CN102400375A - Method for producing modified ultrahigh molecular weight polyethylene fiber by using mutual radiation grafting technology - Google Patents
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Abstract
The invention relates to a method for producing a modified ultrahigh molecular weight polyethylene fiber by using a mutual radiation grafting technology. Operations of a mutual radiation grafting and production operations of an ultrahigh molecular weight polyethylene fiber are connected to form a serialized production technology for preparing and modifying the ultrahigh molecular weight polyethylene fiber. The method comprises specific steps of: drawing the ultrahigh molecular weight polyethylene fiber into a grafting liquid bath by a tractor and dipping in the grafting liquid; carrying out electron beam mutual radiation grafting modification on the dipped ultrahigh molecular weight polyethylene fiber; washing the fiber with water to remove impurities after irradiation; and finally drying to obtain a product. Compared with a prior art, the method of the invention has advantages of convenient operation, industrialized continuous production and promotion of usage of the ultrahigh molecular weight polyethylene fiber in fiber reinforced composite.
Description
Technical field
The present invention relates to a kind of fiber surface modification technology, be intended to improve superhigh molecular weight polyethylene fibers surface adhesion performance, belong to the polymer surface modification field.
Background technology
Ultra-high molecular weight polyethylene (UHMWPE) fiber, it is to succeed in developing late 1970s and get into a kind of high-performance fiber of industrialization the beginning of the eighties, and this kind fiber has height-oriented extended-chain configuration, and density has only 0.97g/cm
3, light weight, chemical stability is good, has very strong chemical inertness, and strong acid, strong base solution and organic solvent have no influence to its intensity; Have good weather, after the 1500h Exposure to Sunlight, the fibre strength conservation rate is still up to 80%, and ultra-violet resistance can be very superior; Lower temperature resistance is good, and serviceability temperature can be low to moderate-150 ℃; In addition, wear-resisting resistance to bend(ing) ability, tension force fatigue behaviour, the anti-cutting performance of superhigh molecular weight polyethylene fibers also are the strongest in the existing high-performance fiber.Bringing into play very important effect in safety, protection, Aeronautics and Astronautics, defence equipment, vehicle manufacturing, shipbuilding industry, sporting world.In addition, superhigh molecular weight polyethylene fibers also has wide application prospect in the civilian industry field as shock resistance, vibration-absorptive material and high-performance light composite.But superhigh molecular weight polyethylene fibers also exists some to treat improved shortcoming, does not have a stronger interaction force (like hydrogen bond) as intermolecular; Creep resistance is poor; Strand is linear structure, does not have phenyl ring isopolarity functional group, causes its fusing point lower; Processing temperature is less than 140 ℃, and the sensitiveness of serviceability temperature is bigger etc.; Particularly as far as the superhigh molecular weight polyethylene fibers composite, fiber is made up of simple methylene, makes fiber surface not only have no the reactivity point; Be difficult to form chemical bonded refractory and close, and methylene is nonpolar, add the highly crystalline that super drawing is shaped, height-oriented smooth surface with resin; Make its surface energy extremely low; Be difficult for being soaked into, do not have coarse surface again, be difficult for producing stronger interaction force between fiber molecule and molecular resin for forming the mechanical engagement point by resin; Cause the cementability of fiber and resin matrix relatively poor; Thereby make phenomenons such as fibre reinforced composites in use are prone to come unstuck, resin matrix cracking, largely limit superhigh molecular weight polyethylene fibers in the particularly application in lightweight structural material field of composite, so superhigh molecular weight polyethylene fibers is carried out surface modification treatment; Improve the interfacial adhesion strength of itself and resin matrix, become one of important topic of composite science research.
