CN104947243A - Preparation method for polypropylene/polyurethane X-ray shielding composite fiber containing lanthanide - Google Patents
Preparation method for polypropylene/polyurethane X-ray shielding composite fiber containing lanthanide Download PDFInfo
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Abstract
The invention discloses a preparation method for polypropylene/polyurethane X-ray shielding composite fiber containing lanthanide and relates to the field of medical shielding X-ray materials. According to the preparation method for the polypropylene/polyurethane X-ray shielding composite fiber containing the lanthanide, a polypropylene/polyurethane composite material is taken as a substrate, lanthanide series compound particles are added, and spinning master batch is obtained through blending extrusion by an extruder and granulation; the obtained spinning master batch is fed into a single screw spinning machine, nascent fiber is obtained through spinning and winding, the adopted spinning temperature is 200-230 DEG C, the screw speed is 20-30 r/min, the winding speed is 6-9 m/min, and the diameters of spinneret orifices are 0.1-0.2 mm; the nascent fiber is dissolved by the adoption of paraxylene at the temperature of 100-110 DEG C for 0.5-1.5 h, and after being washed twice by absolute ethyl alcohol, the processed fiber is dried in an air blasting mode for 10 h under the condition that the temperature of a drying oven is 50 DEG C. According to the preparation method for the polypropylene/polyurethane X-ray shielding composite fiber containing the lanthanide, for improving the effective content of the lanthanide in the fiber, the paraxylene is adopted to dissolve part of polypropylene in the fiber under the heating condition, a polyurethane elastic framework is retained, and the X-ray shielding fiber with the high shielding agent content and both the elasticity and the air permeability is obtained.
Description
Technical field
The present invention relates to medical grade barrier X-ray Material Field, particularly relate to a kind of technology of preparing containing lanthanide series polypropylene/polyurethane X-ray shielding composite fibre.
Background technology
X-ray is that a kind of wavelength is extremely short, the electromagnetic wave that energy is very large, the wavelength of X-ray is (about 0.001 ~ 100nm, the X-ray wavelength medically applied is between 0.001 ~ 0.1nm) shorter than the wavelength of visible ray, its photon energy than visible ray photon energy greatly several ten thousand to hundreds of thousands doubly, very large to harm under being chronically exposed to X-ray radiation.X-ray is widely used at medical domain, as fluoroscopic image, angiocardiography, cardiac angioplasty etc., for a long time, lower by protection degree of concern compared to other occasion X-ray workers China medical X-ray contact worker, be badly in need of high-quality X-ray protection clothing.
Traditional medical X-ray protection material is lead rubber, as everyone knows, lead is harmful element, there are some researches show that it exists weak absorbing to the photoelectron that energy drops on 40 ~ 88keV interval, for reaching shield effectiveness, the often plumbous type shielding agent of a large amount of interpolation, the shielding clothing therefore made is heavier, a lead screen clothing is by 7 kilograms, and the weight of 70 ~ 80% comes from plumbous type shielding agent.Based on this, part researcher wishes that searching one group effectively can make up the weak absorbing of lead element, light weight and harmless X-ray screener.
Due to rare earth 4f electron structure and the special K electron ABSORPTION EDGE (63.3keV from the 38.9keV of lanthanum to lutetium, effectively compensate for plumbous weak absorbing interval), rare earth causes a large amount of concerns of researcher as novel radio-opaque substance, various research method and in succession being reported containing rare earth material.Russ P RU2054439 and RU2028331 have developed rare earth oxide filled rubber X-ray shielding material, and shield effectiveness is good; Beijing University of Chemical Technology professor Liu Li was engaged in the research and development of organically-modified rare earth/rubber Novel protective material in recent years always, and at anti-X, gamma-rays individual protection field achieves substantial progress, the industrialization of some individuals protective clothing kind.Based on the airtight and heavy feature of rubber-based protective materials, bring much inconvenience to user, rubber-like chemical protective clothing very easily to rub human body back, shoulder in the process of dress, and Long-Time Service often can cause user's local skin red and swollen.
