CN104947243B - 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, more particularly to a kind of X of polypropylene/polyurethane containing lanthanide series
The technology of preparing of alpha ray shield composite fibre.
Background technology
X-ray is that a kind of wavelength is extremely short, the very big electromagnetic wave of energy, and the wavelength of X-ray (about in 0.001~100nm, is cured
The X-ray wavelength applied on is about between 0.001~0.1nm) it is more shorter than the wavelength of visible ray, its photon energy is than visible
The photon energy of light is big tens of thousands of to hundreds of thousands times, is chronically exposed to very big to harm under X-radiation.X-ray is in medical science
Field is widely used, such as fluoroscopic image, cardioangiography, cardiac angioplasty, and for a long time, in China, medical X is penetrated
Linear contact lay worker is relatively low by protection degree of concern compared to other occasion X-ray workers, is badly in need of high-quality X-ray protection
Clothing.
Traditional medical X-ray protection material is lead rubber, it is well known that lead is harmful element, there is research
Show it to fall energy in the interval photoelectrons of 40~88keV to there is weak absorbing, to reach shield effectiveness, lead is often added in a large number
Type shielding agent, therefore the shielding clothing made is heavier, based on 7 kilograms, 70~80% weight comes from lead to a lead screen clothing
Type shielding agent.Based on this, part researcher wishes to find one group of weak absorbing that can effectively make up lead element, light weight and to people
The harmless X-ray shield agent of body.
Due to rare earth 4f electron structures and special K electron ABSORPTION EDGE, (38.9keV from lanthanum is to lutecium
63.3keV, the weak absorbing that effectively compensate for lead is interval), rare earth causes researcher as new radio-opaque substance
A large amount of concerns, various research methoies and reported in succession containing rare earth material.Russ P RU2054439 and RU2028331
Rare earth oxide filled rubber X-ray shield material is have developed, shield effectiveness is good；Beijing University of Chemical Technology professor Liu Li was in recent years
The research and development of organically-modified rare earth/rubber novel protective material are always worked on, in anti-X, gamma-rays individual protection field achieves reality
Matter is in progress, the species industrialization of some individuals protective garment.Based on the airtight and heavy feature of rubber-based protective material, give
User brings many inconvenience, and rubber-like biochemical defence suit easily rubs human body back, shoulder during dress, and life-time service is normal
User local skin can be caused red and swollen.
Based on rubber-like protective material disadvantages mentioned above, fiber-like protective material is increasingly becoming new research direction.Tianjin work
Shandong professor learns by screener and polypropene blended prepared radiation resistant fiber in sparetime university, makes non-weaving cloth, and has done X-ray shield
Rate is tested, 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；Japan and Austrian scholar once attempted for barium sulfate being added into viscose glue fibre
Radiation resistant fiber is obtained in dimension, can be used to make X-ray-preventing clothes, shield effectiveness is good, wash resistant.But fiber in the studies above
Be single matrix addition screener to make, cause made by protect the performance of fiber to be limited by single substrate performance, for example
Fibrous mechanical property is poor, and causes difficulty in spinning with screener addition number increase, and wire broken rate increases in spinning process.Phase
Than in single matrix, based on " performance complement effect ", two kinds and above blended compound material matrix have excellent combination property,
Preparing protection fiber using matrices of composite material will be increasingly becoming protective material Trends on Study.
Polypropylene fibre realizes first industrialized production in nineteen sixty by Italian Meng Tekadini companies, in the eighties
Phase, polypropylene fibre world annual production has more than 40 country's production more than 1Mt.The raw material of production polypropylene fibre is also only limited
In isotactic polypropylene, its isotacticity is 97%~98%, it is impossible to less than 96%, and mean molecule quantity is 180000~300000, knot
More than 65%, heat decomposition temperature is 350~380 DEG C to brilliant degree, and fusing point is 158~176 DEG C.The hygroscopicity of polypropylene fibre and close
Degree is conventionally synthesized minimum in fiber, and its regain is 0.03%, and density is 0.90~0.92g/cm3.Polypropylene fibre has
There are high intensity, high tenacity, good chemical resistance and lower-price characteristic, have been widely used in drapery field.
