CN114561061A - POE (polyolefin elastomer) calendered material for X and gamma ray protection and preparation method thereof - Google Patents
POE (polyolefin elastomer) calendered material for X and gamma ray protection and preparation method thereof Download PDFInfo
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- 229920006124 polyolefin elastomer Polymers 0.000 title claims abstract description 181
- 239000000463 material Substances 0.000 title claims abstract description 59
- 230000005251 gamma ray Effects 0.000 title claims abstract description 45
- 238000003490 calendering Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 78
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical class [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000005096 rolling process Methods 0.000 claims abstract description 48
- 150000001621 bismuth Chemical class 0.000 claims abstract description 42
- 150000003657 tungsten Chemical class 0.000 claims abstract description 42
- 150000003481 tantalum Chemical class 0.000 claims abstract description 33
- 238000007731 hot pressing Methods 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 46
- 238000002156 mixing Methods 0.000 claims description 46
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 28
- 229910052797 bismuth Inorganic materials 0.000 claims description 20
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 20
- 238000002844 melting Methods 0.000 claims description 20
- 230000008018 melting Effects 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 20
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims description 19
- 229940075613 gadolinium oxide Drugs 0.000 claims description 19
- 229910052721 tungsten Inorganic materials 0.000 claims description 19
- 239000010937 tungsten Substances 0.000 claims description 19
- 229910052715 tantalum Inorganic materials 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 14
- 238000012986 modification Methods 0.000 claims description 13
- 230000004048 modification Effects 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000003760 magnetic stirring Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 10
- 229920001721 polyimide Polymers 0.000 claims description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 10
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000005453 pelletization Methods 0.000 claims 1
- 230000005855 radiation Effects 0.000 description 6
- 238000000465 moulding Methods 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000000333 X-ray scattering Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000005025 nuclear technology Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0887—Tungsten
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
Abstract
The invention discloses a POE (polyolefin elastomer) rolling material for X and gamma ray protection and a preparation method thereof, relating to the field of ray protection, and the POE rolling material consists of 18-28% of modified gadolinium oxide, 18-28% of modified bismuth, 9-16% of modified tungsten, 9-16% of modified tantalum and the balance of POE particles; the POE rolled material for X and gamma ray protection is of one of a layered rolled plate structure or a mixed rolled plate structure, and the preparation process comprises the following steps: modifying, granulating, hot-pressing to form a plate and calendering to form. The invention has the advantages that: the POE rolled material for X and gamma ray protection has extremely high protection efficiency on rays with different energy intensities, and simultaneously has the surface density of about 2.3kg/m2, and has the advantages of light weight and high efficiency compared with the existing ray protection material.
Description
Technical Field
The invention relates to the field of ray protection, in particular to a POE (polyolefin elastomer) calendered material for X and gamma ray protection and a preparation method thereof.
Background
The development of nuclear technology brings convenience to people and simultaneously generates a lot of radiation hazards, and the radiation protection articles which are light, flexible and excellent in protection performance are hot spots of current research. The radiation protection material is mainly divided into a lead material and a lead-free material. Lead is mainly lead, and although the protective effect is good, the lead has toxicity, poor strength and large low-energy X-ray scattering. The lead-free material mainly comprises a composite material prepared from rare earth elements and heavy metal compounds such as tin, tungsten, bismuth and the like, and has excellent protection effect, light weight and safety.
In the aspect of radiation protection, the range of radiation energy absorption of a protective material filled with a single metal or a compound thereof is relatively limited, and a multilayer protective material prepared by layer-by-layer compounding of different metals or compounds thereof can simultaneously absorb radiation with different energy, so that a composite POE (polyolefin elastomer) rolling material for X and gamma ray protection is provided.
Disclosure of Invention
In order to solve the technical problems, the POE calendering material for X-ray and gamma-ray protection and the preparation method thereof are provided.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
a POE (polyolefin elastomer) calendering material for X and gamma ray protection is composed of the following raw materials in parts by weight:
18-28% of modified gadolinium oxide, 18-28% of modified bismuth, 9-16% of modified tungsten, 9-16% of modified tantalum and the balance of POE particles;
the POE rolling material for X and gamma ray protection is of a layered rolling plate structure or a mixed rolling plate structure.
