CN115521398A - Organic radiation-proof material and formula and preparation method thereof - Google Patents
Organic radiation-proof material and formula and preparation method thereof Download PDFInfo
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- CN115521398A CN115521398A CN202211316174.XA CN202211316174A CN115521398A CN 115521398 A CN115521398 A CN 115521398A CN 202211316174 A CN202211316174 A CN 202211316174A CN 115521398 A CN115521398 A CN 115521398A
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- 239000000463 material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000009472 formulation Methods 0.000 title claims description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
- 239000002184 metal Substances 0.000 claims abstract description 23
- 150000003839 salts Chemical class 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000178 monomer Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000006184 cosolvent Substances 0.000 claims abstract description 14
- 239000003999 initiator Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 5
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 15
- 230000001681 protective effect Effects 0.000 claims description 15
- 230000005855 radiation Effects 0.000 claims description 15
- OIUWEEPWAUVTRR-UHFFFAOYSA-K 2-methylprop-2-enoate samarium(3+) Chemical compound C(C(=C)C)(=O)[O-].[Sm+3].C(C(=C)C)(=O)[O-].C(C(=C)C)(=O)[O-] OIUWEEPWAUVTRR-UHFFFAOYSA-K 0.000 claims description 12
- 229910052772 Samarium Inorganic materials 0.000 claims description 12
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 9
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 9
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical group COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 9
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 9
- VHSHLMUCYSAUQU-UHFFFAOYSA-N 2-hydroxypropyl methacrylate Chemical compound CC(O)COC(=O)C(C)=C VHSHLMUCYSAUQU-UHFFFAOYSA-N 0.000 claims description 6
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 6
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 6
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 3
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 abstract description 7
- 241001391944 Commicarpus scandens Species 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 4
- 230000005484 gravity Effects 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 125000005395 methacrylic acid group Chemical group 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- 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
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The application relates to an organic radiation-proof material, a formula and a preparation method thereof. The formula comprises the following components in percentage by weight: 49.5-84.5% polymerized monomer; 10-30% of a metal salt; 5-20% of cosolvent; 0.5% of initiator. The preparation method comprises the following steps: weighing the raw materials according to the formula; dissolving metal salt in a polymerization monomer to obtain a mixed solution; adding a cosolvent and an initiator into the mixed solution, heating and stirring, and obtaining a mixture after the metal salt powder is completely dissolved; and injecting the mixture into a mold, and heating and curing to obtain the organic radiation-proof material. The preparation method is simple in preparation process and low in cost, the prepared organic radiation-proof material has excellent optical transparency, small specific gravity, high strength and toughness, is not easy to attenuate and easy to use, and the defect that inorganic glass is easy to break under the action of external force in the using process is overcome.
Description
Technical Field
The application relates to an organic radiation-proof material, in particular to an organic radiation-proof material, a formula and a preparation method thereof.
Background
With the rapid development of industry, the demand of radiation-proof materials, especially transparent radiation-proof materials, in the fields of daily life, medical treatment and health and the like is increasing. The existing radiation-proof material mainly comprises a lead plate and an inorganic lead-containing glass plate, wherein the lead plate has excellent radiation-proof performance, but the application range of the radiation-proof material is narrow due to self bulkiness and opacity, and the inorganic lead-containing glass plate has transparency, but the radiation-proof material has poor mechanical property and high cost due to complex preparation and forming process, so the radiation-proof material is difficult to widely use.
Disclosure of Invention
In order to solve the problems in the prior art, embodiments of the present application provide an organic radiation-proof material, and a formula and a preparation method thereof. The specific technical scheme is as follows:
in a first aspect, a formula of an organic radiation-proof material is provided, which comprises the following components in percentage by weight: 49.5-84.5% of polymerized monomers; 10-30% of a metal salt; 5-20% of cosolvent; 0.5% of initiator.
In a first possible implementation of the first aspect, the polymerized monomer is methyl methacrylate.
In a second possible implementation form of the first aspect, the metal salt is one or more of samarium methacrylate and samarium octoate.
In a third possible implementation form of the first aspect, the co-solvent is one or more of methacrylic acid, octanoic acid, beta-hydroxyethyl methacrylate, beta-hydroxypropyl methacrylate, n-butyl methacrylate, dioctyl phthalate.
