CN115746537A - Nuclear radiation protection material with high temperature resistance and preparation method thereof - Google Patents

Nuclear radiation protection material with high temperature resistance and preparation method thereof Download PDF

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CN115746537A
CN115746537A CN202211511308.3A CN202211511308A CN115746537A CN 115746537 A CN115746537 A CN 115746537A CN 202211511308 A CN202211511308 A CN 202211511308A CN 115746537 A CN115746537 A CN 115746537A
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high temperature
nuclear radiation
temperature resistance
radiation protection
coupling agent
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于海剑
李佳男
史杰
赵同
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Zibo Torch Energy Co ltd
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Abstract

The invention belongs to the technical field of protective materials, and particularly relates to a nuclear radiation protective material with high temperature resistance and a preparation method thereof. The nuclear radiation protection material with high temperature resistance is prepared from the following components in parts by weight: 20-100 parts of modified polyphenylene oxide; 10-50 parts of a reinforcing material; 5-40 parts of boron oxide; 50-300 parts of heavy metal protective particles; 5-10 parts of a coupling agent; 1-10 parts of a processing aid; the reinforcing material is carbon fiber electroplated lead, and the fiber length is 1-15 mm. The invention provides a nuclear radiation protection material with high temperature resistance, which has good high temperature resistance, humidity resistance, corrosion resistance and good comprehensive shielding effect.

Description

Nuclear radiation protection material with high temperature resistance and preparation method thereof
Technical Field
The invention belongs to the technical field of protective materials, and particularly relates to a nuclear radiation protective material with high temperature resistance and a preparation method thereof.
Background
With the continuous progress of the nuclear power technology and the continuous expansion of the radiation application field in China, the radiation safety and protection problems brought by the technology become more and more important. When the traditional radiation protection material is used in a high-temperature and irradiation environment, the problems of irradiation aging and thermal aging are serious. The lead-boron polyethylene is a shielding material which is widely used at present, has high hydrogen content, cannot be activated, but has no high temperature resistance, can be softened when the use temperature reaches more than 100 ℃, has poor radiation resistance effect, and is limited to be used in a plurality of environments. Therefore, the lead-boron polyethylene shielding material can be continuously decomposed along with the increase of service time, molecular chains are broken, the mechanical property is reduced, and the shielding material finally loses strength and cannot be used.
CN109762321B discloses a nuclear radiation-proof composite material, which is prepared from polyphenyl ether, impact-resistant polystyrene, modified lead powder, modified lead fiber, composite filler, coupling agent, antioxidant and lubricant. The number average molecular weight of the polyphenyl ether is 5.5-8.0 ten thousand, the thermal deformation temperature is 190-195 ℃ under 0.45MPa, the composite filler is a mixture of silicon dioxide and paraphenylene terephthalamide fiber, and the modified lead fiber is short fiber treated by a coupling agent; the material is obtained by mixing the raw materials in a mixer and then carrying out parallel double-screw extrusion granulation.
CN112011180A discloses a wave-absorbing radiation-proof plastic, which consists of an inorganic mixed component A and an organic mixed component B, wherein the inorganic mixed component A: iron, silver, nickel, zinc and samarium source ion precursors are mixed with rare earth gadolinium source ion precursors as main components, rare earth cerium source ion precursors as surface film main components, and polyethylene glycol (Mr < 2000) as a dispersing agent; organic mixed component B: the composite material comprises polyphenyl ether, nylon 66, UHMWPE, polyacetamide, carbon fiber, carbon black, a compatilizer, a flexibilizer and an auxiliary agent.
Because of different surface polarities and density differences, the affinity of the metal inorganic compound and the resin matrix is poor, chemical bond connection is difficult to form, incompatible components exist in the interface, the gap of the combined interface between the metal inorganic compound and the matrix material is large, and the probability of the action of rays and protective particles can be reduced, so that the metal inorganic compound is easy to precipitate in the resin matrix under high filling, uniform dispersion is difficult to achieve, and the strength of the material is influenced; direct mixing of carbon fibers and polyphenylene ether resin also has the problem of difficult combination, and the problem of uneven dispersion of the materials is difficult to solve by a single mechanical mixing process.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a nuclear radiation protection material with high temperature resistance, good humidity resistance, good corrosion resistance and good comprehensive shielding effect, and also provides a preparation method thereof.
