CN110951135A - Preparation method of thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material - Google Patents
Preparation method of thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material Download PDFInfo
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- CN110951135A CN110951135A CN201910831338.4A CN201910831338A CN110951135A CN 110951135 A CN110951135 A CN 110951135A CN 201910831338 A CN201910831338 A CN 201910831338A CN 110951135 A CN110951135 A CN 110951135A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
- G21F1/02—Selection of uniform shielding materials
- G21F1/10—Organic substances; Dispersions in organic carriers
- G21F1/103—Dispersions in organic carriers
- G21F1/106—Dispersions in organic carriers metallic dispersions
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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
- 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
- C08K2003/2289—Oxides; Hydroxides of metals of cobalt
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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
- 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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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Abstract
The invention discloses a preparation method of a thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material, which comprises the following operation steps: (1) mixing the eucommia ulmoides gum, the ethylene propylene rubber and the high-density polyethylene to obtain a primary rubber compound; (2) mixing the primary mixed rubber, elemental lead, elemental boron, antimony oxide, cobaltosic oxide, zinc oxide, an accelerator, an anti-aging agent and a vulcanizing agent, then carrying out secondary mixing, vulcanizing by a flat vulcanizing machine, adding into a mold, carrying out heat preservation treatment at the temperature of 215-230 ℃ for 120min, and then carrying out hot pressing at high temperature in time to obtain the nuclear shielding material. The preparation method of the thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material provided by the invention is simple to operate and low in cost, and the prepared lead-boron-polyethylene composite nuclear shielding material still has excellent nuclear shielding performance even if the thickness is thinner.
Description
Technical Field
The invention belongs to the technical field of nuclear shielding material preparation, and particularly relates to a preparation method of a thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material.
Background
Nuclear energy has been more and more paid attention to by people as an environment-friendly and efficient energy source, and is widely applied to the fields of nuclear power, nuclear energy, military industry, aerospace, medical treatment and the like. It is known that when a nuclear reaction occurs, neutrons, gamma rays, and other rays which may damage a human body or an instrument are emitted, and therefore, in order to make the nuclear reaction safer for human service, it is necessary to shield the nuclear reaction. Therefore, with the widespread application of nuclear energy and nuclear technology, the development of nuclear shielding materials has become a necessary trend.
The lead-boron-polyethylene is a material which is earlier in research, more in application and better in shielding performance. Polyethylene has high hydrogen content, hydrogen atoms have good slowing effect on fast neutrons, boron atoms can absorb thermal neutrons, and lead atoms have shielding effect on fast neutrons with certain energy and are particularly effective in shielding gamma rays. However, in the prior art, a thinner nuclear shielding material is needed in some occasions, and when the thickness of the common lead-boron polyethylene is less than 5mm, the shielding performance of the common lead-boron polyethylene to gamma rays is only about 18%, which seriously affects the nuclear shielding performance of the lead-boron polyethylene.
Disclosure of Invention
In order to improve the applicability of the nuclear shielding material and improve the nuclear shielding performance of a thinner nuclear shielding material, the invention provides a preparation method of a thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material.
The invention is realized by the following technical scheme.
A preparation method of a thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material comprises the following operation steps:
(1) mixing the eucommia ulmoides gum, the ethylene propylene rubber and the high-density polyethylene according to the mass ratio of 1:1:15-20 to obtain a primary rubber compound;
(2) according to the weight parts, 180-piece primary rubber compound, 80-120 piece simple substance lead, 3-6 piece simple substance boron, 0.5-0.9 piece antimony oxide, 0.1-0.3 piece cobaltosic oxide, 13-18 piece zinc oxide, 1-4 piece accelerant, 5-9 piece anti-aging agent and 4-8 piece vulcanizing agent are mixed and then mixed for the second-stage mixing, then vulcanized by a flat vulcanizing machine, added into a mold, and subjected to heat preservation treatment for 120min in the environment of 215-piece 230 ℃, and then hot-pressed in time at high temperature to prepare the nuclear shielding material.
Specifically, in the step (1), the number average molecular weight of the gutta percha is 4.1 × 104The polydispersity index is 2.7, the weight average molecular weight of the ethylene propylene rubber is 3000-5000, and the density of the high-density polyethylene is 0.949-0.951g/cm3。
Specifically, in the step (1) and the step (2), a torque rheometer device is adopted for mixing, wherein the mixing temperature in the step (1) is 135-140 ℃, the rotation speed is 60r/min, the mixing time is 15-20min, the two-stage mixing temperature in the step (2) is 138-144 ℃, the rotation speed is 60r/min, and the mixing time is 10-15 min.