Based on the above-mentioned shortcoming of rubber-like protective materials, fiber-like protective materials becomes new research direction gradually.Tianjin University of Technology Shandong professor, by screener and polypropene blended obtained radiation resistant fiber, makes non-weaving cloth, and has done the test of X-ray shielding rate, and centering low energy X ray shielding rate can reach more than 90%; In this seminar application publication number CN104532381A patent, rare earth/polypropylene Effect of X-Ray Shielding Fibre is studied; Japanese and Austrian scholar once attempted barium sulfate to be added into obtained radiation resistant fiber in viscose, and can be used for making X-ray-preventing clothes, shield effectiveness is good, wash resistant.But in above-mentioned research fiber be single matrix add screener make, cause the restriction of performance by single substrate performance of the protection fiber made, such as fibrous mechanical property is poor, and causes difficulty in spinning with the increase of screener interpolation number, and in spinning process, wire broken rate increases.Compared to single matrix, based on " performance complement effect ", two kinds and above blended compound material matrix have excellent combination property, adopt matrices of composite material preparation protection fiber will become protective materials Trends on Study gradually.
First polypropylene fibre realizes suitability for industrialized production, the mid-80 in nineteen sixty by Italian Meng Tekadini company, and the annual production of the polypropylene fibre world, more than 1Mt, has more than 40 country to produce.The raw material producing polypropylene fibre is also only limited to isotactic polypropylene, and its isotacticity is 97% ~ 98%, can not lower than 96%, and mean molecule quantity is 180000 ~ 300000, and degree of crystallinity is more than 65%, and heat decomposition temperature is 350 ~ 380 DEG C, and fusing point is 158 ~ 176 DEG C.The hygroscopicity of polypropylene fibre and density are minimum in conventional synthetic fiber, and its regain is 0.03%, and density is 0.90 ~ 0.92g/cm
3.Polypropylene fibre has high strength, high tenacity, good chemical resistance and lower-price characteristic, has been widely used in drapery field.Polyurethane elastomeric fiber, formal name used at school polyurethane fibre, it is the fiber that one has the elasticity of " section " structure good, hard section is reacted by isocyanates and diamine compound and is formed, soft section is made up of long-chain dihydroxy compounds (PTMEG or polyester-diol), it is more soft, fusing point is below 50 DEG C, vitrification point is-50 ~-70 DEG C (polyether-types) and 25 ~ 45 DEG C (polyester-type), different commodity introduce different components, to improve the various performances of fiber in strand.Polyurethane elastomeric fiber, owing to having outstanding stretching, extension and recovery capacity, gives the performances such as goods are capable of expansion and contraction, comfortable fittingness.Polypropylene/polyurethane composite is adopted to be that matrix is prepared X-ray shielding fiber and will be become the new direction of X-ray protection investigation of materials.
Summary of the invention
The object of the present invention is to provide a kind of preparation method containing lanthanide series polypropylene/polyurethane X-ray shielding composite fibre, the method preparation technology is simple, with low cost; Preparation X-ray shielding fiber light weight, nontoxic, mechanics and X-ray shielding properties excellent.