In a fourth possible implementation of the first aspect, the initiator is azobisisobutyronitrile.
In a second aspect, a method for preparing an organic radiation-proof material is provided, which comprises the following steps: weighing raw materials according to the formula of the organic radiation-proof material in any one of the first aspect; dissolving metal salt in a polymerization monomer to obtain a mixed solution; adding a cosolvent and an initiator into the mixed solution, heating and stirring, and obtaining a mixed material after the metal salt powder is completely dissolved; and injecting the mixture into a mold, and heating and curing to obtain the organic radiation-proof material.
In a first possible implementation of the second aspect, dissolving the metal salt in the polymerized monomers comprises the steps of: adding metal salt into the polymerization monomer, heating and stirring at 50-60 deg.C for 10-20min.
In a second possible implementation manner of the second aspect, the heating and stirring temperature of the cosolvent, the initiator and the mixed solution is 70-80 ℃, and after the metal salt powder is completely dissolved, the temperature is reduced to 30 ℃.
In a third possible implementation manner of the second aspect, during the heating curing, the mold is placed in an oven, and is cured at 40-50 ℃ for 10-15h,60-70 ℃ for 5-10h,80-90 ℃ for 5-10h and 125-130 ℃ for 3-5h in sequence.
In a third aspect, there is provided an organic radiation protective material prepared according to the method for preparing an organic radiation protective material of any one of the above first aspects.
Compared with the prior art, the application has the advantages that:
the organic radiation-proof material, the formula and the preparation method thereof have the advantages of simple preparation process and low cost, and the prepared organic radiation-proof material has excellent optical transparency, small specific gravity, high strength and toughness, is not easy to attenuate and easy to use, and overcomes the defect that inorganic glass is easy to break under the action of external force in the use process.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a flow chart of the steps of a method for preparing an organic radiation protective material according to an embodiment of the present application.
Detailed Description
For organic radiation-proof materials, mainly inorganic lead-containing glass plates are used, and the organic radiation-proof materials have transparency, but the organic radiation-proof materials have poor mechanical properties, and the cost is high due to the complex preparation and forming process, so that the organic radiation-proof materials are difficult to widely use.
The organic radiation-proof material prepared by the application overcomes the defect that inorganic glass is easy to break under the action of external force in the using process, has good transparency and radiation-proof performance, and is light in specific gravity and excellent in mechanical property.
To make the objects, technical solutions and advantages of the present application more clear, embodiments of the present application will be described in further detail below with reference to the accompanying drawings.
Please refer to fig. 1, which is a flowchart illustrating steps of a method for preparing an organic radiation protective material according to an embodiment of the present application. As shown in the figure, the preparation method S of the organic radiation protective material includes the following steps S1 to S4. First, in step S1, the raw materials are weighed. Weighing the raw materials according to the weight percentage of 49.5-84.5% of polymerized monomer, 10-30% of metal salt, 5-20% of cosolvent and 0.5% of initiator.
In this embodiment, the polymerized monomer is methyl methacrylate, the metal salt is one or more of samarium methacrylate and samarium octoate, the cosolvent is one or more of methacrylic acid, octanoic acid, beta-hydroxyethyl methacrylate, beta-hydroxypropyl methacrylate, n-butyl methacrylate, and dioctyl phthalate, and the initiator is azobisisobutyronitrile.
The metal salt is dissolved in the polymerized monomer in step S2. Adding metal salt into the polymerization monomer, heating and stirring at a constant temperature of 50-60 ℃ for 10-20min, and dissolving the metal salt into the polymerization monomer at the temperature to obtain a mixed solution. Next, in step S3, a co-solvent and an initiator are added. Adding cosolvent and initiator into the mixed solution, stirring at constant temperature and constant speed of 70-80 ℃, observing the reaction process, obtaining a mixture after the metal salt powder is completely dissolved, and cooling the mixture to 30 ℃.
Finally injection molding and curing are performed in step S4. And injecting the mixture into a mold, then placing the mold into an oven, curing for 10-15h at 40-50 ℃, curing for 5-10h at 60-70 ℃, curing for 5-10h at 80-90 ℃ and curing for 3-5h at 125-130 ℃ in sequence, and removing the mold after curing is finished, thus obtaining the organic radiation-proof material.