At present; Improve the method for the interfacial adhesion strength between superhigh molecular weight polyethylene fibers and resin matrix; Can carry out surface modification through methods such as chemical reagent oxidizes, plasma treatment, Corona discharge Treatment, photooxidation surface modification treatment; Make the activation of superhigh molecular weight polyethylene fibers inactive surfaces layer, realize at nonpolar fiber surface introducing hydroxyl, carboxyl isopolarity group, for example:
Chinese patent document CN1035308A discloses a kind of method that improves superhigh molecular weight polyethylene fibers surface adhesion property.It adopts the method for superhigh molecular weight polyethylene fibers being carried out plasma treatment.The method can effectively improve wettability and the surface adhesion intensity of fiber to resin matrix.But this method appointed condition requires high, and there is difficulty in industrialization, and the improper meeting of treatment conditions causes the mechanical properties decrease of fiber.
People such as Israel Silverstein are at article Composite Science Technology; 1993; 48:151～157 and Journal of Materials Science, 1993, report in 28:4718～4724; Superhigh molecular weight polyethylene fibers is after the perchromic acid etching, and the oxygen content of fiber surface increases gradually.And with the prolongation of handling the time, the variation that falling after rising appears in the interface shear strength of fiber and epoxy resin, behind the processing 4h, interface shear strength reaches maximum.The method is helpful to the surface polarity that improves fiber, but can damage the intensity of superhigh molecular weight polyethylene fibers, reduces its use value in composite, and produces a large amount of waste liquids, and is unfavorable to environmental protection.
American documentation literature USP4870136 discloses a kind of method that improves the fiber surface adhesive property; The method is earlier with a certain proportion of UHMWPE powder, radical initiator, silane compound and diluent melting mixing in the screw rod machine; Carry out the plasticising melt spinning; Cause the silanization graft reaction of accomplishing UHMWPE in the spinning stage through heat, the fiber with spinning carries out hot-stretch in the medium of extractant and crosslinking agent then, in boiling water, accomplishes cross-linking reaction again.The adhesive property of this method gained fiber surface improves; But because it has added a large amount of initators and graft compound and after graft reaction is accomplished, has stretched again in the UHMWPE fiber spinning dope; Thereby cause the tensile fiber multiple lower, the mechanical property of gained UHMWPE fiber is relatively poor.
A kind of method that improves the fiber surface adhesive property is disclosed among the american documentation literature USP6172163.The method be utilize poly high crystalline can, adopt the method for pure physics, the fiber surface amorphous region is dissolved after crystallization and at fiber surface formation one deck " molecular brush " again.Behind the UHMWPE fiber and resin compounded with the processing of this kind method, the fiber adhesive property is greatly improved, but this method operation is loaded down with trivial details, and process conditions are harsh, and deal with improperly and also can cause the UHMWPE fibrous mechanical property significantly to descend.
Chinese patent document CN1693544A discloses a kind of method of the UHMWPE of raising fiber surface cementability.The method is that polar polymer is dissolved in the conventional extractant of UHMWPE gel spun fiber; Process composite extractant; The UHMWPE gel spun fiber is extracted in composite extractant, postprocessing working procedures such as drawn is processed the UHMWPE fiber that adhesive property improves a lot then again.Though this method can keep original intensity of UHMWPE fiber preferably, it is limited that the fiber adhesive strength improves degree, do not reach practical target.
Summary of the invention
The object of the invention is exactly to provide a kind of easy to operate for the defective that overcomes above-mentioned prior art existence; But industrialization is produced continuously, the mutual radiation crosslinking technology that promotes the use of superhigh molecular weight polyethylene fibers in the fibre reinforced composites is produced the method for modified ultra-high molecular weight polyethylene fiber.
The object of the invention can be realized through following technical scheme: the mutual radiation crosslinking technology is produced the method for modified ultra-high molecular weight polyethylene fiber; It is characterized in that; The operation of mutual radiation grafting is linked to each other with the production process of superhigh molecular weight polyethylene fibers; Forming the continuous production technology of superhigh molecular weight polyethylene fibers preparation and modification, specifically is earlier superhigh molecular weight polyethylene fibers to be got into grafting liquid drill traverse stain grafting liquid through the hauling machine traction, again the superhigh molecular weight polyethylene fibers behind the dipping is carried out the graft modification of electron beam mutual radiation; Wash removal impurity behind the fiber irradiation, carry out dried at last and promptly get product.
