CN114634659A - Flexible shielding material and preparation method thereof - Google Patents
Flexible shielding material and preparation method thereof Download PDFInfo
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- CN114634659A CN114634659A CN202210405497.XA CN202210405497A CN114634659A CN 114634659 A CN114634659 A CN 114634659A CN 202210405497 A CN202210405497 A CN 202210405497A CN 114634659 A CN114634659 A CN 114634659A
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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
- C08L7/00—Compositions of natural rubber
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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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0887—Tungsten
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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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a flexible shielding material and a preparation method thereof, wherein the flexible shielding material is prepared from the following raw materials in parts by mass: 100 parts of rubber, 1450-containing materials, 1850 parts of flame retardant, 15-30 parts of flame retardant, 10-25 parts of flame retardant plasticizer, 15-20 parts of filling reinforcing agent, 1-5 parts of functional reinforcing agent, 4-6 parts of zinc oxide, 0.5-2 parts of stearic acid, 0.5-1.5 parts of anti-aging agent and 4.5-8.5 parts of vulcanizing agent. The invention takes two rubbers of natural rubber and chloroprene rubber as flexible material matrixes, shielding fillers are added, and the filling amount of the shielding fillers is more than 90 wt% for higher shielding effect; in order to compensate the reduction of mechanical properties caused by large filling amount of the shielding filler, a certain filling reinforcing agent and a high-efficiency functional reinforcing agent are added, the two reinforcing agents further reinforce the rubber matrix, so that the mechanical properties in the shielding filler high-filling rubber are maintained, and the comprehensive mechanical properties are greatly improved by adding a proper vulcanization system.
Description
Technical Field
The invention relates to a shielding material, in particular to a high-performance flexible shielding material and a preparation method thereof.
Background
With the rapid development of nuclear technology in national defense and civil industries, various high-energy rays (gamma, neutron and the like) are more and more widely applied in the fields of national defense and military, aviation and navigation, industrial exploration, medical health, wireless communication, scientific technology and the like, on one hand, more convenience is provided for human beings, and on the other hand, the health and life safety of the human beings are potentially threatened. Lower radiation dose can cause dizziness, dim eyesight, vomit and the like, and too high radiation dose can cause irreversible damage to tissues and organs of the human body, such as weakened nerve perception, difficult fertility and the like, and can also increase the probability of canceration, distortion and genetic diseases. Therefore, theoretical research and application development of radiation protection materials will become more and more important.
The organic shielding material is a flexible shielding material compounded by heavy metal and organic material, and is mainly used for shielding X rays and gamma rays in the nuclear industry, the national defense industry and the nondestructive testing industry. At present, the flexible shielding material has a single shielding form and a poor shielding effect, a large amount of the flexible shielding material needs to be added to achieve the established shielding effect, and the high loading capacity seriously reduces the mechanical property and the weather resistance of the shielding material, so that the long-term service characteristic of the shielding material is influenced.
In addition, the conventional flexible shielding material is very easy to generate a large amount of heat accumulation in the shielding process, and has a large fire hazard, so that the development of the flexible shielding material with excellent shielding performance and comprehensive performances such as flexibility, flame retardance, fire resistance and mechanical properties is urgently needed.
Disclosure of Invention
Aiming at the problems that the shielding performance and the mechanical performance of the flexible shielding material cannot be simultaneously considered and the flexible shielding material is not fireproof, the invention provides the flexible shielding material and the preparation method thereof, the shielding filler in the flexible shielding material reaches 90 wt%, and the shielding material has various advantages such as excellent shielding performance, mechanical performance, flame retardant performance and the like by adding a flame retardant, a functional assistant and the like.
In order to achieve the above object, one aspect of the present invention provides a flexible shielding material, which is prepared from the following raw materials in parts by mass: 100 parts of rubber, 1450-1850 parts of shielding filler, 15-30 parts of flame retardant, 10-25 parts of flame retardant plasticizer, 15-20 parts of filling reinforcing agent, 1-5 parts of functional reinforcing agent, 4-6 parts of zinc oxide, 0.5-2 parts of stearic acid, 0.5-1.5 parts of anti-aging agent and 4.5-8.5 parts of vulcanizing agent.