Specifically, in the step (2), the average particle sizes of the simple substance lead and the simple substance boron are both 500 nm.
Specifically, in the step (2), the average particle sizes of the antimony oxide and the cobaltosic oxide are both 60-80 nm.
Specifically, in the step (2), the accelerator is zinc di-N-butyldithiocarbamate, the anti-aging agent is N-isopropyl-N-phenyl-p-phenylenediamine, and the vulcanizing agent is sulfur.
According to the technical scheme, the beneficial effects of the invention are as follows:
the preparation method of the thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material provided by the invention is simple to operate and low in cost, and the prepared lead-boron-polyethylene composite nuclear shielding material still has excellent nuclear shielding performance even if the thickness is thinner. In the step (1), after the gutta percha and the ethylene propylene rubber are added into the high-density polyethylene, the mechanical property of the composite nuclear shielding material can be effectively improved, the requirement on the mechanical property of the nuclear shielding material when the thickness is about 2mm is met, and meanwhile, the gutta percha and the ethylene propylene rubber can also effectively improve the uniformity of the hole distribution of the rubber compound at the initial section, so that the elemental lead and the elemental boron can be uniformly distributed in the material, and the nuclear shielding property of the nuclear shielding material is effectively improved; the antimony oxide can effectively improve the dispersity of the elemental boron in the composite material, so that the nuclear shielding material can fully absorb the collision of neutrons, and the nuclear shielding performance of the material is improved; the cobaltosic oxide can effectively improve the absorption performance of the simple substance lead to gamma rays.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
A preparation method of a thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material comprises the following operation steps:
(1) mixing the eucommia ulmoides gum, the ethylene propylene rubber and the high-density polyethylene according to the mass ratio of 1:1:15 to obtain a primary rubber compound, wherein the number average molecular weight of the eucommia ulmoides gum is 4.1 multiplied by 104The polydispersity index is 2.7, the weight average molecular weight of the ethylene propylene rubber is 3000, and the density of the high-density polyethylene is 0.949g/cm3；
(2) Mixing 180 parts of primary rubber compound, 80 parts of elemental lead, 3 parts of elemental boron, 0.5 part of antimony oxide, 0.1 part of cobaltosic oxide, 13 parts of zinc oxide, 1 part of accelerator, 5 parts of antioxidant and 4 parts of vulcanizing agent, then carrying out secondary mixing, vulcanizing by using a flat vulcanizing machine, adding into a mold, carrying out heat preservation treatment in an environment at 215 ℃ for 100min, and carrying out hot pressing in time at high temperature to obtain the nuclear shielding material, wherein the average particle sizes of the elemental lead and the elemental boron are both 500nm, the average particle sizes of the antimony oxide and the cobaltosic oxide are both 60nm, the accelerator is di-N-butyl zinc dithiocarbamate, the antioxidant is N-isopropyl-N-phenyl p-phenylenediamine and the vulcanizing agent is sulfur.
In the step (1) and the step (2), a torque rheometer device is adopted for mixing, wherein the mixing temperature in the step (1) is 135 ℃, the rotating speed is 60r/min, the mixing time is 15min, the two-stage mixing temperature in the step (2) is 138 ℃, the rotating speed is 60r/min, and the mixing time is 10 min.
Example 2
A preparation method of a thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material comprises the following operation steps:
(1) mixing the eucommia ulmoides gum, the ethylene propylene rubber and the high-density polyethylene according to the mass ratio of 1:1:18 to obtain a primary rubber compound, wherein the number average molecular weight of the eucommia ulmoides gum is 4.1 multiplied by 104The polydispersity index is 2.7, the weight average molecular weight of the ethylene propylene rubber is 4000, and the density of the high-density polyethylene is 0.950g/cm3；
(2) According to parts by weight, 200 parts of primary rubber compound, 100 parts of elemental lead, 5 parts of elemental boron, 0.7 part of antimony oxide, 0.2 part of cobaltosic oxide, 15 parts of zinc oxide, 3 parts of accelerator, 7 parts of antioxidant and 6 parts of vulcanizing agent are mixed and then subjected to secondary mixing, then vulcanized by a flat vulcanizing machine, added into a mold, and subjected to heat preservation treatment at 220 ℃ for 110min, and then hot-pressed at high temperature in time to obtain the nuclear shielding material, wherein the average particle sizes of the elemental lead and the elemental boron are both 500nm, the average particle sizes of the antimony oxide and the cobaltosic oxide are both 70nm, the accelerator is zinc di-N-butyldithiocarbamate, the antioxidant is N-isopropyl-N-phenyl-p-phenylenediamine, and the vulcanizing agent is sulfur.