Polyurethane elastomeric fiber, scientific name polyurethane fibre is elastic good fiber that one kind has " section " structure, hard section by
Isocyanates react to be formed with diamine compound, and soft section is made up of long-chain dihydroxy compounds (PTMEG or polyester-diol),
It is relatively soft, and fusing point is below 50 DEG C, and vitrification point is -50~-70 DEG C (polyether-types) and 25~45 DEG C (polyester-type), different
Commodity introduce different components in strand, to improve the various performances of fiber.Polyurethane elastomeric fiber is due to non-
All stretching, extension and recovery capacity, give the performances such as the capable of expansion and contraction, comfortable fittingness of product.Using polypropylene/polyurethane composite
Based on prepare X-ray shield fiber and will become the new direction of X-ray protection investigation of materials.
The content of the invention
It is an object of the invention to provide a kind of system of the X-ray shield of polypropylene/polyurethane containing lanthanide series composite fibre
Preparation Method, the method preparation process is simple is with low cost；The X-ray shield fiber light weight of preparation, nontoxic, mechanics and X-ray screen
Cover function admirable.
To reach above-mentioned purpose, the technical scheme is that：For preparing a kind of polypropylene/polyurethane containing lanthanide series
The preparation method of X-ray shield composite fibre.Its feature is comprised the following steps：
1) pelletize is blended：Based on polypropylene/polyurethane composite, add lanthanide series compound granule, extruded machine
Spinning master batch is obtained after blending extrusion, pelletize.The addition parts by weight of wherein each material：40~60 parts of polypropylene；Polyurethane 40
~60 parts；30~50 parts of lanthanide series compound.Blending condition is：200~220 DEG C of blending temperature, is blended time 5min, screw speed
80~200r/min；
2) prepared by as-spun fibre：Gained spinning master batch is fed into single screw rod spinning-drawing machine, Jing spinning, winding obtain nascent fibre
Dimension, adopts 200~230 DEG C of spinning temperature, 20~30r/min of screw speed to wind 6~9m/min of speed, orifice diameter
For 0.1~0.2mm；
3) dissolution method processes fiber：By above-mentioned steps 2) as-spun fibre for preparing from xylol in temperature 100
0.5~1.5h is dissolved under the conditions of~110 DEG C, by the fiber after process Jing after twice of dehydrated alcohol drip washing in 50 DEG C of bars of oven temperature
10h is dried in air blast under part.
Based on the employing polypropylene/polyurethane composite of the invention, addition lanthanide series prepare X-ray-preventing
As-spun fibre, is the effective content for improving lanthanide series in fiber, is dissolved in fiber under conditions of heating with xylol
Polypropylene segment, retain elastic polyurethane skeleton.This research improves screener content in the fibre using solvent method, retains
Elastic polyurethane skeleton, finally prepares high shielding agent content, has the X-ray shield fiber of elasticity and breathability concurrently.
The X-ray-preventing as-spun fibre for obtaining is cut into into length and is about 5 centimeters of chopped fibers, by chopped fiber by the perpendicular paving of horizontal one layer of paving
One layer of method successively spreads even, suppresses 10 minutes at pressure 4MPa, 100 DEG C of temperature by film laminator, makes thickness for 5mm's
Non-weaving cloth.This pressing film method proposes claim in application publication number CN104532381A patent, and herein this patent does not do
Claim.Thus non-weaving cloth Jing China's Center for Disease Control's radiation protection is determined with Nuclear Safety Institute obtained in fiber,
Method of testing and requirement are pressed the assay method of X-ray protection material fade performance in GBZ/T147-2002 and are performed, material protection
Can be characterized with lead equivalent.Under x-ray tube voltage 120KV, 2.50mm thickness aluminium flake filterconditions, lead equivalent up to 0.25~
0.35mmPb, increasing the thickness of non-weaving cloth can improve the lead equivalent of non-weaving cloth.Fibrous fracture percentage elongation is 30%~50%,
30~40MPa of fracture strength, thus non-weaving cloth density made by fiber is 0.9~1.1g/cm3, it is anti-compared to lead rubber-like
Padded equipment light weight.The lanthanide series compound content in fiber is learnt with Jing thermogravimetrics test analysis residual qualities after xylol dissolution process
150~250% are improve than undissolved before processing.
One of the advantages of the present invention is process is simple, easy to operate, and the technique for being provided without complexity dexterously have found one
Plant and prepare the X-ray shield fiber that high screener filling has elasticity and breathability concurrently.Two is the extruder for using, melt spinning machine
Conventional equipment is, is easy to industrialization production.
Description of the drawings
Fig. 1 is filamentary electrons scanning electron microscope (SEM) image.