Specifically, the rubber comprises the following components in percentage by mass (7-9): the natural rubber and the chloroprene rubber of (1-3).
Specifically, the shielding filler is tungsten powder.
Preferably, the flame retardant is a bromine-antimony system flame retardant, such as decabromodiphenylethane and antimony trioxide, and has a specific and efficient synergistic effect on flame retardance.
Preferably, the flame-retardant plasticizer is one or more of brominated paraffin, bromochlorinated paraffin and chlorinated paraffin.
Specifically, the filling reinforcing agent is one or more of carbon black, white carbon black, titanium dioxide and argil.
Preferably, the functional reinforcing agent is zinc methacrylate, aluminum methacrylate or magnesium methacrylate.
Preferably, the vulcanizing agent comprises the following components in a mass ratio of (2-3): 1 bis-tert-butylperoxyisopropyl benzene and triallyl isocyanurate; or the vulcanizing agent comprises the following components in a mass ratio of (3-4.5): (1.5-2): 1: 1: di-tert-butylperoxyisopropyl benzene, triallyl isocyanurate of (1-2), sulfur, an accelerator and magnesium oxide.
The second aspect of the present invention provides a method for preparing a flexible shielding material, comprising the steps of: adding zinc oxide, stearic acid, an anti-aging agent, a filling reinforcing agent and a flame retardant into rubber in plastication in sequence, uniformly mixing to obtain a rubber compound, adding a shielding material added with a flame-retardant plasticizer into the rubber compound, fully mixing, then adding a functional reinforcing agent and a vulcanizing agent in sequence, uniformly mixing, and finally vulcanizing to obtain the flame-retardant modified rubber;
the rubber is 100 parts, the shielding filler is 1450-1850 parts, the flame retardant is 15-30 parts, the flame-retardant plasticizer is 10-25 parts, the filling reinforcing agent is 15-20 parts, the functional reinforcing agent is 1-5 parts, the zinc oxide is 4-6 parts, the stearic acid is 0.5-2 parts, the anti-aging agent is 0.5-1.5 parts, and the vulcanizing agent is 4.5-8.5 parts.
Specifically, the vulcanization method comprises the following steps: firstly, carrying out forming vulcanization and then carrying out sheet-out vulcanization.
Through the technical scheme, the invention has the following beneficial effects:
1. the invention takes two rubbers of natural rubber and chloroprene rubber as flexible material matrixes, shielding fillers are added, and the filling amount of the shielding fillers is more than 90 wt% for higher shielding effect; in order to compensate the reduction of mechanical properties caused by large filling amount of the shielding filler, a certain filling reinforcing agent and a high-efficiency functional reinforcing agent are added, the two reinforcing agents further reinforce the rubber matrix, so that the mechanical properties in the shielding filler high-filling rubber are maintained, and the comprehensive mechanical properties are greatly improved by adding a proper vulcanization system.
2. In order to ensure efficient flame-retardant effect, a flame retardant is added, and a certain amount of flame-retardant plasticizer is added, so that the flame-retardant performance of the shielding material reaches V-0 level; the flame-retardant plasticizer can play a plasticizing role in materials, so that the shielding filler with high filling amount in the rubber compound is not easy to generate high temperature in open mixing, a rubber matrix is cracked, and the effects of increasing flexibility, reducing hardness and the like are achieved on the vulcanized rubber.
Detailed Description
The following examples are provided to explain the present invention in detail. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
Example 1
Dripping 10 parts of flame-retardant plasticizer brominated paraffin into 1450 parts of tungsten powder; plasticating 90 parts of natural rubber and 10 parts of chloroprene rubber on an open mill, adding a solid auxiliary agent (4 parts of ZnO, 0.5 part of stearic acid and 0.5 part of antioxidant 4010NA) for open milling, and adding 15 parts of carbon black N330 for open milling after uniform open milling; then adding 10 parts of fire retardant decabromodiphenylethane and 5 parts of antimony trioxide for open milling; quickly adding tungsten powder dropwise added with a flame-retardant plasticizer into rubber compound being subjected to open mixing, quickly performing open mixing, adding 1 part of zinc methacrylate, uniformly mixing, finally adding 3 parts of di-tert-butylperoxyisopropyl benzene and 1.5 parts of triallyl isocyanurate, uniformly mixing, packaging in a triangular bag, and discharging; and putting the mixed rubber compound into a mold, vulcanizing on a pressure forming machine, and vulcanizing at 165 ℃ for 15min on a flat vulcanizing machine to obtain the flexible shielding material.
