CN102505158A - High-concentration preparation method for ultra-high molecular weight polyethylene fiber - Google Patents

High-concentration preparation method for ultra-high molecular weight polyethylene fiber Download PDF

Info

Publication number
CN102505158A
CN102505158A CN2011103273967A CN201110327396A CN102505158A CN 102505158 A CN102505158 A CN 102505158A CN 2011103273967 A CN2011103273967 A CN 2011103273967A CN 201110327396 A CN201110327396 A CN 201110327396A CN 102505158 A CN102505158 A CN 102505158A
Authority
CN
China
Prior art keywords
molecular weight
weight polyethylene
ultra
temperature
high molecular
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2011103273967A
Other languages
Chinese (zh)
Inventor
王宗宝
顾群
陈鹏
洪亮
鲁力
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ningbo Institute of Material Technology and Engineering of CAS
Original Assignee
Ningbo Institute of Material Technology and Engineering of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ningbo Institute of Material Technology and Engineering of CAS filed Critical Ningbo Institute of Material Technology and Engineering of CAS
Priority to CN2011103273967A priority Critical patent/CN102505158A/en
Publication of CN102505158A publication Critical patent/CN102505158A/en
Pending legal-status Critical Current

Links

Abstract

The invention relates to a high-concentration preparation method for an ultra-high molecular weight polyethylene fiber. A high-concentration spinning solution is difficult to prepare through the existing method. The method in the invention comprises the following steps: firstly, ultra-high molecular weight polyethylene resin is mixed with antioxidant and solvent, and then the mixture is swelled, so as to obtain a swelling solution; then, the swelling solution is delivered into a twin-screw extruder after being cooled and is extruded by the twin-screw extruder to obtain a high-concentration jelly ultra-high molecular weight polyethylene spinning solution; then, the jelly ultra-high molecular weight polyethylene spinning solution is spun by a metering pump and a spinneret plate, so as to obtain a jelly fiber after sizing in water bath; and finally, 2-4-grade ultra-drafting is carried out on the dried jelly fiber, so as to obtain the ultra-high molecular weight polyethylene fiber. With the adoption of the method, the concentration of the ultra-high molecular weight polyethylene spinning solution is improved, the ultra-high molecular weight polyethylene spinning solution with high intensity and high modulus is obtained, and the production efficiency is improved greatly.