Preferably, the preparation process of the modified gadolinium oxide, the modified bismuth, the modified tungsten and the modified tantalum comprises the following steps:
respectively placing the powder of gadolinium oxide, bismuth, tungsten and tantalum into ethanol, dispersing, then adding a silane coupling agent for modification, stirring, centrifuging, washing and drying to respectively obtain modified gadolinium oxide, modified bismuth, modified tungsten and modified tantalum.
Further, a preparation process of the POE layered rolling material for X and gamma ray protection is provided, which is used for preparing the POE layered rolling material for X and gamma ray protection of the layered rolling plate-shaped structure, and comprises the following steps:
modification: respectively placing powder of gadolinium oxide, bismuth, tungsten and tantalum with the particle size of 50-100nm into ethanol, performing ultrasonic dispersion for 10-20min, then adding octaaminophenyltrioxasilane, performing magnetic stirring for 18-24h, then performing centrifugal operation at the speed of 8000-10000 r/min, then washing for 2-3 times by adopting absolute ethyl alcohol, and then drying at the temperature of 60-70 ℃ for 12-16h to respectively obtain modified gadolinium oxide, modified bismuth, modified tungsten and modified tantalum powder;
and (3) granulation: respectively melting and mixing modified gadolinium oxide, modified bismuth, modified tungsten and modified tantalum powder and POE particles according to the proportion of 1-2:3-4, uniformly stirring, and granulating to respectively obtain modified gadolinium oxide POE particles, modified bismuth POE particles, modified tungsten POE particles and modified tantalum POE particles;
hot pressing to form a plate: respectively placing modified gadolinium oxide POE particles, modified bismuth POE particles, modified tungsten POE particles and modified tantalum POE particles on a polyimide film, and hot-pressing by using a hot press to respectively obtain a modified gadolinium oxide POE plate, a modified bismuth POE plate, a modified tungsten POE plate and a modified tantalum POE plate;
layering and calendaring and forming: and overlapping the modified gadolinium oxide POE plate, the modified bismuth POE plate, the modified tungsten POE plate and the modified tantalum POE plate according to the thickness proportion of 30-35% of the modified gadolinium oxide layer, 30-35% of the modified bismuth layer, 15-20% of the modified tungsten layer and 15-20% of the modified tantalum layer, and rolling by using a roller of a calender to obtain the POE layered rolling material for protecting X and gamma rays.
Optionally, in the granulating step, the melting temperature is 60-80 ℃, the stirring is mechanical stirring, and the stirring time is 2-4 h.
Optionally, in the step of hot pressing to form the plate, the hot pressing temperature is 60 ℃ to 80 ℃.
Optionally, in the step of layered calendering and molding, the calendering parameters are as follows: the temperature of the upper roller is 70-90 ℃, the temperature of the middle roller is 60-80 ℃, the temperature of the lower roller is 50-70 ℃, the roller distance is 1mm, and the rolling speed is 30-50 m/min.
Still further, a preparation process of the POE mixed rolled material for X and gamma ray protection is provided, which is used for preparing the POE rolled material for X and gamma ray protection of the mixed rolled plate-shaped structure, and comprises the following steps:
mixing modification: mixing gadolinium oxide powder, bismuth powder, tungsten powder and tantalum powder with the particle size of 50-100nm according to the mass percentage of 30-35% of gadolinium oxide, 30-35% of bismuth, 15-20% of tungsten and 15-20% of tantalum, placing the mixture into ethanol, performing ultrasonic dispersion for 10-20min, adding octaaminophenyltrioxasilane, performing magnetic stirring for 18-24h, performing centrifugal operation at the speed of 8000r/min-10000r/min, washing for 2-3 times by adopting absolute ethyl alcohol, and drying for 12-16h at the temperature of 60-70 ℃ to obtain modified mixed powder;
mixing and granulating: melting and mixing the modified mixed powder and POE particles according to the proportion of 1-2:3-4, uniformly stirring, and granulating to obtain modified mixed POE particles;
mixing and hot-pressing to form a plate: placing the modified mixed POE particles on a polyimide film, and carrying out hot pressing by using a hot press to obtain a modified mixed POE plate;
mixing, calendaring and forming: and (3) rolling the modified mixed POE plate by a roller of a rolling mill to obtain the POE mixed rolled material for X and gamma ray protection.
