CN111041586A - Preparation process of bulletproof high-strength polyethylene fiber applied to special clothing - Google Patents
Preparation process of bulletproof high-strength polyethylene fiber applied to special clothing Download PDFInfo
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- CN111041586A CN111041586A CN201911384751.7A CN201911384751A CN111041586A CN 111041586 A CN111041586 A CN 111041586A CN 201911384751 A CN201911384751 A CN 201911384751A CN 111041586 A CN111041586 A CN 111041586A
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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
- 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
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a preparation process of bulletproof high-strength polyethylene fibers applied to special clothing, and belongs to the technical field of printing and dyeing textile. When preparing the product, firstly treating the ultrahigh molecular weight polyethylene by using oxygen plasma, then carrying out oxidation treatment by using a sodium periodate solution, then mixing the ultrahigh molecular weight polyethylene, the graphene oxide, the layered silicate and the glass fiber short fiber, and carrying out melt spinning to obtain the product; the glass fiber short fiber is glass fiber short fiber with surface adsorbed with nano silicon dioxide, and graphene oxide can be treated with sodium polystyrene sulfonate before being added. The product obtained by the invention has excellent strength and impact resistance.
Description
Technical Field
The invention relates to the technical field of printing and dyeing textile, in particular to a preparation process of bulletproof high-strength polyethylene fibers applied to special clothing.
Background
A woven structure of ultra-high molecular weight polyethylene fibers has an important influence on the bulletproof performance of a composite material, an ultra-high molecular weight polyethylene fiber orthogonal-laid layer, plain weave, twill weave and weft-knitted biaxial fabric structure is used as a reinforcement, low-density polyethylene is used as a base body, and the bulletproof composite material is prepared.
In addition, although the woven structure of the ultra-high molecular weight polyethylene fibers has an important influence on the bulletproof performance of the composite material, the influence of the performance of the fibers on the bulletproof performance cannot be ignored. When the composite material is impacted by the elastic sheet, the crack can be expanded to the fiber, if the interface bonding strength is weaker, the crack can be transferred to the direction and is expanded along the fiber, and if the crack can be organized to expand through the structure of the fiber or the characteristics of the material or the stress diffusion in the expansion process is weakened, the impact of the elastic sheet on the whole composite material can be properly reduced, and the impact toughness of the product is improved.
Disclosure of Invention
The invention aims to provide a preparation process of bulletproof high-strength polyethylene fibers applied to special clothing, and aims to overcome the defect that the mechanical property of ultrahigh molecular weight polyethylene fibers in the prior art is insufficient.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation process of bulletproof high-strength polyethylene fibers applied to special clothing comprises the following specific preparation steps:
(1) pretreatment of ultrahigh molecular weight polyethylene: treating the ultra-high molecular weight polyethylene with oxygen plasma;
(2) and (3) oxidation: oxidizing the pretreated ultrahigh molecular weight polyethylene by using a sodium periodate solution;
(3) spinning: and mixing the oxidized ultrahigh molecular weight polyethylene, the oxidized graphene and the layered silicate, and carrying out melt spinning to obtain the product.
According to the technical scheme, the ultrahigh molecular weight polyethylene is treated by oxygen plasma, the molecular structure of the ultrahigh molecular weight polyethylene is changed by bombardment of the plasma, so that subsequent sodium periodate oxidation reaction is facilitated, polar oxygen-containing functional groups such as carboxyl, carbonyl and the like are formed at the position bombarded by the plasma, the formed oxygen-containing functional groups and carboxyl, hydroxyl or epoxy in the molecular structure of the graphene oxide can be subjected to dehydration condensation in the heating and melting process to form chemical bonding, the graphene oxide is stably dispersed in an ultrahigh molecular weight polyethylene fiber matrix, a good toughening and reinforcing effect is achieved, in addition, the graphene oxide is of a layered structure, and gaps among layers of the graphene oxide can play a good deformation buffering role when a product is impacted by an elastic sheet, so that the impact resistance of the product is improved.
Further, the spinning in the step (3) comprises the following steps: and mixing the oxidized ultrahigh molecular weight polyethylene, the oxidized graphene, the layered silicate and the glass fiber short fibers, and carrying out melt spinning to obtain the product.
