CN107841796B - Preparation method of ultra-high molecular weight polyethylene fiber and ultra-high molecular weight polyethylene fiber prepared by same - Google Patents
Preparation method of ultra-high molecular weight polyethylene fiber and ultra-high molecular weight polyethylene fiber prepared by same Download PDFInfo
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- CN107841796B CN107841796B CN201610838145.8A CN201610838145A CN107841796B CN 107841796 B CN107841796 B CN 107841796B CN 201610838145 A CN201610838145 A CN 201610838145A CN 107841796 B CN107841796 B CN 107841796B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
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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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Abstract
The invention belongs to the field of fiber preparation technology, and provides a preparation method of an ultrahigh molecular weight polyethylene fiber and the prepared ultrahigh molecular weight polyethylene fiber. The preparation method comprises the following steps: selecting ultra-high molecular weight polyethylene powder, and adding solvent oil, an antioxidant and a modifier into the ultra-high molecular weight polyethylene powder; feeding the spinning solution into a double-screw extruder for blending and extruding; feeding the spinning solution into a filter, and extruding the spinning solution through a spinneret plate by a metering pump; sequentially extracting, drying and primary drawing. The ultra-high molecular weight polyethylene fiber is prepared according to the preparation method. According to the invention, the modifier is added in the spinning solution, so that the rheological property of the spinning solution is increased, the viscosity of the spinning solution is reduced, the spinnability of the product is improved, and the first-level drafting is used for replacing the traditional third-level drafting in the back-end drafting process, so that the product inspection index can meet the requirement, and meanwhile, the energy consumption is reduced, the occupied area and the cost are saved, and the time and the labor are saved.
Description
Technical Field
The invention relates to the field of fiber preparation, in particular to a preparation method of ultra-high molecular weight polyethylene fibers and the ultra-high molecular weight polyethylene fibers prepared by the preparation method.
Background
The ultra-high molecular weight polyethylene fiber belongs to scarce materials worldwide and has large gaps. According to the prediction of experts, the annual market demand of the ultrahigh molecular weight polyethylene fiber in the next 10 years is more than 10 million tons, and the ultrahigh molecular weight polyethylene fiber has huge market potential and broad prospect.
At the end of the last 70 s of the last century, Gel spinning (Gel spinning) was used by the Dusmann company in the Netherlands to spin ultra-high molecular weight polyethylene fibers successfully.
The high-end market for ultra-high molecular weight polyethylene fibers is in the rope net manufacturing industry, followed by the use for ballistic protection sheets (UD). The ultra-high molecular weight polyethylene fiber in China is mainly used for manufacturing stab-resistant armor, body armor, bulletproof helmets, ropes, ocean fishing nets, fishing lines, labor protection and the like, and part of the fiber is exported to countries and regions such as Europe, America, Asia and the like. The national defense field is gradually used in China, the civil field is also popularized and used, and the annual market demand is about more than 10000 tons. With the realization of large-scale industrial production of ultra-high molecular weight polyethylene fibers in China and the reduction of production cost and product price, the research and development of China in the national defense and civil application fields are certainly and rapidly driven, particularly in the civil field (ropes, ocean fishing nets, mariculture and labor protection), the application range is continuously expanded, the society is more and more extensive, and the market demand is kept vigorously increased. The development of the ultra-high molecular weight polyethylene fiber in China has remarkable strategic significance to national defense construction and military equipment.
In the production cost of conventional manufacturers at present, the proportion of power consumption is nearly half, and the energy consumption is huge. Therefore, a method for preparing ultra-high molecular weight polyethylene fiber which can reduce energy consumption is required.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of an ultrahigh molecular weight polyethylene fiber and the prepared ultrahigh molecular weight polyethylene fiber, so as to achieve the purposes of reducing energy consumption and saving cost.
In a first aspect, the present invention provides a method for preparing ultra-high molecular weight polyethylene fibers, comprising the steps of:
selecting ultra-high molecular weight polyethylene powder, and adding solvent oil, an antioxidant and a modifier into the ultra-high molecular weight polyethylene powder to obtain spinning stock solution;
feeding the spinning stock solution into a double-screw extruder for blending and extruding to obtain a spinning solution;
feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain primary gel yarns;
and sequentially extracting, drying and primary drafting the nascent gel filaments to finally obtain the ultra-high molecular weight polyethylene fiber.