Description

A kind of high concentration preparation method of superhigh molecular weight polyethylene fibers
Technical field
The invention belongs to technical field of polymer materials, relate to the high concentration preparation method of a kind of ultra-high molecular weight polyethylene (UHMWPE) fiber.
Background technology
Superhigh molecular weight polyethylene fibers is a kind of high-strength high-modulus fibre that last century, industrialization was succeeded in developing and carried out in early eighties to late nineteen seventies.Superhigh molecular weight polyethylene fibers and carbon fiber, aramid fiber also are called three big high-performance fibers.Because superhigh molecular weight polyethylene fibers has ultralight, high specific strength, high ratio modulus, superior energy absorption, multiple excellent properties such as wear-resisting, corrosion-resistant, fast light preferably, has obtained in fields such as Aero-Space, national defense and military, security protection, ocean engineering, sports equipment, power communication, medical material and civilian nettings using widely.
Superhigh molecular weight polyethylene fibers normally forms through the gel spinning prepared.Gel spinning technology is earlier ultra-high molecular weight polyethylene and suitable solvent to be processed spinning solution, generates gel fiber through after the extrusion molding then, and is again that the solvent extraction in the gel fiber is dry, obtains superhigh molecular weight polyethylene fibers through ultra doubly hot drawing-off at last.
The key technology of existing superhigh molecular weight polyethylene fibers gel spinning technology is the fully homogeneous solution of dissolving of preparation, thereby obtains the spinnability of resin.Yet because it has super high molecular weight, viscosity was very big when all resin raw materials dissolved simultaneously, needed to use the high boiling solvent high-temperature digestion, and it is harsh to prepare uniform consoluet solution condition, so be difficult to the spinning solution of preparation high concentration; And because the solution temperature that resin needs is very high, it is very big that the ultra-high molecular weight polyethylene molecular weight reduces amplitude, and the last performance that generates fiber of influence can only be improved dissolution conditions through the method for further reduction concentration, promotes fibre property.For above-mentioned reasons; Spinning solution concentration only can reach about 10% in the existing gel spinning technology; Unit production efficiency is low, energy consumption is big, manufacturing cost is high, has greatly limited UHMWPE fiber applying at civil areas such as the huge high-strength hawser of demand, industry cloth, fishing net, safety nets.Analysis and research through to polyvinyl resin with super-high molecular weight show; Comprise amorphous fraction, chain-folded lamellae and extended-chain crystal in the resin; Wherein the fusing point of chain-folded lamellae is generally 135~137 ℃; The fusing point of extended-chain crystal is generally 148~150 ℃, and the fusing point of two kinds of crystal exists than big-difference, and because extended-chain crystal is bigger than chain-folded lamellae ordering size; So it is much more difficult that the dissolving of extended-chain crystal is stranded than the dissolving of chain-folded lamellae, and along the extended-chain crystal of fiber axis orientation exactly superhigh molecular weight polyethylene fibers can obtain the structural key of high strength and high-modulus.Therefore; If in the preparation process of ultra-high molecular weight polyethylene spinning solution, keep the extended-chain crystal in the resin not dissolved; Just utilize its high rigidity to form the characteristic of similar liquid crystal solution; Can reduce the viscosity of ultra-high molecular weight polyethylene spinning solution significantly, improve its flowability, and reduce owing to the high molecular weight that causes of spinning solution preparation temperature reduces significantly.Adopt this kind method preparation the gel fiber that contains extended-chain crystal we can type of being called gel spun fiber.For the ultra-high molecular weight polyethylene extended-chain crystal that spinning solution prepared keep in the process along the fiber axially-aligned; In the forming process of class gel spun fiber, adopt the shower nozzle drawing-off; And directly extract drying after the process cold bath; Make stretching field effect lower edge gel fiber axially-aligned and the fixed orientation of extended-chain crystal, in order to obtain stable stretching field, the spinnerets of preferred hyperboloid shape guide hole in the shower nozzle drawing-off; Make frozen glue solution continuously smooth ground get into spinneret orifice, guarantee the continous-stable of stretching field.Adopt said method; Break through the technical bottleneck that only can under narrower solution concentration, obtain the resin spinnability at present; Develop and novel UHMWPE fiber high concentration preparation technology; And the concentration of dope that improves in the UHMWPE fiber production process is reduction UHMWPE fiber production and application cost, improves production capacity, realizes the important channel of the energy-saving and emission-reduction of fiber production process, environmental protection low-carbon (LC).
Summary of the invention
The objective of the invention is the deficiency to prior art, a kind of production efficiency is high, the high concentration spinning process of the preparation superhigh molecular weight polyethylene fibers of good product quality and provide.
The concrete steps of the inventive method are:
Step (1). with antioxidant and molecular weight greater than 8 * 10 5Polyvinyl resin with super-high molecular weight press mass ratio 0.1~1:100 and mix; Mix with solvent stirring at normal temperature in mulser; Every kilogram of polyvinyl resin with super-high molecular weight adds 1.5~5.67 kilograms of solvents; Put into the swelling still then and stir swelling, obtain swelling solution, swelling temperature is that 70~110 ℃, swelling time are 30~180 minutes;