According to the technical scheme, the glass fiber short fibers are further introduced into the ultrahigh molecular weight polyethylene fiber matrix, when strong elastic sheet impact force is applied, fracture failure of the product is usually gradually expanded from the crack, the short fibers can have a good blocking effect at the crack, further expansion of the crack is avoided, in addition, no obvious interaction force exists between the short fibers, the short fibers can be well dispersed in a system, the short fibers can be filled in a better density with the same mass of addition, so that the short fibers are continuously blocked by the short fibers in the crack expansion process, and the impact resistance of the product is effectively improved.
Further, the preparation process of the glass fiber short fiber comprises the following steps: mixing nano silicon dioxide, a silane coupling agent and an ethanol solution for reaction, and then filtering, washing and drying to obtain modified nano silicon dioxide; and heating, stirring and reacting the modified nano-silica, the anhydrous alcohol and the glass fiber short fibers, filtering and drying.
According to the technical scheme, the smooth surface of the glass fiber is further coated with the nano silicon dioxide, so that the roughness of the surface of the glass fiber is improved, after the nano silicon dioxide is added into a product, a macromolecular chain of the linear ultrahigh molecular weight polyethylene fiber and the nano silicon dioxide on the surface of the glass fiber are favorably wound and attached, and in the stress process of the product, the mutual slippage of all components is effectively avoided, and the overall mechanical property of the product is improved.
Further, the preparation process of the graphene oxide is as follows: mixing graphene oxide, sodium polystyrene sulfonate and deionized water, carrying out ultrasonic reaction, and carrying out spray drying.
According to the technical scheme, the sodium polystyrene sulfonate is further utilized to modify the graphene oxide, in the treatment process, benzene rings in the molecular structure of the sodium polystyrene sulfonate can interact with the graphene oxide conjugate zone to be adsorbed, so that negative charges are charged at the edge of the graphene oxide lamellar structure, the interlayer spacing of the graphene oxide lamellar structure is widened due to the mutual repulsion of the same charges, the widened interlayer spacing can better play a role in deformation buffering when a product is impacted by an elastic sheet, and the impact resistance of the product is further improved.
Further, the phyllosilicate is acid-modified sepiolite.
Further, the preparation process of the acid modified sepiolite comprises the following steps: mixing sepiolite and hydrochloric acid, carrying out hydrothermal reaction, filtering, washing and drying.
Further, the oxygen plasma treatment is as follows: and (3) in a plasma reactor, under the conditions of controlling the oxygen pressure to be 40-60 Pa and the oxygen flow to be 8-10 mL/min, carrying out plasma treatment for 20-30 min.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Modified glass fiber short fiber: according to the weight parts, sequentially taking 10-20 parts of nano silicon dioxide, 8-10 parts of silane coupling agent KH-560 and 80-120 parts of ethanol solution with the mass fraction of 10-90%, mixing, stirring and reacting for 30-60 min under the condition that the stirring rotating speed is 100-500 r/min, filtering, washing and drying to obtain modified nano silicon dioxide; and sequentially taking 10-15 parts of modified nano silicon dioxide, 80-100 parts of absolute ethyl alcohol and 30-50 parts of a material with a length-diameter ratio of 5: 1, heating, stirring and reacting for 45-60 min at the temperature of 55-65 ℃ and the stirring speed of 300-500 r/min after mixing, filtering and drying to obtain modified glass fiber short fibers;
modified graphene oxide: according to the weight parts, 10-30 parts of graphene oxide, 3-5 parts of sodium polystyrene sulfonate and 80-150 parts of deionized water are sequentially taken, mixed, subjected to ultrasonic reaction for 30-60 min under the condition that the ultrasonic frequency is 40-80 kHz, and then subjected to spray drying to obtain modified graphene oxide;
acid-modified sepiolite: mixing sepiolite and hydrochloric acid with the mass fraction of 1-10% in a mass ratio of 1: 5-1: 10, mixing, pouring into a hydrothermal kettle, carrying out hydrothermal reaction for 2-4 h at the temperature of 150-200 ℃, filtering, washing a filter cake with deionized water until a washing liquid is neutral, transferring the filter cake into a drying oven, and drying at the temperature of 100-110 ℃ until the weight is constant to obtain the acid modified sepiolite;
transferring the ultra-high molecular weight polyethylene into a plasma reactor, and carrying out plasma treatment for 20-30 min in an oxygen atmosphere under the conditions that the oxygen pressure is controlled to be 40-60 Pa and the oxygen flow is 8-10 mL/min;
and (2) treating the ultrahigh molecular weight polyethylene subjected to oxygen plasma treatment and a sodium periodate solution with the mass fraction of 3-10% in a mass ratio of 1: 5-1: 10, heating, stirring and reacting for 45-60 min under the conditions that the temperature is 55-75 ℃ and the rotating speed is 300-500 r/min;
according to the weight parts, 80-100 parts of oxidized ultrahigh molecular weight polyethylene, 8-10 parts of modified graphene oxide, 3-5 parts of acid modified sepiolite and 8-10 parts of modified glass fiber short fiber are sequentially taken, stirred and mixed, subjected to melt spinning, stretched and rolled to obtain the product.