In the step (1) and the step (2), a torque rheometer device is adopted for mixing, wherein the mixing temperature in the step (1) is 138 ℃, the rotating speed is 60r/min, the mixing time is 18min, the two-stage mixing temperature in the step (2) is 140 ℃, the rotating speed is 60r/min, and the mixing time is 13 min.
Example 3
A preparation method of a thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material comprises the following operation steps:
(1) mixing the eucommia ulmoides gum, the ethylene propylene rubber and the high-density polyethylene according to the mass ratio of 1:1:20 to obtain a primary rubber compound, wherein the number average molecular weight of the eucommia ulmoides gum is 4.1 multiplied by 104The polydispersity index is 2.7, the weight average molecular weight of the ethylene propylene rubber is 5000, and the density of the high-density polyethylene is 0.951g/cm3；
(2) According to parts by weight, 220 parts of primary rubber compound, 120 parts of elemental lead, 6 parts of elemental boron, 0.9 part of antimony oxide, 0.3 part of cobaltosic oxide, 18 parts of zinc oxide, 4 parts of accelerator, 9 parts of antioxidant and 8 parts of vulcanizing agent are mixed and then subjected to secondary mixing, then vulcanized by a flat vulcanizing machine, added into a mold, and subjected to heat preservation treatment at 230 ℃ for 120min, and then hot-pressed at high temperature in time to obtain the nuclear shielding material, wherein the average particle sizes of the elemental lead and the elemental boron are both 500nm, the average particle sizes of the antimony oxide and the cobaltosic oxide are both 80nm, the accelerator is zinc di-N-butyldithiocarbamate, the antioxidant is N-isopropyl-N-phenyl-p-phenylenediamine, and the vulcanizing agent is sulfur.
In the step (1) and the step (2), a torque rheometer device is adopted for mixing, wherein the mixing temperature in the step (1) is 140 ℃, the rotating speed is 60r/min, the mixing time is 20min, the two-stage mixing temperature in the step (2) is 144 ℃, the rotating speed is 60r/min, and the mixing time is 15 min.
Comparative example 1
The operation steps in the step (1) are completely the same as those in the example 1 except that no gutta-percha or ethylene propylene rubber is added.
Comparative example 2
The operation of step (2) was the same as that of example 2 except that antimony oxide was not added.
Comparative example 3
The operation of step (3) was carried out in the same manner as in example 3 except that no tricobalt tetroxide was added.
The lead boron polyethylene composite nuclear shielding material with the thickness of 2mm is prepared by the methods of each example and the comparative example respectively, then the absorption performance of the lead boron polyethylene composite nuclear shielding material to neutrons and gamma rays is tested, and the test results are shown in table 1:
TABLE 1 absorption Performance test of Nuclear Shielding materials for neutrons and Gamma rays
| Item | Neutron absorption rate% | Gamma ray absorption rate% | Flexural strength, MPa |
| Example 1 | 98.3 | 33.7 | 15.9 |
| Comparative example 1 | 92.1 | 24.2 | 13.0 |
| Example 2 | 98.7 | 34.1 | 16.4 |
| Comparative example 2 | 93.7 | 31.3 | 15.8 |
| Example 3 | 99.0 | 34.8 | 16.5 |
| Comparative example 3 | 96.4 | 20.1 | 16.1 |
Wherein, during testing neutron shielding performance, the experiment is a pulse nuclear reactor, the neutron energy is 0.042 +/-0.01 eV, and during testing the absorption performance of gamma rays, the experiment gamma ray source is60Co, dose is about 300Gy, and radiation energy is 1.17MeV and 1.33 MeV.