Described solvent is one or more in decahydronaphthalenes, tetrahydronaphthalene, paraffin oil, kerosene, the white oil.
Step (2). swelling solution is delivered in the material storage kettle, is cooled to 30~60 ℃, send into double screw extruder then, extrude the class frozen glue ultra-high molecular weight polyethylene spinning solution that obtains high concentration.This step is to utilize chain-folded lamellae and extended-chain crystal fusing point in the polyvinyl resin with super-high molecular weight to differ bigger characteristics, adopts the method that the dissolving of the chain-folded lamellae in the UHMWPE resin is kept extended-chain crystal to prepare the class frozen glue ultra-high molecular weight polyethylene spinning solution of resin crystal block section dissolving.
The inlet temperature of described double screw extruder is that 80~130 ℃, the temperature of middle extruding lysing segment are that 130~180 ℃, outlet temperature are 160~180 ℃, and the slewing rate of double screw extruder is 30~400r/min.
Step (3). with class frozen glue ultra-high molecular weight polyethylene spinning solution process measuring pump and spinnerets spinning, typing type of obtaining gel fiber in water-bath, the vertical range between the spinnerets and the tank water surface is 1~8 centimetre; In the spinning process, apply 1.5~6 times drawing-off between the spinnerets and the tank water surface, make extended-chain crystal in stretching field effect lower edge the gel fiber axially-aligned; Type gel fiber directly extracts through after the water-bath, drying, make extended-chain crystal along fiber axis to orientation and arrange fixingly, extraction temperature is that 20~60 ℃, baking temperature are 20~60 ℃;
The guide hole of described spinnerets is half hyperboloid shape, and its minimum-value aperture is that 0.5~1.5mm, draw ratio are 2~20, the angle of outlet is 0.5~2o; Also can be cylindrical or conical, its minimum-value aperture be that 0.5~1.5mm, draw ratio are 2~20.
Step (4). dried type gel fiber is carried out 2~4 grades of ultra doubly hot drawing-offs, obtain superhigh molecular weight polyethylene fibers, the temperature of hot drawing-off is that 80~150 ℃, the general times of hot drawing-off are 10~60 times.
The present invention is employed in dissolving chain-folded lamellae in the preparation process of ultra-high molecular weight polyethylene spinning solution and keeps extended-chain lamellae; And (strand does not have orientation in the fiber of the dry back of the gel spun fiber of the gel spinning prepared of crystal CL extraction usually to make the novel high density spinning technique route that extended-chain lamellae is able to keep in the preparation process of superhigh molecular weight polyethylene fibers; And the dry back of the gel spun fiber of the novel spinning prepared of high concentration extraction is higher along the fiber axis degree of orientation; And its degree of crystallinity brings up to 48% from 30% of common gel spun fiber; Show the extended-chain crystals that exist in the gel spun fiber of high concentration spinning technique preparation in a large number along the fiber axially-aligned); Improved the concentration (20~40%) of ultra-high molecular weight polyethylene spinning solution; Obtain the superhigh molecular weight polyethylene fibers of high strength (more than the 28cN/dtex) high-modulus (more than the 1000cN/dtex), greatly improved production efficiency.
The specific embodiment
Further describe the working of an invention mode through embodiment below, but scope of the present invention not only is limited to these case study on implementation, these case study on implementation of being given only are illustrative, and are unintelligible for being limitation of the present invention.The ordinary skill of this area is according to the content of invention, and some nonessential improvement and adjustment that invention is made still belong to protection scope of the present invention.
The molecular weight of the polyvinyl resin with super-high molecular weight in following examples is greater than 8 * 10 5Used antioxidant is the conventional antioxidant of super high molecular weight polyethylene gel spinning technique; Like 2,6-di-t-butyl-4-sylvan, 3-(3,5-di-t-butyl-4-hydroxy benzenes) propionic acid stearyl, tricresyl phosphite (dodecyl) ester, tricresyl phosphite (octadecyl) ester, three sulfo-tricresyl phosphite (dodecyl) esters, tricresyl phosphite (2; 4-dimethyl benzene) ester or tricresyl phosphite (2,4-di-tert-butyl) ester.
Embodiment 1
10kg polyvinyl resin with super-high molecular weight, 40kg decahydronaphthalenes and 10g antioxidant stirring at normal temperature in mulser is even; Put into the swelling still then; Be heated to 70 ℃; Stirred swelling 180 minutes, suspension is delivered to material storage kettle through pipeline, send into double screw extruder after making suspension in material storage kettle, be cooled to 30 ℃ to push dissolving.Wherein, the inlet temperature of double screw extruder is 80 ℃, and the temperature of middle extruding lysing segment is 130 ℃, and outlet temperature is 160 ℃, and the velocity of rotation of double screw extruder is 30r/min.Suspension through twin-screw extruding dissolving to be prepared into concentration be 20% uniform ultra-high molecular weight polyethylene class frozen glue solution.With type of the obtaining gel spun fiber of in water-bath, finalizing the design behind this type of frozen glue solution process measuring pump and the spinnerets; Wherein, the spinnerets guide hole is cylindrical, and the aperture is that 1mm, draw ratio are 10; Vertical range between the spinnerets and the tank water surface is 1 centimetre, applies 1.5 times shower nozzle drawing-off.Type gel fiber directly extracts through after the water-bath, drying, and wherein, extraction temperature is that 20 ℃, baking temperature are 20 ℃.Dried gel spun fiber is carried out the two levels of thermal drawing-off, and wherein, the hot drawing temperature of one-level is 80 ℃, and drafting multiple is 4 times, and the hot drawing temperature of secondary is 120 ℃, and drafting multiple is 2.5 times, after hot drawing-off, obtains superhigh molecular weight polyethylene fibers.