The beneficial effects of the organic radiation protective material, its formulation and preparation method will be described in the following specific examples 1 to 3.
Example 1
1. Weighing the following components in percentage by weight: 82.5% of methyl methacrylate, 5% of samarium methacrylate and 5% of samarium octoate, 2.5% of beta-hydroxypropyl methacrylate, 2.5% of methacrylic acid and 2% of dioctyl phthalate, 0.5% of azobisisobutyronitrile.
2. Adding the weighed samarium methacrylate and samarium octoate into methyl methacrylate, heating and stirring at the constant temperature of 50 ℃ for 20min to obtain a mixed solution.
3. Adding the weighed methacrylic acid-beta-hydroxypropyl, methacrylic acid, dioctyl phthalate and azodiisobutyronitrile into the mixed solution, stirring at constant temperature and constant speed of 70 ℃, observing the reaction process, and cooling the mixed material to 30 ℃ after the samarium methacrylate and samarium octoate powder are completely dissolved;
4. the mixture was poured into a mold, which was then placed in an oven and cured at 45 ℃ for 10h,60 ℃ for 6h,85 ℃ for 6h, and 125 ℃ for 4h.
5. And removing the mold after curing is finished to obtain the finished product of the organic radiation-proof material.
6. The transmittance of the organic radiation-proof material is 88.35%, the haze is 0.71%, the tensile strength is 73.2MPa, the lead equivalent is 0.1Pbmm, and the bending deformation temperature is 105.3 ℃.
Example 2
1. Weighing the following components in percentage by weight: 67.5% of methyl methacrylate, 10% of samarium methacrylate and 10% of samarium octoate, 5% of beta-hydroxypropyl methacrylate, 5% of methacrylic acid and 2% of dioctyl phthalate, 0.5% of azobisisobutyronitrile.
2. Adding the weighed samarium methacrylate and samarium octoate into methyl methacrylate, heating and stirring at the constant temperature of 50 ℃ for 20min to obtain a mixed solution.
3. Adding the weighed methacrylic acid-beta-hydroxypropyl, methacrylic acid, dioctyl phthalate and azodiisobutyronitrile into the mixed solution, stirring at constant temperature and constant speed of 70 ℃, observing the reaction process, and cooling the mixed material to 30 ℃ after the samarium methacrylate and samarium octoate powder are completely dissolved;
4. the mixture was poured into a mold, which was then placed in an oven and cured at 45 ℃ for 10h,60 ℃ for 6h,85 ℃ for 6h, and 125 ℃ for 4h.
5. And removing the mold after curing is finished to obtain the finished product of the organic radiation-proof material.
6. The transmittance of the tested organic radiation-proof material is 86.12%, the haze is 0.63%, the tensile strength is 68.5MPa, the lead equivalent is 0.4Pbmm, and the bending deformation temperature is 113.8 ℃.
Example 3
1. Weighing the following components in percentage by weight: 52.5 percent of methyl methacrylate, 15 percent of samarium methacrylate and 15 percent of samarium octoate, 7.5 percent of beta-hydroxypropyl methacrylate, 7.5 percent of methacrylic acid and 2 percent of dioctyl phthalate, and 0.5 percent of azobisisobutyronitrile.
2. Adding the weighed samarium methacrylate and samarium octoate into methyl methacrylate, heating and stirring at the constant temperature of 50 ℃ for 20min to obtain a mixed solution.
3. Adding the weighed methacrylic acid-beta-hydroxypropyl, methacrylic acid, dioctyl phthalate and azodiisobutyronitrile into the mixed solution, stirring at constant temperature and constant speed of 70 ℃, observing the reaction process, and cooling the mixed material to 30 ℃ after the samarium methacrylate and samarium octoate powder are completely dissolved;
4. the mixture was poured into a mold, which was then placed in an oven and cured at 45 ℃ for 10h,60 ℃ for 6h,85 ℃ for 6h, and 125 ℃ for 4h.
5. And removing the mold after curing is finished to obtain the finished product of the organic radiation-proof material.