Example 1
Modified glass fiber short fiber: according to the weight parts, sequentially taking 10 parts of nano-silica, 8 parts of silane coupling agent KH-560 and 80 parts of ethanol solution with the mass fraction of 10%, mixing, stirring and reacting for 30min under the condition that the stirring speed is 100r/min, and filtering, washing and drying to obtain modified nano-silica; then according to the parts by weight, sequentially taking 10 parts of modified nano silicon dioxide, 80 parts of absolute ethyl alcohol, and 30 parts of a silicon dioxide/silicon dioxide composite material with the length-diameter ratio of 5: 1, mixing, heating, stirring and reacting for 45min at the temperature of 55 ℃ and the stirring speed of 300r/min, filtering and drying to obtain modified glass fiber short fibers;
modified graphene oxide: according to the weight parts, 10 parts of graphene oxide, 3 parts of sodium polystyrene sulfonate and 80 parts of deionized water are sequentially taken, mixed, subjected to ultrasonic reaction for 30min under the condition that the ultrasonic frequency is 40kHz, and then subjected to spray drying to obtain modified graphene oxide;
acid-modified sepiolite: mixing sepiolite and hydrochloric acid with the mass fraction of 1% according to the mass ratio of 1: 5, mixing, pouring into a hydrothermal kettle, carrying out hydrothermal reaction for 2 hours at the temperature of 150 ℃, filtering, washing a filter cake with deionized water until a washing liquid is neutral, transferring the filter cake into a drying oven, and drying at the temperature of 100 ℃ to constant weight to obtain the acid modified sepiolite;
transferring the ultra-high molecular weight polyethylene into a plasma reactor, and carrying out plasma treatment for 20min in an oxygen atmosphere under the conditions that the oxygen pressure is controlled to be 40Pa and the oxygen flow is 8 mL/min;
and (2) mixing the ultra-high molecular weight polyethylene treated by the oxygen plasma with a sodium periodate solution with the mass fraction of 3% according to the mass ratio of 1: 5, after mixing, heating, stirring and reacting for 45min at the temperature of 55 ℃ and the rotating speed of 300 r/min;
according to the weight parts, 80 parts of oxidized ultrahigh molecular weight polyethylene, 8 parts of modified graphene oxide, 3 parts of acid modified sepiolite and 8 parts of modified glass fiber short fiber are sequentially taken, stirred and mixed, subjected to melt spinning, stretched and rolled to obtain the product.
