CN111154151B - Preparation method of radiation-proof rubber - Google Patents
Preparation method of radiation-proof rubber Download PDFInfo
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- CN111154151B CN111154151B CN202010025115.1A CN202010025115A CN111154151B CN 111154151 B CN111154151 B CN 111154151B CN 202010025115 A CN202010025115 A CN 202010025115A CN 111154151 B CN111154151 B CN 111154151B
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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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- 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
- C08K2201/001—Conductive additives
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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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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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
Abstract
A preparation method of radiation-proof rubber belongs to the technical field of rubber material manufacture. The preparation method of the radiation-proof rubber comprises the following steps: uniformly mixing raw rubber, zinc oxide, stearic acid, sulfur, an accelerator, an anti-aging agent, a plasticizer, a lead-plated carbon nanotube and other materials to obtain a rubber compound; and vulcanizing the rubber compound in a vulcanizing machine to obtain the radiation-proof rubber product. The radiation-proof rubber prepared by the invention has X-ray shielding performance and excellent physical and mechanical properties of a high-molecular rubber material, and is wide in application field; the preparation method is simple and can be used for industrial production.
Description
Technical Field
The invention relates to a technology in the field of rubber materials, in particular to a preparation method of radiation-proof rubber.
Background
With the continuous progress of human science and technology, various rays which are contacted by human beings are more and more, and the problems of environmental pollution and damage to the human beings caused by radioactivity are more and more concerned by the society. Lead is a metal capable of effectively blocking X rays, gamma rays and high-intensity rays, and is widely applied to a radiation shielding material of a radiation hot spot. The radiation-proof protective clothing and the radiation-proof sealing material for the human body are mainly lead clothes or lead rubber and the like.
Chinese patent application No. CN201910246027.1 discloses a lead rubber. This lead rubber adopts a large amount of lead powder to fill and makes, when having increased rubber weight, seriously influences the physical properties of rubber, and a large amount of lead powder also has the pollution to the environment, on the other hand if the filling volume of lead powder is not enough not to play the radiation protection effect again.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of radiation-proof rubber, which is characterized in that lead is plated on the surface of a carbon nano tube, and then a three-dimensional network is formed in the rubber through the carbon nano tube, so that the radiation-proof rubber is beneficial to shielding X rays.
The invention comprises the following steps:
1) weighing raw rubber, zinc oxide, stearic acid, sulfur, an accelerator, an anti-aging agent, a plasticizer and lead-plated carbon nanotubes according to the weight ratio for later use;
2) uniformly mixing all the components to obtain a mixed rubber with all the components uniformly dispersed in rubber;
3) and vulcanizing the rubber compound in a vulcanizing machine to obtain the radiation-proof rubber product.
Preferably, the raw rubber is one or more of NR, IR, IIR, BR, SBR, CR, NBR, Q and FPM.
Preferably, the weight ratio of the rubber raw rubber to the lead-plated carbon nano tube is 100 (10-50), and the proportion of the rest materials is the conventional proportion in the prior art.
Preferably, the diameter of the carbon nanotube used for the lead-plated carbon nanotube is 50-200nm, and the length is 5-10 μm.
Preferably, the thickness of the lead plating layer in the lead-plated carbon nanotube is 10nm-5 μm, and the lead plating layer can be simple substance lead and/or lead oxide.
Technical effects
Compared with the prior art, the invention plates lead on the surface of the carbon nano tube, the lead-plated carbon nano tube is used in rubber to prepare radiation-proof rubber, and the lead-plated carbon nano tube forms a three-dimensional conductive shielding network in the rubber, thereby improving the lead equivalent of the radiation-proof rubber;
assuming that the diameter of a single carbon nanotube is 100nm, the length is 10 μm, and the density of the carbon nanotube is 2g/cm3The thickness of the surface lead-plated layer is 20nm, and the density of lead is 11.34g/cm3Then, it is deduced according to the following formula:
VCNT＝πr2L，VPb/CNT＝π(r+d)2L；
ρPb/CNT＝(mCNT+mPb)/VPb/CNT＝(ρPbVPb+ρCVCNT)/VPb/CNT，VPb/CNT＝π(r+d)2L；
i.e. pPb/CNT＝ρPb-r2(ρPb-ρCNT)/(r+d)2＝11.34-2500*(11.34-2)/4900＝6.57g/cm3；
Wherein r is the radius of the carbon nano tube, L is the length of the carbon nano tube, and d is the thickness of the lead plating layer;
the density of the lead-plated carbon nano tube is almost half of that of lead, namely the filling amount of lead is reduced by half, so that the problem of excessive filling amount of lead and other shielding materials is solved, the density of a radiation-proof rubber product is reduced, the strength of the radiation-proof rubber is ensured, and the application field of the radiation-proof rubber is favorably expanded.
Drawings
FIG. 1 is an SEM photograph of a surface-plated lead-containing carbon nanotube according to example 1 of the present invention;
FIG. 2 is an SEM photograph of a carbon nanotube coated with lead oxide according to example 2 of the present invention;
fig. 3 is a schematic diagram of a simulation of the dispersion of lead-plated carbon nanotubes in rubber.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description. It should be understood that these examples are for illustrative purposes and are not intended to limit the scope of the present invention. The conditions used in the examples may be further adjusted according to the conditions of the particular manufacturer, and the conditions not specified are generally the conditions in routine experiments.