Optionally, in the mixing and granulating step, the melting temperature is 60-80 ℃, the stirring is mechanical stirring, and the stirring time is 2-4 h.
Optionally, in the step of mixing and hot-pressing to form the plate, the hot-pressing temperature is 60-80 ℃.
Optionally, in the step of mixing, calendering and molding, the calendering parameters are as follows: the temperature of the upper roller is 70-90 ℃, the temperature of the middle roller is 60-80 ℃, the temperature of the lower roller is 50-70 ℃, the roller distance is 1mm, and the rolling speed is 30-50 m/min.
Compared with the prior art, the invention has the advantages that:
according to the invention, the powder of gadolinium oxide, bismuth, tungsten and tantalum is modified by octaaminophenyltrioxasilane, then is melted and mixed with POE elastic particles to prepare modified POE particles, and then is hot-pressed and calendered to prepare the POE calendered material containing gadolinium oxide, bismuth, tungsten and tantalum for ray protection, so that X rays and gamma rays with various energies can be effectively protected, and the requirements of different application scenes and different protection grades are met.
Drawings
FIG. 1 is a flow chart of a process for preparing POE layered calendered material for X, gamma ray protection in the present invention;
FIG. 2 is a flow chart of a process for preparing POE mixed calendered material for X, gamma ray protection in the present invention;
FIG. 3 is an SEM image of a POE layered calendered material for X, gamma ray protection in the present invention;
FIG. 4 is an SEM image of the POE mixed rolled material for X-ray and gamma-ray protection in the invention.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
The first embodiment is as follows:
a preparation process of POE layered calendered material for X, gamma ray protection comprises the following steps:
modification: respectively placing powder of gadolinium oxide, bismuth, tungsten and tantalum with the particle size of 50nm into ethanol, performing ultrasonic dispersion for 10min, then adding octaaminophenyltrioxasilane, performing magnetic stirring for 18h, then performing centrifugal operation at the speed of 8000r/min, then washing for 2 times by using absolute ethyl alcohol, and then drying for 16h at the temperature of 60 ℃ to respectively obtain modified gadolinium oxide, modified bismuth, modified tungsten and modified tantalum powder;
and (3) granulation: respectively melting and mixing modified gadolinium oxide, modified bismuth, modified tungsten and modified tantalum powder and POE particles according to the ratio of 3:2, then melting and mixing at 60 ℃, mechanically stirring for 2h, and then granulating to respectively obtain modified gadolinium oxide POE particles, modified bismuth POE particles, modified tungsten POE particles and modified tantalum POE particles;
hot pressing to form a plate: respectively placing modified gadolinium oxide POE particles, modified bismuth POE particles, modified tungsten POE particles and modified tantalum POE particles on a polyimide film, and carrying out hot pressing at 60 ℃ to respectively obtain a modified gadolinium oxide POE plate, a modified bismuth POE plate, a modified tungsten POE plate and a modified tantalum POE plate;
layering and calendaring and forming: after the modified gadolinium oxide POE plate, the modified bismuth POE plate, the modified tungsten POE plate and the modified tantalum POE plate are overlapped according to the thickness proportion of a modified gadolinium oxide layer of 30 percent, a modified bismuth layer of 30 percent, a modified tungsten layer of 20 percent and a modified tantalum layer of 20 percent, the materials are rolled by a roller of a calender to obtain X, and the POE layered rolling material for gamma ray protection has the following rolling technological parameters: the temperature of the upper roll is 70 ℃, the temperature of the middle roll is 60 ℃, the temperature of the lower roll is 50 ℃, the roll spacing is 1mm, and the rolling speed is 30 m/min.