The fracture strength of described superhigh molecular weight polyethylene fibers is higher than 20cN/dtex, and modulus is higher than 600cN/dtex, and molecular weight is 500,000～8,000,000, and the speed controlling of described traction is 2～15m/min.
Described grafting liquid is by graft modification monomer, swelling agent, polymerization inhibitor and solvent composition.
Described graft modification monomer is the various acrylic monomers of existing superhigh molecular weight polyethylene fibers graft modification; Described swelling agent be selected from chloroform, dichloroethanes and trichloro-ethylene one of them; Described polymerization inhibitor is Cu
2+Or Fe
2+Salt; Described solvent is deionized water, ethanol or acetone.
Described grafting liquid is benchmark with the solvent, and said graft modification monomer concentration is 1～20mol/L, and said swelling agent concentration is 0.03～5mol/L, and said inhibitor concentration is 0.001～0.06mol/L.
The radiation dose rate average out to 5～70KGy/S of described electron beam mutual radiation grafting, irradiation reaction atmosphere is selected N
2, Ar or C
2H
2A kind of in the gas.
Described washing is ultrasonic washing, the ultrasonic energy 1kW～5kW of ultrasonic washing, and washing temperature is 25～40 ℃.
The temperature of described dried is 25～50 ℃.
Compared with prior art; The present invention introduces the mutual radiation graft process on existing fiberline; Utilize the new technology of mutual radiation grafting to realize online modification to superhigh molecular weight polyethylene fibers; Also online simultaneously coupling washing and dry aided process; Ultrasonic washing is intended to remove the impurity such as homopolymers of the superhigh molecular weight polyethylene fibers surface adhesion after the mutual radiation graft modification, and dry purpose is drying fibrous, realizes that the industrialization of modified ultra-high molecular weight polyethylene fiber is produced continuously.
Advantage of the present invention is the surface modification of super-high molecular-weight polyethylene fiber surface effect obvious; Keep the intensity of superhigh molecular weight polyethylene fibers self constant basically simultaneously; The adhesive property of fiber and resin matrix improves significantly; This method is easy to operate, but industrialization produce continuously, with the use that promotes superhigh molecular weight polyethylene fibers in the fibre reinforced composites.
Description of drawings
Fig. 1 produces sketch map continuously for modified ultra-high molecular weight polyethylene fiber of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is elaborated.
As shown in Figure 1; Mutual radiation crosslinking technology of the present invention prepares the serialization commercial production sketch map of modified ultra-high molecular weight polyethylene fiber; The operation of mutual radiation grafting is linked to each other with the production process of superhigh molecular weight polyethylene fibers; Forming the continuous production technology of superhigh molecular weight polyethylene fibers preparation and modification, specifically is earlier superhigh molecular weight polyethylene fibers 1 to be got into grafting liquid bath 3 dipping grafting liquid through hauling machine 2 tractions, and the superhigh molecular weight polyethylene fibers after will flooding again carries out the graft modification of electron beam mutual radiation; The device of described mutual radiation grafting comprises that concrete blocks case 4, electronics tube 5, filament 6, scanning coil 7 and flying-spot tube 8; Electronics tube 5, filament 6, scanning coil 7 and flying-spot tube 8 all are arranged on concrete and block in the case 4, and filament 6 is arranged in the electronics tube 5, and scanning coil 7 is arranged on electronics tube 5 belows; Flying-spot tube 8 is arranged on scanning coil 7 belows; Flying-spot tube 8 sends the superhigh molecular weight polyethylene fibers that is impregnated with maceration extract of its below of high-power electron beam 9 irradiation, promptly it is carried out the mutual radiation graft modification, and fiber irradiation is laggard to be gone in the ultrasonic washing pool 10 to wash removal impurity; In drying box 11, carry out dried at last and promptly get product, the product that obtains is delivered to the fibrous composite manufacturing procedure.
Following examples are based on that said method and device carry out.