Optionally, the primary drawing has a drawing magnification of 10-100 and a drawing temperature of 120-.
Optionally, the weight average molecular weight of the ultra-high molecular weight polyethylene powder is 1 × 106－6×106。
Further, the weight average molecular weight of the ultra-high molecular weight polyethylene powder is 2 x 106－5×106。
Further, the weight average molecular weight of the ultra-high molecular weight polyethylene powder is 3X 106。
Optionally, the solvent oil comprises the following components in parts by weight: 70-95 parts of cycloalkanes and 5-30 parts of chain hydrocarbons, wherein the cycloalkanes and the chain hydrocarbons each contain 25-50 carbon atoms.
Optionally, the antioxidant is selected from any one or more than two of 2, 6-di-tert-butylphenol, 2, 4, 6-tri-tert-butylphenol or triphenyl phosphite, wherein the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 0.1-1: 200.
optionally, the modifier is selected from one or more than two of acid anhydride, diamine, dihydric alcohol, dibasic acid, polyalcohol and polybasic acid, wherein the mass ratio of the modifier to the ultra-high molecular weight polyethylene powder is 0.1-1: 100.
optionally, the twin screw extruder has a length to diameter ratio of at least 40.
In a second aspect, the ultra-high molecular weight polyethylene fiber provided by the invention is prepared by the preparation method of the ultra-high molecular weight polyethylene fiber, wherein the crystallinity of the polyethylene fiber is more than 75%, the orientation degree is more than 90%, the breaking strength is more than 38g/d, and the modulus is more than 1500 g/d.
According to the preparation method of the ultra-high molecular weight polyethylene fiber and the ultra-high molecular weight polyethylene fiber prepared by the preparation method, the modifier is added into the spinning solution, so that the rheological property of the spinning solution is increased, the viscosity of the spinning solution is reduced, the spinnability of the product is improved, and the traditional three-level drafting is replaced by the primary drafting in the back drafting process, so that the product inspection index can meet the requirement, the energy consumption is reduced, the occupied area and the cost are saved, and the time and the labor are saved.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or portions are generally identified by like reference numerals. In the drawings, elements or portions are not necessarily drawn to scale.
Fig. 1 shows a flow chart of a method for preparing ultra-high molecular weight polyethylene fibers according to an embodiment of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
Fig. 1 shows a flow chart of a method for preparing ultra-high molecular weight polyethylene fibers according to an embodiment of the present invention. Referring to fig. 1, the method comprises the following steps:
step 1, selecting ultra-high molecular weight polyethylene powder, and adding solvent oil, an antioxidant and a modifier into the ultra-high molecular weight polyethylene powder to obtain a spinning solution;
step 2, feeding the spinning stock solution into a double-screw extruder for blending and extruding to obtain a spinning solution;
step 3, feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain primary gel yarns;
and 4, sequentially extracting, drying and primary drafting the nascent gel filaments to finally obtain the ultra-high molecular weight polyethylene fibers.
According to the preparation method of the ultra-high molecular weight polyethylene fiber and the ultra-high molecular weight polyethylene fiber prepared by the preparation method, the modifier is added into the spinning solution, so that the rheological property of the spinning solution is increased, the viscosity of the spinning solution is reduced, the spinnability of the product is improved, and the traditional three-level drafting is replaced by the primary drafting in the later drafting process, so that the product inspection index can meet the requirement, the energy consumption is reduced, the occupied area and the cost are saved, and the time and the labor are saved.
The three-stage drafting adopts four groups of drafting rollers and three hot boxes to draft the product, and the three hot boxes are respectively arranged between the adjacent drafting rollers. And the primary drafting adopts two groups of drafting rollers and a hot box to draft the product, and the hot box is arranged between the two groups of drafting rollers. The primary drafting can reduce the floor area of the drafting equipment while ensuring the performance of products, and can also greatly save electric energy.
Wherein the drafting multiplying power of the primary drafting is 10-100, and the drafting temperature is 120-200 ℃.
Wherein the weight average molecular weight of the ultra-high molecular weight polyethylene powder is 1 x 106－6×106. Further, the weight average molecular weight of the ultra-high molecular weight polyethylene powder is 2 x 106－5×106. Further, the weight average molecular weight of the ultra-high molecular weight polyethylene powder is 3X 106。
Wherein the solvent oil comprises the following components in parts by weight: 70-95 parts of cycloalkanes and 5-30 parts of chain hydrocarbons, wherein the cycloalkanes and the chain hydrocarbons each contain 25-50 carbon atoms.
