CN111349341A - Ray-shielding organic silicon material and preparation method thereof - Google Patents
Ray-shielding organic silicon material and preparation method thereof Download PDFInfo
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
- C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5425—Silicon-containing compounds containing oxygen containing at least one C=C bond
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- C08K5/00—Use of organic ingredients
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- C08K5/544—Silicon-containing compounds containing nitrogen
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- C08K5/00—Use of organic ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
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- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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Abstract
The invention relates to a ray-shielding organic silicon material which comprises the following raw materials in parts by weight: 100 parts of hydroxyl-terminated polydimethylsiloxane, 5-200 parts of reinforcing filler, 300 parts of shielding filler 200-8 parts of cross-linking agent, 0.1-3 parts of catalyst and 0.1-1.5 parts of silane coupling agent. The invention has good ray shielding effect and excellent operation performance.
Description
Technical Field
The invention relates to the technical field of shielding materials, in particular to an organic silicon material for shielding rays and a preparation method thereof.
Background
With the development of the nuclear industry, the scenes of application of nuclear materials are more and more. In many applications, protective materials are indispensable, and the updating of protective materials is also an extremely important research subject. For radiation protection of X, gamma and the like, protective materials used in the early stage generally contain lead, and with the environmental protection requirement, the search for more environment-friendly shielding materials is gradually becoming a consensus.
At present, most of basic polymers applied to shielding materials in the available patent documents are carbon compounds such as epoxy, polyurethane, acrylic acid and the like, and the prepared products have the defects of weather resistance, high and low temperature resistance and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an organosilicon material for shielding rays and a preparation method thereof, and the prepared product has better shielding property.
In order to achieve the purpose, the invention adopts the technical scheme that:
a ray-shielding organic silicon material comprises the following raw materials in parts by weight: 100 parts of hydroxyl-terminated polydimethylsiloxane, 5-200 parts of reinforcing filler, 300 parts of shielding filler 200-8 parts of cross-linking agent, 0.1-3 parts of catalyst and 0.1-1.5 parts of silane coupling agent.
The viscosity of the hydroxyl-terminated polydimethylsiloxane is 1000-80000 CS.
The reinforcing filler is one or more of white carbon black, calcium carbonate, aluminum oxide, aluminum hydroxide and silicon micropowder.
The shielding filler is one or more of lanthanum carbonate, cerium carbonate, cesium carbonate, lanthanum oxide, cerium oxide and cesium oxide.
The cross-linking agent is alkoxy silane.
The alkoxy silane is one or more of methyl trimethoxy silane, vinyl trimethoxy silane, ethyl trimethoxy silane, vinyl triethoxy silane, methyl triethoxy silane, ethyl orthosilicate, methyl tributyrinoxime silane and vinyl tributyrinoxime silane.
The catalyst is a titanate catalyst or an organic tin catalyst.
A method of preparing a radiation-shielding silicone material as described above, comprising the steps of:
(1) mixing hydroxyl-terminated polydimethylsiloxane, reinforcing filler treated by stearic acid and shielding filler, and keeping the mixture for 3 hours at the temperature of 150 ℃ and the vacuum degree of less than-0.98 MPa;
(2) cooling to room temperature, adding a cross-linking agent, and keeping for 30 minutes under the condition that the vacuum degree is less than-0.95 MPa;
(3) adding a silane coupling agent and a catalyst, and keeping for 45 minutes under the condition that the vacuum degree is less than-0.95 MPa to obtain the organosilicon material for shielding rays.
Compared with the prior art, the invention has the following beneficial effects:
the high and low temperature resistance and the weather resistance of the organic silicon polymer are obviously superior to those of carbon-based compounds such as epoxy polyurethane and the like. The prepared product has good construction performance, room temperature curing, simple and convenient process, good ray shielding effect, no lead and more environmental protection.
Detailed Description
The invention discloses a ray-shielding organic silicon material which comprises the following raw materials in parts by weight: 100 parts of hydroxyl-terminated polydimethylsiloxane, 5-200 parts of reinforcing filler, 300 parts of shielding filler 200-8 parts of cross-linking agent, 0.1-3 parts of catalyst and 0.1-1.5 parts of silane coupling agent.