Mechanics Performance Testing is carried out in sampling to fiber, and the result lists in table 1.
Embodiment 2
10kg polyvinyl resin with super-high molecular weight, 15kg tetrahydronaphthalene, 20g antioxidant stirring at normal temperature in mulser is even; Put into the swelling still then; Be heated to 80 ℃; Stirred swelling 150 minutes, suspension is delivered to material storage kettle through pipeline, send into double screw extruder after making suspension in material storage kettle, be cooled to 40 ℃ to push dissolving.Wherein, the inlet temperature of double screw extruder is 90 ℃, and the temperature of middle extruding lysing segment is 140 ℃, and outlet temperature is 160 ℃, and the velocity of rotation of double screw extruder is 60r/min.Suspension through twin-screw extruding dissolving to be prepared into concentration be 20% uniform ultra-high molecular weight polyethylene class frozen glue solution.With type of the obtaining gel spun fiber of in water-bath, finalizing the design behind this type of frozen glue solution process measuring pump and the spinnerets; Wherein, the spinnerets guide hole is conical, and the minimum-value aperture is that 0.5mm, draw ratio are 20; Vertical range between the spinnerets and the tank water surface is 2 centimetres, applies 2 times shower nozzle drawing-off.Type gel fiber directly extracts through after the water-bath, drying, and wherein, extraction temperature is that 30 ℃, baking temperature are 30 ℃.Dried gel spun fiber is carried out three grades of hot drawing-offs, and wherein, the hot drawing temperature of one-level is 80 ℃; Drafting multiple is 4 times; The hot drawing temperature of secondary is 120 ℃, and drafting multiple is 2.5 times, and three grades of hot drawing temperatures are 150 ℃; Drafting multiple is 1.8 times, after hot drawing-off, obtains superhigh molecular weight polyethylene fibers.
Mechanics Performance Testing is carried out in sampling to fiber, and the result lists in table 1.
Embodiment 3
10kg polyvinyl resin with super-high molecular weight, 20kg paraffin oil, 30g antioxidant stirring at normal temperature in mulser is even; Put into the swelling still then; Be heated to 90 ℃; Stirred swelling 120 minutes, suspension is delivered to material storage kettle through pipeline, send into double screw extruder after making suspension in material storage kettle, be cooled to 40 ℃ to push dissolving.Wherein, the inlet temperature of double screw extruder is 100 ℃, and the temperature of middle extruding lysing segment is 150 ℃, and outlet temperature is 170 ℃, and the velocity of rotation of double screw extruder is 90r/min.Suspension through twin-screw extruding dissolving to be prepared into concentration be 25% uniform ultra-high molecular weight polyethylene class frozen glue solution.With type of the obtaining gel spun fiber of in water-bath, finalizing the design behind this type of frozen glue solution process measuring pump and the spinnerets; Wherein, the spinnerets guide hole is conical, and the minimum-value aperture is that 1.5mm, draw ratio are 2; Vertical range between the spinnerets and the tank water surface is 3 centimetres, applies 3 times shower nozzle drawing-off.Type gel fiber directly extracts through after the water-bath, drying, and wherein, extraction temperature is that 40 ℃, baking temperature are 40 ℃.Dried gel spun fiber is carried out three grades of hot drawing-offs, and wherein, the hot drawing temperature of one-level is 90 ℃; Drafting multiple is 4 times; The hot drawing temperature of secondary is 130 ℃, and drafting multiple is 3 times, and three grades of hot drawing temperatures are 150 ℃; Drafting multiple is 1.8 times, after hot drawing-off, obtains superhigh molecular weight polyethylene fibers.
Mechanics Performance Testing is carried out in sampling to fiber, and the result lists in table 1.
Embodiment 4
10kg polyvinyl resin with super-high molecular weight, 30kg kerosene, 40g antioxidant stirring at normal temperature in mulser is even; Put into the swelling still then; Be heated to 100 ℃; Stirred swelling 60 minutes, suspension is delivered to material storage kettle through pipeline, send into double screw extruder after making suspension in material storage kettle, be cooled to 45 ℃ to push dissolving.Wherein, the inlet temperature of double screw extruder is 110 ℃, and the temperature of middle extruding lysing segment is 160 ℃, and outlet temperature is 170 ℃, and the velocity of rotation of double screw extruder is 120r/min.Suspension through twin-screw extruding dissolving to be prepared into concentration be 30% uniform ultra-high molecular weight polyethylene class frozen glue solution.With type of the obtaining gel spun fiber of in water-bath, finalizing the design behind this type of frozen glue solution process measuring pump and the spinnerets; Wherein, the spinnerets guide hole is conical, and the minimum-value aperture is that 1mm, draw ratio are 5; Vertical range between the spinnerets and the tank water surface is 4 centimetres, applies 4 times shower nozzle drawing-off.Type gel fiber directly extracts through after the water-bath, drying, and wherein, extraction temperature is that 50 ℃, baking temperature are 50 ℃.Dried gel spun fiber is carried out three grades of hot drawing-offs, and wherein, the hot drawing temperature of one-level is 100 ℃; Drafting multiple is 5 times; The hot drawing temperature of secondary is 130 ℃, and drafting multiple is 3 times, and three grades of hot drawing temperatures are 150 ℃; Drafting multiple is 1.8 times, after hot drawing-off, obtains superhigh molecular weight polyethylene fibers.
Mechanics Performance Testing is carried out in sampling to fiber, and the result lists in table 1.
Embodiment 5
