CN106757410A - A kind of spinneret orifice and its processing method - Google Patents
A kind of spinneret orifice and its processing method Download PDFInfo
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- CN106757410A CN106757410A CN201611004384.XA CN201611004384A CN106757410A CN 106757410 A CN106757410 A CN 106757410A CN 201611004384 A CN201611004384 A CN 201611004384A CN 106757410 A CN106757410 A CN 106757410A
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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
- D01D4/00—Spinnerette packs; Cleaning thereof
- D01D4/02—Spinnerettes
- D01D4/022—Processes or materials for the preparation of spinnerettes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
-
- 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Silicon Polymers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to a kind of spinneret orifice and its processing method, with spinneret as fixed bed, with polysiloxanes treatment fluid as flow fluid, under the conditions of 70~85 DEG C, flow fluid is flowed out from the spinneret orifice of spinneret, primary solidification is then carried out under the conditions of 95~120 DEG C, then solidified again at 200~230 DEG C, final curing finally is carried out at 260~280 DEG C, the spinneret orifice of low-surface-energy is obtained after cooling.Spinneret orifice is the spinneret orifice of the low-surface-energy being surface-treated by polysiloxanes treatment fluid, and the surface of spinneret orifice can En≤35mJ/cm2, surface roughness Ra≤0.2 μm, surface static contact angle WCA >=85 °.Spinneret orifice of the invention, with low-surface-energy feature, can improve spinneret orifice smoothness and reduce coefficient of friction, and using the spinneret of spinneret orifice of the invention, the cleaning frequency extends to original more than 4 times.
Description
Technical field
The invention belongs to spinneret technical field, it is related to a kind of spinneret orifice and its processing method, it is more particularly to a kind of low
The spinneret orifice and its processing method of surface energy.
Background technology
China is chemical fibre big country, and chemical fibre is the important raw material of field of textiles, from for the yield of chemical fibre, China in 2014
Chemical fibre yield reaches 43,900,000 tons.The production of current fibers material based on melt-spinning technology, the transition and upgrade in chemical fibre field
Main development direction is promoted to produce energy-efficient and fiber quality.The lifting of melt spinning technology turns for chemical fibre field
Type upgrading has great facilitation.
Existing melt spinning technology problem present in application process is concentrated mainly on spinning speed and lifts limited, life
Produce improved efficiency unobvious：Rheological resistance and windage resistance in fiber forming process, in melt spinning process of manufacture,
Because the appearance of the phenomenons such as lousiness, broken end causes the generation of certain amount waste silk, with the increase of chemical fibre production capacity, in production process
Waste silk doses also can accordingly increase.And the waste silk rate level of China's chemical fibre whole industry is 10kg/t, therefore there is hundreds of thousands every year
The generation of the chemical fiber waste filament of ton, causes the serious wasting of resources.Therefore how simply and effectively this part waste silk material of reuse, right
In raw material dosage is saved, production cost is reduced, improve the economic benefit of enterprise, suffer from larger realistic meaning.
For the problem present on, it is necessary to melt spinning technical optimization, lifting melt spinning speed, reducing energy consumption
Fiber quality is further lifted simultaneously.Wherein during melt spinning, the distribution of force for spinning fiber in journey is melt spinning skill
Art core, for the effect that melt forming and quality regulation and control play key.Journey research angle is spun from fiber, works as melting
When spinning technique changes, the changes in distribution for spinning power in journey can be caused.Generally, fiber spin in journey the power that is subject to
Based on rheological resistance, windage resistance, both power have directly influence to the lifting for spinning speed.Chinese patent CN
Problem in 102206879 A for the above designs negative pressure spinning condition (0.01~0.001MPa) in fiber forming process,
The spinning speed of fiber is lifted by way of reducing windage resistance, but is lacked necessity for the rheological resistance suffered by melt and is examined
Consider, and it is one of key factor that rheological resistance spins speed with the lifting of quality for fiber.The structure pair of spinneret in filament spinning component
Rheological resistance suffered by melt have directly affect, and then regulate and control fiber formation process.