For achieving the above object, technical scheme of the present invention is: for the preparation of a kind of preparation method containing lanthanide series polypropylene/polyurethane X-ray shielding composite fibre.Its feature comprises the following steps:
1) blended granulation: with polypropylene/polyurethane composite for matrix, adds lanthanide series compound particle, obtains spinning master batch after extruder blending extrusion, granulation.The wherein interpolation parts by weight of each material: polypropylene 40 ~ 60 parts; Polyurethane 40 ~ 60 parts; Lanthanide series compound 30 ~ 50 parts.Blending condition is: blending temperature 200 ~ 220 DEG C, blended time 5min, screw speed 80 ~ 200r/min;
2) as-spun fibre preparation: by gained spinning master batch feeding singe screw spinning machine, through spinning, winding obtain as-spun fibre, adopt spinning temperature 200 ~ 230 DEG C, screw speed 20 ~ 30r/min, winding speed 6 ~ 9m/min, orifice diameter is 0.1 ~ 0.2mm;
3) dissolution method process fiber: by above-mentioned steps 2) as-spun fibre for preparing selects paraxylene to dissolve 0.5 ~ 1.5h under temperature 100 ~ 110 DEG C of conditions, by the fiber after process after absolute ethyl alcohol drip washing twice under oven temperature 50 DEG C of conditions air blast dry 10h.
The employing polypropylene/polyurethane composite of the invention is matrix, add lanthanide series and prepare X-ray-preventing as-spun fibre, for improving the effective content of lanthanide series in fiber, under the condition of heating, dissolving the polypropylene segment in fiber with paraxylene, retain elastic polyurethane skeleton.This research adopts solvent method to improve screener content in the fibre, remains elastic polyurethane skeleton, finally prepares high screener content, has the X-ray shielding fiber of elasticity and gas permeability concurrently.
The X-ray-preventing as-spun fibre obtained is cut into length and is about 5 centimeters of staple fibres, the method that staple fibre erects paving one deck by horizontal paving one deck is successively spread even, by film laminator at pressure 4MPa, suppress 10 minutes at temperature 100 DEG C, make the non-weaving cloth that thickness is 5mm.This pressing film method proposes claim in application publication number CN104532381A patent, and this patent does not do claim herein.The non-weaving cloth that fiber is obtained thus measures through the radiation protection of Chinese Center for Disease Control and Nuclear Safety Institute, the assay method that X-ray protection material attenuate performance in GBZ/T147-2002 is pressed in method of testing and requirement performs, and material protection performance characterizes with lead equivalent.Under x-ray tube voltage 120KV, 2.50mm thickness aluminium flake filter condition, lead equivalent can reach 0.25 ~ 0.35mmPb, and the thickness increasing non-weaving cloth can improve the lead equivalent of non-weaving cloth.Fibrous fracture percentage elongation is 30% ~ 50%, fracture strength 30 ~ 40MPa, and the non-weaving cloth density that fiber is made thus is 0.9 ~ 1.1g/cm
3, compared to plumbous rubber-like vest light weight.Improve 150 ~ 250% than before non-dissolution process with the lanthanide series compound content learnt in fiber through thermogravimetric test analysis residual qualities after paraxylene dissolution process.
One of advantage of the present invention is that technique is simple, easy and simple to handle, does not adopt complicated technique namely to have found dexterously and a kind ofly prepares high screener and fill the X-ray shielding fiber having elasticity and gas permeability concurrently.Two is the extruders used, and melt spinning machine is conventional equipment, is convenient to industrialization and produces.
Accompanying drawing explanation
Fig. 1 is filamentary electrons ESEM (SEM) image.
By blending weight fraction polypropylene 50 parts, polyurethane 50 parts, after the blended obtained master batch of lanthana 40 parts adopts melt spinning method to obtain as-spun fibre, through paraxylene at 105 DEG C of filamentary electrons ESEM (SEM) images obtained after dissolving 0.5h as shown in the figure, wherein blending condition: temperature 210 DEG C, time 5min, screw speed 100r/min.Spinning condition: spinning temperature 210 DEG C, screw speed 25r/min, winding speed 8m/min, orifice diameter 0.1mm.Be can be observed the pore structure of fiber surface by figure, this structure provides possibility for the vest making good air permeability.
Detailed description of the invention
Continue to describe the present invention below in conjunction with example, institute's example of chatting only illustratively use of the present invention, the present invention is not limited to down and chats embodiment.Lanthanide series compound particle recommends particle diameter <10 micron.