Example 1
The preparation process of this example is as follows:
1) preparing the carbon nano tube with the surface plated with lead: a. CNT in weight ratio: mixing the raw materials, performing ultrasonic dispersion on the raw materials, and coating the mixture on the surface of the copper foil, wherein the deionized water is 3: 17; b. putting a section of copper foil coated with the carbon nano tube into a self-made low-temperature vacuum cold-state sputtering instrument, pre-filling a high-purity Pb target in the sputtering instrument, uniformly advancing the copper foil at the speed of 1cm/s, sputtering the copper foil at the power of 14W, taking down the carbon nano tube on the surface of the copper foil after the sputtering is finished to obtain the carbon nano tube with the uniformly plated lead on the surface, wherein m isCNT:mPb＝1:1, and a small amount of lead oxide is allowed to be contained in the lead layer due to the limitation of the preparation process;
2) weighing the materials according to the following formula and then mixing the materials:
100g of natural rubber, 5g of zinc oxide, 1g of stearic acid, 2.5g of sulfur, 1.5g of accelerator DM, 1.5g of accelerator EZ, 0.5g of antioxidant RD, 1.5g of antioxidant A, 5g of paraffin oil, 30g of carbon black and 20g of surface-plated lead carbon nanotubes;
3) mixing uniformly, standing for 2h, vulcanizing at 150 ℃ for 30min to obtain the radiation-proof rubber, wherein the dispersion condition of the lead-plated carbon nano tubes in the rubber is shown in figure 3.
Example 2
The preparation process of this example is as follows:
1) preparing the carbon nano tube with the surface plated with the lead oxide:
a. CNT according to weight ratio: mixing the raw materials, performing ultrasonic dispersion on the raw materials, and coating the mixture on the surface of the copper foil, wherein the ratio of deionized water to deionized water is 10: 7; b. putting the mixture into a rotary furnace, introducing nitrogen at the temperature of 320 ℃ in the rotary furnace at the rate of 200sccm, and reacting for 2 hours to obtain the carbon nano tube with the surface uniformly plated with the lead oxide, wherein m isCNT:mPbO＝1:1.1；
2) Weighing the materials according to the following formula and then mixing the materials:
100g of natural rubber, 5g of zinc oxide, 2g of stearic acid, 2.5g of sulfur, 1.5g of accelerator DM, 1.5g of accelerator EZ, 0.5g of antioxidant RD, 1.5g of antioxidant A, 5g of paraffin oil, 30g of carbon black and 20g of carbon nano tube with the surface plated with lead oxide;
3) mixing uniformly, standing for 2h, and vulcanizing at 150 ℃ for 30min to obtain the radiation-proof rubber.
Analyzing the carbon nanotubes with the surface plated with lead prepared in example 1 and the carbon nanotubes with the surface plated with lead oxide prepared in example 2 by using a scanning electron microscope to obtain SEM photographs, which are respectively shown in fig. 1 and 2; lead is uniformly distributed on the surface of the carbon nano tube to form a layer of film.
The properties of the radiation protective rubbers obtained in examples 1 and 2 are shown in Table 1 below.
TABLE 1 Property Table of radiation-proof rubber
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (4)
1. The preparation method of the radiation-proof rubber is characterized by comprising the following steps:
1) weighing raw rubber, zinc oxide, stearic acid, sulfur, an accelerator, an anti-aging agent, a plasticizer and a lead-plated carbon nano tube according to a weight ratio for later use, wherein the thickness of a lead coating in the lead-plated carbon nano tube is 10nm-5 mu m, and the lead coating in the lead-plated carbon nano tube is elemental lead and/or an oxide of lead;
2) uniformly mixing the components to obtain a mixed rubber with all the components uniformly dispersed in the rubber;
3) and vulcanizing the rubber compound in a vulcanizing machine to obtain the radiation-proof rubber product.
2. The method for preparing the radiation-proof rubber according to claim 1, wherein the raw rubber is one or more of NR, IR, IIR, BR, SBR, CR, NBR and FPM.
3. The preparation method of the radiation-proof rubber according to claim 1, wherein the weight ratio of the raw rubber to the lead-plated carbon nanotube is 100 (10-50).
4. The method for preparing the radiation-proof rubber according to claim 1, wherein the diameter of the carbon nanotube used for the lead-plated carbon nanotube is 50-200nm, and the length is 5-10 μm.
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| CN112048109A (en) * | 2020-08-18 | 2020-12-08 | 赛福纳米科技(徐州)有限公司 | Radiation-proof flexible rubber and preparation process thereof |
| CN113061296B (en) * | 2021-03-16 | 2022-06-17 | 重庆市金盾橡胶制品有限公司 | Carbon nanotube tread rubber and preparation method thereof |
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| CN101440010B (en) * | 2007-11-23 | 2013-01-16 | 深圳大学 | Lead / carbon nano-tube composite powder and preparation thereof |
| CN101642709B (en) * | 2008-08-04 | 2011-07-20 | 深圳大学 | CuO-PbO/carbon nano-tube composite powder and preparation method thereof |
| CN101362389B (en) * | 2008-09-28 | 2012-04-25 | 北京理工大学 | Wide band electromagnetic wave-shielded polyethylene compound film containing nickel-plating carbon nanotube and preparation method thereof |
| US20140225039A1 (en) * | 2013-02-11 | 2014-08-14 | Industrial Technology Research Institute | Radiation shielding composite material including radiation absorbing material and method for preparing the same |
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