CN113214558B - High-use-temperature accident-condition-resistant anti-irradiation material and preparation method thereof - Google Patents
High-use-temperature accident-condition-resistant anti-irradiation material and preparation method thereof Download PDFInfo
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- 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
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- C08K13/02—Organic and inorganic ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
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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
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/068—Ultra high molecular weight polyethylene
Abstract
The invention discloses a high-service-temperature accident-condition-resistant anti-radiation material and a preparation method thereof, and solves the technical problems that the existing shielding material taking a polyethylene material as a base body can be plasticized and collapsed in a short time at the temperature of an accident-condition environment, cannot keep a shielding function, flows and aggravates the unsafe condition in a pile. The radiation-resistant composite additive is compounded by nanometer rare earth oxide and an organic radiation-resistant composite system. The invention has the advantages of good mechanical property and radiation resistance of the radiation-resistant material.
Description
Technical Field
The invention relates to the technical field of nuclear radiation protection, in particular to a high-use-temperature accident-resistant working condition anti-irradiation material and a preparation method thereof.
Background
The lead-boron polyethylene can simultaneously shield gamma rays, slow fast neutrons and absorb thermal neutrons, the hydrogen content of the polyethylene reaches 14%, the molding processability is excellent, and the fillability to lead and boron carbide materials is excellent, so the lead-boron polyethylene material is an ideal comprehensive radiation field shielding material. The method is widely applied to shielding of a primary loop and a secondary loop in model engineering.
At present, the technology for preparing the lead-boron polyethylene is mature, but the polyethylene used in the technology is mostly high-density polyethylene or low-density polyethylene, and the polyethylene is easy to deform or plasticize and flow at high temperature. As a shielding material used for a primary circuit, after the shielding material is used for a long time and the temperature exceeds 80 ℃, the material can deform, so that a gap of a shielding body becomes large, and radiation leakage is caused. Particularly, under the accident condition, the environmental temperature can reach over 180 ℃, and the shielding material taking the traditional polyethylene material as the matrix can be plasticized and collapsed in a short time under the accident condition environmental temperature, can not keep the shielding function at all, and generates flowing, so that the insecurity in the pile is aggravated.
In order to solve the problem of low use temperature of polyethylene-based shielding materials, shielding materials using polypropylene-based, epoxy-based, and engineering plastics such as polyether ether ketone, polyphenylene sulfide, polyimide, etc. as a base have been developed. The polypropylene material has poor irradiation resistance due to the chain segment structure, and the material can be quickly irradiated and deteriorated under the irradiation environment, so that the performance is reduced, the service life is shortened, and the use safety of the material is influenced. The epoxy resin-based shielding material is a casting type thermosetting material, is suitable for shielding containers and special-shaped positions, and has the defect that casting bubbles, layering and other defects easily influence the shielding performance when parts such as shielding plates, shielding bodies and the like are prepared. Engineering plastics are high-temperature resistant materials, but are difficult to machine and form, high in cost, particularly the materials are low in hydrogen content, usually about 4%, and have large influence on the moderating performance of fast neutrons, so that the application field of the materials is limited.
Therefore, in view of the above problems, there is a need to improve the temperature resistance and radiation resistance of polyethylene base materials without affecting the shielding properties and processability.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the shielding material taking the existing polyethylene material as the matrix can be plasticized and collapsed in a short time at the temperature of the accident working condition environment, cannot keep the shielding function, and flows to aggravate the insecurity in the reactor.
The invention is realized by the following technical scheme:
the high-service-temperature accident-condition-resistant anti-radiation material comprises ultrahigh-molecular-weight polyethylene, shielding substance filler and an anti-radiation composite additive, wherein the anti-radiation composite additive is formed by compounding a nano rare earth oxide and an organic anti-radiation composite system.