Wherein the antioxidant is selected from any one or more than two of 2, 6-di-tert-butylphenol, 2, 4, 6-tri-tert-butylphenol or triphenyl phosphite, wherein the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 0.1-1: 200.
wherein the modifier is selected from one or more than two of anhydride, diamine, dihydric alcohol, dibasic acid, polyalcohol and polybasic acid, wherein the mass ratio of the modifier to the ultra-high molecular weight polyethylene powder is 0.1-1: 100.
wherein the twin-screw extruder has a length to diameter ratio of at least 40.
Wherein, the extraction adopts microwave oscillation to assist the extraction, so as to ensure the extraction effect.
Wherein, the drying adopts a drying mode of top air suction and bottom side air supply, thereby ensuring the drying effect.
The ultrahigh molecular weight polyethylene fiber provided by the invention is prepared by the preparation method of the ultrahigh molecular weight polyethylene fiber, the crystallinity of the polyethylene fiber is more than 75%, the orientation degree is more than 90%, the breaking strength is more than 38g/d, and the modulus is more than 1500 g/d.
The following examples are provided for the preparation of ultra-high molecular weight polyethylene fibers of the present invention.
Example 1
1. Selecting ultra-high molecular weight polyethylene powder with weight average molecular weight of 450 ten thousand, and adding solvent oil, antioxidant and modifier into the ultra-high molecular weight polyethylene powder to obtain spinning solution. Wherein the solvent oil comprises 70 parts of naphthene and 5 parts of chain hydrocarbon, the naphthene contains 25 carbon atoms, the chain hydrocarbon contains 50 carbon atoms respectively, the antioxidant is 2, 6-ditert-butyl phenol, and the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 1: 2000. the modifier is acid anhydride, and the mass ratio of the modifier to the ultrahigh molecular weight polyethylene powder is 1: 100.
2. and feeding the spinning solution into a double-screw extruder for blending and extruding to obtain a spinning solution.
3. And (3) feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain the nascent gel silk.
4. Sequentially extracting, drying and primary drawing the nascent gel silk, wherein the drawing multiplying power of the primary drawing is 10, the drawing temperature is 200 ℃, and the drying air volume is 30000m3/h。
Example 2
1. Selecting ultra-high molecular weight polyethylene powder with weight average molecular weight of 400 ten thousand, and adding solvent oil, antioxidant and modifier into the ultra-high molecular weight polyethylene powder to obtain spinning solution. Wherein the solvent oil comprises 75 parts of naphthene and 10 parts of chain hydrocarbon, the naphthene contains 28 carbon atoms, the chain hydrocarbon contains 49 carbon atoms respectively, the antioxidant is 2, 4, 6-tributylphenol, and the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 1: 1000. the modifier is diamine, and the mass ratio of the modifier to the ultrahigh molecular weight polyethylene powder is 9: 1000.
2. and feeding the spinning solution into a double-screw extruder for blending and extruding to obtain a spinning solution.
3. And (3) feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain the nascent gel silk.
4. Sequentially extracting, drying and primary drawing the nascent gel silk, wherein the drawing multiplying power of the primary drawing is 20, the drawing temperature is 200 ℃, and the drying air volume is 29000m3/h。
Example 3
1. Selecting ultra-high molecular weight polyethylene powder with the weight-average molecular weight of 500 ten thousand, and adding solvent oil, an antioxidant and a modifier into the ultra-high molecular weight polyethylene powder to obtain spinning solution. Wherein the solvent oil comprises 80 parts of cycloparaffin and 15 parts of chain hydrocarbon, the cycloparaffin contains 30 carbon atoms, the chain hydrocarbon contains 44 carbon atoms respectively, the antioxidant is triphenyl phosphite, and the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 3: 2000. the modifier is dihydric alcohol, and the mass ratio of the modifier to the ultrahigh molecular weight polyethylene powder is 1: 125.
2. and feeding the spinning solution into a double-screw extruder for blending and extruding to obtain a spinning solution.