The nuclear radiation protection material with high temperature resistance is prepared from the following components in parts by weight:
Figure BDA0003969184610000021
the reinforcing material is carbon fiber electroplated lead, and the length of the fiber is 1 mm-15 mm; the treatment method for carbon fiber electroplating lead comprises the following steps: firstly, adopting a mixed solution of acrylic acid and sulfuric acid as a grafting liquid, adding carbon fibers to be modified to ensure that the carbon fibers are completely immersed in the liquid, then slowly adding a potassium permanganate solution, keeping the solution from discoloring before and after the addition, and carrying out a grafting reaction; and taking the reacted carbon fiber out of the solution, repeatedly washing the carbon fiber with deionized water for a plurality of times, putting the carbon fiber into boiling water, boiling and drying. During electrolysis, the carbon fiber is used as a cathode, and lead metal ions in the plating solution are deposited on the surface of the carbon fiber under the action of direct current to form a compact metal plating layer, so that carbon fiber electroplated lead is obtained.
The modified polyphenyl ether is vinyl benzyl ether modified thermosetting polyphenyl ether resin with five-functionality and more than five-functionality, the molecular weight is 1000-4000 g/mol, and the heat distortion temperature is more than 200 ℃. The structural formula is as follows:
Figure BDA0003969184610000022
the heavy metal protection particles are one or more of lead compounds, tungsten powder and a mixture of the tungsten powder and iron powder. The lead compound is one of lead monoxide, lead carbonate and lead nitrate.
The coupling agent is one of phthalate ester coupling agent, aluminum-titanium composite coupling agent and aluminum-zirconium acid ester coupling agent.
The processing aid comprises an end-capping reagent, an antioxidant and an anti-aging agent in a weight ratio of (1-2) to (1-2).
The end capping agent is one of phenyl salicylate, salicylic carbonate and linear polysalicylate.
The anti-aging agent is one of acetyl phenylhydrazine, 2, 6-tertiary butyl-4-methylphenol and docosanol ester.
The antioxidant is one of diphenyl isooctyl phosphite, antioxidant 1010 (tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester) and bis (2, 4-di-tert-butylphenol) pentaerythritol diphosphite.
The preparation method of the nuclear radiation protection material with high temperature resistance comprises the following steps:
(1) Pretreatment: mixing a silane coupling agent with ethanol at room temperature, performing ultrasonic dispersion for 10-20 min, adding heavy metal protective particles, performing ultrasonic dispersion for 40-60 min, evaporating, and drying for 4-5 h to obtain a surface-modified inorganic metal filler A;
(2) Mixing the reinforcing material and boron oxide, adding a coupling agent, mixing and reacting for 5-6 h, and drying at 60-80 ℃ for 4-5 h to obtain a mixture B;
(3) Adding the inorganic metal filler A, the mixture B, the processing aid and the modified polyphenyl ether into a high-speed mixer, mixing for 20-40 min at the temperature of 60-80 ℃, and cooling to room temperature to obtain powder C;
(4) Carrying out hot-press molding on the powder C by adopting a melt compression molding process, cooling to room temperature, and then demolding;
(5) And carrying out secondary curing molding on the demoulded material to obtain the nuclear radiation protection material with high temperature resistance.
The mass ratio of the silane coupling agent to the heavy metal protective particles in the step (1) is (1.
The conditions of the molding process in the step (4) are as follows: the pressure is 10-20 MPa, the temperature is 220-280 ℃, and the molding time is 100-150 min.
The secondary curing molding in the step (5) adopts gradient temperature rise, and the temperature and the molding time are respectively 200 ℃/2h, 220 ℃/2h and 240 ℃/16-24 h.
The silane coupling agent is one of KH560, KH550 and KH 570.