The high service temperature of the invention particularly means that the shape can be kept without collapsing and the function can be kept when the accident working condition is about 200 ℃, and the safety and the reliability of the shielding body are improved. Meanwhile, the temperature can be increased from room temperature to about 120 ℃ after long-term use, so that the long-term use is realized without deformation and ray beam leakage.
The invention utilizes the characteristics of good heat resistance and extremely poor plasticizing fluidity at high temperature of the ultra-high molecular weight polyethylene to ensure that the polyethylene-based shielding material can not deform after being used for a long time under the condition of higher temperature, can keep the shape under the working condition of an accident, and improves the radiation resistance of the material through the cooperation with the radiation-resistant composite additive, wherein the radiation-resistant composite additive is formed by compounding nano rare earth oxide and an organic radiation-resistant composite system, is an organic-inorganic composite material, has good heat resistance of the nano rare earth oxide and is distributed in the organic radiation-resistant composite system, after being distributed in the ultra-high molecular weight polyethylene, the organic radiation-resistant composite system can form a membrane when being irradiated, and can slow down the chain segment fracture of the polyethylene, and the rare earth oxide can absorb partial radiation and is beneficial to transferring heat, so that the local heat and the irradiation energy are reduced, the irradiation damage is reduced, and the heat resistance and the irradiation resistance are improved together. On the other hand, the nanometer rare earth oxide has shielding effect on low-energy rays, and is distributed in the polyethylene matrix to be mixed with the shielding material filler, so that the shielding function is integrally improved.
The invention preferably selects a high-use-temperature anti-accident working condition anti-radiation material, the organic anti-radiation composite system is a polyolefin anti-aging composite system, the polyolefin anti-aging composite system comprises a phenol anti-aging agent and a phosphite ester anti-aging agent, the mass ratio of the phenol anti-aging agent to the phosphite ester anti-aging agent is 1: 5-3: 4, the phenol anti-aging agent and the phosphite ester anti-aging agent are sold in the market, and the mass ratio of the nano rare earth oxide to the polyolefin anti-aging composite system is 1-5: 100.
furthermore, the rare earth oxide is yttrium oxide, and the organic anti-radiation composite system is prepared by compounding a plurality of phenols and phosphite stabilizers.
The invention preferably selects an anti-irradiation material with high service temperature and accident-resistant working condition, and the addition amount of the anti-irradiation composite additive is 1-2.5% of the total mass.
The invention preferably selects a high-use-temperature accident-resistant working condition anti-radiation material which comprises the following components in percentage by mass:
ultra-high molecular weight polyethylene: 15-50 percent
Radiation-resistant composite additive: 1 to 2.5 percent;
the rest is shielding material filler.
The invention preferably selects a high-use-temperature accident-condition-resistant anti-radiation material, and the molecular weight of the ultra-high molecular weight polyethylene is 300-900 ten thousand.
The invention preferably selects a high-use-temperature accident-condition-resistant anti-radiation material, and the molecular weight of the ultra-high molecular weight polyethylene is 500-900 ten thousand.
The inventor shows that when the molecular weight is more than 500 ten thousand, the heat resistance and the radiation resistance are better through the result of mixing the ultrahigh molecular weight polyethylene with different molecular weights and the radiation resistance composite additive.
A preparation method of a high-use-temperature accident-condition-resistant anti-radiation material comprises the following steps:
step 1: ball-milling the nano rare earth oxide and polyolefin anti-aging composite system to obtain an irradiation-resistant composite additive;
step 2: diluting the radiation-resistant composite additive and adding the diluted radiation-resistant composite additive into a shielding material filler;
and step 3: and mixing to obtain the anti-irradiation material.
The invention preferably discloses a preparation method of an anti-irradiation material with high service temperature and accident-resistant working condition, wherein in the step 1, ethanol is added as a dispersing agent during ball milling, the addition amount of the ethanol is 2-10% of the sum of the mass of a nano rare earth oxide and polyolefin anti-aging composite system, and the ratio of the total mass of the nano rare earth oxide and polyolefin anti-aging composite system to a grinding ball is 1: 8-20.