10kg polyvinyl resin with super-high molecular weight, 56.7kg white oil, 100g antioxidant stirring at normal temperature in mulser is even; Put into the swelling still then; Be heated to 100 ℃; Stirred swelling 60 minutes, suspension is delivered to material storage kettle through pipeline, send into double screw extruder after making suspension in material storage kettle, be cooled to 50 ℃ to push dissolving.Wherein, the inlet temperature of double screw extruder is 120 ℃, and the temperature of middle extruding lysing segment is 170 ℃, and outlet temperature is 170 ℃, and the velocity of rotation of double screw extruder is 150r/min.Suspension through twin-screw extruding dissolving to be prepared into concentration be 35% uniform ultra-high molecular weight polyethylene class frozen glue solution.With type of the obtaining gel spun fiber of in water-bath, finalizing the design behind this type of frozen glue solution process measuring pump and the spinnerets; Wherein, The spinnerets guide hole is half hyperboloid shape; The minimum-value aperture is that 0.5mm, draw ratio are 20, the angle of outlet is 1o, and the vertical range between the spinnerets and the tank water surface is 5 centimetres, applies 5 times shower nozzle drawing-off.Type gel fiber directly extracts through after the water-bath, drying, and wherein, extraction temperature is that 60 ℃, baking temperature are 60 ℃.Dried gel spun fiber is carried out three grades of hot drawing-offs, and wherein, the hot drawing temperature of one-level is 110 ℃; Drafting multiple is 6 times; The hot drawing temperature of secondary is 130 ℃, and drafting multiple is 3 times, and three grades of hot drawing temperatures are 150 ℃; Drafting multiple is 1.8 times, after hot drawing-off, obtains superhigh molecular weight polyethylene fibers.
Mechanics Performance Testing is carried out in sampling to fiber, and the result lists in table 1.
Embodiment 6
10kg polyvinyl resin with super-high molecular weight, 25kg decahydronaphthalenes, 25kg tetrahydronaphthalene, 80g antioxidant stirring at normal temperature in mulser is even; Put into the swelling still then; Be heated to 110 ℃; Stirred swelling 30 minutes, suspension is delivered to material storage kettle through pipeline, send into double screw extruder after making suspension in material storage kettle, be cooled to 60 ℃ to push dissolving.Wherein, the inlet temperature of double screw extruder is 130 ℃, and the temperature of middle extruding lysing segment is 180 ℃, and outlet temperature is 180 ℃, and the velocity of rotation of double screw extruder is 200r/min.Suspension through twin-screw extruding dissolving to be prepared into concentration be 35% uniform ultra-high molecular weight polyethylene class frozen glue solution.With type of the obtaining gel spun fiber of in water-bath, finalizing the design behind this type of frozen glue solution process measuring pump and the spinnerets; Wherein, The spinnerets guide hole is half hyperboloid shape; The minimum-value aperture is that 1mm, draw ratio are 10, the angle of outlet is 0.5o, and the vertical range between the spinnerets and the tank water surface is 6 centimetres, applies 5 times shower nozzle drawing-off.Type gel spun fiber directly extracts through after the water-bath, drying, and wherein, extraction temperature is that 40 ℃, baking temperature are 60 ℃.Dried gel spun fiber is carried out three grades of hot drawing-offs, and wherein, the hot drawing temperature of one-level is 120 ℃; Drafting multiple is 7 times; The hot drawing temperature of secondary is 135 ℃, and drafting multiple is 3.4 times, and three grades of hot drawing temperatures are 150 ℃; Drafting multiple is 1.8 times, after hot drawing-off, obtains superhigh molecular weight polyethylene fibers.
Mechanics Performance Testing is carried out in sampling to fiber, and the result lists in table 1.。
Embodiment 7
10kg polyvinyl resin with super-high molecular weight, 15kg white oil, 15kg paraffin oil, 15kg kerosene, 60g antioxidant stirring at normal temperature in mulser is even; Put into the swelling still then; Be heated to 110 ℃; Stirred swelling 90 minutes, suspension is delivered to material storage kettle through pipeline, send into double screw extruder after making suspension in material storage kettle, be cooled to 60 ℃ to push dissolving.Wherein, the inlet temperature of double screw extruder is 130 ℃, and the temperature of middle extruding lysing segment is 180 ℃, and outlet temperature is 180 ℃, and the velocity of rotation of double screw extruder is 400r/min.Suspension through twin-screw extruding dissolving to be prepared into concentration be 40% uniform ultra-high molecular weight polyethylene class frozen glue solution.With type of the obtaining gel spun fiber of in water-bath, finalizing the design behind this type of frozen glue solution process measuring pump and the spinnerets; Wherein, The spinnerets guide hole is half hyperboloid shape; The minimum-value aperture is that 1.5mm, draw ratio are 2, the angle of outlet is 2o, and the vertical range between the spinnerets and the tank water surface is 8 centimetres, applies 6 times shower nozzle drawing-off.Type gel spun fiber directly extracts through after the water-bath, drying, and wherein, extraction temperature is that 50 ℃, baking temperature are 60 ℃.Dried gel spun fiber is carried out the hot drawing-off of level Four, and wherein, the hot drawing temperature of one-level is 90 ℃; Drafting multiple is 4 times, and the hot drawing temperature of secondary is 120 ℃, and drafting multiple is 3 times; Three grades of hot drawing temperatures are 135 ℃, and drafting multiple is 2.5 times, and three grades of hot drawing temperatures are 150 ℃; Drafting multiple is 2 times, after hot drawing-off, obtains superhigh molecular weight polyethylene fibers.
Mechanics Performance Testing is carried out in sampling to fiber, and the result lists in table 1.
Table 1, the superhigh molecular weight polyethylene fibers embodiment performance table of comparisons
? Concentration (%) Hot drawing-off general times Fiber number (dtex) Intensity (cN/dtex) Modulus (cN/dtex) Percentage elongation (%)
Embodiment 1 20 10.0 5.0 28.1 1023 5.0
Embodiment 2 20 18.0 4.5 28.9 1086 4.6
Embodiment 3 25 21.6 4.2 29.2 1123 4.4
Embodiment 4 30 27.0 3.6 29.7 1176 4.1
Embodiment 5 35 32.4 4.0 30.5 1210 3.6
Embodiment 6 35 42.8 4.0 31.2 1244 3.2
Embodiment 7 40 60.0 2.2 33.7 1325 2.4