The content of the invention
The present invention is not enough for existing research, fully takes into account rheological resistance and spins journey to fiber with spinning boundary layer environment
The mechanism of action of stress, to the treatment of spinneret face low resistance, reduces rheological resistance of the melt at spinneret, greatly promotes spinning
Speed, while designing spinning boundary environment, fiber can realize orientation and the crystallization of matching under high speed spinning, reach fabric
The lifting of matter.The technical problems to be solved by the invention are to provide a kind of spinneret orifice and its processing method, are a kind of low surfaces
Spinneret orifice of energy and preparation method thereof.
A kind of processing method of spinneret orifice of the invention, is stream with polysiloxanes treatment fluid with spinneret as fixed bed
Hydrodynamic, under the conditions of 70~85 DEG C, makes flow fluid be flowed out from the spinneret orifice of spinneret, then enters under the conditions of 95~120 DEG C
Row primary solidification, then solidified again at 200~230 DEG C, final curing finally is carried out at 260~280 DEG C, obtain low after cooling
The spinneret orifice of surface energy.
As preferred technical scheme：
A kind of processing method of spinneret orifice as described above, the polysiloxanes treatment fluid by weight, each component
For：
A kind of processing method of spinneret orifice as described above, the preparation method of the polysiloxanes treatment fluid is in proportion
Ludox and Alumina gel are added, then pH value is adjusted with catalyst, the pH value of system is maintained 2~4.5, then added again
Enter solvent and siloxanes, then the 15~20min that is hydrolyzed at normal temperatures, system is then put into 45~80 DEG C again carries out high temperature contracting
Close, reaction maintains 30~75min, reaction to add auxiliary agent after terminating, and after being stirred 5~10min, the system for the treatment of is cooled to room
Temperature, obtains required polysiloxanes treatment fluid.
A kind of processing method of spinneret orifice as described above, the siloxanes is MTMS, methyl three
One or more of Ethoxysilane, ethyl triethoxysilane, trim,ethylchlorosilane or phenyl triethoxysilane.
A kind of processing method of spinneret orifice as described above, the preferred MTMS of siloxanes, phenyl
The mixture of triethoxysilane and trim,ethylchlorosilane, and corresponding volume ratio is 1:0.05~0.25:0.05~0.1.
A kind of processing method of spinneret orifice as described above, the Ludox is alkaline silica sol, and its pH value is 10.3
± 0.2, the solid content of Ludox is 30~45wt%, and average grain diameter is 30~50nm.
A kind of processing method of spinneret orifice as described above, the Alumina gel is alkaline Alumina gel, its pH value is 9.6 ±
0.2, the solid content of Alumina gel is 20~35wt%, and average grain diameter is 45~65nm.
A kind of processing method of spinneret orifice as described above, the solvent is the mixed solvent of alcohol and water, and alcohol is unitary
Alcohol or dihydroxylic alcohols；Wherein monohydric alcohol is ethanol, isopropanol or butanol, and dihydroxylic alcohols is ethylene glycol or 1,3-PD；And unitary
Alcohol is 1.25~1.60 with the volume ratio of water:1, dihydroxylic alcohols is 0.75~1.0 with the volume ratio of water:1；
The catalyst is one or two the mixture in formic acid, acetic acid, hydrochloric acid, phosphoric acid and nitric acid；
The auxiliary agent is the mixture of levelling agent BYK 310, defoamer BYK 025 and surface hardening anti-wear agent T801；Its
The mass ratio of middle levelling agent, defoamer and surface hardening anti-wear agent is 1:1~5:0.25~0.5.
A kind of processing method of spinneret orifice as described above, the flow velocity that flow fluid flows out from the spinneret orifice of spinneret is
0.01~10L/min, the time is 0.5~5min；The primary solidification time is 15~20min；Again hardening time be 20~
25min；The final curing time is 5~10min；Cooling uses natural cooling.
Present invention also offers a kind of spinneret orifice, the spinneret orifice is to be surface-treated by polysiloxanes treatment fluid
Low-surface-energy spinneret orifice, the surface of spinneret orifice can En≤35mJ/cm2, surface roughness Ra≤0.2 μm, surface is quiet
State contact angle WCA >=85 °.
Spinneret orifice of the invention, including conventional circular hole and various irregularly-shaped holes, the irregularly-shaped hole be triangular form, trilobal cross,
The micropores such as hollow type, platypelloid type, cross, rich font, " 8 " font, Y-shaped, " H " type.
Spinneret orifice of the invention including and be not limited to melt spinning, wet spinning, electrostatic spinning etc. it is spinning jet used or
The spinneret orifice of spinneret passage.