Example two:
a preparation process of POE layered calendered material for X, gamma ray protection comprises the following steps:
modification: respectively placing powder of gadolinium oxide, bismuth, tungsten and tantalum with the particle size of 70nm into ethanol, performing ultrasonic dispersion for 15min, then adding octaaminophenyltrioxasilane, performing magnetic stirring for 20h, then performing centrifugal operation at the speed of 9000r/min, then washing for 3 times by using absolute ethyl alcohol, and then drying for 14h at the temperature of 65 ℃ to respectively obtain modified gadolinium oxide, modified bismuth, modified tungsten and modified tantalum powder;
and (3) granulation: respectively melting and mixing modified gadolinium oxide, modified bismuth, modified tungsten and modified tantalum powder and POE particles according to the proportion of 7:3, then melting and mixing at 70 ℃, mechanically stirring for 3h, and then granulating to respectively obtain modified gadolinium oxide POE particles, modified bismuth POE particles, modified tungsten POE particles and modified tantalum POE particles;
hot pressing to form a plate: respectively placing modified gadolinium oxide POE particles, modified bismuth POE particles, modified tungsten POE particles and modified tantalum POE particles on a polyimide film, and hot-pressing at 70 ℃ to respectively obtain a modified gadolinium oxide POE plate, a modified bismuth POE plate, a modified tungsten POE plate and a modified tantalum POE plate;
layering and calendaring and forming: after the modified gadolinium oxide POE plate, the modified bismuth POE plate, the modified tungsten POE plate and the modified tantalum POE plate are overlapped according to the thickness proportion of a modified gadolinium oxide layer 33%, a modified bismuth layer 33%, a modified tungsten layer 17% and a modified tantalum layer 17%, rolling by a roller of a calender to obtain the POE layered rolling material for gamma ray protection, wherein the rolling technological parameters are as follows: the temperature of the upper roll is 80 ℃, the temperature of the middle roll is 70 ℃, the temperature of the lower roll is 60 ℃, the roll spacing is 1mm, and the rolling speed is 40 m/min.
Example three:
a preparation process of POE layered calendered material for X, gamma ray protection comprises the following steps:
modification: respectively placing powder of gadolinium oxide, bismuth, tungsten and tantalum with the particle size of 100nm into ethanol, performing ultrasonic dispersion for 20min, then adding octaaminophenyltrioxasilane, performing magnetic stirring for 24h, then performing centrifugal operation at the speed of 10000r/min, then washing for 2 times by adopting absolute ethanol, and then drying at the temperature of 70 ℃ for 12h to respectively obtain modified gadolinium oxide, modified bismuth, modified tungsten and modified tantalum powder;
and (3) granulation: respectively melting and mixing modified gadolinium oxide POE particles, modified bismuth POE particles, modified tungsten POE particles and modified tantalum POE particles according to the ratio of 4:1, then melting and mixing at 80 ℃, mechanically stirring for 4h, and then granulating to respectively obtain modified gadolinium oxide POE particles, modified bismuth POE particles, modified tungsten POE particles and modified tantalum POE particles;
hot pressing to form a plate: respectively placing modified gadolinium oxide POE particles, modified bismuth POE particles, modified tungsten POE particles and modified tantalum POE particles on a polyimide film, and carrying out hot pressing at 80 ℃ to respectively obtain a modified gadolinium oxide POE plate, a modified bismuth POE plate, a modified tungsten POE plate and a modified tantalum POE plate;
layering and calendaring and forming: after the modified gadolinium oxide POE plate, the modified bismuth POE plate, the modified tungsten POE plate and the modified tantalum POE plate are overlapped according to the thickness proportion of 35 percent of the modified gadolinium oxide layer, 35 percent of the modified bismuth layer, 15 percent of the modified tungsten layer and 15 percent of the modified tantalum layer, the materials are rolled by a roller of a calender to obtain X, and the POE layered rolling materials for gamma ray protection have the following rolling technological parameters: the temperature of the upper roller is 90 ℃, the temperature of the middle roller is 80 ℃, the temperature of the lower roller is 70 ℃, the roller spacing is 1mm, and the rolling speed is 50 m/min.