Claims (5)

1. the high concentration preparation method of a superhigh molecular weight polyethylene fibers is characterized in that the concrete steps of this method are:
Step (1). with antioxidant and molecular weight greater than 8 * 10 5Polyvinyl resin with super-high molecular weight press mass ratio 0.1~1:100 and mix; Mix with solvent stirring at normal temperature in mulser; Every kilogram of polyvinyl resin with super-high molecular weight adds 1.5~5.67 kilograms of solvents; Put into the swelling still then and stir swelling, obtain swelling solution, swelling temperature is that 70~110 ℃, swelling time are 30~180 minutes;
Step (2). swelling solution is delivered in the material storage kettle, is cooled to 30~60 ℃, send into double screw extruder then, extrude the class frozen glue ultra-high molecular weight polyethylene spinning solution that obtains high concentration;
Step (3). with class frozen glue ultra-high molecular weight polyethylene spinning solution process measuring pump and spinnerets spinning, typing type of obtaining gel fiber in water-bath, the vertical range between the spinnerets and the tank water surface is 1~8 centimetre; In the spinning process, apply 1.5~6 times drawing-off between the spinnerets and the tank water surface; Type gel fiber directly extracts through after the water-bath, drying, and extraction temperature is that 20~60 ℃, baking temperature are 20~60 ℃;
Step (4). dried type gel fiber is carried out 2~4 grades of ultra doubly hot drawing-offs, obtain superhigh molecular weight polyethylene fibers, the temperature of hot drawing-off is that 80~150 ℃, the general times of hot drawing-off are 10~60 times.
2. the high concentration preparation method of a kind of superhigh molecular weight polyethylene fibers as claimed in claim 1 is characterized in that the solvent described in the step (1) is one or more in decahydronaphthalenes, tetrahydronaphthalene, paraffin oil, kerosene, the white oil.
3. the high concentration preparation method of a kind of superhigh molecular weight polyethylene fibers as claimed in claim 1; The inlet temperature that it is characterized in that the double screw extruder described in the step (2) is that 80~130 ℃, the temperature of middle extruding lysing segment are that 130~180 ℃, outlet temperature are 160~180 ℃, and the slewing rate of double screw extruder is 30~400r/min.
4. the high concentration preparation method of a kind of superhigh molecular weight polyethylene fibers as claimed in claim 1; The guide hole that it is characterized in that the described spinnerets of step (3) is half hyperboloid shape, and its minimum-value aperture is that 0.5~1.5mm, draw ratio are 2~20, the angle of outlet is 0.5~2o.
5. the high concentration preparation method of a kind of superhigh molecular weight polyethylene fibers as claimed in claim 1 is characterized in that the guide hole of the described spinnerets of step (3) is cylindrical or conical, and its minimum-value aperture is that 0.5~1.5mm, draw ratio are 2~20.
CN2011103273967A 2011-10-25 2011-10-25 High-concentration preparation method for ultra-high molecular weight polyethylene fiber Pending CN102505158A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2011103273967A CN102505158A (en) 2011-10-25 2011-10-25 High-concentration preparation method for ultra-high molecular weight polyethylene fiber