Spinneret material is stainless steel.
Spinneret orifice of the invention, also including spinneret orifice that composite spinning is spinning jet used.
A kind of spinneret orifice of the invention, is the spinneret orifice processed by low-surface-energy polysiloxanes treatment fluid,
Spinneret orifice surface crater in itself is filled by low-surface-energy material, and spinneret orifice surface is smooth, spinning melt and spinneret orifice
Coefficient of friction reduction.
Beneficial effect：
Spinneret orifice of the invention, with low-surface-energy feature, improves spinneret orifice smoothness and reduces coefficient of friction.
Spinneret orifice of the invention, using surface cure step by step is carried out after silicone monomers hydrolytic condensation, both ensure that
The dimensional stability and low-surface-energy characteristic of spinneret orifice, at the same can also improve solidification after polysiloxanes build structure turn
Become, improve spinneret orifice case hardness and crocking resistance.
Using the spinneret of spinneret orifice of the invention, the cleaning frequency extends to original more than 4 times.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
Embodiment 1
10 parts of pH value are that 10.1, solid content is first by weight by a kind of processing method of spinneret orifice
30wt%, average grain diameter are that 9.4, solid content is that 20wt%, average grain diameter are for the alkaline silica sol and 10 parts of pH value of 30nm
The alkaline Alumina gel mixing of 45nm, is subsequently adding 5 parts of first acid as catalyst regulation system pH value, pH value is maintained 2, Ran Houjia
Enter the mixed solvent of 10 parts of ethanol and water, ethanol is 1.25 with the volume ratio of water:1, then add 30 parts of methyl trimethoxy epoxides
Silane, then the 15min that is hydrolyzed at normal temperatures, system is then put into 45 DEG C again carries out pyrocondensation, and reaction maintains 30min,
Reaction adds 1 part of mass ratio after terminating be 1:1:0.25 levelling agent BYK 310, defoamer BYK 025 and surface hardening is resistance to
The mixture auxiliary agent of grinding agent T801, after being stirred 5min, the system for the treatment of is cooled to room temperature, obtains polysiloxanes treatment fluid.
With spinneret as fixed bed, with polysiloxanes treatment fluid as flow fluid, under the conditions of 70 DEG C, flow fluid is set to exist
Flowed out from the circular spinneret orifice of spinneret with the flow velocity of 0.01L/min in 0.5min, then carried out under the conditions of 95 DEG C preliminary
Solidification 15min, then solidified 20min again at 200 DEG C, final curing 5min finally is carried out at 260 DEG C, obtained after natural cooling
The spinneret orifice of low-surface-energy.Test shows that the surface energy En of the spinneret orifice of the spinneret orifice of the low-surface-energy for preparing is
35mJ/cm2, surface roughness Ra is 0.2 μm, and surface static contact angle WCA is 85 °.
Embodiment 2
20 parts of pH value are that 10.5, solid content is first by weight by a kind of processing method of spinneret orifice
45wt%, average grain diameter are that 9.8, solid content is that 35wt%, average grain diameter are for the alkaline silica sol and 20 parts of pH value of 50nm
The alkaline Alumina gel mixing of 65nm, is subsequently adding 8 parts of second acid as catalyst regulation system pH value, pH value is maintained 4.5, then
The mixed solvent of 20 parts of isopropanols and water is added, isopropanol is 1.42 with the volume ratio of water:1, then add 40 parts of methyl three
Ethoxysilane, then the 20min that is hydrolyzed at normal temperatures, system is then put into 80 DEG C again carries out pyrocondensation, and reaction is maintained
75min, reaction adds 3 parts of mass ratioes after terminating be 1:5:0.5 levelling agent BYK 310, defoamer BYK 025 and surface increase
The mixture auxiliary agent of hard anti-wear agent T801, after being stirred 10min, the system for the treatment of is cooled to room temperature, obtains polysiloxanes treatment fluid.
With spinneret as fixed bed, with polysiloxanes treatment fluid as flow fluid, under the conditions of 85 DEG C, make flow fluid in 5min
The interior flow velocity with 10L/min is flowed out from the triangular form spinneret orifice of spinneret, and primary solidification is then carried out under the conditions of 120 DEG C
20min, then solidified 25min again at 230 DEG C, final curing 10min finally is carried out at 280 DEG C, obtain low after natural cooling
The spinneret orifice of surface energy.Test shows that the surface energy En of the spinneret orifice of the spinneret orifice of the low-surface-energy for preparing is 34mJ/
cm2, surface roughness Ra is 0.15 μm, and surface static contact angle WCA is 86 °.