3. And (3) feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain the nascent gel silk.
4. Sequentially extracting, drying and primary drawing the nascent gel silk, wherein the drawing multiplying power of the primary drawing is 30, the drawing temperature is 190 ℃, and the drying air volume is 31000m3/h。
Example 4
1. Selecting ultra-high molecular weight polyethylene powder with the weight-average molecular weight of 600 ten thousand, and adding solvent oil, an antioxidant and a modifier into the ultra-high molecular weight polyethylene powder to obtain spinning solution. Wherein the solvent oil comprises 85 parts of cycloparaffins and 20 parts of chain hydrocarbons, the cycloparaffins contain 32 carbon atoms, the chain hydrocarbons contain 39 carbon atoms respectively, the antioxidant is a mixture of 2, 6-di-tert-butylphenol and 2, 4, 6-tri-tert-butylphenol, and the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 1: 500. the modifier is dibasic acid, and the mass ratio of the modifier to the ultrahigh molecular weight polyethylene powder is 7: 1000.
2. and feeding the spinning solution into a double-screw extruder for blending and extruding to obtain a spinning solution.
3. And (3) feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain the nascent gel silk.
4. Sequentially extracting, drying and primary drawing the as-spun gel filaments, wherein the drawing ratio of the primary drawing is 40, the drawing temperature is 180 ℃, and the drying air volume is 28000m3/h。
Example 5
1. Selecting ultra-high molecular weight polyethylene powder with the weight-average molecular weight of 300 ten thousand, and adding solvent oil, an antioxidant and a modifier into the ultra-high molecular weight polyethylene powder to obtain spinning solution. Wherein the solvent oil comprises 90 parts of cycloalkane and 25 parts of chain hydrocarbon, the cycloalkane contains 36 carbon atoms, the chain hydrocarbon contains 37 carbon atoms respectively, the antioxidant is a mixture of 2, 6-ditert-butyl phenol and triphenyl phosphite, and the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 1: 400. the modifier is polyhydric alcohol, and the mass ratio of the modifier to the ultrahigh molecular weight polyethylene powder is 3: 500.
2. and feeding the spinning solution into a double-screw extruder for blending and extruding to obtain a spinning solution.
3. And (3) feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain the nascent gel silk.
4. Sequentially extracting, drying and primary drawing the as-spun gel filaments, wherein the drawing multiplying power of the primary drawing is 50, the drawing temperature is 170 ℃, and the drying air volume is 32000m3/h。
Example 6
1. Selecting ultra-high molecular weight polyethylene powder with the weight-average molecular weight of 200 ten thousand, and adding solvent oil, an antioxidant and a modifier into the ultra-high molecular weight polyethylene powder to obtain spinning solution. Wherein the solvent oil comprises 95 parts of cycloalkane and 30 parts of chain hydrocarbon, the cycloalkane contains 39 carbon atoms, the chain hydrocarbon contains 34 carbon atoms respectively, the antioxidant is a mixture of 2, 4, 6-tributylphenol and triphenyl phosphite, and the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 3: 1000. the modifier is polybasic acid, and the mass ratio of the modifier to the ultrahigh molecular weight polyethylene powder is 1: 200.
2. and feeding the spinning solution into a double-screw extruder for blending and extruding to obtain a spinning solution.
3. And (3) feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain the nascent gel silk.
4. Sequentially extracting, drying and primary drawing the nascent gel silk, wherein the drawing multiplying power of the primary drawing is 60, the drawing temperature is 160 ℃, and the drying air volume is 27000m3/h。
Example 7
1. Selecting ultra-high molecular weight polyethylene powder with the weight-average molecular weight of 100 ten thousand, and adding solvent oil, an antioxidant and a modifier into the ultra-high molecular weight polyethylene powder to obtain spinning solution. Wherein the solvent oil comprises 87 parts of naphthenic hydrocarbon and 18 parts of chain hydrocarbon, the naphthenic hydrocarbon contains 42 carbon atoms, the chain hydrocarbon contains 30 carbon atoms respectively, the antioxidant is a mixture of 2, 6-ditert-butyl phenol, 2, 4, 6-tritert-butyl phenol and triphenyl phosphite, and the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 7: 2000. the modifier is a mixture of anhydride and diamine, and the mass ratio of the modifier to the ultrahigh molecular weight polyethylene powder is 1: 250.
2. and feeding the spinning solution into a double-screw extruder for blending and extruding to obtain a spinning solution.