6. The transmittance of the tested organic radiation-proof material is 80.06%, the haze is 0.92%, the tensile strength is 61.8MPa, the lead equivalent is 0.6Pbmm, and the bending deformation temperature is 122.4 ℃.
In summary, the present application provides an organic radiation protective material, a formula thereof and a preparation method thereof. The preparation method is simple in process and low in cost, the prepared organic radiation-proof material has excellent optical transparency, small specific gravity, high strength and toughness, is not easy to attenuate and easy to use, and the defect that inorganic glass is easy to break under the action of external force in the using process is overcome.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a … …" does not exclude the presence of another identical element in a process, method, article, or apparatus that comprises the element.
While the present embodiments have been described with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise embodiments described above, which are meant to be illustrative and not restrictive, and that various changes may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The formula of the organic radiation-proof material is characterized by comprising the following components in percentage by weight:
49.5-84.5% polymerized monomer;
10-30% of a metal salt;
5-20% of cosolvent;
0.5% of initiator.
2. The formulation of organic radiation protective materials of claim 1 wherein said polymeric monomer is methyl methacrylate.
3. The formulation of organic radiation protective materials of claim 1 wherein said metal salt is one or more of samarium methacrylate and samarium octoate.
4. The formulation of organic radiation protective material according to claim 1, wherein the cosolvent is one or more of methacrylic acid, octanoic acid, beta-hydroxyethyl methacrylate, beta-hydroxypropyl methacrylate, n-butyl methacrylate, and dioctyl phthalate.
5. The formulation of organic radiation protective materials of claim 1 wherein said initiator is azobisisobutyronitrile.
6. The preparation method of the organic radiation-proof material is characterized by comprising the following steps:
weighing the raw materials according to the formula of the organic radiation-proof material as claimed in any one of the claims 1 to 5;
dissolving the metal salt in the polymerization monomer to obtain a mixed solution;
adding the cosolvent and the initiator into the mixed solution, heating and stirring, and obtaining a mixture after the metal salt powder is completely dissolved;
and injecting the mixture into a mold, and heating and curing to obtain the organic radiation-proof material.
7. The method for preparing organic radiation protective material according to claim 6, wherein dissolving said metal salt in said polymerized monomer comprises the following steps: adding the metal salt into the polymerization monomer, and heating and stirring at 50-60 ℃ for 10-20min.
8. The method for preparing organic radiation-proof material according to claim 6, wherein the heating and stirring temperature of the cosolvent, the initiator and the mixed solution is 70-80 ℃, and after the metal salt powder is completely dissolved, the temperature is reduced to 30 ℃.
9. The method for preparing organic radiation protective material according to claim 6, wherein in the heating curing, the mold is placed in an oven, and curing is performed at 40-50 ℃ for 10-15h,60-70 ℃ for 5-10h,80-90 ℃ for 5-10h and 125-130 ℃ for 3-5h in sequence.
10. An organic radiation protective material prepared according to the method for preparing an organic radiation protective material according to any one of the preceding claims 6-9.
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| CN202211316174.XA CN115521398A (en) | 2022-10-26 | 2022-10-26 | Organic radiation-proof material and formula and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558426A (en) * | 2011-10-16 | 2012-07-11 | 浙江吉利汽车研究院有限公司 | Leadless radiation-proof organic glass and preparation method thereof |
| US20140316090A1 (en) * | 2011-11-25 | 2014-10-23 | Jx Nippon Oil & Energy Corporation | Method for producing methacrylic resin for optical film |
| CN104262527A (en) * | 2014-10-08 | 2015-01-07 | 天津儒创新材料科技有限公司 | Radiation-resistant liquid organic glass |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558426A (en) * | 2011-10-16 | 2012-07-11 | 浙江吉利汽车研究院有限公司 | Leadless radiation-proof organic glass and preparation method thereof |
| US20140316090A1 (en) * | 2011-11-25 | 2014-10-23 | Jx Nippon Oil & Energy Corporation | Method for producing methacrylic resin for optical film |
| CN104262527A (en) * | 2014-10-08 | 2015-01-07 | 天津儒创新材料科技有限公司 | Radiation-resistant liquid organic glass |
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Application publication date: 20221227 |