CN104558703B - A kind of tungsten-based composite material and preparation method thereof applied to alpha ray shield - Google Patents
A kind of tungsten-based composite material and preparation method thereof applied to alpha ray shield Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0011—Combinations of extrusion moulding with other shaping operations combined with compression moulding
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
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- C08K2201/00—Specific properties of additives
- C08K2201/016—Additives defined by their aspect ratio
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The tungsten-based composite material and preparation method thereof that the present invention relates to a kind of applied to alpha ray shield, the tungsten-based composite material include the component of following parts by weight：100 parts by weight of rubber；- 2000 parts by weight of 200 parts by weight of tungsten powder；- 50 parts by weight of 0.5 parts by weight of tungsten fiber；- 250 parts by weight of -150 parts by weight of 0.5 parts by weight of blanc fixe and/or 0.5 parts by weight of rareearth oxidate powder；- 6 parts by weight of 0.5 parts by weight of compatilizer；- 9 parts by weight of 3 parts by weight of activator；- 50 parts by weight of 0.5 parts by weight of plasticizer；- 3 parts by weight of 0.5 parts by weight of anti-aging agent；- 0.5 parts by weight of 0.05 parts by weight of antiscorching agent；- 3 parts by weight of 0.5 parts by weight of vulcanization accelerator；- 3 parts by weight of 0.5 parts by weight of vulcanizing agent.Preparation method prepares including (1) feed proportioning.(2) prepared by mixed fillers.(3) rubber compounding.(4) extrusion calendaring.(5) vulcanization forming.The composite material is free of lead, has good ray shielding performance, physical mechanical property etc..
Description
Technical field
The tungsten-based composite material and preparation method thereof that the present invention relates to a kind of applied to alpha ray shield, belongs to advanced functional
Composite Materials Design and preparation field.
Background technology
With the improvement of modern science and technology, in the nuclear power energy, medical detection, military war, aerospace, the people's livelihood
The various basic research and technological development that the fields such as security are unfolded around nuclear energy and ray applications are continuously increased, and thus ray is anti-
Shield seems further important.Such as in nuclear power field, the reactor of nuclear power plant is a huge radioactive source, fuel fission and core
Waste material will produce a large amount of ray radiation.Therefore, it is necessary to radiation-resistant glass be carried out to its equipment and operating personnel, to avoid various
The generation of possible accident.In another example in core medical field, the x-ray inspection equipment of medical space, CT examination equipment increase year by year,
The local irradiation dosage that patient is subject to during primary diagnosis is equivalent to the decades of times of natural radiation year equivalent dose, the office of radiotherapy
Portion's dosage bigger, the dosage of a course for the treatment of are equivalent to thousands of times of diagnosis.Therefore, patient and the frequently doctor of behaviour's Medical Equipment for Radiotherapy
Shield personnel must carry out effective alpha ray shield, to reduce accidental exposure harm.
Traditional core radiation shielding material is mainly metallic lead and its polymer composites, is inhaled with good energy
Characteristic is received, has preferable shield effectiveness to low energy and sigmatron and gamma-rays, it is at low cost and easy to process.However, lead sheet
Body fusing point is low, has bio-toxicity, can form lead steam in higher temperature, leaded exhaust gas, waste water, waste residue etc. pollute air,
Water source and crops, seriously jeopardize health.According to European Union《It is harmful into using certain about being limited in electronic and electrical equipment
The instruction (RoHS instructions) divided》,《Waste electronic andelectrical equipment instructs (WEEE instructions)》And《The registration of chemicals is assessed, is awarded
Power and limitation (REACH regulations)》, lead is listed in limitation one of the harmful substance that uses and pay high attention to.With China's ecology text
Bright construction and environmental improvement measure are constantly reinforced, and positive closing successively is not had the processing factory of lead subsequent processing ability by country,
Therefore unleaded shielding material will will appear larger demand, and research replaces lead to be applied to alpha ray shield field gesture with other materials
It must go.
The atomic number of tungsten is 74, density 19.35g/cm3, there is good ray shielding performance, and do not generate secondary
Electron radiation is the choosing of the ideal for doing Shielding Materials for Nuclear Radiation.It will be appreciated, however, that tungsten is high-melting-point refractory metal,
Sintered state toughness plasticity is poor, and forming is difficult and cost is higher, it is difficult to prepare that shape is more complicated to apply part, therefore
Using when be subject to many limitations.Japanese Tomita applied for a patent EP1338626 in 2001, the patent with polyamide (PA6,
PA66 and PA12) it is polymeric matrix, using tungsten powder as screener, is had using the composite material of injection moulding preparation and preferably penetrated
Line shielding properties, but it is not used to the occasion of flexible requirement, and small dimension product can only be prepared, the scope of application is limited
System.