Embodiment 1
The hauling speed of control superhigh molecular weight polyethylene fibers is 5m/min, and through the grafting liquid bath, the grafting liquid in this grafting liquid bath is by deionized water, acrylic acid, trichloro-ethylene, CuSO
4Form.With the deionized water is benchmark, and acrylic acid concentration is 6mol/L, and the concentration of trichloro-ethylene is 1mol/L, CuSO
4Concentration be 0.002mol/L.Adopt JJ-2 type electrostatic accelerator, at room temperature, N
2Under the atmosphere superhigh molecular weight polyethylene fibers that is impregnated with above-mentioned grafting liquid is carried out irradiation, the mean dose rate is 25KGy/S.Fiber behind the irradiation is with 1.5kW, 30 ℃ the ultrasonic washing of pure water, and then drying under 38 ℃ of air conditionses can make described superhigh molecular weight polyethylene fibers.
The hauling speed of control superhigh molecular weight polyethylene fibers is 8m/min, and through the grafting liquid bath, the grafting liquid in this grafting liquid bath is by deionized water, methacrylic acid, dichloroethanes, CuSO
4Form.With the deionized water is benchmark, and the concentration of methacrylic acid is 10mol/L, and the concentration of dichloroethanes is 2.5mol/L, CuSO
4Concentration be 0.01mol/L.Adopt JJ-2 type electrostatic accelerator, at room temperature, N
2Under the atmosphere superhigh molecular weight polyethylene fibers that is impregnated with above-mentioned grafting liquid is carried out irradiation, the mean dose rate is 40KGy/S.Fiber behind the irradiation is with 1.7kW, 35 ℃ the ultrasonic washing of pure water, and then drying under 40 ℃ of air conditionses can make described superhigh molecular weight polyethylene fibers.
The hauling speed of control superhigh molecular weight polyethylene fibers is 10m/min, and through the grafting liquid bath, the grafting liquid in this grafting liquid bath is by deionized water, methyl acrylate, trichloro-ethylene, CuSO
4Form.With the deionized water is benchmark, and the concentration of methyl acrylate is 15mol/L, and the concentration of trichloro-ethylene is 4.2mol/L, CuSO
4Concentration be 0.05mol/L.Adopt JJ-2 type electrostatic accelerator, under room temperature, Ar atmosphere, the superhigh molecular weight polyethylene fibers that is impregnated with above-mentioned grafting liquid is carried out irradiation, the mean dose rate is 60KGy/S.Fiber behind the irradiation is with 2.0kW, 40 ℃ the ultrasonic washing of pure water, and then drying under 42 ℃ of air conditionses can make described superhigh molecular weight polyethylene fibers.
The mechanical property of superhigh molecular weight polyethylene fibers and surface adhesion performance are seen table 1 and table 2 before and after the irradiation grafting modification.
The mechanical property of superhigh molecular weight polyethylene fibers before and after the modification of table 1 irradiation grafting
| Sample | Fracture strength (cN/dtex) | Elastic modelling quantity (cN/dtex) | Extension at break (%) |
| Irradiation fiber not | 28.14 | 1150 | 2.05 |
| Embodiment 1 fiber | 26.29 | 1143 | 2.31 |
| |
25.70 | 1120 | 2.18 |
| |
26.10 | 1133 | 2.25 |
The mechanical property of fiber adopts the DXLL-3000 electronic tension tester to measure, and the folder distance is 600mm.Draw speed is 250mm/min.Try to achieve the ultimate strength and the extension at break of fiber, and try to achieve the elastic modelling quantity of fiber by the slope of S-S curve straight line start-up portion.
The surface adhesion performance of superhigh molecular weight polyethylene fibers before and after the modification of table 2 irradiation grafting
| Sample | Irradiation fiber not | Embodiment 1 | Embodiment | 2 | Embodiment | 3 fibers |
| Maximum pull-out strength (MPa) | 0.55 | ?0.85 | ?0.91 | ?0.93 |
The surface adhesion performance test methods of fiber is following:
After epoxy resin (trade mark E-51) and curing agent (trade mark 593) mixed by 100: 26, pour in the high disk of 5mm, let fiber vertical hanging to be measured pass disc centre and at room temperature solidify 8hr.Solidify the back and on LLY-6 type tensometer, carries out the filament pull, measure superhigh molecular weight polyethylene fibers and adhesive property resin, draw speed is 1mm/min.