By 50 parts of weight fraction polypropylene is blended, 50 parts of polyurethane, 40 parts of blendings of lanthana are obtained master batch using melting spinning
Silk legal system is obtained after as-spun fibre, Jing xylol in 105 DEG C of filamentary electrons scanning electron microscope (SEM) images obtained after dissolving 0.5h
As illustrated, wherein blending condition：210 DEG C of temperature, time 5min, screw speed 100r/min.Spinning condition：Spinning temperature
210 DEG C, screw speed 25r/min winds speed 8m/min, orifice diameter 0.1mm.The hole of fiber surface can be observed by figure
Gap structure, this structure provides possibility for the protective clothing for making good air permeability.
Specific embodiment
Continue to describe the present invention with reference to example, chat example and only use as the explanation present invention, the present invention is not limited to
Under chat embodiment.Lanthanide series compound granule recommends particle diameter<10 microns.
Embodiment 1
1) pelletize is blended：Based on polypropylene/polyurethane composite, addition lanthana, extruded machine blending extrusion,
Obtain preparing fiber master batch after pelletize.The addition parts by weight of wherein each material：40 parts of polypropylene；60 parts of polyurethane；Lanthana
30 parts.Blending condition is：200 DEG C of blending temperature, is blended time 5min, screw speed 80r/min；
2) prepared by as-spun fibre：Gained fiber master batch is fed into single screw rod spinning-drawing machine, Jing spinning, winding obtain nascent fibre
Dimension, adopts 200 DEG C of spinning temperature, screw speed 20r/min to wind speed 9m/min, and orifice diameter is 0.2mm；
3) dissolution method processes fiber：By above-mentioned steps 2) as-spun fibre for preparing from xylol in temperature 100
1.5h is dissolved under the conditions of DEG C, air blast is dried under the conditions of 50 DEG C of oven temperature Jing after twice of dehydrated alcohol drip washing by the fiber after process
10h。
The X-ray-preventing as-spun fibre for obtaining is cut into into length and is about 5 centimeters of chopped fibers, by chopped fiber by the perpendicular paving of horizontal one layer of paving
One layer of method successively spreads even, suppresses 10 minutes at pressure 4MPa, 100 DEG C of temperature by film laminator, makes thickness for 5mm's
Non-weaving cloth.Thus non-weaving cloth Jing China's Center for Disease Control's radiation protection is determined with Nuclear Safety Institute obtained in fiber,
Method of testing and requirement are pressed the assay method of X-ray protection material fade performance in GBZ/T147-2002 and are performed, material protection
Can be characterized with lead equivalent.Under x-ray tube voltage 120KV, 2.50mm thickness aluminium flake filterconditions, lead equivalent is reachable
0.25mmPb, increasing the thickness of non-weaving cloth can improve the lead equivalent of non-weaving cloth.Fibrous fracture percentage elongation is 40%, and fracture is strong
Degree 40MPa, thus non-weaving cloth density made by fiber is 0.9g/cm3.Jing thermogravimetric test analysis residual qualities are learnt in fiber
Lanthanide series compound content improve 150% than undissolved before processing.
Embodiment 2
1) pelletize is blended：Based on polypropylene/polyurethane composite, addition lanthana, extruded machine blending extrusion,
Obtain preparing fiber master batch after pelletize.The addition parts by weight of wherein each material：50 parts of polypropylene；50 parts of polyurethane；Lanthana
40 parts.Blending condition is：210 DEG C of blending temperature, is blended time 5min, screw speed 100r/min；
2) prepared by as-spun fibre：Gained fiber master batch is fed into single screw rod spinning-drawing machine, Jing spinning, winding obtain nascent fibre
Dimension, adopts 210 DEG C of spinning temperature, screw speed 25r/min to wind speed 8m/min, and orifice diameter is 0.1mm.