Invention content
It is an object of the invention to design a kind of tungsten-based composite material and preparation method thereof applied to alpha ray shield.This is multiple
Condensation material is free of lead, has good ray shielding performance, physical mechanical property etc., and environmental-friendly, flexible easy processing can answer
Alpha ray shield for nuclear industry, core medical treatment, precision instrument, electric mechanical, nuke rubbish and nuclear crisis pollutant storage container etc.
Field.
The specific technical solution of the present invention is as follows：
A kind of tungsten-based composite material applied to alpha ray shield, each component and its weight percent content are：
100 parts by weight of rubber；
- 2000 parts by weight of 200 parts by weight of tungsten powder；
- 50 parts by weight of 0.5 parts by weight of tungsten fiber；
- 250 parts by weight of -150 parts by weight of 0.5 parts by weight of blanc fixe and/or 0.5 parts by weight of rareearth oxidate powder；
- 6 parts by weight of 0.5 parts by weight of compatilizer；
- 9 parts by weight of 3 parts by weight of activator；
- 50 parts by weight of 0.5 parts by weight of plasticizer；
- 3 parts by weight of 0.5 parts by weight of anti-aging agent；
- 0.5 parts by weight of 0.05 parts by weight of antiscorching agent；
- 3 parts by weight of 0.5 parts by weight of vulcanization accelerator；
- 3 parts by weight of 0.5 parts by weight of vulcanizing agent.
Wherein, rubber be preferably one kind in natural rubber, butadiene-styrene rubber, EP rubbers, neoprene, nitrile rubber or
Several mixtures.
Tungsten powder is a kind of tungsten powder of 0.4 μm -20 μm of Fisher particle size or the mixture of several tungsten powders.Its parts by weight preferably can be with
It is 400,600,800,1000,1200,1400,1600,1800 parts.
Tungsten fiber is 10 μm -30 μm of diameter, a kind of tungsten fiber of draw ratio 50-150 or the mixture of several tungsten fibers.Its
Parts by weight preferably can be 5,10,15,20,25,30,35,40,45 parts.
Blanc fixe is a kind of blanc fixe of 0.1 μm -5 μm of Fisher particle size or the mixture of several blanc fixes.Its is heavy
It can be 10,20,30,40,50,60,70,80,90,100,110,120,130,140 parts to measure part preferably.
Rare earth oxide is erbium oxide, lanthana, gadolinium oxide, neodymia, cerium oxide, the oxygen of 0.4 μm -20 μm of Fisher particle size
Change the mixture of praseodymium, a kind of rareearth oxidate powder in samarium oxide or several rareearth oxidate powders.Its parts by weight preferably can be
10,20,40,60,80,100,120,140,160,180,200,220,240 parts.
Wherein, lead member is all free of in activator, anti-aging agent, antiscorching agent, plasticizer, compatilizer, vulcanization accelerator, vulcanizing agent
Element.The prior art may be used in these.It is, however, preferable that
Contain zinc oxide, preferably indirect process zinc oxide in activator.
Antiscorching agent is preferably sulfonamide antiscorchiag agent, more preferably N- cyclohexyl thiophthalamides.
Plasticizer is preferably one kind in aromatic naphtha, naphthenic oil or paraffin oil.
Compatilizer is preferably silane coupling agent.
The preparation method of the above-mentioned tungsten-based composite material applied to alpha ray shield, step are：
(1) feed proportioning prepares：Various raw materials are weighed up quality by formula, and by rubber such as anti-aging agent, vulcanization accelerators
Pellet in auxiliary agent is crushed powdering.
(2) prepared by mixed fillers：By fillers such as tungsten powder, tungsten fiber, blanc fixe, rareearth oxidate powders in vacuum drying chamber
Middle vacuum drying, and it is uniformly mixed obtained mixed fillers in a vacuum high speed mixer.
(3) rubber compounding：Rubber, activator, anti-aging agent, antiscorching agent, mixed fillers, plasticising are sequentially added in mixer
Agent, compatilizer, vulcanization accelerator, vulcanizing agent etc., after mixing is uniform, open mill mill clot, and lower item is parked.
(4) extrusion calendaring：Adhesive tape input pin cold feed extruder will be parked, with fluid pressure type wide cut head extrusion, and
It is rolled into sheet material through calender, after cutting edge cools down, (preferred, to be padded with high-strength double-sided release paper) is padded with paper or cloth and is received
Volume is parked.