Embodiment 1
1) blended granulation: with polypropylene/polyurethane composite for matrix, adds lanthana, obtains preparing fiber master batch after extruder blending extrusion, granulation.The wherein interpolation parts by weight of each material: polypropylene 40 parts; Polyurethane 60 parts; Lanthana 30 parts.Blending condition is: blending temperature 200 DEG C, blended time 5min, screw speed 80r/min;
2) as-spun fibre preparation: by gained fiber master batch feeding singe screw spinning machine, obtain as-spun fibre through spinning, winding, institute adopts spinning temperature 200 DEG C, screw speed 20r/min, and reel speed 9m/min, and orifice diameter is 0.2mm;
3) dissolution method process fiber: by above-mentioned steps 2) as-spun fibre for preparing selects paraxylene to dissolve 1.5h under temperature 100 DEG C of conditions, by the fiber after process after absolute ethyl alcohol drip washing twice under oven temperature 50 DEG C of conditions air blast dry 10h.
The X-ray-preventing as-spun fibre obtained is cut into length and is about 5 centimeters of staple fibres, the method that staple fibre erects paving one deck by horizontal paving one deck is successively spread even, by film laminator at pressure 4MPa, suppress 10 minutes at temperature 100 DEG C, make the non-weaving cloth that thickness is 5mm.The non-weaving cloth that fiber is obtained thus measures through the radiation protection of Chinese Center for Disease Control and Nuclear Safety Institute, the assay method that X-ray protection material attenuate performance in GBZ/T147-2002 is pressed in method of testing and requirement performs, and material protection performance characterizes with lead equivalent.Under x-ray tube voltage 120KV, 2.50mm thickness aluminium flake filter condition, lead equivalent can reach 0.25mmPb, and the thickness increasing non-weaving cloth can improve the lead equivalent of non-weaving cloth.Fibrous fracture percentage elongation is 40%, fracture strength 40MPa, and the non-weaving cloth density that fiber is made thus is 0.9g/cm
3.The lanthanide series compound content learnt in fiber through thermogravimetric test analysis residual qualities improves 150% than before non-dissolution process.
Embodiment 2
1) blended granulation: with polypropylene/polyurethane composite for matrix, adds lanthana, obtains preparing fiber master batch after extruder blending extrusion, granulation.The wherein interpolation parts by weight of each material: polypropylene 50 parts; Polyurethane 50 parts; Lanthana 40 parts.Blending condition is: blending temperature 210 DEG C, blended time 5min, screw speed 100r/min;
2) as-spun fibre preparation: by gained fiber master batch feeding singe screw spinning machine, obtain as-spun fibre through spinning, winding, institute adopts spinning temperature 210 DEG C, screw speed 25r/min, and reel speed 8m/min, and orifice diameter is 0.1mm.
3) dissolution method process fiber: by above-mentioned steps 2) as-spun fibre for preparing selects paraxylene to dissolve 0.5h under temperature 105 DEG C of conditions, by the fiber after process after absolute ethyl alcohol drip washing twice under oven temperature 50 DEG C of conditions air blast dry 10h;
The X-ray-preventing as-spun fibre obtained is cut into length and is about 5 centimeters of staple fibres, the method that staple fibre erects paving one deck by horizontal paving one deck is successively spread even, by film laminator at pressure 4MPa, suppress 10 minutes at temperature 100 DEG C, make the non-weaving cloth that thickness is 5mm.The non-weaving cloth that fiber is obtained thus measures through the radiation protection of Chinese Center for Disease Control and Nuclear Safety Institute, the assay method that X-ray protection material attenuate performance in GBZ/T147-2002 is pressed in method of testing and requirement performs, and material protection performance characterizes with lead equivalent.Under x-ray tube voltage 120KV, 2.50mm thickness aluminium flake filter condition, lead equivalent can reach 0.30mmPb, and the thickness increasing non-weaving cloth can improve the lead equivalent of non-weaving cloth.Fibrous fracture percentage elongation is 35%, fracture strength 35MPa, and the non-weaving cloth density that fiber is made thus is 1.0g/cm
3.The lanthanide series compound content learnt in fiber through thermogravimetric test analysis residual qualities improves 250% than before non-dissolution process.