According to the invention, the uniformity and embeddability of the nano rare earth oxide and polyolefin anti-aging composite system in the radiation-resistant composite additive are improved through ball milling, and the dispersion of the nano rare earth oxide in the polyolefin anti-aging composite system is improved through adding ethanol as a diluent and a dispersant.
When the shielding material filler is lead powder and boron carbide powder, the mixing in the step 3 is two-step mixing, wherein in the first step, the lead powder and the boron carbide powder are mixed and sprayed with diluted radiation-resistant composite additive, and in the second step, the ultrahigh molecular weight polyethylene is mixed with the material obtained in the first step.
Furthermore, the purity of the lead powder is more than 99.99%, and the boron carbide powder is more than the grade II of the core, so that the secondary activation dose of the material reactor core shielding is reduced.
The invention preferably selects a preparation method of the anti-radiation material with high use temperature and accident-resistant working condition, and the second step of mixing adopts double-speed mixing with low speed and high speed, and the mixing is repeated for 2-3 times to obtain the lead-boron polyethylene material.
The invention improves the mixing uniformity of the whole material by two-step mixing and matching with low-speed-high-speed interval mixing.
The lead-boron polyethylene material can be used for plate forming by hot press forming or extrusion forming, wherein the hot press forming can be adopted when the functional filling materials are more, and the extrusion forming can be adopted when the functional filling materials are less. The hot-press molding process comprises the steps of mold preheating, mold release agent spraying, material paving, hot-press molding, cold-press molding and mold release, and the extrusion molding process comprises the steps of feeding, extruding, cooling molding and fixed-length cutting.
The thickness of the hot-press formed plate is 10 mm-500 mm, and the thickness of the extrusion formed plate is 2 mm-50 mm.
The invention has the following advantages and beneficial effects:
1. the invention adopts ultra-high molecular weight polyethylene and the radiation-resistant composite additive which is compounded by the nanometer rare earth oxide and the organic radiation-resistant composite system, thereby improving the heat resistance and the radiation resistance of the material.
2. According to the invention, more than 500 ten thousand ultrahigh molecular weight polyethylene is selected as an anti-irradiation matrix, and is matched with an anti-irradiation composite additive formed by ball-milling and compounding a nano yttrium oxide and polyolefin anti-aging composite system, so that the mechanical property of the obtained anti-irradiation material is improved, and the Vicat softening point is improved to 131 ℃.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1
A preparation method of a high-use-temperature accident-condition-resistant anti-radiation material comprises the following steps:
step 1, preparation of radiation-resistant composite additive
Weighing a nano yttrium oxide and polyolefin anti-aging composite system according to a mass ratio of 3:100, putting the nano yttrium oxide and polyolefin anti-aging composite system into a ball milling tank, adding 8% of ethanol into the material, adding zirconia grinding balls for ball milling, wherein the mass ratio of the nano yttrium oxide and polyolefin anti-aging composite system to the grinding balls is 1:10, the ball milling speed is 800 r/min, the ball milling time is 12 hours, and screening and discharging to obtain an irradiation-resistant composite additive;
the polyolefin anti-aging composite system is formed by mixing a phenol anti-aging agent and a phosphite ester anti-aging agent according to the mass ratio of 1: 5;
step 2, mixing lead powder and boron carbide powder
Weighing 78 wt% of lead powder and 2 wt% of boron carbide powder according to the proportion, mixing in a conical mixer, and then adding 2 wt% of radiation-resistant composite additive for mixing to obtain a mixed material;
wherein, the addition amounts of the lead powder, the boron carbide powder and the radiation-resistant composite additive are calculated by the final material;
step 3, mixing the mixed material obtained in the step 2 with ultrahigh molecular weight to obtain a final material
And (2) mixing the ultrahigh molecular weight polyethylene with the molecular weight of 500 ten thousand with the material in the step (2), wherein the ultrahigh molecular weight polyethylene accounts for 18 wt% of the final material, and the ultrahigh molecular weight polyethylene is mixed at a low speed and a high speed, wherein the low speed is 650r/min, the low speed is 2-5min, the high speed is 1300r/min, the high speed is 1-2min, and the low speed and the high speed are repeated for 3 times to finally obtain the material to be molded.