(5) vulcanization forming：Double-sided release paper is led out, calendered sheet is imported into drum vulcanizer vulcanization forming, export winding.
The beneficial effects of the invention are as follows：
1. the present invention is with the function powders such as tungsten powder, tungsten fiber, barite, rare earth oxide and the standby tungsten base ray of rubber system
Shielding composite has excellent screening ability (lead equivalent is in 0.30mmPb or more) to X-ray and gamma-rays, and belongs to green
Color material is free of lead element, environmentally safe, no biotoxicity, soft easy processing (elongation at break is 500% or more).
2. making composite material have good ray shielding performance compared with the function powder of fine grain and tungsten fiber in the present invention
While, excellent physical mechanical property is had both, nuclear industry, core medical treatment, precision instrument, electric mechanical, nuke rubbish are can be applied to
And the alpha ray shield field of nuclear crisis pollutant storage container etc..
3. powder plasticizing extrusion/calendering/sulfurization technology that the present invention uses, big rule can not be produced by overcoming in foregoing invention
The shortcomings of lattice product, production efficiency are low, density uniformity is poor, poor dimensional precision, poor alpha ray shield effect.
4. the tungsten-based composite material applied to alpha ray shield that the present invention is invented not only functionally realizes core ray
The requirement of shielding, and formally overturned the application mode of tungsten and its alloy and be difficult to forming the problem of, to make
Material product design has higher flexibility.
Specific implementation mode
With reference to specific embodiment, the invention will be further described.
In following embodiment, it is N- cyclohexyl thiophthalamides that activator, which is all zinc oxide, anti-aging agent DNP, antiscorching agent,
(CTP), plasticizer is paraffin oil, compatilizer is silane coupling agent.Accelerator M, vulcanizing agent S.
Embodiment 1
Tungsten-based composite material formula applied to alpha ray shield is：
The preparation method of the tungsten-based composite material applied to alpha ray shield, step are：
(1) feed proportioning prepares：Various raw materials are weighed up quality by formula, and by the grain in anti-aging agent, vulcanization accelerator
Material is crushed powdering.
(2) prepared by mixed fillers：Three kinds of tungsten powders are dried in vacuo in vacuum drying chamber, and in a vacuum high speed mixer
It is uniformly mixed obtained mixed fillers.
(3) rubber compounding：Rubber, activator, anti-aging agent, antiscorching agent are sequentially added in mixer at 90 DEG C -110 DEG C
CTP, mixed fillers, silane coupling agent, vulcanization accelerator, vulcanizing agent etc., after mixing is uniform, 50 DEG C of -60 DEG C of mills of open mill are beaten
Volume, and lower item is parked.
(4) extrusion calendaring：Adhesive tape input pin cold feed extruder will be parked, with 50 DEG C -90 of fluid pressure type wide cut head
It DEG C squeezes out, and is rolled into sheet material through calender, after cutting edge cools down, pad winding is made with high-strength double-sided release paper and is parked.
(5) vulcanization forming：Double-sided release paper is led out, calendered sheet 140 DEG C -150 DEG C of drum vulcanizer of importing is sulfided into
Shape, export winding.
The physical mechanical property and radiation protection performance of the tungsten matrix composite sheet applied to alpha ray shield of gained are such as
Under：
Embodiment 2
Tungsten-based composite material formula applied to alpha ray shield is：
The preparation method of the tungsten-based composite material applied to alpha ray shield, step are：
(1) feed proportioning prepares：Various raw materials are weighed up quality by formula, and by the grain in anti-aging agent, vulcanization accelerator
Material is crushed powdering.
(2) prepared by mixed fillers：Tungsten powder, gadolinium oxide powder are dried in vacuo in vacuum drying chamber, and mixed in vacuum high speed
Obtained mixed fillers are uniformly mixed in conjunction machine.
(3) rubber compounding：Rubber, activator, anti-aging agent, antiscorching agent are sequentially added in mixer at 90 DEG C -110 DEG C
CTP, mixed fillers, silane coupling agent, vulcanization accelerator, vulcanizing agent etc., after mixing is uniform, 50 DEG C of -60 DEG C of mills of open mill are beaten
Volume, and lower item is parked.
(4) extrusion calendaring：Adhesive tape input pin cold feed extruder will be parked, with 50 DEG C -90 of fluid pressure type wide cut head
It DEG C squeezes out, and is rolled into sheet material through calender, after cutting edge cools down, pad winding is made with high-strength double-sided release paper and is parked.