Example 2
25 parts of flame-retardant plasticizer brominated chlorcosane is added into 1850 parts of tungsten powder; plasticating 80 parts of natural rubber and 20 parts of chloroprene rubber on an open mill, adding a solid auxiliary agent (6 parts of ZnO, 2 parts of stearic acid and 1.5 parts of antioxidant 4010NA) for open milling, and adding 20 parts of white carbon black for open milling after the open milling is uniform; then adding 20 parts of fire retardant decabromodiphenylethane and 10 parts of antimony trioxide for open milling; quickly adding tungsten powder dropwise added with a flame-retardant plasticizer into rubber compound being subjected to open mixing, quickly performing open mixing, adding 5 parts of aluminum methacrylate after the open mixing is sufficient, uniformly mixing, finally adding 5 parts of di-tert-butylperoxyisopropyl benzene and 2.5 parts of triallyl isocyanurate, after the open mixing is uniform, packaging in a triangular bag, and discharging; and putting the mixed rubber compound into a mold, vulcanizing on a pressure forming machine, and vulcanizing at 165 ℃ for 15min on a flat vulcanizing machine to obtain the flexible shielding material.
Example 3
Dripping 10 parts of flame-retardant plasticizer bromochloroparaffin and 5 parts of chloroparaffin into 1500 parts of tungsten powder; plasticating 70 parts of natural rubber and 30 parts of chloroprene rubber on an open mill, adding a solid auxiliary agent (5 parts of ZnO, 1 part of stearic acid and 1 part of antioxidant 4010NA) for open milling, and adding 15 parts of carbon black N330 for open milling after the open milling is uniform; then adding 10 parts of fire retardant decabromodiphenylethane and 5 parts of antimony trioxide for open milling; quickly adding tungsten powder dropwise added with a flame-retardant plasticizer into rubber compound being subjected to open mixing, quickly performing open mixing, adding 2 parts of magnesium methacrylate, uniformly mixing, finally adding 3 parts of di-tert-butylperoxyisopropyl benzene, 1.5 parts of triallyl isocyanurate, 1 part of sulfur, 1 part of accelerator DM and 2 parts of MgO, performing triangular bag making, and discharging the sheet; and putting the mixed rubber compound into a mold, vulcanizing on a pressure forming machine, and vulcanizing at 165 ℃ for 15min on a flat vulcanizing machine to obtain the flexible shielding material.
Example 4
Dripping 20 parts of flame-retardant plasticizer brominated paraffin into 1800 parts of tungsten powder; plasticating 70 parts of natural rubber and 30 parts of chloroprene rubber on an open mill, adding a solid auxiliary agent (5 parts of ZnO, 1 part of stearic acid and 1 part of antioxidant 4010NA) for open milling, and adding 15 parts of carbon black N330 for open milling after the open milling is uniform; then adding 10 parts of fire retardant decabromodiphenylethane and 5 parts of antimony trioxide for open milling; quickly adding tungsten powder dropwise added with a flame-retardant plasticizer into rubber compound being subjected to open mixing, quickly performing open mixing, adding 1 part of zinc methacrylate and 1 part of magnesium methacrylate, uniformly mixing, finally adding 4.5 parts of di-tert-butylperoxyisopropyl benzene, 2 parts of triallyl isocyanurate, 1 part of sulfur, 1 part of accelerator DM and 1 part of MgO, performing triangular bag making after uniform open mixing, and discharging sheets; and putting the mixed rubber compound into a mold, vulcanizing on a pressure forming machine, and vulcanizing at 165 ℃ for 15min on a flat vulcanizing machine to obtain the flexible shielding material.