3. And (3) feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain the nascent gel silk.
4. Sequentially extracting, drying and primary drawing the nascent gel silk, wherein the drawing multiplying power of the primary drawing is 70, the drawing temperature is 150 ℃, and the drying air volume is 33000m3/h。
Example 8
1. Selecting ultrahigh molecular weight polyethylene powder with weight average molecular weight of 550 ten thousand, and adding solvent oil, antioxidant and modifier to obtain spinning solution. The solvent oil comprises 92 parts of cycloparaffin and 12 parts of chain hydrocarbon, the cycloparaffin contains 46 carbon atoms, the chain hydrocarbon contains 28 carbon atoms respectively, the antioxidant is 2, 6-ditert-butyl phenol, and the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 1: 250. The modifier is a mixture of dihydric alcohol and dibasic acid, and the mass ratio of the modifier to the ultrahigh molecular weight polyethylene powder is 3: 1000.
2. and feeding the spinning solution into a double-screw extruder for blending and extruding to obtain a spinning solution.
3. And (3) feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain the nascent gel silk.
4. Sequentially extracting, drying and primary drawing the as-spun gel filaments, wherein the drawing multiplying power of the primary drawing is 80, the drawing temperature is 140 ℃, and the drying air volume is 26000m3/h。
Example 9
1. Selecting ultra-high molecular weight polyethylene powder with the weight-average molecular weight of 350 ten thousand, and adding solvent oil, an antioxidant and a modifier into the ultra-high molecular weight polyethylene powder to obtain spinning solution. Wherein the solvent oil comprises 78 parts of cycloalkanes and 24 parts of chain hydrocarbons, the cycloalkanes contain 48 carbon atoms, the chain hydrocarbons respectively contain 26 carbon atoms, the antioxidant is 2, 4, 6-tributylphenol, and the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 9: 2000. the modifier is a mixture of polyalcohol and polybasic acid, and the mass ratio of the modifier to the ultrahigh molecular weight polyethylene powder is 1: 500.
2. and feeding the spinning solution into a double-screw extruder for blending and extruding to obtain a spinning solution.
3. And (3) feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain the nascent gel silk.
4. Sequentially extracting, drying and primary drawing the as-spun gel filaments, wherein the drawing multiplying power of the primary drawing is 90, the drawing temperature is 130 ℃, and the drying air volume is 34000m3/h。
Example 10
1. Selecting ultra-high molecular weight polyethylene powder with weight average molecular weight of 450 ten thousand, and adding solvent oil, antioxidant and modifier into the ultra-high molecular weight polyethylene powder to obtain spinning solution. Wherein the solvent oil comprises 88 parts of cycloparaffin and 28 parts of chain hydrocarbon, the cycloparaffin contains 50 carbon atoms, the chain hydrocarbon contains 25 carbon atoms respectively, the antioxidant is triphenyl phosphite, and the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 1: 200. the modifier is a mixture of acid anhydride, diamine, dihydric alcohol, dibasic acid, polybasic acid and polybasic acid, and the mass ratio of the modifier to the ultrahigh molecular weight polyethylene powder is 1: 1000.
2. and feeding the spinning solution into a double-screw extruder for blending and extruding to obtain a spinning solution.
3. And (3) feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain the nascent gel silk.
4. Sequentially extracting, drying and primary drawing the as-spun gel filaments, wherein the drawing ratio of the primary drawing is 100, the drawing temperature is 120 ℃, and drying is carried outThe dry air volume is 30000m3/h。
Table 1 shows the performance parameters of the ultra-high molecular weight polyethylene fibers obtained in examples 1 to 10. Referring to Table 1, it can be seen that the polyethylene fiber has a fiber fineness of 2000-4000D, a crystallinity of more than 75%, an orientation degree of more than 90%, a breaking strength of more than 38g/D, and a modulus of more than 1500 g/D.