(5) vulcanization forming：Double-sided release paper is led out, calendered sheet 140 DEG C -150 DEG C of drum vulcanizer of importing is sulfided into
Shape, export winding.
The physical mechanical property and radiation protection performance of the tungsten matrix composite sheet applied to alpha ray shield of gained are such as
Under：
Embodiment 3
Tungsten-based composite material formula applied to alpha ray shield is：
The preparation method of the tungsten-based composite material applied to alpha ray shield, step are：
(1) feed proportioning prepares：Various raw materials are weighed up quality by formula, and by the grain in anti-aging agent, vulcanization accelerator
Material is crushed powdering.
(2) prepared by mixed fillers：Tungsten powder, blanc fixe are dried in vacuo in vacuum drying chamber, and mixed in vacuum high speed
Obtained mixed fillers are uniformly mixed in conjunction machine.
(3) rubber compounding：Rubber, activator, anti-aging agent, antiscorching agent are sequentially added in mixer at 90 DEG C -110 DEG C
CTP, mixed fillers, silane coupling agent, vulcanization accelerator, vulcanizing agent etc., after mixing is uniform, 50 DEG C of -60 DEG C of mills of open mill are beaten
Volume, and lower item is parked.
(4) extrusion calendaring：Adhesive tape input pin cold feed extruder will be parked, with 50 DEG C -90 of fluid pressure type wide cut head
It DEG C squeezes out, and is rolled into sheet material through calender, after cutting edge cools down, pad winding is made with high-strength double-sided release paper and is parked.
(5) vulcanization forming：Double-sided release paper is led out, calendered sheet 140 DEG C -150 DEG C of drum vulcanizer of importing is sulfided into
Shape, export winding.
The physical mechanical property and radiation protection performance of the tungsten matrix composite sheet applied to alpha ray shield of gained are such as
Under：
Embodiment 4
Tungsten-based composite material formula applied to alpha ray shield is：
The preparation method of the tungsten-based composite material applied to alpha ray shield, step are：
(1) feed proportioning prepares：Various raw materials are weighed up quality by formula, and by the grain in anti-aging agent, vulcanization accelerator
Material is crushed powdering.
(2) prepared by filler：Tungsten powder, gadolinium oxide powder, blanc fixe, tungsten fiber are dried in vacuo in vacuum drying chamber.
(3) rubber compounding：Rubber, activator, anti-aging agent, antiscorching agent are sequentially added in mixer at 90 DEG C -110 DEG C
CTP, mixed fillers, silane coupling agent, paraffin oil, vulcanization accelerator, vulcanizing agent etc., after mixing is uniform, 50 DEG C -60 DEG C of open mill
Mill clot, and lower item is parked.
(4) extrusion calendaring：Adhesive tape input pin cold feed extruder will be parked, with 50 DEG C -90 of fluid pressure type wide cut head
It DEG C squeezes out, and is rolled into sheet material through calender, after cutting edge cools down, pad winding is made with high-strength double-sided release paper and is parked.
(5) vulcanization forming：Double-sided release paper is led out, calendered sheet 170 DEG C -180 DEG C of drum vulcanizer of importing is sulfided into
Shape, export winding.
The physical mechanical property and radiation protection performance of the tungsten matrix composite sheet applied to alpha ray shield of gained are such as
Under：
Claims (10)
1. a kind of tungsten-based composite material applied to alpha ray shield consists of the following compositions by weight：
100 parts by weight of rubber；
- 500 parts by weight of 200 parts by weight of tungsten powder；
- 50 parts by weight of 0.5 parts by weight of tungsten fiber；
- 250 parts by weight of 120 parts by weight of rareearth oxidate powder or -150 parts by weight of 0.5 parts by weight of blanc fixe and rare earth oxide
- 250 parts by weight of 120 parts by weight of powder；
- 6 parts by weight of 0.5 parts by weight of compatilizer；
- 9 parts by weight of 3 parts by weight of activator；
- 50 parts by weight of 0.5 parts by weight of plasticizer；
- 3 parts by weight of 0.5 parts by weight of anti-aging agent；
- 0.5 parts by weight of 0.05 parts by weight of antiscorching agent；
- 3 parts by weight of 0.5 parts by weight of vulcanization accelerator；
- 3 parts by weight of 0.5 parts by weight of vulcanizing agent；
Wherein, the tungsten powder is a kind of tungsten powder of 0.4 μm -20 μm of Fisher particle size or the mixture of several tungsten powders；The tungsten
Fiber is 10 μm -30 μm of diameter, a kind of tungsten fiber of draw ratio 50-150 or the mixture of several tungsten fibers；The barite
Powder is a kind of blanc fixe of 0.1 μm -5 μm of Fisher particle size or the mixture of several blanc fixes；The rareearth oxidate powder
Fisher particle size is 0.4 μm -20 μm.