With maximum pull-out strength (τ
Max) represent the adhesive property of fiber and epoxy resin.τ
MaxMay be defined as:
τ
max＝F
max/πNDL
F in the formula
MaxFor the fiber maximum is extracted brute force (N); The N-number of fiber; D-fibre diameter (mm); L-epoxy resin soaks and buries length (mm).
Embodiment 4
Get fracture strength and be higher than 20cN/dtex; Modulus is higher than 600cN/dtex; Molecular weight is 500,000～8,000,000 superhigh molecular weight polyethylene fibers; The hauling speed of control superhigh molecular weight polyethylene fibers is 2m/min, and through the grafting liquid bath, the grafting liquid in this grafting liquid bath is by ethanol, methyl acrylate, chloroform, FeSO
4Form.With ethanol is benchmark, and the concentration of methyl acrylate is 1mol/L, and the concentration of chloroform is 0.03mol/L, FeSO
4Concentration be 0.001mol/L.Adopt JJ-2 type electrostatic accelerator, at room temperature, C
2H
2Under the atmosphere superhigh molecular weight polyethylene fibers that is impregnated with above-mentioned grafting liquid is carried out irradiation, the mean dose rate is 5KGy/S.Fiber behind the irradiation is with 1.0kW, 25 ℃ the ultrasonic washing of pure water, and then drying under 25 ℃ of air conditionses can make described superhigh molecular weight polyethylene fibers.
The hauling speed of control superhigh molecular weight polyethylene fibers is 15m/min, and through the grafting liquid bath, the grafting liquid in this grafting liquid bath is by acetone, acrylic acid, trichloro-ethylene, Fe (NO
3)
2Form.With acetone is benchmark, and acrylic acid concentration is 20mol/L, and the concentration of trichloro-ethylene is 5mol/L, Fe (NO
3)
2Concentration be 0.06mol/L.Adopt JJ-2 type electrostatic accelerator, under room temperature, Ar atmosphere, the superhigh molecular weight polyethylene fibers that is impregnated with above-mentioned grafting liquid is carried out irradiation, the mean dose rate is 70KGy/S.Fiber behind the irradiation is with 5.0kW, 40 ℃ the ultrasonic washing of pure water, and then drying under 50 ℃ of air conditionses can make described superhigh molecular weight polyethylene fibers.
Claims (8)
1. the mutual radiation crosslinking technology is produced the method for modified ultra-high molecular weight polyethylene fiber; It is characterized in that; The operation of mutual radiation grafting is linked to each other with the production process of superhigh molecular weight polyethylene fibers; Forming the continuous production technology of superhigh molecular weight polyethylene fibers preparation and modification, specifically is earlier superhigh molecular weight polyethylene fibers to be got into grafting liquid drill traverse stain grafting liquid through the hauling machine traction, again the superhigh molecular weight polyethylene fibers behind the dipping is carried out the graft modification of electron beam mutual radiation; Wash removal impurity behind the fiber irradiation, carry out dried at last and promptly get product.
2. mutual radiation crosslinking technology according to claim 1 is produced the method for modified ultra-high molecular weight polyethylene fiber; It is characterized in that; The fracture strength of described superhigh molecular weight polyethylene fibers is higher than 20cN/dtex; Modulus is higher than 600cN/dtex, and molecular weight is 500,000～8,000,000, and the speed controlling of described traction is 2～15m/min.
3. mutual radiation crosslinking technology according to claim 1 is produced the method for modified ultra-high molecular weight polyethylene fiber, it is characterized in that described grafting liquid is by graft modification monomer, swelling agent, polymerization inhibitor and solvent composition.
4. mutual radiation crosslinking technology according to claim 3 is produced the method for modified ultra-high molecular weight polyethylene fiber, it is characterized in that, described graft modification monomer is the various acrylic monomers of existing superhigh molecular weight polyethylene fibers graft modification; Described swelling agent be selected from chloroform, dichloroethanes and trichloro-ethylene one of them; Described polymerization inhibitor is Cu
2+Or Fe
2+Salt; Described solvent is deionized water, ethanol or acetone.