Specifically, the preparation method of the nuclear radiation protection material with the high temperature resistance comprises the following steps:
(1) Firstly, mixing a silane coupling agent and ethanol at room temperature, performing ultrasonic dispersion for 10-20 min, adding heavy metal protective particle powder, performing ultrasonic dispersion for 40-60 min, evaporating excessive solvent, and drying the heavy metal protective particles treated by the coupling agent in an electric heating oven for 4-5 h to obtain a surface-modified inorganic metal filler A;
(2) Mixing the reinforcing material and boron oxide, adding a coupling agent, mixing and reacting for 5-6 h, and drying at 60-80 ℃ for 4-5 h to obtain a mixture B;
(3) Adding the inorganic metal filler A, the mixture B, the processing aid and the polyphenyl ether into a high-speed mixer, mixing for 20-40 min at the temperature of 60-80 ℃, and cooling to room temperature to obtain powder C;
(4) Carrying out hot pressing molding on the powder C for 100-150 min by adopting a melt compression molding process under the conditions of 10-20 MPa and 220-280 ℃, cooling to room temperature, and then demoulding;
(5) And putting the demoulded material into an electric heating oven, and carrying out secondary curing forming by adopting a gradient heating method, wherein the temperature and the forming time are respectively 200 ℃/2h, 220 ℃/2h and 240 ℃/16-24 h.
According to the invention, the polyphenyl ether resin is a vinyl benzyl ether modified thermosetting polyphenyl ether resin with five or more functionality, the mechanical property and the heat resistance of the material are superior to those of a common polyphenyl ether material, the processing difficulty is low, and the material is easy to mold; the reinforcing material is carbon fiber with a metalized surface (carbon fiber is plated with lead), the surface metallization of the carbon fiber can improve the wettability and chemical compatibility of the carbon fiber and a base material, the metalized carbon fiber has excellent performances such as high specific strength, high specific modulus and good toughness, and the shielding material obtained by using the surface metalized carbon fiber as a filler has a good shielding effect. The carbon fiber electroplating is a process for processing the surface of the carbon fiber by using an electrolysis method. Before electroplating, the carbon fiber is subjected to surface treatment to improve the surface activity of the carbon fiber, and the metal deposition is to obtain electrons from an external power supply.
The modified polyphenyl ether is adopted as a raw material, so that the modified polyphenyl ether is high-temperature resistant, and has excellent mechanical property, excellent dielectric property, shielding and irradiation resistance, flame retardance, corrosion resistance, organic solvent resistance and acid and alkali resistance. The nuclear radiation protection material with high temperature resistance prepared by the invention aims at the severe physical and chemical environment with high radioactivity, high humidity and high heat and strong corrosion in the nuclear reactor cabin, and has the advantages of high temperature resistance, radiation resistance, acid and alkali corrosion resistance and the like. In the application aspect, the material is suitable for being used as a nuclear reactor radiation protection layer, and meets the development requirement of novel nuclear reactor secondary shielding on high-temperature resistant radiation protection materials. The nuclear radiation protection material can provide effective radiation protection, and is excellent in heat resistance, flame retardance, mechanical property, temperature resistance and irradiation resistance.
Compared with the prior art, the invention has the beneficial effects that:
(1) The nuclear radiation protection material prepared by the invention has the neutron ray shielding rate of 80-85 percent, has the protection performance of gamma rays, has the gamma ray shielding coefficient of more than 1.9 and the thermal decomposition temperature of more than 380 ℃, and has the thermal aging performance that the discontinuous use temperature reaches more than 205 ℃ and the continuous use temperature reaches more than 120 ℃.
(2) The nuclear radiation protection material prepared by the invention has excellent weather resistance, is stable to ultraviolet light, gamma rays and neutron rays, has basically unchanged intensity and modulus after irradiation, can be used as a structural shielding material, and can be used at high temperature for a long time.
(3) The nuclear radiation protection material prepared by the invention has good processability, can be made into plates or other special-shaped pieces according to requirements, solves the problems of poor neutron ray protection effect, poor heat resistance, poor mechanical property, poor dielectric property, poor corrosion resistance and poor flame retardance of lead-based shielding products, is comprehensively applied to secondary shielding of a nuclear reactor cabin, and can be widely applied to other key engineering fields.