Example 2
Modified glass fiber short fiber: taking 15 parts of nano-silica, 9 parts of silane coupling agent KH-560 and 100 parts of 50% ethanol solution in sequence by weight, mixing, stirring and reacting for 50min at the stirring speed of 300r/min, filtering, washing and drying to obtain modified nano-silica; and then according to the parts by weight, sequentially taking 12 parts of modified nano silicon dioxide, 90 parts of absolute ethyl alcohol, 40 parts of a silicon dioxide/silicon dioxide composite material with the length-diameter ratio of 5: 1, mixing, heating, stirring and reacting for 50min at the temperature of 60 ℃ and the stirring speed of 400r/min, filtering and drying to obtain modified glass fiber short fibers;
modified graphene oxide: according to the weight parts, 20 parts of graphene oxide, 4 parts of sodium polystyrene sulfonate and 120 parts of deionized water are sequentially taken, mixed, subjected to ultrasonic reaction for 50min under the condition that the ultrasonic frequency is 50kHz, and then subjected to spray drying to obtain modified graphene oxide;
acid-modified sepiolite: mixing sepiolite and 5% hydrochloric acid according to a mass ratio of 1: 8, mixing, pouring into a hydrothermal kettle, carrying out hydrothermal reaction for 3 hours at the temperature of 180 ℃, filtering, washing a filter cake with deionized water until a washing liquid is neutral, transferring the filter cake into a drying oven, and drying at the temperature of 105 ℃ to constant weight to obtain the acid modified sepiolite;
transferring the ultra-high molecular weight polyethylene into a plasma reactor, and carrying out plasma treatment for 25min in an oxygen atmosphere under the conditions that the oxygen pressure is controlled to be 50Pa and the oxygen flow is 9 mL/min;
and (2) mixing the ultra-high molecular weight polyethylene treated by the oxygen plasma with a sodium periodate solution with the mass fraction of 5% according to the mass ratio of 1: 8, mixing, heating, stirring and reacting for 50min at the temperature of 65 ℃ and the rotating speed of 400 r/min;
according to the weight parts, 90 parts of oxidized ultrahigh molecular weight polyethylene, 9 parts of modified graphene oxide, 4 parts of acid modified sepiolite and 9 parts of modified glass fiber short fiber are sequentially taken, stirred and mixed, and then melt spinning, stretching and rolling are carried out, so as to obtain the product.
Example 3
Modified glass fiber short fiber: according to the weight parts, 20 parts of nano-silica, 10 parts of silane coupling agent KH-560 and 120 parts of 90% ethanol solution are sequentially taken, mixed and stirred for reaction for 60min under the condition that the stirring speed is 500r/min, and then filtered, washed and dried to obtain modified nano-silica; and then according to the parts by weight, sequentially taking 15 parts of modified nano silicon dioxide, 100 parts of absolute ethyl alcohol, 50 parts of modified nano silicon dioxide with the length-diameter ratio of 5: 1, mixing, heating, stirring and reacting for 60min at the temperature of 65 ℃ and the stirring speed of 500r/min, filtering and drying to obtain modified glass fiber short fibers;
modified graphene oxide: according to the weight parts, 30 parts of graphene oxide, 5 parts of sodium polystyrene sulfonate and 150 parts of deionized water are sequentially taken, mixed, subjected to ultrasonic reaction for 60min under the condition that the ultrasonic frequency is 80kHz, and then subjected to spray drying to obtain modified graphene oxide;
acid-modified sepiolite: mixing sepiolite and 10% hydrochloric acid according to a mass ratio of 1: 10, mixing and pouring the mixture into a hydrothermal kettle, carrying out hydrothermal reaction for 4 hours at the temperature of 200 ℃, filtering, washing a filter cake with deionized water until a washing liquid is neutral, transferring the filter cake into a drying oven, and drying the filter cake to constant weight at the temperature of 110 ℃ to obtain acid modified sepiolite;
transferring the ultra-high molecular weight polyethylene into a plasma reactor, and carrying out plasma treatment for 30min in an oxygen atmosphere under the conditions that the oxygen pressure is controlled to be 60Pa and the oxygen flow is 10 mL/min;
and (2) mixing the ultra-high molecular weight polyethylene treated by the oxygen plasma with a sodium periodate solution with the mass fraction of 10% according to the mass ratio of 1: 10, heating, stirring and reacting for 60min at the temperature of 75 ℃ and the rotating speed of 500 r/min;
according to the weight parts, 100 parts of oxidized ultrahigh molecular weight polyethylene, 10 parts of modified graphene oxide, 5 parts of acid modified sepiolite and 10 parts of modified glass fiber short fiber are sequentially taken, stirred and mixed, and then melt spinning, stretching and rolling are carried out, so as to obtain the product.
Comparative example 1
This comparative example compared to example 1, no nanosilica was added and the remaining conditions were kept unchanged.
Comparative example 2
In comparison with example 1, no graphene oxide was added, and the remaining conditions were maintained.
Comparative example 3
This comparative example compared to example 1, no acid modified sepiolite was added and the remaining conditions remained the same.