Wherein, the viscosity of the hydroxyl-terminated polydimethylsiloxane (107 glue) is 1000-. The reinforcing filler is one or more of white carbon black, calcium carbonate, alumina, aluminum hydroxide and silicon micropowder. The shielding filler is lanthanum carbonate, cerium carbonate, cesium carbonate, lanthanum oxide, cerium oxide or cesium oxide, and the shielding material is low in cost, belongs to a non-lead substance and is more environment-friendly.
As the silane coupling agent, two or more of KH540 (gamma-aminopropyl trimethoxysilane), KH550 (gamma-aminopropyl triethoxysilane), KH560 (gamma-2, 3-glycidoxy) propyl trimethoxysilane), KH792 (N- (β -aminoethyl) -gamma-aminopropyl trimethoxysilane), KH570 (gamma-methacryloxypropyl trimethoxysilane), KH580 (gamma-methacryloxypropyl trimethoxysilane), IPTS (isocyanatopropyltriethoxysilane) may be used.
Based on the same inventive concept, the invention also discloses a preparation method of the ray-shielding organic silicon material, which comprises the following steps:
(1) mixing hydroxyl-terminated polydimethylsiloxane, reinforcing filler treated by stearic acid and shielding filler, and keeping the mixture for 3 hours at the temperature of 150 ℃ and the vacuum degree of less than-0.98 MPa;
(2) cooling to below 45 ℃, adding a cross-linking agent, and keeping for 30 minutes under the condition that the vacuum degree is less than-0.95 MPa;
(3) adding a silane coupling agent and a catalyst, and keeping for 45 minutes under the condition that the vacuum degree is less than-0.95 MPa to obtain the organosilicon material for shielding rays.
In order to detail the present invention, the following examples are given to illustrate the invention
Example one
In this example, the raw materials and composition of the radiation-shielding silicone material are as follows (parts by weight): 100 parts of 800-viscosity 107 glue, 6 parts of methyltrimethoxysilane, 100 parts of light calcium carbonate, 100 parts of lanthanum carbonate, 100 parts of cesium carbonate, 7.6 parts of titanate chelate and 2.4 parts of silane coupling agent mixture. Wherein the silane coupling agent mixture is prepared by mixing KH550 and KH560 according to the weight ratio of 1: 1, mixing, sealing and standing at room temperature for 5 days; the titanate chelate is a propylene glycol acetoacetate ethyl titanate chelate which is a conventional product in the market.
The preparation process of this example is as follows:
uniformly mixing 107 glue, reinforcing filler and shielding material in a power mixer, and keeping for 3 hours at the temperature of 150 ℃ under the vacuum-0.98 MPa; cooling, adding methyltrimethoxysilane when the temperature is reduced to below 45 ℃, stirring for 30min under vacuum-0.95 MPa, adding the mixture of the titanate chelate and the silane coupling agent, stirring for 30min under vacuum-0.95 MPa, and subpackaging to a sealed tube to finish the preparation.
The preparation methods of the second to sixth examples are the same, except that the raw materials and the weight fractions of the radiation-shielding organosilicon materials are slightly different, and the details are shown in table 1.
TABLE 1
And curing the ray-shielding organosilicon materials obtained in the six embodiments at room temperature for 7 days, and then carrying out product performance test. The test method is as follows:
extrusion Rate test methods: GB-T13477.3-2017 building sealing material test method part 3 method for determining extrusion property of sealing material by using standard apparatus
The hardness test method comprises the following steps: GB/T531.1-2008 vulcanized rubber or thermoplastic rubber press-in hardness test method;
elongation/tensile strength test method: GB/T528-2009 vulcanizates or thermoplastic rubbers;
the ray shielding test method comprises the following steps: reference is made to GB/T16363-1996X-ray protective material shielding performance and a detection method. The test results are shown in table 2:
| item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 6 |
| Extrusion Rate ml/min | 181 | 156 | 230 | 116 | 138 | 267 |
| Hardness, Shore A | 50 | 48 | 35 | 42 | 54 | 32 |
| Elongation percentage of% | 140 | 210 | 260 | 240 | 190 | 360 |
| Tensile strength, Mpa | 1.4 | 1.8 | 1.9 | 2.5 | 2.3 | 1.8 |
| Specific lead equivalent, mmPb, 120kV,2.5mmAl | 0.27 | 0.29 | 0.10 | 0.32 | 0.38 | 0 |
TABLE 2
In Table 2, the larger the value of the specific lead equivalent, the better the shielding property is. As can be seen from table 1 and table 2, the addition of the radiation shielding material can enhance the shielding function of the material against radiation; in the embodiments 1-5, the larger the addition amount of the shielding material is, the better the shielding effect is, and the shielding effect is remarkably improved after the shielding material is added to a certain degree; but the addition amount of the shielding material can influence the workability of the material; by adjusting the ratio of 107 adhesive viscosity to the reinforcing filler in the formula, the organic silicon material with good ray shielding effect and excellent construction performance can be realized.