Detailed Description
The present invention is further illustrated by the following examples. The parts by weight in the following examples and comparative examples are by mass. The raw materials and reagents are all obtained from the market.
The carbon fiber electrolytic lead used in the following examples, which is 1mm to 15mm in length, was treated by the following methods: firstly, adopting a mixed solution of acrylic acid and sulfuric acid as a grafting liquid, adding carbon fibers to be modified, ensuring that the carbon fibers are completely immersed in the liquid, then slowly adding a potassium permanganate solution, keeping the solution from discoloring before and after the addition, and carrying out a grafting reaction; and taking the reacted carbon fiber out of the solution, repeatedly washing the carbon fiber with deionized water for a plurality of times, boiling the carbon fiber in boiling water, drying the carbon fiber, taking the carbon fiber as a cathode during electrolysis, and depositing metal ions in the plating solution on the surface of the carbon fiber under the action of direct current to form a compact metal plating layer.
Example 1
The nuclear radiation protection material with the high temperature resistance is prepared from the following components in parts by weight:
Figure BDA0003969184610000041
Figure BDA0003969184610000051
the molecular weight of the modified polyphenylene ether is 1000g/mol, and the heat distortion temperature is 250 ℃.
The preparation method of the nuclear radiation protection material with the high temperature resistance comprises the following steps:
(1) Firstly, mixing a silane coupling agent KH550 with ethanol at room temperature, performing ultrasonic dispersion for 15min, then adding lead monoxide powder, performing ultrasonic dispersion for 50min, evaporating excessive solvent, and drying a metal shielding agent treated by the coupling agent in an electric heating oven at 130 ℃ for 4h to obtain a surface-modified inorganic metal filler A; the mass ratio of the silane coupling agent KH550 to the lead monoxide is (1;
(2) Mixing carbon fiber electroplated lead and boron oxide, adding a phthalate ester coupling agent, mixing and reacting for 5 hours, and drying at 70 ℃ for 4 hours to obtain a mixture B;
(3) Adding the inorganic metal filler A, the mixture B, phenyl salicylate, diphenyl isooctyl phosphite, acetyl phenylhydrazine and modified polyphenyl ether into a high-speed mixer, mixing for 30min at 70 ℃, and cooling to room temperature to obtain powder C;
(4) Hot-pressing the powder C for 120min by adopting a melt compression molding process under the conditions of 15MPa and 250 ℃, cooling to room temperature, and demolding;
(5) And putting the demoulded material into an electric heating oven, carrying out secondary curing molding, and obtaining the nuclear radiation protection material with high temperature resistance by adopting a gradient heating method, wherein the temperature and the molding time are respectively 200 ℃/2h, 220 ℃/2h and 240 ℃/18 h.
Example 2
The nuclear radiation protection material with high temperature resistance is prepared from the following components in parts by weight:
Figure BDA0003969184610000052
the molecular weight of the modified polyphenylene oxide is 4000g/mol, and the heat distortion temperature is 300 ℃.
The preparation method of the nuclear radiation protection material with high temperature resistance comprises the following steps:
(1) Firstly, mixing a silane coupling agent KH560 with ethanol at room temperature, performing ultrasonic dispersion for 10min, then adding a mixture of tungsten powder and iron powder, performing ultrasonic dispersion for 60min, evaporating excessive solvent, and drying a metal shielding agent treated by the coupling agent in an electric heating oven at 120 ℃ for 5h to obtain a surface-modified inorganic metal filler A; the mass ratio of the silane coupling agent KH560 to the mixture of the tungsten powder and the iron powder is (1.5;
(2) Mixing carbon fiber electroplated lead and boron oxide, adding an aluminum zirconium acid ester coupling agent, mixing and reacting for 6 hours, and drying at 60 ℃ for 5 hours to obtain a mixture B;
(3) Adding an inorganic metal filler A, a mixture B, salicylic carbonate, bis (2, 4-di-tert-butylphenol) pentaerythritol diphosphite, 2, 6-tertiary butyl-4-methylphenol and modified polyphenylene oxide into a high-speed mixer, mixing for 40min at 60 ℃, and cooling to room temperature to obtain powder C;
(4) Carrying out hot pressing molding on the powder C for 150min under the conditions of 10MPa and 220 ℃ by adopting a melt compression molding process, cooling to room temperature, and then demolding;
(5) And (3) putting the demoulded material into an electric heating oven, carrying out secondary curing forming, and obtaining the nuclear radiation protection material with high temperature resistance by adopting a gradient heating method, wherein the temperature and the forming time are respectively 200 ℃/2h, 220 ℃/2h and 240 ℃/24 h.