5. mutual radiation crosslinking technology according to claim 3 is produced the method for modified ultra-high molecular weight polyethylene fiber; It is characterized in that; Described grafting liquid is benchmark with the solvent; Said graft modification monomer concentration is 1～20mol/L, and said swelling agent concentration is 0.03～5mol/L, and said inhibitor concentration is 0.001～0.06mol/L.
6. mutual radiation crosslinking technology according to claim 1 is produced the method for modified ultra-high molecular weight polyethylene fiber, it is characterized in that, and the radiation dose rate average out to 5～70KGy/S of described electron beam mutual radiation grafting, irradiation reaction atmosphere is selected N
2, Ar or C
2H
2A kind of in the gas.
7. mutual radiation crosslinking technology according to claim 1 is produced the method for modified ultra-high molecular weight polyethylene fiber, it is characterized in that described washing is ultrasonic washing, the ultrasonic energy 1kW～5kW of ultrasonic washing, and washing temperature is 25～40 ℃.
8. mutual radiation crosslinking technology according to claim 1 is produced the method for modified ultra-high molecular weight polyethylene fiber, it is characterized in that the temperature of described dried is 25～50 ℃.
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Cited By (6)
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| CN102644196A (en) * | 2012-04-29 | 2012-08-22 | 中国人民解放军总后勤部军需装备研究所 | Processing method for improving hydrophilicity of polyester fiber and fabric of polyester fiber |
| CN104818541A (en) * | 2015-05-22 | 2015-08-05 | 江苏神鹤科技发展有限公司 | Crosslinked ultrahigh molecular weight polyethylene fiber and wet preparation method thereof |
| CN104846446A (en) * | 2015-05-22 | 2015-08-19 | 江苏神鹤科技发展有限公司 | Crosslinked polyethylene fiber with ultrahigh molecular weight and dry preparation method for crosslinked polyethylene fiber |
| CN108166151A (en) * | 2018-02-05 | 2018-06-15 | 成都天府轨谷科技有限公司 | A kind of defensive superhigh molecular weight polyethylene fibers braided fabric in field |
| CN111749016A (en) * | 2020-07-03 | 2020-10-09 | 江苏扬农化工集团有限公司 | Polyethylene polymerization grafting impregnation liquid and ultrahigh molecular weight polyethylene polymerization grafting modification method |
| CN113481723A (en) * | 2021-06-28 | 2021-10-08 | 上海化工研究院有限公司 | Modified ultra-high molecular weight polyethylene fiber and UD cloth |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104846446A (en) * | 2015-05-22 | 2015-08-19 | 江苏神鹤科技发展有限公司 | Crosslinked polyethylene fiber with ultrahigh molecular weight and dry preparation method for crosslinked polyethylene fiber |
| CN104846446B (en) * | 2015-05-22 | 2018-10-02 | 江苏神鹤科技发展有限公司 | Crosslinked superhigh molecular weight polyethylene fibers and its dry type preparation method |
| CN108166151A (en) * | 2018-02-05 | 2018-06-15 | 成都天府轨谷科技有限公司 | A kind of defensive superhigh molecular weight polyethylene fibers braided fabric in field |
| CN108166151B (en) * | 2018-02-05 | 2019-08-27 | 成都天府轨谷科技有限公司 | A kind of defensive ultra high molecular weight polyethylene fiber braided fabric in field |
| CN111749016A (en) * | 2020-07-03 | 2020-10-09 | 江苏扬农化工集团有限公司 | Polyethylene polymerization grafting impregnation liquid and ultrahigh molecular weight polyethylene polymerization grafting modification method |
| CN111749016B (en) * | 2020-07-03 | 2022-12-09 | 江苏扬农化工集团有限公司 | Polyethylene polymerization graft impregnation liquid and method for polymerization graft modification of ultrahigh molecular weight polyethylene |
| CN113481723A (en) * | 2021-06-28 | 2021-10-08 | 上海化工研究院有限公司 | Modified ultra-high molecular weight polyethylene fiber and UD cloth |
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Application publication date: 20120404 |