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2011103273967A CN102505158A (en) 2011-10-25 2011-10-25 High-concentration preparation method for ultra-high molecular weight polyethylene fiber

Publications (1)

Publication Number Publication Date
CN102505158A true CN102505158A (en) 2012-06-20

Family

ID=46217286

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2011103273967A Pending CN102505158A (en) 2011-10-25 2011-10-25 High-concentration preparation method for ultra-high molecular weight polyethylene fiber

Country Status (1)

Country Link
CN (1) CN102505158A (en)

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103243404A (en) * 2013-05-03 2013-08-14 中国科学院宁波材料技术与工程研究所 Preparation method of ultrahigh molecular weight polyethylene nanometer composite material
CN106319667A (en) * 2016-08-19 2017-01-11 中国科学院化学研究所 Fiber prepared with solubilizing type ultra-high molecular weight ultrathin polyethylene and preparation method thereof
CN106498532A (en) * 2016-10-21 2017-03-15 东华大学 A kind of preparation method of superhigh molecular weight polyethylene fibers
CN106555240A (en) * 2016-11-23 2017-04-05 中国纺织科学研究院 A kind of preparation method and fiber of high-performance polyethylene fibres
CN106591981A (en) * 2017-02-21 2017-04-26 青岛信泰科技有限公司 Production device of compound graphene high-strength high-mold polyethylene fiber and preparation method thereof
CN108623818A (en) * 2018-06-06 2018-10-09 深圳大学 Ultra-high molecular weight polyethylene and its chemistry auxiliary dissolving method and application
CN108950711A (en) * 2018-09-06 2018-12-07 山东莱威新材料有限公司 A kind of superhigh molecular weight polyethylene flat silk and preparation method thereof
CN109306061A (en) * 2018-06-06 2019-02-05 深圳大学 The preparation method and ultra high molecular weight polyethylene fiber of ultra-high molecular weight polyethylene spinning solution
CN110658036A (en) * 2019-09-05 2020-01-07 上海化工研究院有限公司 Preparation of UHMWPE dilute solution and method for detecting dissolution degree of UHMWPE dilute solution
CN110867548A (en) * 2018-08-27 2020-03-06 中国石油化工股份有限公司 Polyethylene and separator and use
CN111005079A (en) * 2019-12-18 2020-04-14 黑龙江金源仑特种纤维有限公司 Method for manufacturing ultra-high molecular weight polyethylene monofilament fiber
CN111254511A (en) * 2020-01-19 2020-06-09 上海化工研究院有限公司 Low-temperature spun superfine denier ultra-high molecular weight polyethylene fiber and preparation method thereof
CN112111802A (en) * 2019-06-20 2020-12-22 北京鼎中新材料技术研究院有限公司 Ultrahigh-strength ultrahigh molecular weight polyethylene fiber and manufacturing method thereof
KR20210028286A (en) * 2016-08-19 2021-03-11 인스티튜트 오브 케미스트리, 차이니즈 아카데미 오브 사이언시즈 Ultra-high molecular weight, ultra-fine particle size polyethylene, preparation method therefor and use thereof
CN112725918A (en) * 2020-12-23 2021-04-30 中国纺织科学研究院有限公司 Preparation method of polyethylene fiber and fiber
CN115323518A (en) * 2022-05-27 2022-11-11 宁波大学 Preparation method of ultra-high molecular weight polyethylene fiber

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1190137A (en) * 1997-12-10 1998-08-12 中国纺织大学 Continuous preparation of homogeneous solution of superhigh molecular weight polythene
CN101967688A (en) * 2010-09-21 2011-02-09 中国科学院宁波材料技术与工程研究所 Method for preparing ultrahigh molecular weight polyethylene fibers

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1190137A (en) * 1997-12-10 1998-08-12 中国纺织大学 Continuous preparation of homogeneous solution of superhigh molecular weight polythene
CN101967688A (en) * 2010-09-21 2011-02-09 中国科学院宁波材料技术与工程研究所 Method for preparing ultrahigh molecular weight polyethylene fibers