Embodiment 3
1) blended granulation: with polypropylene/polyurethane composite for matrix, adds lanthana, obtains preparing fiber master batch after extruder blending extrusion, granulation.The wherein interpolation parts by weight of each material: polypropylene 60 parts; Polyurethane 40 parts; Lanthana 50 parts.Blending condition is: blending temperature 220 DEG C, blended time 5min, screw speed 200r/min;
2) as-spun fibre preparation: by gained fiber master batch feeding singe screw spinning machine, obtain as-spun fibre through spinning, winding, institute adopts spinning temperature 230 DEG C, screw speed 30r/min, and reel speed 6m/min, and orifice diameter is 0.1mm;
3) dissolution method process fiber: by above-mentioned steps 2) as-spun fibre for preparing selects paraxylene to dissolve 1h under temperature 110 DEG C of conditions, by the fiber after process after absolute ethyl alcohol drip washing twice under oven temperature 50 DEG C of conditions air blast dry 10h.
The X-ray-preventing as-spun fibre obtained is cut into length and is about 5 centimeters of staple fibres, the method that staple fibre erects paving one deck by horizontal paving one deck is successively spread even, by film laminator at pressure 4MPa, suppress 10 minutes at temperature 100 DEG C, make the non-weaving cloth that thickness is 5mm.The non-weaving cloth that fiber is obtained thus measures through the radiation protection of Chinese Center for Disease Control and Nuclear Safety Institute, the assay method that X-ray protection material attenuate performance in GBZ/T147-2002 is pressed in method of testing and requirement performs, and material protection performance characterizes with lead equivalent.Under x-ray tube voltage 120KV, 2.50mm thickness aluminium flake filter condition, lead equivalent can reach 0.35mmPb, and the thickness increasing non-weaving cloth can improve the lead equivalent of non-weaving cloth.Fibrous fracture percentage elongation is 31%, fracture strength 35MPa, and the non-weaving cloth density that fiber is made thus is 1.1g/cm
3.The lanthanide series compound content learnt in fiber through thermogravimetric test analysis residual qualities improves 250% than before non-dissolution process.
Claims (1)
1. containing the preparation method of lanthanide series polypropylene/polyurethane X-ray shielding composite fibre, one kind is characterized in that step is as follows:
1) blended granulation: with polypropylene/polyurethane composite for matrix, adds lanthanide series compound particle, obtains spinning master batch after extruder blending extrusion, granulation; The wherein interpolation parts by weight of each material: polypropylene 40 ~ 60 parts; Polyurethane 40 ~ 60 parts; Lanthanide series compound 30 ~ 50 parts; Blending condition is: blending temperature 200 ~ 220 DEG C, blended time 5min, screw speed 80 ~ 200r/min;
2) as-spun fibre preparation: by gained spinning master batch feeding singe screw spinning machine, through spinning, winding obtain as-spun fibre, adopt spinning temperature 200 ~ 230 DEG C, screw speed 20 ~ 30r/min, winding speed 6 ~ 9m/min, orifice diameter is 0.1 ~ 0.2mm;
3) dissolution method process fiber: by above-mentioned steps 2) as-spun fibre for preparing selects paraxylene to dissolve 0.5 ~ 1.5h under temperature 100 ~ 110 DEG C of conditions, by the fiber after process after absolute ethyl alcohol drip washing twice under oven temperature 50 DEG C of conditions air blast dry 10h.
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| CN114687202A (en) * | 2022-04-20 | 2022-07-01 | 西安工程大学 | X-ray-proof shielding fabric and preparation method and application thereof |
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