Example four:
a preparation process of POE mixed calendaring material for X, gamma ray protection comprises the following steps:
mixing modification: mixing powder of gadolinium oxide, bismuth, tungsten and tantalum with the particle size of 50nm according to the mass percentage of 30% of gadolinium oxide, 30% of bismuth, 20% of tungsten and 20% of tantalum, placing the mixture into ethanol, performing ultrasonic dispersion for 10min, adding octaaminophenyltrioxasilane, performing magnetic stirring for 18h, performing centrifugal operation at the speed of 8000r/min, washing for 2 times by using absolute ethyl alcohol, and drying at the temperature of 60 ℃ for 16h to obtain modified mixed powder;
mixing and granulating: melting and mixing the modified mixed powder and POE particles according to the ratio of 3:2, then melting and mixing at 60 ℃, mechanically stirring for 2 hours, and then granulating to obtain modified mixed POE particles;
mixing and hot-pressing to form a plate: placing the modified mixed POE particles on a polyimide film to carry out hot pressing at 60 ℃ to obtain a modified mixed POE plate;
mixing, calendaring and molding: and (3) rolling the modified mixed POE plate by a roller of a rolling mill to obtain the POE mixed rolled material for X and gamma ray protection, wherein the rolling technological parameters are as follows: the temperature of the upper roll is 70 ℃, the temperature of the middle roll is 60 ℃, the temperature of the lower roll is 50 ℃, the roll spacing is 1mm, and the rolling speed is 30 m/min.
Example five:
mixing modification: mixing powder of gadolinium oxide, bismuth, tungsten and tantalum with the particle size of 70nm according to the mass percent of 33% of gadolinium oxide, 33% of bismuth, 17% of tungsten and 17% of tantalum, then placing the mixture into ethanol, performing ultrasonic dispersion for 15min, then adding octaaminophenyltrioxasilane, performing magnetic stirring for 20h, then performing centrifugal operation at the speed of 9000r/min, then washing for 3 times by using absolute ethyl alcohol, and then drying for 14h at the temperature of 65 ℃ to obtain modified mixed powder;
mixing and granulating: melting and mixing the modified mixed powder and POE particles according to the proportion of 7:3, then melting and mixing at 70 ℃, mechanically stirring for 3h, and then granulating to obtain modified mixed POE particles;
mixing and hot-pressing to form a plate: placing the modified mixed POE particles on a polyimide film to carry out hot pressing at 70 ℃ to obtain a modified mixed POE plate;
mixing, calendaring and forming: and (3) rolling the modified mixed POE plate by a roller of a rolling mill to obtain the POE mixed rolled material for X and gamma ray protection, wherein the rolling technological parameters are as follows: the temperature of the upper roll is 70 ℃, the temperature of the middle roll is 60 ℃, the temperature of the lower roll is 50 ℃, the roll spacing is 1mm, and the rolling speed is 30 m/min.
Example six:
mixing modification: mixing powder of gadolinium oxide, bismuth, tungsten and tantalum with the particle size of 90nm according to the mass percent of 35% of gadolinium oxide, 35% of bismuth, 15% of tungsten and 15% of tantalum, placing the mixture into ethanol, performing ultrasonic dispersion for 20min, adding octaaminophenyltrioxasilane, performing magnetic stirring for 24h, performing centrifugal operation at the speed of 10000r/min, washing for 2 times by using absolute ethyl alcohol, and drying at the temperature of 70 ℃ for 12h to obtain modified mixed powder;
mixing and granulating: melting and mixing the modified mixed powder and POE particles according to the ratio of 4:1, then melting and mixing at 80 ℃, mechanically stirring for 4 hours, and then granulating to obtain modified mixed POE particles;
mixing and hot-pressing to form a plate: placing the modified mixed POE particles on a polyimide film to carry out hot pressing at 80 ℃ to obtain a modified mixed POE plate;
mixing, calendaring and forming: and (3) rolling the modified mixed POE plate by a roller of a rolling mill to obtain the POE mixed rolled material for X and gamma ray protection, wherein the rolling technological parameters are as follows: the temperature of the upper roller is 90 ℃, the temperature of the middle roller is 80 ℃, the temperature of the lower roller is 70 ℃, the roller spacing is 1mm, and the rolling speed is 50 m/min.