2. a kind of tungsten-based composite material applied to alpha ray shield according to claim 1, which is characterized in that the rare earth
Oxide includes at least one of erbium oxide, lanthana, gadolinium oxide, neodymia, cerium oxide, praseodymium oxide, samarium oxide.
3. a kind of tungsten-based composite material applied to alpha ray shield according to claim 1, which is characterized in that the work
Agent, anti-aging agent, antiscorching agent, plasticizer, compatilizer, vulcanization accelerator, vulcanizing agent are all free of lead element.
4. a kind of tungsten-based composite material applied to alpha ray shield according to claim 1 or 3, which is characterized in that described
Activator contain zinc oxide.
5. a kind of tungsten-based composite material applied to alpha ray shield according to claim 4, which is characterized in that the oxidation
Zinc is indirect process zinc oxide.
6. a kind of tungsten-based composite material applied to alpha ray shield according to claim 1 or 3, which is characterized in that described
Antiscorching agent be sulfonamide antiscorchiag agent.
7. a kind of tungsten-based composite material applied to alpha ray shield according to claim 6, which is characterized in that the secondary sulphur
Amides antiscorching agent is N- cyclohexyl thio phthalimides.
8. a kind of tungsten-based composite material applied to alpha ray shield according to claim 1 or 3, which is characterized in that described
Plasticizer be aromatic naphtha, naphthenic oil or paraffin oil in one kind.
9. a kind of tungsten-based composite material applied to alpha ray shield according to claim 1 or 3, which is characterized in that described
Compatilizer be silane coupling agent.
10. a kind of preparation method of tungsten-based composite material applied to alpha ray shield according to claim 1, step
For：
(1) feed proportioning prepares：Various raw materials are weighed up quality by formula, and by activator, anti-aging agent, antiscorching agent, plasticizer,
Compatilizer, vulcanization accelerator, vulcanizing agent pellet are crushed powdering respectively；
(2) prepared by mixed fillers：Tungsten powder, tungsten fiber, blanc fixe, rare earth oxide are dried in vacuo in vacuum drying chamber,
And it is uniformly mixed obtained mixed fillers in a vacuum high speed mixer；
(3) rubber compounding：Sequentially added in mixer rubber, activator, anti-aging agent, antiscorching agent, mixed fillers, compatilizer,
Plasticizer, vulcanization accelerator, vulcanizing agent, after mixing is uniform, open mill mill clot, and lower item is parked；
(4) extrusion calendaring：Adhesive tape input pin cold feed extruder will be parked, with fluid pressure type wide cut head extrusion, and through pressure
Prolong machine and be rolled into sheet material, after cutting edge cools down, pad winding is made with paper or cloth and is parked；
(5) vulcanization forming：Paper or cloth are led out, calendered sheet is imported into drum vulcanizer vulcanization forming, export winding.
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| CN106128537B (en) * | 2016-07-29 | 2019-01-08 | 何天泽 | A kind of radiation protection red copper stereotype |
| CN107910089A (en) * | 2017-11-17 | 2018-04-13 | 南京核安核能科技有限公司 | A kind of protective garment of the unleaded radiation of novel flexible |
| CN114634659B (en) * | 2022-04-18 | 2023-08-08 | 扬州大学 | Flexible shielding material and preparation method thereof |
| CN115181428A (en) * | 2022-08-25 | 2022-10-14 | 中广核工程有限公司 | Organic silicon composite material and preparation method and application thereof |
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| WO2009004710A1 (en) * | 2007-07-02 | 2009-01-08 | Ohara Inc. | Glass composition |
| CN101570606A (en) * | 2009-06-15 | 2009-11-04 | 北京化工大学 | Overall lead-free X-ray shielding rubber compound material |
| CN102585330A (en) * | 2012-01-18 | 2012-07-18 | 厦门虹鹭钨钼工业有限公司 | Tungsten-polymer composite material and preparation method thereof |
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| WO2009004710A1 (en) * | 2007-07-02 | 2009-01-08 | Ohara Inc. | Glass composition |
| CN101570606A (en) * | 2009-06-15 | 2009-11-04 | 北京化工大学 | Overall lead-free X-ray shielding rubber compound material |
| CN102585330A (en) * | 2012-01-18 | 2012-07-18 | 厦门虹鹭钨钼工业有限公司 | Tungsten-polymer composite material and preparation method thereof |
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