200 is with the central axes bilateral symmetry of deaeration autoclave body 1) so that No. four water conservancy diversion samming arcwall faces 6 are cut in same level
Each point on face is consistent with the heat transfer distances between the heating agent in heating agent inner cavity, thus No. four water conservancy diversion samming arcwall faces 6 is same
The temperature of each point on horizontal cross-section is also consistent, so, melt is spread out in membrane process in the flowing of No. four water conservancy diversion samming arcwall faces 6,
The heated scoring path of solution on No. four water conservancy diversion samming arcwall faces 6 is identical, the heating temperature of the solution on same level section also phase
Together, and since the heat build-up area of No. four water conservancy diversion samming arcwall faces is big, so melt is at the flowing booth of No. four water conservancy diversion samming arcwall faces 6
The even temperature effect better to third level de-aeration than first order deaeration is able to achieve in membrane process；
The solution for flowing into No. four water conservancy diversion samming arcwall faces 6 forms the film of 1.8mm thickness on No. four water conservancy diversion samming arcwall faces 6, melts
Body is in the flowing booth membrane process on No. four water conservancy diversion samming arcwall faces 6, and remaining micro-molecular gas and part bubble be again in melt
Secondary rupture, realizes deaeration again, this is fourth stage deaeration.
Step 7, spinning pump 63 is opened, the speed of spinning pump is 24rpm, and melt enters 1 bottom of deaeration autoclave body
Spinning pump 63, then be pumped into filament spinning component through spinning pump 63, start spinning.
Embodiment 2:
The present embodiment difference from example 1 is that:
Melt to deaeration is the preceramic polymer polyaluminocarbosilane (PACS) of aluminum-containing silicon carbide fiber, softening point 220
℃。
The heat medium temperature in the heating agent inner cavity 200 of viscous/deaeration integrated device is set according to the softening point to spinning polymer,
Heat medium temperature is set as 310 DEG C, is started heating agent circulatory system soaking time 3 hours.When the deaeration kettle of equal viscous/deaeration integrated devices
Vacuum degree in inner cavity 100 is -80kPa, closes the valve on the first vacuum connection tube 22.Fuel gauge pump 23 speed be
20rpm, spinning pump pump speed are 19rpm.
Remaining is the same as embodiment 1.
The technical means disclosed in the embodiments of the present invention and device, are not limited to the above technical means, and further include by the above skill
Technical solution composed by art feature equivalent replacement.Unaccomplished matter of the invention belongs to the common knowledge of those skilled in the art.
Claims (8)
1. viscous/deaeration integrated device, including deaeration autoclave body (1) of Preceramic Polymers spinning melt, deaeration autoclave body (1)
Top be equipped with autoclave body upper cover (2), the closed cavity that the inner wall of deaeration autoclave body (1) and the lower surface of autoclave body upper cover (2) surround
For deaeration kettle inner cavity (100), which is characterized in that the top of deaeration autoclave body (1) or autoclave body upper cover (2) are pumped equipped with fuel gauge
(23), the bottom of deaeration autoclave body (1) is equipped with spinning pump (63), is disposed with from top to bottom in deaeration kettle inner cavity (100)
No.1 umbrella shape guide face (3), No. two anti-umbrella shape guide faces (4), No. three umbrella shape guide faces (5), No. four water conservancy diversion samming arcwall faces
(6), No.1 umbrella shape guide face (3), No. two anti-umbrella shape guide faces (4), No. three umbrella shape guide faces (5) with deaeration autoclave body (1)
The junction of inner wall connection, No.1 umbrella shape guide face (3) and deaeration autoclave body (1) inner wall is equipped with the first overflow seam (8), No. two anti-umbrellas
The center of shape guide face (4), which is equipped with, collects hole, and collection hole is through-hole, No. three umbrella shape guide faces (5) and deaeration autoclave body (1) inner wall
Junction is stitched equipped with the second overflow, and No. four water conservancy diversion samming arcwall faces (6) are the arc inner wall face of deaeration autoclave body (1) lower part；No.1
Umbrella shape guide face (3), No. two anti-umbrella shape guide faces (4), No. three umbrella shape guide faces (5) and No. four water conservancy diversion samming arcwall faces (6) are equal
With the central axes bilateral symmetry of deaeration autoclave body (1).