Comparative example 1
Plasticating 70 parts of natural rubber and 30 parts of chloroprene rubber on an open mill, adding a solid auxiliary agent (5 parts of ZnO, 1 part of SA and 1 part of anti-4010 NA) for open milling, and adding 15 parts of carbon black N330 for open milling after uniform open milling; then adding 10 parts of fire retardant decabromodiphenylethane and 5 parts of antimony trioxide for open milling; rapidly adding 1500 parts of tungsten powder into the rubber compound which is being subjected to open mixing, rapidly opening the rubber compound to ensure that 2 parts of zinc methacrylate are added after the rubber compound is fully opened, uniformly mixing, finally adding 3 parts of di-tert-butylperoxyisopropyl benzene serving as a vulcanizing agent and 1.5 parts of triallyl isocyanurate, packaging into triangular bags after the rubber compound is uniformly opened, and discharging sheets; and putting the mixed rubber compound into a mold, vulcanizing on a pressure forming machine, and vulcanizing at 165 ℃ for 15min on a flat vulcanizing machine to obtain the sheet.
Comparative example 2
15 parts of flame-retardant plasticizer brominated paraffin is dripped into 1500 parts of tungsten powder; plasticating 70 parts of natural rubber and 30 parts of chloroprene rubber on an open mill, adding a solid auxiliary agent (5 parts of ZnO, 1 part of SA and 1 part of anti-4010 NA) for open milling, and adding 17 parts of carbon black N330 for open milling after uniform open milling; then adding 10 parts of fire retardant decabromodiphenylethane and 5 parts of antimony trioxide for open milling; quickly adding tungsten powder dropwise added with a flame-retardant plasticizer into mixed rubber which is being subjected to open mixing, quickly performing open mixing to ensure that the mixed rubber is fully subjected to open mixing, finally adding 3 parts of di-tert-butylperoxyisopropyl benzene serving as a vulcanizing agent and 1.5 parts of triallyl isocyanurate, uniformly performing open mixing, packaging in a triangular bag, and discharging; and putting the mixed rubber compound into a mold, vulcanizing on a pressure forming machine, and vulcanizing at 165 ℃ for 15min on a flat vulcanizing machine to obtain the sheet.
Comparative example 3
15 parts of flame-retardant plasticizer brominated paraffin is dripped into 1500 parts of tungsten powder; plasticating 70 parts of natural rubber and 30 parts of chloroprene rubber on an open mill, adding a solid auxiliary agent (5 parts of ZnO, 1 part of SA and 1 part of 4010NA) for open milling, and after uniform open milling, adding 10 parts of flame retardant decabromodiphenylethane and 5 parts of antimony trioxide for open milling; rapidly adding the tungsten powder dropwise added with the brominated paraffin into the rubber compound being subjected to open mixing, rapidly performing open mixing to ensure that 17 parts of zinc methacrylate is added after the open mixing is sufficient, uniformly mixing, finally adding 3 parts of di-tert-butylperoxyisopropyl benzene and 1.5 parts of triallyl isocyanurate serving as vulcanizing agents, performing triangular bag forming after uniform open mixing, and discharging tablets; and putting the mixed rubber compound into a mold, vulcanizing on a pressure forming machine, and vulcanizing at 165 ℃ for 15min on a flat vulcanizing machine to obtain sheets.
The flexible shielding materials prepared in examples 1 to 4 and comparative examples 1 to 3 were measured for shielding performance (linear damping coefficient of Cs 137), mechanical properties (tensile strength, elongation at break and shore hardness), and flame retardancy (flame retardancy rating of vertical burning test) and the results are shown in table 1.
TABLE 1 Flexible Shielding Material Performance test results
As can be seen from table 1, the flexible shielding material prepared in the examples of the present invention has excellent shielding properties, mechanical and mechanical properties, and flame retardancy, while the mechanical properties, especially tensile strength, are greatly reduced in the shielding material prepared without using the flame retardant plasticizer (comparative example 1), the functional reinforcing agent (comparative example 2), and the filler reinforcing agent (comparative example 3).
The preferred embodiments of the present invention have been described in detail with reference to the examples, but the present invention is not limited to the details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that, in the above embodiments, the various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, the present invention does not separately describe various possible combinations.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The flexible shielding material is characterized by being prepared from the following raw materials in parts by mass: 100 parts of rubber, 1450-containing materials, 1850 parts of flame retardant, 15-30 parts of flame retardant, 10-25 parts of flame retardant plasticizer, 15-20 parts of filling reinforcing agent, 1-5 parts of functional reinforcing agent, 4-6 parts of zinc oxide, 0.5-2 parts of stearic acid, 0.5-1.5 parts of anti-aging agent and 4.5-8.5 parts of vulcanizing agent.