Embodiment 3
15 parts of pH value are that 10.3, solid content is first by weight by a kind of processing method of spinneret orifice
35wt%, average grain diameter are that 9.6, solid content is that 30wt%, average grain diameter are for the alkaline silica sol and 15 parts of pH value of 40nm
The alkaline Alumina gel mixing of 50nm, is subsequently adding 6 parts of salt acid as catalyst regulation system pH value, pH value is maintained 3, Ran Houjia
Enter the mixed solvent of 15 parts of butanol and water, butanol is 1.60 with the volume ratio of water:1, then add 35 parts of ethyl triethoxies
Silane, then the 18min that is hydrolyzed at normal temperatures, system is then put into 50 DEG C again carries out pyrocondensation, and reaction maintains 40min,
Reaction adds 2 parts of mass ratioes after terminating be 1:1:0.25 levelling agent BYK 310, defoamer BYK 025 and surface hardening is resistance to
The mixture auxiliary agent of grinding agent T801, after being stirred 8min, the system for the treatment of is cooled to room temperature, obtains polysiloxanes treatment fluid.
With spinneret as fixed bed, with polysiloxanes treatment fluid as flow fluid, under the conditions of 80 DEG C, make flow fluid in 3min
The interior flow velocity with 5L/min is flowed out from the trilobal cross spinneret orifice of spinneret, and primary solidification is then carried out under the conditions of 100 DEG C
18min, then solidified 22min again at 210 DEG C, final curing 8min finally is carried out at 270 DEG C, low table is obtained after natural cooling
The spinneret orifice of face energy.Test shows that the surface energy En of the spinneret orifice of the spinneret orifice of the low-surface-energy for preparing is 32mJ/
cm2, surface roughness Ra is 0.1 μm, and surface static contact angle WCA is 88 °.
Embodiment 4
18 parts of pH value are that 10.3, solid content is first by weight by a kind of processing method of spinneret orifice
40wt%, average grain diameter are that 9.6, solid content is that 30wt%, average grain diameter are for the alkaline silica sol and 18 parts of pH value of 45nm
The alkaline Alumina gel mixing of 60nm, is subsequently adding 7 parts of phosphoric acid does catalyst regulation system pH value, pH value is maintained 4.5, then
The mixed solvent of 18 parts of ethylene glycol and water is added, ethylene glycol is 0.75 with the volume ratio of water:1, then add 38 parts of trimethyls
Chlorosilane, then the 18min that is hydrolyzed at normal temperatures, system is then put into 70 DEG C again carries out pyrocondensation, and reaction is maintained
70min, reaction adds 3 parts of mass ratioes after terminating be 1:5:0.5 levelling agent BYK 310, defoamer BYK 025 and surface increase
The mixture auxiliary agent of hard anti-wear agent T801, after being stirred 10min, the system for the treatment of is cooled to room temperature, obtains polysiloxanes treatment fluid.
With spinneret as fixed bed, with polysiloxanes treatment fluid as flow fluid, under the conditions of 80 DEG C, make flow fluid in 4min
The interior flow velocity with 8L/min is flowed out from the hollow type spinneret orifice of spinneret, and primary solidification is then carried out under the conditions of 110 DEG C
18min, then solidified 24min again at 220 DEG C, final curing 8min finally is carried out at 270 DEG C, low table is obtained after natural cooling
The spinneret orifice of face energy.Test shows that the surface energy En of the spinneret orifice of the spinneret orifice of the low-surface-energy for preparing is 34mJ/
cm2, surface roughness Ra is 0.2 μm, and surface static contact angle WCA is 88 °.