2. viscous/deaeration integrated device, the feature of Preceramic Polymers spinning melt according to claim 1 exist
In, inert atmosphere is installed in autoclave body upper cover (2) and enters pipe (21) and the first vacuum connection tube (22), inert atmosphere enter pipe (21) and
Valve is respectively arranged on first vacuum connection tube (22), inert atmosphere enters the external inert atmosphere storage tank in one end of pipe (21), indifferent gas
The other end that atmosphere enters pipe (21) is connected to deaeration kettle inner cavity (100), the external vacuum system in one end of the first vacuum connection tube (22), the
The other end of one vacuum connection tube (22) is connected to deaeration kettle inner cavity (100).
3. viscous/deaeration integrated device of Preceramic Polymers spinning melt according to claim 1 or 2, special
Sign is, heating agent inner cavity (200) between the inner wall of deaeration autoclave body (1) and the outside wall surface of deaeration autoclave body (1), heating agent inner cavity
(200) with the central axes bilateral symmetry of deaeration autoclave body (1)；The top of deaeration autoclave body (1) is equipped with and is connected to heating agent inner cavity (200)
Heating agent entrance (10), the lower part of deaeration autoclave body (1) are equipped with the heating agent outlet (11) being connected to heating agent inner cavity (200), deaeration autoclave body
(1) outside wall surface periphery is equipped with insulating layer (7), and heating agent entrance (10) and heating agent outlet (11) run through insulating layer (7).
4. viscous/deaeration integrated device of Preceramic Polymers spinning melt according to claim 1 or 2, special
Sign is, the first snorkel (31) is housed on No.1 umbrella shape guide face (3), the upper end of the first snorkel (31) extend out to No.1 umbrella
The top of shape guide face (3), the lower end of the first snorkel (31) extend out to the top of No. two anti-umbrella shape guide faces (4)；No. three umbrellas
The second snorkel (32) are housed on shape guide face (5), the upper end of the second snorkel (32) extend out to No. three umbrella shape guide faces (5)
Top, the lower end of the second snorkel (32) are protruded into the space that No. four water conservancy diversion samming arcwall faces (6) surround；
Deaeration autoclave body (1) is equipped with the second vacuum connection tube (61) and third vacuum connection tube (62), the second vacuum connection tube
(61) and third vacuum connection tube (62) is symmetrically set in the central axes two sides of deaeration autoclave body (1), the second vacuum connection tube (61)
Upper end and the upper end of third vacuum connection tube (62) extend out to the top of No.1 umbrella shape guide face (3), the second vacuum connection tube
(61) lower end of upper end and third vacuum connection tube (62) extend out to the top of No. three umbrella shape guide faces (5).
5. being carried out using viscous/deaeration integrated device of Preceramic Polymers spinning melt as described in claim 1-4 equal
The method of viscous/deaeration, which comprises the steps of:
Step 1, the heating agent entrance (10) of viscous/deaeration integrated device and the heating agent of the heating agent circulatory system are exported and is connected, viscous/
The heating agent outlet (11) of deaeration integrated device is connect with the heating agent entrance of the heating agent circulatory system, according to the softening point to spinning polymer
Heat medium temperature is set, heat medium temperature is 80 DEG C higher than the softening point to spinning polymer~and 120 DEG C；Start the heating agent circulatory system and keeps the temperature 1-
4 hours, heating agent flowed into heating agent inner cavity (200) through heating agent entrance (10), and holding temperature is equal to heat medium temperature；
By the first vacuum connection tube (22) external vacuum system of viscous/deaeration integrated device, the first vacuum connection tube is opened
(22) valve on opens vacuum system, when the vacuum degree in the deaeration kettle inner cavity (100) of viscous/deaeration integrated device is-
When 70kPa~-85kPa, the valve on the first vacuum connection tube (22) is closed, closes and removes vacuum system；By indifferent gas
Atmosphere enters the external inert atmosphere storage tank of pipe (21), opens inert atmosphere and enters the valve on pipe (21), fills into deaeration kettle inner cavity (100)
Enter inert gas, the rate that is filled with of inert gas is 1-10L/min, according to the volume and inert gas of deaeration kettle inner cavity (100)
The rate that is filled with acquire in deaeration kettle inner cavity (100) full of the time needed for inert gas, be full of when in deaeration kettle inner cavity (100)
When inert gas, the valve that is again turned on the first vacuum connection tube (22)；Inert atmosphere, which enters pipe (21), to be continued into deaeration kettle
It is filled with inert gas in chamber (100), extra inert gas is flowed from the first vacuum connection tube (22) in deaeration kettle inner cavity (100)
Out；
Step 2, starting fuel gauge pump (23) and spinning pump (63) pump (23) by fuel gauge to spinning polymer melt
It is pumped into deaeration kettle inner cavity (100)；The revolving speed that fuel gauge pumps (23) determines that feed is counted according to the revolving speed of spinning pump (63)
The fast 3%-7% of revolving speed of the rotating ratio spinning pump 63 of amount pump 23；
Step 3, spinning melt be pumped by fuel gauge pump (23) in deaeration kettle inner cavity (100) to spinning polymer melt,