Example 3
The nuclear radiation protection material with high temperature resistance is prepared from the following components in parts by weight:
Figure BDA0003969184610000061
the molecular weight of the modified polyphenylene ether is 2000g/mol, and the heat distortion temperature is 280 ℃.
The preparation method of the nuclear radiation protection material with the high temperature resistance comprises the following steps:
(1) Firstly, mixing a silane coupling agent KH570 with ethanol at room temperature, performing ultrasonic dispersion for 20min, then adding tungsten powder, performing ultrasonic dispersion for 40min, evaporating excessive solvent, and drying a metal shielding agent treated by the coupling agent in an electric heating oven at 140 ℃ for 5h to obtain a surface-modified inorganic metal filler A; the mass ratio of the silane coupling agent KH570 to the tungsten powder is (1.5;
(2) Mixing carbon fiber electroplated lead and boron oxide, adding an aluminum-titanium composite coupling agent, mixing and reacting for 5 hours, and drying at 80 ℃ for 4 hours to obtain a mixture B;
(3) Adding the inorganic metal filler A, the mixture B, the linear polysalicylate, the antioxidant 1010, the docosanol ester and the modified polyphenyl ether into a high-speed mixer, mixing for 20min at 80 ℃, and cooling to room temperature to obtain powder C;
(4) Carrying out hot pressing molding on the powder C for 100min under the conditions of 20MPa and 280 ℃ by adopting a melt compression molding process, cooling to room temperature, and then demolding;
(5) And (3) putting the demoulded material into an electric heating oven, carrying out secondary curing forming, and obtaining the nuclear radiation protection material with high temperature resistance by adopting a gradient heating method, wherein the temperature and the forming time are respectively 200 ℃/2h, 220 ℃/2h and 240 ℃/16 h.
Comparative example 1
An epoxy resin-based protective material is prepared from the following components in parts by weight:
Figure BDA0003969184610000071
a preparation method of an epoxy resin-based shielding material comprises the following steps:
(1) Respectively adding boron nitride and lead powder into 100 parts by weight of multifunctional epoxy resin, heating to 60 ℃, uniformly stirring, and carrying out vacuum defoaming for 1h at 60 ℃, wherein the obtained component is marked as a component A;
(2) Respectively adding the carbon fiber subjected to surface treatment and a diluent into a curing agent, heating to 60 ℃, uniformly stirring, and carrying out vacuum defoamation for 1h at 60 ℃, wherein the obtained component is marked as a component B;
(3) Uniformly mixing the component A and the component B, heating to 60 ℃, uniformly stirring, carrying out vacuum defoamation for 1.0h at 60 ℃, and discharging to obtain a mixture;
(4) Pouring the mixture into a mold preheated to 60 ℃ for curing molding, and cooling and demolding after curing molding to obtain the epoxy resin shielding material;
(5) Wherein, the curing and forming comprises the following specific operations: firstly, the mixture is solidified for 1h at 80 ℃, then is heated to 120 ℃ at the heating rate of 1-10 ℃/min, and is solidified for 2h at 120 ℃.
Comparative example 2
The modified polyphenylene ether was replaced with a conventional polyphenylene ether in the same manner as in example 1 using the same starting materials and by the same preparation method as in example 1.
Comparative example 3
The same raw materials as those in example 1 were used, and carbon fiber plated with lead was replaced with ordinary carbon fiber, and the preparation method was the same as that in example 1.
Comparative example 4
The same raw material as in example 1, except that step (1) of the production method of example 1 was omitted, and the lead monoxide powder was directly mixed with the reinforcing material and boron oxide in step (2).