Embodiment 5
10 parts of pH value are that 10.1, solid content is first by weight by a kind of processing method of spinneret orifice
30wt%, average grain diameter are that 9.4, solid content is that 20wt%, average grain diameter are for the alkaline silica sol and 10 parts of pH value of 30nm
The alkaline Alumina gel mixing of 45nm, is subsequently adding 5 parts of nitre acid as catalyst regulation system pH value, pH value is maintained 2, Ran Houjia
Enter the mixed solvent of 10 parts of 1,3-PDs and water, 1,3-PD is 1.0 with the volume ratio of water:1, then add 30 parts of benzene
Ethyl triethoxy silicane alkane, then the 15min that is hydrolyzed at normal temperatures, system is then put into 45 DEG C again carries out pyrocondensation, reaction
It is 1 to maintain 30min, reaction that 1 part of mass ratio is added after terminating:1:0.25 levelling agent BYK 310, the and of defoamer BYK 025
The mixture auxiliary agent of surface hardening anti-wear agent T801, after being stirred 5min, the system for the treatment of is cooled to room temperature, obtains at polysiloxanes
Reason liquid.
With spinneret as fixed bed, with polysiloxanes treatment fluid as flow fluid, under the conditions of 70 DEG C, flow fluid is set to exist
Flowed out from the platypelloid type spinneret orifice of spinneret with the flow velocity of 0.01L/min in 0.5min, then carried out under the conditions of 95 DEG C just
Step solidification 15min, then solidified 20min again at 200 DEG C, final curing 5min finally is carried out at 260 DEG C, after natural cooling
To the spinneret orifice of low-surface-energy.Test shows that the surface energy En of the spinneret orifice of the spinneret orifice of the low-surface-energy for preparing is
32mJ/cm2, surface roughness Ra is 0.2 μm, and surface static contact angle WCA is 85 °.
Embodiment 6
15 parts of pH value are that 10.3, solid content is first by weight by a kind of processing method of spinneret orifice
40wt%, average grain diameter are that 9.6, solid content is that 30wt%, average grain diameter are for the alkaline silica sol and 15 parts of pH value of 40nm
The alkaline Alumina gel mixing of 60nm, is subsequently adding the mixture as catalyst regulation system pH value of 6 parts of formic acid and acetic acid, makes pH value
3 are maintained, formic acid is 1 with the mass ratio of acetic acid:1, it is subsequently adding the volume of the mixed solvent of 15 parts of ethanol and water, ethanol and water
Than being 1.25:1, then add the mixture of 35 parts of MTMSs and MTES, corresponding body
Product is than being 1:1, then the 18min that is hydrolyzed at normal temperatures, system is then put into 70 DEG C again carries out pyrocondensation, and reaction is maintained
60min, reaction adds 2 parts of mass ratioes after terminating be 1:5:0.5 levelling agent BYK 310, defoamer BYK 025 and surface increase
The mixture auxiliary agent of hard anti-wear agent T801, after being stirred 8min, the system for the treatment of is cooled to room temperature, obtains polysiloxanes treatment fluid.
With spinneret as fixed bed, with polysiloxanes treatment fluid as flow fluid, under the conditions of 80 DEG C, make flow fluid in 4min
The interior flow velocity with 8L/min is flowed out from the cross spinneret orifice of spinneret, and primary solidification is then carried out under the conditions of 100 DEG C
18min, then solidified 24min again at 220 DEG C, final curing 8min finally is carried out at 270 DEG C, low table is obtained after natural cooling
The spinneret orifice of face energy.Test shows that the surface energy En of the spinneret orifice of the spinneret orifice of the low-surface-energy for preparing is 33mJ/
cm2, surface roughness Ra is 0.2 μm, and surface static contact angle WCA is 87 °.
Embodiment 7
10 parts of pH value are that 10.1, solid content is first by weight by a kind of processing method of spinneret orifice
30wt%, average grain diameter are that 9.4, solid content is that 20wt%, average grain diameter are for the alkaline silica sol and 10 parts of pH value of 30nm
The alkaline Alumina gel mixing of 45nm, is subsequently adding the mixture of 5 parts of hydrochloric acid and phosphoric acid, makees catalyst regulation system pH value, makes pH
Value maintains 2, and hydrochloric acid is 1 with the mass ratio of phosphoric acid:2, it is subsequently adding the mixed solvent of 10 parts of isopropanols and water, isopropanol and water
Volume ratio be 1.42:1, then add 30 parts of MTMSs, phenyl triethoxysilane and trimethylchloro-silicanes
The mixture of alkane, corresponding volume ratio is 1:0.05:0.05, then the 15min that is hydrolyzed at normal temperatures, system is put into again then
45 DEG C carry out pyrocondensation, and it is 1 that reaction maintains 30min, reaction that 1 part of mass ratio is added after terminating:1:0.25 levelling agent BYK
310th, the mixture auxiliary agent of defoamer BYK 025 and surface hardening anti-wear agent T801, after being stirred 5min, the system for the treatment of is cooled to
Room temperature, obtains polysiloxanes treatment fluid.