TABLE 1 Properties of ultra high molecular weight polyethylene fibers obtained in examples 1-10
| Test items | Fiber fineness (D) | Breaking Strength (g/d) | Degree of crystallinity | Degree of orientation | Modulus (g/d) |
| Example 1 | 2400 | 38 | 75.2％ | 91.7％ | 1510 |
| Example 2 | 2600 | 41 | 76.1％ | 92.0％ | 1530 |
| Example 3 | 2800 | 42 | 75.8％ | 92.3％ | 1620 |
| Example 4 | 2400 | 41 | 76.8％ | 93.3％ | 1610 |
| Example 5 | 2000 | 43 | 75.7％ | 92.4％ | 1580 |
| Example 6 | 3000 | 42 | 75.6％ | 92.7％ | 1610 |
| Example 7 | 4000 | 41 | 76.4％ | 92.9％ | 1590 |
| Example 8 | 3500 | 42 | 77.2％ | 92.0％ | 1530 |
| Example 9 | 3600 | 43 | 75.8％ | 92.8％ | 1550 |
| Example 10 | 3800 | 41 | 75.9％ | 91.9％ | 1570 |
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. In all examples shown and described herein, unless otherwise specified, any particular value should be construed as merely illustrative, and not restrictive, and thus other examples of example embodiments may have different values.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (7)
1. A preparation method of ultra-high molecular weight polyethylene fiber is characterized by comprising the following steps:
selecting ultra-high molecular weight polyethylene powder, and adding solvent oil, an antioxidant and a modifier into the ultra-high molecular weight polyethylene powder to obtain spinning stock solution;
feeding the spinning stock solution into a double-screw extruder for blending and extruding to obtain a spinning solution;
feeding the spinning solution into a filter, and extruding the spinning solution through a metering pump and a spinneret plate to obtain primary gel yarns;
sequentially extracting, drying and primary drafting the as-spun gel filaments to finally obtain the ultra-high molecular weight polyethylene fibers;
the drafting magnification of the primary drafting is 10-100, and the drafting temperature is 120-200 ℃;
the antioxidant is selected from any one or more than two of 2, 6-di-tert-butylphenol, 2, 4, 6-tri-tert-butylphenol or triphenyl phosphite, wherein the mass ratio of the antioxidant to the ultrahigh molecular weight polyethylene powder is 0.1-1: 200 of a carrier;
the modifier is selected from one or more than two of anhydride, diamine, dihydric alcohol, dibasic acid, polybasic acid and polybasic acid, wherein the mass ratio of the modifier to the ultra-high molecular weight polyethylene powder is 0.1-1: 100.
2. the method of claim 1, wherein the weight average molecular weight of the ultra-high molecular weight polyethylene powder is 1 x 106－6×106。
3. The method of claim 2, wherein the weight average molecular weight of the ultra-high molecular weight polyethylene powder is 2 x 106－5×106。
4. The method of claim 3, wherein the weight average molecular weight of the ultra-high molecular weight polyethylene powder is 3X 106。
5. The method for preparing ultra-high molecular weight polyethylene fiber according to claim 1, wherein the solvent oil comprises the following components in parts by weight: 70-95 parts of cycloalkanes and 5-30 parts of chain hydrocarbons, wherein the cycloalkanes and the chain hydrocarbons each contain 25-50 carbon atoms.
6. Process for the preparation of ultra-high molecular weight polyethylene fibres according to any one of claims 1 to 5, characterised in that the twin-screw extruder has an aspect ratio of at least 40.
7. Ultra-high molecular weight polyethylene fiber obtainable by the process for the preparation of ultra-high molecular weight polyethylene fiber according to any of claims 1 to 6, wherein the polyethylene fiber has a crystallinity of more than 75%, an orientation degree of more than 90%, a breaking strength of more than 38g/d and a modulus of more than 1500 g/d.
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| CN109306541B (en) * | 2018-09-14 | 2020-06-05 | 上海化工研究院有限公司 | Preparation method of high-strength high-modulus polyethylene fiber |
| CN112111802B (en) * | 2019-06-20 | 2022-06-10 | 李乾坤 | Ultrahigh-strength ultrahigh molecular weight polyethylene fiber and manufacturing method thereof |
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| CN101775666A (en) * | 2010-01-22 | 2010-07-14 | 东华大学 | Preparation method of high-strength high-modulus polyethylene fiber |
| EP2639346A1 (en) * | 2010-11-08 | 2013-09-18 | Ningbo Dacheng Advanced Material Co., Ltd | Preparation method for ultrahigh molecular weight polyethylene fiber |
| CN105734708A (en) * | 2014-12-12 | 2016-07-06 | 北京同益中特种纤维技术开发有限公司 | Preparation method of cut-resistant ultrahigh-molecular-weight polyethylene fiber |
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