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103243404B (en) * 2013-05-03 2015-03-25 中国科学院宁波材料技术与工程研究所 Preparation method of ultrahigh molecular weight polyethylene nanometer composite material
CN103243404A (en) * 2013-05-03 2013-08-14 中国科学院宁波材料技术与工程研究所 Preparation method of ultrahigh molecular weight polyethylene nanometer composite material
CN106319667A (en) * 2016-08-19 2017-01-11 中国科学院化学研究所 Fiber prepared with solubilizing type ultra-high molecular weight ultrathin polyethylene and preparation method thereof
US11530281B2 (en) 2016-08-19 2022-12-20 Institute Of Chemistry, Chinese Academy Of Sciences Ultra-high molecular weight, ultra-fine particle size polyethylene, preparation method therefor and use thereof
KR102317083B1 (en) * 2016-08-19 2021-10-25 인스티튜트 오브 케미스트리, 차이니즈 아카데미 오브 사이언시즈 Ultra-high molecular weight, ultra-fine particle size polyethylene, preparation method therefor and use thereof
KR20210028286A (en) * 2016-08-19 2021-03-11 인스티튜트 오브 케미스트리, 차이니즈 아카데미 오브 사이언시즈 Ultra-high molecular weight, ultra-fine particle size polyethylene, preparation method therefor and use thereof
CN106498532A (en) * 2016-10-21 2017-03-15 东华大学 A kind of preparation method of superhigh molecular weight polyethylene fibers
CN106555240B (en) * 2016-11-23 2020-04-07 中国纺织科学研究院有限公司 Preparation method of high-performance polyethylene fiber and fiber
CN106555240A (en) * 2016-11-23 2017-04-05 中国纺织科学研究院 A kind of preparation method and fiber of high-performance polyethylene fibres
CN106591981A (en) * 2017-02-21 2017-04-26 青岛信泰科技有限公司 Production device of compound graphene high-strength high-mold polyethylene fiber and preparation method thereof
CN108623818A (en) * 2018-06-06 2018-10-09 深圳大学 Ultra-high molecular weight polyethylene and its chemistry auxiliary dissolving method and application
CN109306061A (en) * 2018-06-06 2019-02-05 深圳大学 The preparation method and ultra high molecular weight polyethylene fiber of ultra-high molecular weight polyethylene spinning solution
CN110867548B (en) * 2018-08-27 2023-06-06 中国石油化工股份有限公司 Polyethylene and separator and use
CN110867548A (en) * 2018-08-27 2020-03-06 中国石油化工股份有限公司 Polyethylene and separator and use
CN108950711A (en) * 2018-09-06 2018-12-07 山东莱威新材料有限公司 A kind of superhigh molecular weight polyethylene flat silk and preparation method thereof
CN112111802B (en) * 2019-06-20 2022-06-10 李乾坤 Ultrahigh-strength ultrahigh molecular weight polyethylene fiber and manufacturing method thereof
CN112111802A (en) * 2019-06-20 2020-12-22 北京鼎中新材料技术研究院有限公司 Ultrahigh-strength ultrahigh molecular weight polyethylene fiber and manufacturing method thereof
CN110658036A (en) * 2019-09-05 2020-01-07 上海化工研究院有限公司 Preparation of UHMWPE dilute solution and method for detecting dissolution degree of UHMWPE dilute solution
CN110658036B (en) * 2019-09-05 2022-05-06 上海化工研究院有限公司 Preparation of UHMWPE dilute solution and method for detecting dissolution degree of UHMWPE dilute solution
CN111005079B (en) * 2019-12-18 2021-09-03 黑龙江金源仑特种纤维有限公司 Method for manufacturing ultra-high molecular weight polyethylene monofilament fiber
CN111005079A (en) * 2019-12-18 2020-04-14 黑龙江金源仑特种纤维有限公司 Method for manufacturing ultra-high molecular weight polyethylene monofilament fiber
CN111254511B (en) * 2020-01-19 2022-11-08 上海化工研究院有限公司 Low-temperature spun superfine denier ultra-high molecular weight polyethylene fiber and preparation method thereof
CN111254511A (en) * 2020-01-19 2020-06-09 上海化工研究院有限公司 Low-temperature spun superfine denier ultra-high molecular weight polyethylene fiber and preparation method thereof
CN112725918A (en) * 2020-12-23 2021-04-30 中国纺织科学研究院有限公司 Preparation method of polyethylene fiber and fiber
CN115323518A (en) * 2022-05-27 2022-11-11 宁波大学 Preparation method of ultra-high molecular weight polyethylene fiber

Similar Documents

Publication Publication Date Title
CN102505158A (en) High-concentration preparation method for ultra-high molecular weight polyethylene fiber
CN101230499B (en) Coloured high-strength polyethylene fibre and method for manufacturing same
CN101328626A (en) Method for continuously preparing regenerated cellulose fibre
CN106544747B (en) A kind of ultra-high molecular weight polyethylene colored fibers manufacturing method
CN103305954A (en) Method for preparing ultra-high molecular weight polyethylene fiber
CN101886295A (en) Ultra-high molecular weight polyethylene colored fibers and preparation method thereof
WO2012062053A1 (en) Preparation method for ultrahigh molecular weight polyethylene fiber
CN104419996A (en) Production method of ultrahigh molecular weight polyethylene fiber
CN102226300B (en) Preparation method of high strength polyethylene fiber and special device thereof
CN103866416B (en) A kind of preparation method of ultra-high molecular weight polyethylene colored fibers
CN103352266B (en) Preparation method for cellulose and thermoplastic polymer skin-core type composite fiber
CN110079881B (en) Preparation method of environment-friendly high-strength high-modulus polyethylene fiber
US20180134851A1 (en) Process for preparing cellulose solution and equipment therefor
CN101235551A (en) High-shearing ultra-high molecular weight polythene continuous dissolving spinning method
CN101575743B (en) Preparation method of spinning solution of ultra-high molecular weight polyethylene fiber
CN101967686B (en) Method for preparing ultra-high molecular weight polyethylene fiber spinning solution
CN109385689A (en) A kind of spinning process that ultra-high molecular weight polyethylene is blended
CN101718003B (en) Method for producing ultra-high molecular weight polyethylene colored fine denier fiber
CN108004605A (en) Strong porous superhigh molecular weight polyethylene fibers and preparation method in one kind
CN101736411A (en) Method for preparing polyacrylonitrile spinning solution for carbon fiber
CN102644126B (en) Preparation method for high-strength polyethylene fibers with net structures
CN101787577A (en) Novel method for preparing gel fiber
CN101307507A (en) High-strength high-modulo ultra-high molecular weight polyethylene hollow flat fiber preparation method
CN104278338B (en) Gel spinning method for manufacturing aramid fiber III
CN103122489A (en) Ultrahigh molecular weight polyethylene monofilament combination and stretching forming method

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20120620