With spinneret as fixed bed, with polysiloxanes treatment fluid as flow fluid, under the conditions of 70 DEG C, flow fluid is set to exist
Flowed out from the rich font spinneret orifice of spinneret with the flow velocity of 0.01L/min in 0.5min, then carried out under the conditions of 95 DEG C just
Step solidification 15min, then solidified 20min again at 200 DEG C, final curing 5min finally is carried out at 260 DEG C, after natural cooling
To the spinneret orifice of low-surface-energy.Test shows that the surface energy En of the spinneret orifice of the spinneret orifice of the low-surface-energy for preparing is
34.8mJ/cm2, surface roughness Ra is 0.19 μm, and surface static contact angle WCA is 85 °.
Embodiment 8
20 parts of pH value are that 10.5, solid content is first by weight by a kind of preparation method of spinneret orifice
45wt%, average grain diameter are that 9.8, solid content is that 35wt%, average grain diameter are for the alkaline silica sol and 20 parts of pH value of 50nm
The alkaline Alumina gel mixing of 65nm, is subsequently adding the mixture as catalyst regulation system pH value of 8 parts of phosphoric acid and nitric acid, makes pH value
4.5 are maintained, phosphoric acid is 2 with the mass ratio of nitric acid:1, it is subsequently adding the mixed solvent of 20 parts of 1,3-PDs and water, 1,3- third
Glycol is 1.0 with the volume ratio of water:1, then add 38 parts of MTMSs, phenyl triethoxysilane and front threes
The mixture of base chlorosilane, and corresponding volume ratio is 1:0.25:0.1, then the 20min that is hydrolyzed at normal temperatures, then again
System is put into 80 DEG C and carries out pyrocondensation, and it is 1 that reaction maintains 75min, reaction that 3 parts of mass ratioes are added after terminating:5:0.5 stream
The mixture auxiliary agent of flat agent BYK 310, defoamer BYK 025 and surface hardening anti-wear agent T801, after being stirred 10min, treats
System is cooled to room temperature, obtains polysiloxanes treatment fluid.
With spinneret as fixed bed, with polysiloxanes treatment fluid as flow fluid, under the conditions of 85 DEG C, make flow fluid in 5min
The interior flow velocity with 10L/min is flowed out from " 8 " font spinneret orifice of spinneret, and primary solidification is then carried out under the conditions of 120 DEG C
20min, then solidified 25min again at 230 DEG C, final curing 10min finally is carried out at 280 DEG C, obtain low after natural cooling
The spinneret orifice of surface energy.Test shows that the surface energy En of the spinneret orifice of the spinneret orifice of the low-surface-energy for preparing is 35mJ/
cm2, surface roughness Ra is 0.18 μm, and surface static contact angle WCA is 86 °.
Embodiment 9
20 parts of pH value are that 10.5, solid content is first by weight by a kind of preparation method of spinneret orifice
45wt%, average grain diameter are that 9.8, solid content is that 35wt%, average grain diameter are for the alkaline silica sol and 20 parts of pH value of 50nm
The alkaline Alumina gel mixing of 65nm, is subsequently adding the mixture as catalyst regulation system pH value of 8 parts of phosphoric acid and nitric acid, makes pH value
4.5 are maintained, phosphoric acid is 2 with the mass ratio of nitric acid:1, it is subsequently adding the mixed solvent of 20 parts of 1,3-PDs and water, 1,3- third
Glycol is 1.0 with the volume ratio of water:1, then add 34 parts of MTMSs, phenyl triethoxysilane and front threes
The mixture of base chlorosilane, and corresponding volume ratio is 1:0.15:0.08, then the 20min that is hydrolyzed at normal temperatures, then again
System is put into 80 DEG C and carries out pyrocondensation, and it is 1 that reaction maintains 75min, reaction that 3 parts of mass ratioes are added after terminating:5:0.5 stream
The mixture auxiliary agent of flat agent BYK 310, defoamer BYK 025 and surface hardening anti-wear agent T801, after being stirred 10min, treats
System is cooled to room temperature, obtains polysiloxanes treatment fluid.