It uniformly spreads under the effect of gravity and forms film on No.1 umbrella shape guide face (3), melt is on No.1 umbrella shape guide face (3)
In the membrane process of flowing booth, remaining micro-molecular gas and part bubbles burst in melt realize first order deaeration；
Step 4, the melt flowed down from No.1 umbrella shape guide face is connect through No.1 umbrella shape guide face (3) with deaeration autoclave body (1) inner wall
The first overflow seam (8) at place flows down, and after flowing through kettle wall, flows directly on No. 2 reversed umbrella shape guide faces (4) and forms film, melt
In the flowing booth membrane process on No. two anti-umbrella shape guide faces, remaining micro-molecular gas and part bubbles burst in melt are real
Existing second level deaeration；
Step 5, the melt flowed down from No. two anti-umbrella shape guide faces (4), the collection hole through No. two anti-umbrella shape guide face (4) centers
It flows down, flows directly on No. three umbrella shape guide faces (5) and form film, film is spread out in flowing of the melt on No. three umbrella shape guide faces (5)
In the process, remaining micro-molecular gas and part bubbles burst in melt realize third level deaeration；
No.1 umbrella shape guide face, No. two anti-umbrella shape guide faces and No. three umbrella shape guide faces are mainly used for deaeration, while subsidiary samming
Effect；In first order deaeration, second level deaeration and third level de-aeration, melt flows separately through No.1 umbrella shape guide face, two
When number anti-umbrella shape guide face and No. three umbrella shape guide faces, due to the symmetry, in particular to No.1 umbrella shape guide face, No. two of autoclave body
Anti- umbrella shape guide face and No. three umbrella shape guide faces with the central axes bilateral symmetry and heating agent inner cavity (200) of deaeration autoclave body (1) with
The central axes bilateral symmetry of deaeration autoclave body (1), hence for No.1 umbrella shape guide face, No. two anti-umbrella shape guide faces and No. three umbrella shapes
Guide face, it is consistent with the heat transfer distances between the heating agent in heating agent inner cavity in each point on same level section, thus No.1 umbrella
The temperature of each point on the same level section of shape guide face is consistent, each on the same level section of No. two anti-umbrella shape guide faces
The temperature of point, the temperature of each point on the same level section of No. three umbrella shape guide faces are consistent, so, melt is led in No.1 umbrella shape
In the flowing booth membrane process of stream interface, No. two anti-umbrella shape guide faces and No. three umbrella shape guide faces, the heated scoring path of solution is identical, same
The heating temperature of solution on horizontal cross-section is also identical, to realize during first order deaeration to the third level is steeped
Temperature；
Step 6, while No. four water conservancy diversion samming arcwall faces (6) increase the volume of deaeration kettle inner cavity, heat build-up area is increased,
Thus it is viscous to be mainly used for samming for No. four water conservancy diversion samming arcwall faces (6), while subsidiary deaeration acts on；From No. three umbrella shape guide faces
(5) melt flowed down on flows down, directly through No. three umbrella shape guide faces (5) and the second overflow seam of deaeration autoclave body (1) inner wall junction
It connects and flows into No. four water conservancy diversion samming arcwall faces (6), when solution flows through No. four big water conservancy diversion samming arcwall faces of heat build-up area, due to autoclave body
Symmetry, in particular to No. four water conservancy diversion samming arcwall faces (6) with the central axes of deaeration autoclave body (1) bilateral symmetry and heating agent
Inner cavity (200) is with the central axes bilateral symmetry of deaeration autoclave body (1), so that No. four water conservancy diversion samming arcwall faces (6) are cut in same level
Each point on face is consistent with the heat transfer distances between the heating agent in heating agent inner cavity, thus No. four water conservancy diversion samming arcwall faces (6) is same
The temperature of each point on one horizontal cross-section is also consistent, so, melt spreads out membrane process in the flowing of No. four water conservancy diversion samming arcwall faces (6)
In, the heated scoring path of the solution on No. four water conservancy diversion samming arcwall faces (6) is identical, the heating temperature of the solution on same level section
Also identical, and since the heat build-up area of No. four water conservancy diversion samming arcwall faces (6) is big, so melt is in No. four water conservancy diversion samming arcwall faces
(6) even temperature effect better to third level de-aeration than first order deaeration is able to achieve in flowing booth membrane process；
The solution for flowing into No. four water conservancy diversion samming arcwall faces (6) forms film on No. four water conservancy diversion samming arcwall faces (6), and melt exists
In flowing booth membrane process on No. four water conservancy diversion samming arcwall faces, remaining micro-molecular gas and part bubble are broken again in melt
It splits, realizes deaeration again, this is fourth stage deaeration；
Step 7, start spinning pump, melt enters the spinning pump (63) of deaeration autoclave body (1) bottom, then through spinning measuring
Pump (63) is pumped into filament spinning component, starts spinning.