And (3) carrying out hot press molding on the materials to prepare an ultrahigh molecular weight radiation-resistant polyethylene plate body, and carrying out performance detection.
The hot press molding method of the ultra-high molecular weight radiation-resistant polyethylene plate comprises the following manufacturing steps:
1) and (3) loading a mold: pouring the material to be molded into a mold;
2) pre-pressing: prepressing on a press at the pressure of 6MPa, and maintaining the pressure for 2 hours;
3) preheating: putting the prepressed die filled with the raw materials into a press, setting the temperature of the press to be 190 ℃, keeping the pressure to be 10MPa, and setting the preheating time to be 10 hours;
4) hot pressing: hot pressing for 15 hours under the conditions of 15MPa and 180 ℃;
5) cold pressing and shaping: transferring the die and the sample into a cold pressing machine, keeping the pressure consistent with the hot pressing, and cold pressing for 5 hours;
6) and demolding to obtain the lead boron polyethylene sheet.
Example 2
The difference between this example and example 1 is that the lead powder content is 40 wt%, the boron carbide powder content is 10 wt%, the ultra-high molecular weight polyethylene content is 47.5 wt%, and the irradiation resistance additive is 2.5 wt%.
Example 3
This example is different from example 1 in that the molecular weight of the ultra-high molecular weight polyethylene is 300 ten thousand.
Example 4
This example differs from example 1 in that the ultra-high molecular weight polyethylene has a molecular weight of 900 ten thousand.
Comparative example 1
This example differs from example 1 in that the ultra-high molecular weight polyethylene has a molecular weight of 150 ten thousand and in that an irradiation resistant additive is added.
Comparative example 2
This example differs from example 1 in that the radiation resistant additive is 0%.
Comparative example 3
This example differs from example 1 in that the radiation resistant additive is only a polyolefin anti-aging composite system and does not contain yttria.
Comparative example 4
This example differs from example 1 in that the radiation resistant additive is only yttria and does not contain a polyolefin anti-aging composite system.
Comparative example 5
This example differs from example 1 in that the polyethylene is a regular polyethylene and does not contain the radiation resistant additive of example 1.
The mechanical properties and vicat softening points of the lead-boron polyethylene sheets obtained in the above examples 1 to 3 and comparative examples 1 to 4 were measured, and the results are shown in table 1:
TABLE 1
From the above detection data, it can be seen that:
(1) from the performance test data of examples 1-4 and comparative example, it can be seen that as the molecular weight increases, the mechanical properties, especially impact properties, of the material are improved, indicating that the toughness of the material is higher.
(2) From the performance test data of example 1 and comparative example 2, it can be seen that the performance of the ultra-high molecular weight lead-boron polyethylene obtained by using only 500 ten thousand of ultra-high molecular weight polyethylene without adding the radiation-resistant additive is obviously reduced after irradiation.
(3) From the performance test data of example 1 and comparative examples 3 and 4, it can be seen that the radiation-resistant additive is poor in performance when only the polypropylene anti-aging composite system is added without yttrium oxide, or when only yttrium oxide is added without polypropylene anti-aging composite system.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. The high-service-temperature accident-condition-resistant anti-radiation material is characterized by comprising ultrahigh molecular weight polyethylene, shielding substance filler and an anti-radiation composite additive, wherein the anti-radiation composite additive is formed by compounding a nano rare earth oxide and an organic anti-radiation composite system; the organic anti-irradiation composite system is a polyolefin anti-aging composite system, and the mass ratio of the nano rare earth oxide to the polyolefin anti-aging composite system is 1-5: 100, the rare earth oxide is yttrium oxide, the organic anti-radiation complex system is formed by compounding a plurality of phenols and phosphite stabilizers, and the mass ratio of the phenols to the phosphite stabilizers is 1: 5-3: 4.