With spinneret as fixed bed, with polysiloxanes treatment fluid as flow fluid, under the conditions of 85 DEG C, make flow fluid in 5min
The interior flow velocity with 10L/min is flowed out from the Y-shaped spinneret orifice of spinneret, and primary solidification is then carried out under the conditions of 120 DEG C
20min, then solidified 25min again at 230 DEG C, final curing 10min finally is carried out at 280 DEG C, obtain low after natural cooling
The spinneret orifice of surface energy.Test shows that the surface energy En of the spinneret orifice of the spinneret orifice of the low-surface-energy for preparing is
34.5mJ/cm2, surface roughness Ra is 0.17 μm, and surface static contact angle WCA is 85.6 °.
Embodiment 10
16 parts of pH value are that 10.3, solid content is first by weight by a kind of processing method of spinneret orifice
40wt%, average grain diameter are that 9.6, solid content is that 30wt%, average grain diameter are for the alkaline silica sol and 17 parts of pH value of 40nm
The alkaline Alumina gel mixing of 60nm, is subsequently adding the mixture as catalyst regulation system pH value of 6 parts of formic acid and nitric acid, makes pH value
3 are maintained, formic acid is 1 with the mass ratio of nitric acid:1, it is subsequently adding the volume of the mixed solvent of 18 parts of ethanol and water, ethanol and water
Than being 1.25:1, then add the mixture of 35 parts of MTMSs and MTES, corresponding body
Product is than being 1:1, then the 18min that is hydrolyzed at normal temperatures, system is then put into 70 DEG C again carries out pyrocondensation, and reaction is maintained
60min, reaction adds 2 parts of mass ratioes after terminating be 1:3:0.3 levelling agent BYK 310, defoamer BYK 025 and surface increase
The mixture auxiliary agent of hard anti-wear agent T801, after being stirred 8min, the system for the treatment of is cooled to room temperature, obtains polysiloxanes treatment fluid.
With spinneret as fixed bed, with polysiloxanes treatment fluid as flow fluid, under the conditions of 80 DEG C, make flow fluid in 4min
The interior flow velocity with 8L/min is flowed out from " H " the type spinneret orifice of spinneret, and primary solidification is then carried out under the conditions of 100 DEG C
18min, then solidified 24min again at 220 DEG C, final curing 8min finally is carried out at 270 DEG C, low table is obtained after natural cooling
The spinneret orifice of face energy.Test shows that the surface energy En of the spinneret orifice of the spinneret orifice of the low-surface-energy for preparing is 34mJ/
cm2, surface roughness Ra is 0.19 μm, and surface static contact angle WCA is 86 °.
Claims (10)
1. a kind of processing method of spinneret orifice, it is characterized in that：It is flowing with polysiloxanes treatment fluid with spinneret as fixed bed
Liquid, under the conditions of 70~85 DEG C, makes flow fluid be flowed out from the spinneret orifice of spinneret, is then carried out under the conditions of 95~120 DEG C
Primary solidification, then solidified again at 200~230 DEG C, final curing finally is carried out at 260~280 DEG C, low table is obtained after cooling
The spinneret orifice of face energy.
2. a kind of processing method of spinneret orifice according to claim 1, it is characterised in that the polysiloxanes treatment fluid
By weight, each group is divided into：
3. a kind of processing method of spinneret orifice according to claim 2, it is characterised in that the polysiloxanes treatment fluid
Preparation method to be proportionally added into Ludox and Alumina gel, then adjust pH value with catalyst, the pH value of system is maintained 2
~4.5, solvent and siloxanes are then added, then the 15~20min that is hydrolyzed at normal temperatures, system is then put into 45 again~
80 DEG C carry out pyrocondensation, and reaction maintains 30~75min, reaction to add auxiliary agent after terminating, after being stirred 5~10min, treats
System is cooled to room temperature, obtains required polysiloxanes treatment fluid.
4. the processing method of a kind of spinneret orifice according to Claims 2 or 3, it is characterised in that the siloxanes is first
Base trimethoxy silane, MTES, ethyl triethoxysilane, trim,ethylchlorosilane and phenyltriethoxy silane
One or more of alkane.