The POE rolled materials for X and gamma ray protection prepared in the examples are tested for protection efficiency under different ray energies, and the results are shown in the following table:
from the results in the table, the POE rolled material for X-ray and gamma-ray protection prepared by the invention has extremely high protection efficiency on rays with different energy intensities, and simultaneously has the surface density of about 2.3kg/m2, and has the advantages of light weight and high efficiency compared with the existing ray protection materials.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The POE (polyolefin elastomer) calendered material for X and gamma ray protection is characterized by comprising the following raw materials in parts by weight:
18-28% of modified gadolinium oxide, 18-28% of modified bismuth, 9-16% of modified tungsten, 9-16% of modified tantalum and the balance of POE particles;
the POE rolling material for X and gamma ray protection is of a layered rolling plate structure or a mixed rolling plate structure.
2. The POE (polyolefin elastomer) calendered material for X, gamma ray protection according to claim 1, wherein the preparation process of the modified gadolinium oxide, the modified bismuth, the modified tungsten and the modified tantalum comprises the following steps:
respectively placing the powder of gadolinium oxide, bismuth, tungsten and tantalum into ethanol, dispersing, then adding a silane coupling agent for modification, stirring, centrifuging, washing and drying to respectively obtain modified gadolinium oxide, modified bismuth, modified tungsten and modified tantalum.
3. A process for preparing a POE laminated rolled material for X, γ ray protection, which is used for the preparation of the POE laminated rolled material for X, γ ray protection of the laminated rolled plate-like structure as claimed in claim 1, comprising the steps of:
modification: respectively placing powder of gadolinium oxide, bismuth, tungsten and tantalum with the particle size of 50-100nm into ethanol, performing ultrasonic dispersion for 10-20min, then adding octaaminophenyltrioxasilane, performing magnetic stirring for 18-24h, then performing centrifugal operation at the speed of 8000-10000 r/min, then washing for 2-3 times by adopting absolute ethyl alcohol, and then drying at the temperature of 60-70 ℃ for 12-16h to respectively obtain modified gadolinium oxide, modified bismuth, modified tungsten and modified tantalum powder;
and (3) granulation: respectively melting and mixing modified gadolinium oxide, modified bismuth, modified tungsten and modified tantalum powder and POE particles according to the proportion of 1-2:3-4, uniformly stirring, and granulating to respectively obtain modified gadolinium oxide POE particles, modified bismuth POE particles, modified tungsten POE particles and modified tantalum POE particles;
hot pressing to form a plate: respectively placing modified gadolinium oxide POE particles, modified bismuth POE particles, modified tungsten POE particles and modified tantalum POE particles on a polyimide film, and hot-pressing by using a hot press to respectively obtain a modified gadolinium oxide POE plate, a modified bismuth POE plate, a modified tungsten POE plate and a modified tantalum POE plate;
layering and calendaring and forming: and (3) overlapping the modified gadolinium oxide POE plate, the modified bismuth POE plate, the modified tungsten POE plate and the modified tantalum POE plate according to the thickness proportion of 30-35% of the modified gadolinium oxide layer, 30-35% of the modified bismuth layer, 15-20% of the modified tungsten layer and 15-20% of the modified tantalum layer, and rolling by using a roller of a calender to obtain the POE layered rolling material for protecting X and gamma rays.
4. The process for preparing POE (polyolefin elastomer) layered and calendered material for X and gamma ray protection according to claim 3, wherein the melting temperature in the granulation step is 60-80 ℃, the stirring is mechanical stirring, and the stirring time is 2-4 h.