2. The high-use-temperature accident-condition-resistant radiation-resistant material as claimed in claim 1, wherein the addition amount of the radiation-resistant composite additive is 1-2.5% of the total mass.
3. The high-use-temperature accident-resistant working condition radiation-resistant material as claimed in claim 1, which is characterized by comprising the following components in percentage by mass:
ultra-high molecular weight polyethylene: 15-50 percent
Radiation-resistant composite additive: 1 to 2.5 percent;
the rest is shielding material filler.
4. The high-service-temperature accident-resistant radiation-resistant material as claimed in claim 1, wherein the molecular weight of said ultra-high molecular weight polyethylene is 300-900 ten thousand.
5. The high-service-temperature accident-resistant radiation-resistant material as claimed in claim 1, wherein the molecular weight of said ultra-high molecular weight polyethylene is 500-900 ten thousand.
6. A method for preparing the high-use-temperature accident-resistant condition radiation-resistant material according to any one of claims 1 to 5, which comprises the following steps:
step 1: ball-milling the nano rare earth oxide and polyolefin anti-aging composite system to obtain an irradiation-resistant composite additive;
step 2: diluting the radiation-resistant composite additive and adding the diluted radiation-resistant composite additive into a shielding material filler;
and step 3: and mixing to obtain the anti-irradiation material.
7. The preparation method of the high-service-temperature accident-condition-resistant radiation-resistant material as claimed in claim 6, wherein in the step 1, ethanol is added as a dispersing agent during ball milling, the addition amount of the ethanol is 2-10% of the sum of the nano rare earth oxide and the polyolefin anti-aging composite system, and the ratio of the total mass of the nano rare earth oxide and the polyolefin anti-aging composite system to the grinding balls is 1: 8-20.
8. The method for preparing the high-use-temperature accident-condition-resistant radiation-resistant material according to claim 6 or 7, wherein when the shielding material fillers are lead powder and boron carbide powder, the mixing material in the step 3 is mixed in two steps, wherein in the first step, the lead powder and the boron carbide powder are mixed and sprayed with the diluted radiation-resistant composite additive, and in the second step, the ultrahigh molecular weight polyethylene is mixed with the material obtained in the first step.
9. The method for preparing the high-use-temperature accident-resistant radiation-resistant material as claimed in claim 8, wherein the second mixing step is a two-speed mixing step of low speed and high speed, and is repeated for 2-3 times.
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| JPH032695A (en) * | 1989-05-31 | 1991-01-09 | Nisshin Steel Co Ltd | Radiation shielding material with high heat removal efficiency |
| CN102496396B (en) * | 2011-11-16 | 2013-11-06 | 哈尔滨工业大学 | Rare earth/ tungsten/ polyethylene composite gradient nuclear radiation prevention material and production method thereof |
| CN105482225B (en) * | 2015-12-30 | 2019-03-12 | 上海师范大学 | A kind of anti-nuclear radiation rare earth composite material and preparation method thereof |
| CN107910088A (en) * | 2017-10-12 | 2018-04-13 | 上海师范大学 | A kind of rare-earth-based flexible core radiation protection material and its preparation method and application |
| CN109411103A (en) * | 2018-10-24 | 2019-03-01 | 中国船舶重工集团公司第七〇九研究所 | One heavy metal species-rare earth nano composite shielding material and its preparation method and application |
| CN110358177A (en) * | 2019-08-07 | 2019-10-22 | 中国核动力研究设计院 | A kind of Boron-containing-PE stick and its preparation process |
| CN112724487A (en) * | 2020-12-22 | 2021-04-30 | 武汉第二船舶设计研究所(中国船舶重工集团公司第七一九研究所) | High-temperature-resistant modified polyethylene-based shielding material and preparation method thereof |
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