6. being carried out according to claim 5 using viscous/deaeration integrated device of Preceramic Polymers spinning melt equal
The method of viscous/deaeration, which is characterized in that in the step 3, spinning melt is uniformly spread under the effect of gravity leads in No.1 umbrella shape
On stream interface (3), the film of 0.5 mm -3.5mm thickness is formed；
In the step 4, the melt flowed down from No.1 umbrella shape guide face, through in No.1 umbrella shape guide face (3) and deaeration autoclave body (1)
The first overflow seam (8) of wall junction flows down, and after flowing through kettle wall, flows directly on No. 2 reversed umbrella shape guide faces (4), forms 0.5
The film of mm -3.5mm thickness；
In the step 5, the melt flowed down from No. two anti-umbrella shape guide faces (4), through No. two anti-umbrella shape guide face (4) centers
It collects hole to flow down, flow directly on No. three umbrella shape guide faces (5), form the film of 0.5 mm -3.5mm thickness；
In the step 6, the solution of No. four water conservancy diversion samming arcwall faces (6) is flowed into, is formed on No. four water conservancy diversion samming arcwall faces (6)
The film of 0.5 mm -3.5mm thickness.
7. being carried out according to claim 6 using viscous/deaeration integrated device of Preceramic Polymers spinning melt equal
The method of viscous/deaeration, which is characterized in that in the step 3, spinning melt is uniformly spread under the effect of gravity leads in No.1 umbrella shape
On stream interface (3), the film of 1.5mm~2.0mm thickness is formed；
In the step 4, the melt flowed down from No.1 umbrella shape guide face, through in No.1 umbrella shape guide face (3) and deaeration autoclave body (1)
The first overflow seam (8) of wall junction flows down, and after flowing through kettle wall, flows directly on No. 2 reversed umbrella shape guide faces (4), is formed
The film of 1.5mm~2.0mm thickness；
In the step 5, the melt flowed down from No. two anti-umbrella shape guide faces (4), through No. two anti-umbrella shape guide face (4) centers
It collects hole to flow down, flow directly on No. three umbrella shape guide faces (5), form the film of 1.5mm~2.0mm thickness；
In the step 6, the solution of No. four water conservancy diversion samming arcwall faces (6) is flowed into, is formed on No. four water conservancy diversion samming arcwall faces (6)
The film of 1.5mm~2.0mm thickness.
8. being carried out according to claim 7 using viscous/deaeration integrated device of Preceramic Polymers spinning melt equal
The method of viscous/deaeration, which is characterized in that in the step 3, spinning melt is uniformly spread under the effect of gravity leads in No.1 umbrella shape
On stream interface (3), the film of 1.8mm thickness is formed；
In the step 4, the melt flowed down from No.1 umbrella shape guide face, through in No.1 umbrella shape guide face (3) and deaeration autoclave body (1)
The first overflow seam (8) of wall junction flows down, and after flowing through kettle wall, flows directly on No. 2 reversed umbrella shape guide faces (4), is formed
The film of 1.8mm thickness；
In the step 5, the melt flowed down from No. two anti-umbrella shape guide faces (4), through No. two anti-umbrella shape guide face (4) centers
It collects hole to flow down, flow directly on No. three umbrella shape guide faces (5), form the film of 1.8mm thickness；
In the step 6, the solution of No. four water conservancy diversion samming arcwall faces (6) is flowed into, is formed on No. four water conservancy diversion samming arcwall faces (6)
The film of 1.8mm thickness.
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