2. The flexible shielding material of claim 1, wherein the rubber comprises, by mass, a ratio of (7-9): the natural rubber and the chloroprene rubber of (1-3).
3. The flexible shielding material of claim 1, wherein the shielding filler is tungsten powder.
4. The flexible shielding material of claim 1, wherein the flame retardant is a bromine-antimony system flame retardant.
5. The flexible shielding material of claim 1, wherein the flame retardant plasticizer is one or more of brominated paraffin, bromochlorinated paraffin, and chlorinated paraffin.
6. The flexible shielding material of claim 1, wherein the filling reinforcing agent is one or more of carbon black, white carbon black, titanium dioxide and kaolin.
7. The flexible shielding material of claim 1, wherein the functional strengthening agent is zinc methacrylate, aluminum methacrylate, magnesium methacrylate.
8. The flexible shielding material of claim 1, wherein the vulcanizing agent comprises, in mass ratios of (2-3): 1 bis-tert-butylperoxyisopropyl benzene and triallyl isocyanurate; or
The vulcanizing agent comprises the following components in percentage by mass (3-4.5): (1.5-2): 1: 1: di-tert-butylperoxyisopropyl benzene, triallyl isocyanurate of (1-2), sulfur, an accelerator and magnesium oxide.
9. A preparation method of a flexible shielding material is characterized by comprising the following steps: adding zinc oxide, stearic acid, an anti-aging agent, a filling reinforcing agent and a flame retardant into rubber in plastication in sequence, uniformly mixing to obtain a rubber compound, adding a shielding filler added with a flame-retardant plasticizer into the rubber compound, fully mixing, adding a functional reinforcing agent and a vulcanizing agent in sequence, uniformly mixing, and finally vulcanizing to obtain the flame-retardant modified flame-retardant rubber;
the rubber is 100 parts, the shielding filler is 1450-1850 parts, the flame retardant is 15-30 parts, the flame-retardant plasticizer is 10-25 parts, the filling reinforcing agent is 15-20 parts, the functional reinforcing agent is 1-5 parts, the zinc oxide is 4-6 parts, the stearic acid is 0.5-2 parts, the anti-aging agent is 0.5-1.5 parts, and the vulcanizing agent is 4.5-8.5 parts.
10. The method of making a flexible shielding material of claim 9, wherein the curing process comprises: firstly, carrying out forming vulcanization and then carrying out sheet-out vulcanization.
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CN104194165A (en) * | 2014-08-26 | 2014-12-10 | 安徽蓝德集团股份有限公司 | Low-voltage power cable rubber material |
CN104558703A (en) * | 2014-11-27 | 2015-04-29 | 厦门虹鹭钨钼工业有限公司 | Tungsten-base composite material applied to ray shielding and preparation method thereof |
CN106589490A (en) * | 2016-11-25 | 2017-04-26 | 华南理工大学 | Unsaturated carboxylate reinforced magnetic rubber and preparation method thereof |
CN110746705A (en) * | 2019-11-04 | 2020-02-04 | 山东康迪泰克工程橡胶有限公司 | Flame-retardant ozone-resistant lower cover rubber, preparation method and tubular conveying belt |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102532632A (en) * | 2010-10-19 | 2012-07-04 | 维扬斯科技公司 | Fluid resistant high temperature hose |
CN104194165A (en) * | 2014-08-26 | 2014-12-10 | 安徽蓝德集团股份有限公司 | Low-voltage power cable rubber material |
CN104558703A (en) * | 2014-11-27 | 2015-04-29 | 厦门虹鹭钨钼工业有限公司 | Tungsten-base composite material applied to ray shielding and preparation method thereof |
CN106589490A (en) * | 2016-11-25 | 2017-04-26 | 华南理工大学 | Unsaturated carboxylate reinforced magnetic rubber and preparation method thereof |
CN110746705A (en) * | 2019-11-04 | 2020-02-04 | 山东康迪泰克工程橡胶有限公司 | Flame-retardant ozone-resistant lower cover rubber, preparation method and tubular conveying belt |
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