5. The process for preparing POE (polyolefin elastomer) layered and rolled material for X and gamma ray protection according to claim 3, wherein the hot pressing temperature in the step of hot pressing to form the plate is 60-80 ℃.
6. The process for preparing POE (polyolefin elastomer) layered and rolled material for X and gamma ray protection according to claim 3, wherein in the step of layered and rolled forming, the rolling parameters are as follows: the temperature of the upper roller is 70-90 ℃, the temperature of the middle roller is 60-80 ℃, the temperature of the lower roller is 50-70 ℃, the roller distance is 1mm, and the rolling speed is 30-50 m/min.
7. A process for preparing a POE mixed rolled material for X, γ ray protection, which is used for preparing the POE mixed rolled material for X, γ ray protection of the mixed rolled plate-shaped structure as claimed in claim 1, comprising the following steps:
mixing modification: mixing powder of gadolinium oxide, bismuth, tungsten and tantalum with the particle size of 50-100nm according to the mass percentage of 30-35% of gadolinium oxide, 30-35% of bismuth, 15-20% of tungsten and 15-20% of tantalum, placing the mixture into ethanol, performing ultrasonic dispersion for 10-20min, adding octaaminophenyltrioxasilane, performing magnetic stirring for 18-24h, performing centrifugal operation at the speed of 8000r/min-10000r/min, washing for 2-3 times by using absolute ethyl alcohol, and drying for 12-16h at the temperature of 60-70 ℃ to obtain modified mixed powder;
mixing and granulating: melting and mixing the modified mixed powder and POE particles according to the proportion of 1-2:3-4, uniformly stirring, and granulating to obtain modified mixed POE particles;
mixing and hot-pressing to form a plate: placing the modified mixed POE particles on a polyimide film, and carrying out hot pressing by using a hot press to obtain a modified mixed POE plate;
mixing, calendaring and forming: and (3) rolling the modified mixed POE plate by a roller of a rolling mill to obtain the POE mixed rolled material for X and gamma ray protection.
8. The process for preparing POE (polyolefin elastomer) mixed and calendered material for X and gamma ray protection as claimed in claim 7, wherein the melting temperature in the mixing and pelletizing step is 60-80 ℃, the stirring is mechanical stirring, and the stirring time is 2-4 h.
9. The process for preparing POE (polyolefin elastomer) mixed and rolled material for X and gamma ray protection according to claim 7, wherein the hot pressing temperature in the step of mixing and hot pressing to form the plate is 60-80 ℃.
10. The process for preparing POE (polyolefin elastomer) mixed and rolled material for X and gamma ray protection according to claim 7, wherein in the step of mixed and rolled forming, the rolling parameters are as follows: the temperature of the upper roller is 70-90 ℃, the temperature of the middle roller is 60-80 ℃, the temperature of the lower roller is 50-70 ℃, the roller distance is 1mm, and the rolling speed is 30-50 m/min.
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|---|---|---|---|---|
| EP0780207A2 (en) * | 1995-12-23 | 1997-06-25 | Tarkett Aktiengesellschaft | Method for the fabrication of multilayer polyolefin coverings having foamed interlayers |
| KR101890267B1 (en) * | 2017-03-07 | 2018-10-01 | 라스고 주식회사 | Method for preparing lead-free radiation sheilding sheet |
| CN113696369A (en) * | 2021-09-08 | 2021-11-26 | 西安工程大学 | Preparation method of X-ray and gamma-ray protective body based on thermoplastic elastomer |
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2022
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|---|---|---|---|---|
| EP0780207A2 (en) * | 1995-12-23 | 1997-06-25 | Tarkett Aktiengesellschaft | Method for the fabrication of multilayer polyolefin coverings having foamed interlayers |
| KR101890267B1 (en) * | 2017-03-07 | 2018-10-01 | 라스고 주식회사 | Method for preparing lead-free radiation sheilding sheet |
| CN113696369A (en) * | 2021-09-08 | 2021-11-26 | 西安工程大学 | Preparation method of X-ray and gamma-ray protective body based on thermoplastic elastomer |
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