Performance test
The nuclear radiation protective material with high temperature resistance prepared in the above example and the protective material prepared in the comparative example were tested according to the following standards:
a. irradiation resistance: determination of tensile Properties of plastics according to GB/T1040.1-2006 part 1: the tensile strength of the material after 14 days of heat ageing at 220 ℃ was tested according to the method specified in general guidelines.
b. Heat aging performance: determination of tensile Properties of plastics according to GB/T1040.1-2006 part 1: the method specified in general rules, test run 10 5 Tensile strength of the material after Gy gamma irradiation.
c. Neutron shielding rate (thickness 20 mm): choose to use 252 The Cf neutron source is used for testing, and the average energy of neutrons is 2.13MAnd the eV slowing ball and the He-3 proportional counter form a neutron detector, and the shielding rate of the shielding material to neutrons is calculated according to the neutron count before and after the neutrons pass through the material.
d. Gamma ray shielding absorption rate: choose to use 60 The Co gamma radioactive source, the average energy of which is 1.25MeV, tests the gamma dose, and calculates the absorptivity of the shielding material to the gamma ray according to the dose before and after the gamma ray passes through the material (2 cm thick).
e. Heat distortion temperature: the heat distortion temperature of the material was measured according to the method specified in GB/T1634-2004 "measurement of Plastic deformation temperature under load".
f. Thermal decomposition temperature: and performing DSC test by using a differential thermal analyzer, wherein the temperature range is 25-1000 ℃, the temperature rise rate is 20K/min, the purging atmosphere is nitrogen, and the rate is 20mL/min.
j. The flame retardant property is as follows: the vertical burning behavior of the material (3 mm sample) was determined according to the method specified in GB/T2408-2008 "determination of burning behavior of plastics-horizontal and vertical methods".
The test results are shown in table 1.
TABLE 1 test results
Figure BDA0003969184610000081
Figure BDA0003969184610000091
It can also be seen from table 1 that the flame retardant properties of the materials prepared in examples 1-3 of the present invention can reach UL94V-0 level, which indicates that the shielding materials prepared in the present invention have good flame retardant properties; gamma ray of the materials prepared in examples 1 to 3 of the invention: ( 60 Co) is superior to the material prepared in the comparative example 1 in both shielding rate and neutron shielding rate, and shows that the shielding material prepared by the invention has good gamma ray and neutron shielding performance.
In addition, pass through 10 5 The tensile strength of examples 1-3 after Gy gamma irradiation is much higher than that of comparative example 1This shows that the prepared shielding material has good radiation resistance; after the heat aging test of 220 ℃/14 days, the tensile strength of the examples 1-3 is much higher than that of the comparative example 1, which shows that the shielding material prepared by the invention has good heat resistance.
Of course, the foregoing is merely exemplary of the invention and is not to be construed as limiting the scope of the embodiments of the invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit of the present invention should be included in the scope of the present invention.

Claims (10)

1. A nuclear radiation protection material with high temperature resistance is characterized in that: the composition is prepared from the following components in parts by weight:
Figure FDA0003969184600000011
the reinforcing material is carbon fiber electroplated lead, and the length of the fiber is 1 mm-15 mm;
the modified polyphenyl ether is vinyl benzyl ether modified thermosetting polyphenyl ether resin with five-functionality and more than five-functionality, the molecular weight is 1000-4000 g/mol, and the heat distortion temperature is more than 200 ℃.
2. The nuclear radiation protective material with high temperature resistance according to claim 1, characterized in that: the heavy metal protection particles are one of lead compounds, tungsten powder and a mixture of the tungsten powder and iron powder.
3. The nuclear radiation protection material with high temperature resistance according to claim 1, characterized in that: the coupling agent is one of phthalate ester coupling agent, aluminum-titanium composite coupling agent and aluminum-zirconium acid ester coupling agent.
4. The nuclear radiation protective material with high temperature resistance according to claim 1, characterized in that: the processing aid comprises an end-capping reagent, an antioxidant and an anti-aging agent, and the weight ratio of the end-capping reagent to the anti-aging agent is (1-2) to (1-2).
5. The nuclear radiation protective material with high temperature resistance according to claim 4, characterized in that: the end capping agent is one of phenyl salicylate, salicylic carbonate and linear polysalicylate.