5. a kind of processing method of spinneret orifice according to claim 4, it is characterised in that the preferred methyl of siloxanes
The mixture of trimethoxy silane, phenyl triethoxysilane and trim,ethylchlorosilane, and corresponding volume ratio is 1:0.05~
0.25:0.05~0.1.
6. the processing method of a kind of spinneret orifice according to Claims 2 or 3, it is characterised in that the Ludox is alkali
Property Ludox, its pH value is 10.3 ± 0.2, and the solid content of Ludox is 30~45wt%, and average grain diameter is 30~50nm.
7. the processing method of a kind of spinneret orifice according to Claims 2 or 3, it is characterised in that the Alumina gel is alkali
Property Alumina gel, its pH value is 9.6 ± 0.2, and the solid content of Alumina gel is 20~35wt%, and average grain diameter is 45~65nm.
8. the processing method of a kind of spinneret orifice according to Claims 2 or 3, it is characterised in that the solvent be alcohol with
The mixed solvent of water, alcohol is monohydric alcohol or dihydroxylic alcohols；And monohydric alcohol and the volume ratio of water are 1.25~1.60:1, dihydroxylic alcohols with
The volume ratio of water is 0.75~1.0:1；
Wherein monohydric alcohol is ethanol, isopropanol or butanol, and dihydroxylic alcohols is ethylene glycol or 1,3-PD；
The catalyst is one or two the mixture in formic acid, acetic acid, hydrochloric acid, phosphoric acid or nitric acid；
The auxiliary agent is the mixture of levelling agent BYK 310, defoamer BYK 025 and surface hardening anti-wear agent T801；Wherein flow
The mass ratio of flat agent, defoamer and surface hardening anti-wear agent is 1:1~5:0.25~0.5.
9. a kind of processing method of spinneret orifice according to claim 1, it is characterised in that spray of the flow fluid from spinneret
The flow velocity of silk micropore outflow is 0.01~10L/min, and the time is 0.5~5min；The primary solidification time is 15~20min；Again
Hardening time is 20~25min；The final curing time is 5~10min；Cooling uses natural cooling.
10. one kind spinneret orifice according to obtained in any one of claim 1-9 processing method, it is characterized in that：The spinneret is micro-
It is the spinneret orifice of the low-surface-energy being surface-treated by polysiloxanes treatment fluid that hole is, the surface of spinneret orifice can En≤
35mJ/cm2, surface roughness Ra≤0.2 μm, surface static contact angle WCA >=85 °.
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| CN1037158A (en) * | 1988-12-12 | 1989-11-15 | 营口市熊岳制药厂 | Preparation techlonogy for polydipheny dimethyl linear siloxane |
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| CN101139463A (en) * | 2007-10-18 | 2008-03-12 | 江苏盛虹化纤有限公司 | Silicone oil beneficial to improving board repairing quality |
| CN101235202A (en) * | 2008-02-29 | 2008-08-06 | 北京化工大学 | Silicon oil antioxidant |
| JP2011208321A (en) * | 2010-03-30 | 2011-10-20 | Kb Seiren Ltd | Method for producing fiber |
| CN104893806A (en) * | 2015-06-23 | 2015-09-09 | 东莞市佳丹润滑油有限公司 | Special nonflammable atomization silicon oil for spinneret plates of chemical fiber factories and preparation method of special nonflammable atomization silicon oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1037158A (en) * | 1988-12-12 | 1989-11-15 | 营口市熊岳制药厂 | Preparation techlonogy for polydipheny dimethyl linear siloxane |
| CN1709976A (en) * | 2004-06-18 | 2005-12-21 | 江苏日出化工有限公司 | Environment-friendly atomized silicone oil |
| CN101139463A (en) * | 2007-10-18 | 2008-03-12 | 江苏盛虹化纤有限公司 | Silicone oil beneficial to improving board repairing quality |
| CN101235202A (en) * | 2008-02-29 | 2008-08-06 | 北京化工大学 | Silicon oil antioxidant |
| JP2011208321A (en) * | 2010-03-30 | 2011-10-20 | Kb Seiren Ltd | Method for producing fiber |
| CN104893806A (en) * | 2015-06-23 | 2015-09-09 | 东莞市佳丹润滑油有限公司 | Special nonflammable atomization silicon oil for spinneret plates of chemical fiber factories and preparation method of special nonflammable atomization silicon oil |
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