3) dissolution method processes fiber：By above-mentioned steps 2) as-spun fibre for preparing from xylol in temperature 105
0.5h is dissolved under the conditions of DEG C, air blast is dried under the conditions of 50 DEG C of oven temperature Jing after twice of dehydrated alcohol drip washing by the fiber after process
10h；
The X-ray-preventing as-spun fibre for obtaining is cut into into length and is about 5 centimeters of chopped fibers, by chopped fiber by the perpendicular paving of horizontal one layer of paving
One layer of method successively spreads even, suppresses 10 minutes at pressure 4MPa, 100 DEG C of temperature by film laminator, makes thickness for 5mm's
Non-weaving cloth.Thus non-weaving cloth Jing China's Center for Disease Control's radiation protection is determined with Nuclear Safety Institute obtained in fiber,
Method of testing and requirement are pressed the assay method of X-ray protection material fade performance in GBZ/T147-2002 and are performed, material protection
Can be characterized with lead equivalent.Under x-ray tube voltage 120KV, 2.50mm thickness aluminium flake filterconditions, lead equivalent is reachable
0.30mmPb, increasing the thickness of non-weaving cloth can improve the lead equivalent of non-weaving cloth.Fibrous fracture percentage elongation is 35%, and fracture is strong
Degree 35MPa, thus non-weaving cloth density made by fiber is 1.0g/cm3.Jing thermogravimetric test analysis residual qualities are learnt in fiber
Lanthanide series compound content improve 250% than undissolved before processing.
Embodiment 3
1) pelletize is blended：Based on polypropylene/polyurethane composite, addition lanthana, extruded machine blending extrusion,
Obtain preparing fiber master batch after pelletize.The addition parts by weight of wherein each material：60 parts of polypropylene；40 parts of polyurethane；Lanthana
50 parts.Blending condition is：220 DEG C of blending temperature, is blended time 5min, screw speed 200r/min；
2) prepared by as-spun fibre：Gained fiber master batch is fed into single screw rod spinning-drawing machine, Jing spinning, winding obtain nascent fibre
Dimension, adopts 230 DEG C of spinning temperature, screw speed 30r/min to wind speed 6m/min, and orifice diameter is 0.1mm；
3) dissolution method processes fiber：By above-mentioned steps 2) as-spun fibre for preparing from xylol in temperature 110
1h is dissolved under the conditions of DEG C, air blast is dried under the conditions of 50 DEG C of oven temperature Jing after twice of dehydrated alcohol drip washing by the fiber after process
10h。
The X-ray-preventing as-spun fibre for obtaining is cut into into length and is about 5 centimeters of chopped fibers, by chopped fiber by the perpendicular paving of horizontal one layer of paving
One layer of method successively spreads even, suppresses 10 minutes at pressure 4MPa, 100 DEG C of temperature by film laminator, makes thickness for 5mm's
Non-weaving cloth.Thus non-weaving cloth Jing China's Center for Disease Control's radiation protection is determined with Nuclear Safety Institute obtained in fiber,
Method of testing and requirement are pressed the assay method of X-ray protection material fade performance in GBZ/T147-2002 and are performed, material protection
Can be characterized with lead equivalent.Under x-ray tube voltage 120KV, 2.50mm thickness aluminium flake filterconditions, lead equivalent is reachable
0.35mmPb, increasing the thickness of non-weaving cloth can improve the lead equivalent of non-weaving cloth.Fibrous fracture percentage elongation is 31%, and fracture is strong
Degree 35MPa, thus non-weaving cloth density made by fiber is 1.1g/cm3.Jing thermogravimetric test analysis residual qualities are learnt in fiber
Lanthanide series compound content improve 250% than undissolved before processing.
Claims (1)
1. a kind of preparation method of the X-ray shield of polypropylene/polyurethane containing lanthanide series composite fibre it is characterized in that step such as
Under：
1) pelletize is blended：Based on polypropylene/polyurethane composite, add lanthanide series compound granule, extruded machine blending
Spinning master batch is obtained after extrusion, pelletize；The addition parts by weight of wherein each material：40~60 parts of polypropylene；Polyurethane 40~60
Part；30~50 parts of lanthanide series compound；Blending condition is：200~220 DEG C of blending temperature, blending time 5min, screw speed 80~
200r/min；
2) prepared by as-spun fibre：Gained spinning master batch is fed into single screw rod spinning-drawing machine, Jing spinning, winding obtain as-spun fibre, institute
Using 200~230 DEG C of spinning temperature, 20~30r/min of screw speed, 6~9m/min of speed is wound, orifice diameter is 0.1
~0.2mm；
3）Dissolution method processes fiber：By above-mentioned steps 2）The as-spun fibre for preparing is from xylol in temperature 100~110
0.5~1.5h is dissolved under the conditions of DEG C, by the fiber after process Jing after twice of dehydrated alcohol drip washing under the conditions of 50 DEG C of oven temperature
10h is dried in air blast.
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