6. The nuclear radiation protection material with high temperature resistance according to claim 4, characterized in that: the anti-aging agent is one of acetyl phenylhydrazine, 2, 6-tertiary butyl-4-methylphenol and docosanol ester.
7. A method for preparing the nuclear radiation protection material with the high temperature resistance performance of any one of claims 1 to 6, wherein the method comprises the following steps: the method comprises the following steps:
(1) Pretreatment: mixing a silane coupling agent and ethanol at room temperature, performing ultrasonic dispersion for 10-20 min, adding heavy metal protective particles, performing ultrasonic dispersion for 40-60 min, evaporating, and drying for 4-5 h to obtain a surface-modified inorganic metal filler A;
(2) Mixing the reinforcing material and boron oxide, adding a coupling agent, mixing and reacting for 5-6 h, and drying at 60-80 ℃ for 4-5 h to obtain a mixture B;
(3) Adding the inorganic metal filler A, the mixture B, the processing aid and the modified polyphenyl ether into a high-speed mixer, mixing for 20-40 min at the temperature of 60-80 ℃, and cooling to room temperature to obtain powder C;
(4) Carrying out hot-press molding on the powder C by adopting a melt compression molding process, cooling to room temperature, and then demolding;
(5) And carrying out secondary curing molding on the demoulded material to obtain the nuclear radiation protection material with high temperature resistance.
8. The method for preparing the nuclear radiation protection material with high temperature resistance according to claim 7, wherein the method comprises the following steps: the mass ratio of the silane coupling agent to the heavy metal protective particles in the step (1) is (1.
9. The method for preparing the nuclear radiation protection material with the high temperature resistance according to claim 7, wherein the method comprises the following steps: the conditions of the molding process in the step (4) are as follows: the pressure is 10-20 MPa, the temperature is 220-280 ℃, and the molding time is 100-150 min.
10. The method for preparing the nuclear radiation protection material with high temperature resistance according to claim 7, wherein the method comprises the following steps: the secondary curing molding in the step (5) adopts gradient temperature rise, and the temperature and the molding time are respectively 200 ℃/2h, 220 ℃/2h and 240 ℃/16-24 h.
CN202211511308.3A 2022-11-29 2022-11-29 Nuclear radiation protection material with high temperature resistance and preparation method thereof Pending CN115746537A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117877994A (en) * 2024-02-02 2024-04-12 深圳市安信达存储技术有限公司 Packaging method of embedded memory chip by adopting high-resistance material reinforcement process

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104928738A (en) * 2015-05-21 2015-09-23 中国科学院山西煤炭化学研究所 Continuous metal electroplating method and device for carbon fiber tows
CN106317787A (en) * 2016-09-13 2017-01-11 北京市射线应用研究中心 High-temperature-resistant epoxy resin-based neutron and gamma-ray shielding composite material and preparation method thereof
CN106609032A (en) * 2015-10-22 2017-05-03 广东生益科技股份有限公司 Polyphenylene ether resin composition and prepreg containing same, laminated board and printed-circuit board
CN109762321A (en) * 2018-12-19 2019-05-17 青岛科凯达橡塑有限公司 A kind of anti-nuclear radiation composite material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104928738A (en) * 2015-05-21 2015-09-23 中国科学院山西煤炭化学研究所 Continuous metal electroplating method and device for carbon fiber tows
CN106609032A (en) * 2015-10-22 2017-05-03 广东生益科技股份有限公司 Polyphenylene ether resin composition and prepreg containing same, laminated board and printed-circuit board
CN106317787A (en) * 2016-09-13 2017-01-11 北京市射线应用研究中心 High-temperature-resistant epoxy resin-based neutron and gamma-ray shielding composite material and preparation method thereof
CN109762321A (en) * 2018-12-19 2019-05-17 青岛科凯达橡塑有限公司 A kind of anti-nuclear radiation composite material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117877994A (en) * 2024-02-02 2024-04-12 深圳市安信达存储技术有限公司 Packaging method of embedded memory chip by adopting high-resistance material reinforcement process

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