Comparative example 4
In comparison with example 1, graphene oxide is not modified, and the remaining conditions remain the same.
Comparative example 5
The sepiolite was not modified in this comparative example compared to example 1, and the remaining conditions remained unchanged.
The products obtained in examples 1 to 3 and comparative examples 1 to 5 were subjected to performance tests, the specific test modes and test results are as follows:
the breaking strength of the fiber is measured by using a universal electronic material testing machine, and the testing conditions are as follows: the length of the sample is 1000mm, the effective length of the sample is 500mm, the stretching speed is 300mm/min, and the pre-tension is the mass of the length of the fiber (250). During the test, the effective data is at least 5 times, and an average value is taken. The breaking strength was calculated as:
breaking strength ═ filament maximum tensile breaking strength x sample length ÷ (9 × 9.8 × sample mass)
The specific test results are as follows:
| detecting items | Stretching temperature/. degree.C | Breaking strength/g/dtex |
| Example 1 | 80 | 10.2 |
| Example 2 | 75 | 11.6 |
| Example 3 | 70 | 12.6 |
| Detecting items | Stretching temperature/. degree.C | Breaking strength/g/dtex |
| Comparative example 1 | 80 | 5.5 |
| Comparative example 2 | 80 | 5.2 |
| Comparative example 3 | 80 | 5.1 |
| Comparative example 4 | 80 | 6.2 |
| Comparative example 5 | 80 | 6.5 |
As can be seen from the detection results in Table 1, compared with the test results of the comparative example, the technical scheme of the application has an obvious effect of improving the mechanical properties of the product.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference thereto is therefore intended to be embraced therein.
Claims (7)
1. A preparation process of bulletproof high-strength polyethylene fibers applied to special clothing is characterized by comprising the following specific preparation steps:
(1) pretreatment of ultrahigh molecular weight polyethylene: treating the ultra-high molecular weight polyethylene with oxygen plasma;
(2) and (3) oxidation: oxidizing the pretreated ultrahigh molecular weight polyethylene by using a sodium periodate solution;
(3) spinning: and mixing the oxidized ultrahigh molecular weight polyethylene, the oxidized graphene and the layered silicate, and carrying out melt spinning to obtain the product.
2. The process for preparing the bulletproof high-strength polyethylene fiber applied to special clothing according to claim 1, wherein the spinning in the step (3) comprises the following steps: and mixing the oxidized ultrahigh molecular weight polyethylene, the oxidized graphene, the layered silicate and the glass fiber short fibers, and carrying out melt spinning to obtain the product.
3. The preparation process of the bulletproof high-strength polyethylene fiber applied to special clothing according to claim 2, wherein the preparation process of the glass fiber short fiber is as follows: mixing nano silicon dioxide, a silane coupling agent and an ethanol solution for reaction, and then filtering, washing and drying to obtain modified nano silicon dioxide; and heating, stirring and reacting the modified nano-silica, the anhydrous alcohol and the glass fiber short fibers, filtering and drying.
4. The process for preparing the bulletproof high-strength polyethylene fiber applied to special clothing according to any one of claims 1 or 2, wherein the preparation process of the graphene oxide is as follows: mixing graphene oxide, sodium polystyrene sulfonate and deionized water, carrying out ultrasonic reaction, and carrying out spray drying.
5. The process for preparing the bulletproof high-strength polyethylene fiber applied to special clothing according to any one of the claims 1 or 2, wherein the phyllosilicate is acid-modified sepiolite.
6. The preparation process of the bulletproof high-strength polyethylene fiber applied to special clothing according to claim 5, wherein the preparation process of the acid modified sepiolite comprises the following steps: mixing sepiolite and hydrochloric acid, carrying out hydrothermal reaction, filtering, washing and drying.
7. The process for preparing the bulletproof high-strength polyethylene fiber applied to special clothing according to claim 1, wherein the oxygen plasma treatment comprises the following steps: and (3) in a plasma reactor, under the conditions of controlling the oxygen pressure to be 40-60 Pa and the oxygen flow to be 8-10 mL/min, carrying out plasma treatment for 20-30 min.
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| CN115028883A (en) * | 2022-06-10 | 2022-09-09 | 龚伟锋 | Preparation method of flame-retardant silica aerogel |
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