As can be seen from table 1, the thickness of the lead boron polyethylene composite nuclear shielding material prepared by the invention is only 2mm, the applicability of the nuclear shielding material is enhanced, and the nuclear shielding material has excellent nuclear shielding performance, wherein the experimental data of the example 1 and the comparative example 1 show that the gutta percha and the ethylene propylene rubber can effectively improve the uniformity of the hole distribution of the rubber compound at the initial stage, so that the elemental lead and the elemental boron can be uniformly distributed in the material, and the nuclear shielding performance of the nuclear shielding material is effectively improved; the experimental data of the embodiment 2 and the comparative example 2 show that the antimony oxide can effectively improve the dispersity of the elemental boron in the composite material, so that the nuclear shielding material can fully absorb the collision of neutrons, and the nuclear shielding performance of the material is improved; from the experimental data of example 3 and comparative example 3, it can be known that cobaltosic oxide can effectively improve the absorption performance of elemental lead on gamma rays.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art should understand that they can make various changes, modifications, additions and substitutions within the spirit and scope of the present invention.
Claims (6)
1. A preparation method of a thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material is characterized by comprising the following operation steps:
(1) mixing the eucommia ulmoides gum, the ethylene propylene rubber and the high-density polyethylene according to the mass ratio of 1:1:15-20 to obtain a primary rubber compound;
(2) according to the weight parts, 180-piece primary rubber compound, 80-120 piece simple substance lead, 3-6 piece simple substance boron, 0.5-0.9 piece antimony oxide, 0.1-0.3 piece cobaltosic oxide, 13-18 piece zinc oxide, 1-4 piece accelerant, 5-9 piece anti-aging agent and 4-8 piece vulcanizing agent are mixed and then mixed for the second-stage mixing, then vulcanized by a flat vulcanizing machine, added into a mold, and subjected to heat preservation treatment for 120min in the environment of 215-piece 230 ℃, and then hot-pressed in time at high temperature to prepare the nuclear shielding material.
2. The method for preparing the thin-walled high-performance lead-boron-polyethylene composite nuclear shielding material as claimed in claim 1, wherein in the step (1), the number average molecular weight of the gutta percha is 4.1 x 104The polydispersity index is 2.7, the weight average molecular weight of the ethylene propylene rubber is 3000-5000, and the density of the high-density polyethylene is 0.949-0.951g/cm3。
3. The method as claimed in claim 1, wherein the step (1) and the step (2) both use a torque rheometer device for mixing, wherein the mixing temperature in the step (1) is 135-.
4. The method for preparing the thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material as claimed in claim 1, wherein in the step (2), the average particle sizes of elemental lead and elemental boron are both 500 nm.
5. The method for preparing the thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material as claimed in claim 1, wherein in the step (2), the average particle sizes of the antimony oxide and the cobaltosic oxide are both 60-80 nm.
6. The method for preparing the thin-wall high-performance lead-boron-polyethylene composite nuclear shielding material according to claim 1, wherein in the step (2), the accelerator is zinc di-N-butyl dithiocarbamate, the anti-aging agent is N-isopropyl-N-phenyl-p-phenylenediamine, and the vulcanizing agent is sulfur.
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Citations (5)
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| CN102693767A (en) * | 2012-05-21 | 2012-09-26 | 北京富迪创业科技有限公司 | Ultra-thin neutron radiation preventive composite shielding material and preparation method thereof |
| CN103183861A (en) * | 2013-03-21 | 2013-07-03 | 中国船舶重工集团公司第七一九研究所 | Composite shielding material with neutorn-gamma comprehensive shielding effect |
| CN104409124A (en) * | 2014-11-26 | 2015-03-11 | 北京富迪创业科技有限公司 | High-filling composite shielding material for radiation mixing fields and preparation method of high-filling composite shielding material |
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| CN107652509A (en) * | 2017-09-28 | 2018-02-02 | 哈尔滨工业大学 | A kind of lead-boron polythene composite material and preparation method thereof |
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| CN102693767A (en) * | 2012-05-21 | 2012-09-26 | 北京富迪创业科技有限公司 | Ultra-thin neutron radiation preventive composite shielding material and preparation method thereof |
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| CN107033472A (en) * | 2017-05-24 | 2017-08-11 | 北京市射线应用研究中心 | A kind of self-adhering-type gamma-rays rubber composite shielding material and preparation method and application |
| CN107652509A (en) * | 2017-09-28 | 2018-02-02 | 哈尔滨工业大学 | A kind of lead-boron polythene composite material and preparation method thereof |
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