The above description is only exemplary of the present invention and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above exemplary embodiments according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (8)
1. A radiation-shielding silicone material characterized by: the raw materials comprise the following components in parts by weight: 100 parts of hydroxyl-terminated polydimethylsiloxane, 5-200 parts of reinforcing filler, 300 parts of shielding filler 200-8 parts of cross-linking agent, 0.1-3 parts of catalyst and 0.1-1.5 parts of silane coupling agent.
2. A radiation-shielding silicone material according to claim 1, wherein: the viscosity of the hydroxyl-terminated polydimethylsiloxane is 1000-80000 CS.
3. A radiation-shielding silicone material according to claim 1, wherein: the reinforcing filler is one or more of white carbon black, calcium carbonate, aluminum oxide, aluminum hydroxide and silicon micropowder.
4. A radiation-shielding silicone material according to claim 1, wherein: the shielding filler is one or more of lanthanum carbonate, cerium carbonate, cesium carbonate, lanthanum oxide, cerium oxide and cesium oxide.
5. A radiation-shielding silicone material according to claim 1, wherein: the cross-linking agent is alkoxy silane.
6. A radiation-shielding silicone material according to claim 5, wherein: the alkoxy silane is one or more of methyl trimethoxy silane, vinyl trimethoxy silane, ethyl trimethoxy silane, vinyl triethoxy silane, methyl triethoxy silane, ethyl orthosilicate, methyl tributyrinoxime silane and vinyl tributyrinoxime silane.
7. A radiation-shielding silicone material according to claim 1, wherein: the catalyst is a titanate catalyst or an organic tin catalyst.
8. A method of preparing a radiation shielding silicone material of claim 1, wherein: the method comprises the following steps:
mixing hydroxyl-terminated polydimethylsiloxane, reinforcing filler treated by stearic acid and shielding filler, and keeping the mixture for 3 hours at the temperature of 150 ℃ and the vacuum degree of less than-0.98 MPa;
cooling to room temperature, adding a cross-linking agent, and keeping for 30 minutes under the condition that the vacuum degree is less than-0.95 MPa;
adding a silane coupling agent and a catalyst, and keeping for 45 minutes under the condition that the vacuum degree is less than-0.95 MPa to obtain the organosilicon material for shielding rays.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760172A (en) * | 2008-12-24 | 2010-06-30 | 湖北回天胶业股份有限公司 | Single-component dealcoholization-type organic silicon sealant |
| CN106928726A (en) * | 2017-03-13 | 2017-07-07 | 成都德信安创新医疗技术有限公司 | A kind of rubber composition and preparation method thereof |
| CN109338741A (en) * | 2018-10-16 | 2019-02-15 | 济南平安环保设备有限公司 | Leadless X-ray protection plate and preparation method thereof |
-
2020
- 2020-04-16 CN CN202010300893.7A patent/CN111349341A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760172A (en) * | 2008-12-24 | 2010-06-30 | 湖北回天胶业股份有限公司 | Single-component dealcoholization-type organic silicon sealant |
| CN106928726A (en) * | 2017-03-13 | 2017-07-07 | 成都德信安创新医疗技术有限公司 | A kind of rubber composition and preparation method thereof |
| CN109338741A (en) * | 2018-10-16 | 2019-02-15 | 济南平安环保设备有限公司 | Leadless X-ray protection plate and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 中国材料研究学会: "《中国战略性新兴产业新材料环境工程材料》", 30 November 2018, 中国铁道出版社 * |
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