CN107903347B - Plastic scintillator and initiator-free preparation method thereof - Google Patents
Plastic scintillator and initiator-free preparation method thereof Download PDFInfo
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- CN107903347B CN107903347B CN201711215389.1A CN201711215389A CN107903347B CN 107903347 B CN107903347 B CN 107903347B CN 201711215389 A CN201711215389 A CN 201711215389A CN 107903347 B CN107903347 B CN 107903347B
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- 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
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
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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
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/12—Monomers containing a branched unsaturated aliphatic radical or a ring substituted by an alkyl radical
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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
- C08F120/00—Homopolymers 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
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/12—Esters of monohydric alcohols or phenols
- C08F120/14—Methyl esters, e.g. methyl (meth)acrylate
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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
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- 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
- C08K5/01—Hydrocarbons
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/35—Heterocyclic compounds having nitrogen in the ring having also oxygen in the ring
- C08K5/353—Five-membered rings
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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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The invention discloses a plastic scintillator and a preparation method thereof without an initiator. The components of the plastic scintillator comprise a base material, a first scintillation substance and a wave-shifting agent, the prepared plastic scintillator has large light yield and short fast decay time, and both indexes are superior to those of the plastic scintillator which is doped with the first scintillation substance and the wave-shifting agent with the same concentration and contains an initiator. The initiator-free preparation method of the plastic scintillator does not need to add an initiator in the preparation process, has simple preparation process and high yield, and is suitable for industrial popularization.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a plastic scintillator and a preparation method thereof.
Background
With the development of scientific technology and economic level, the requirements for a detector capable of accurately detecting various particle properties and energies are higher and higher, and various advantages of the plastic scintillator enable the plastic scintillator to be widely used in the scintillation detector. However, as the application field and range of the scintillation detector are continuously expanded, the requirements for the shape, performance and the like of the plastic scintillator are different according to different application purposes and different places.
A commercially available plastic scintillator generally consists of three parts, a base material, a first scintillating substance and a wave-shifting agent, which are dissolved in a plastic matrix monomer and polymerized. To accelerate the polymerization rate, initiators are often added to accelerate the polymerization. However, the addition of the initiator is equivalent to the introduction of impurities, which may degrade the properties of the plastic scintillator, such as luminous intensity, light yield, and the like. Meanwhile, initiators such as Azobisisobutyronitrile (AIBN) and the like can release gas during polymerization, so that a cavity can be formed in a capillary when a matrix monomer is polymerized in the capillary, and a uniform capillary optical fiber with a long length is not easy to prepare. At present, there is a need to develop a plastic scintillator without adding an initiator in the preparation process to meet the requirements of engineering application.
Disclosure of Invention
The invention aims to solve the technical problem of a plastic scintillator, and the invention aims to provide a preparation method of the plastic scintillator without an initiator.
The plastic scintillator of the present invention has a composition including a base material, a first scintillating substance, and a wave-shifting agent;
the matrix material is formed by polymerizing unsaturated matrix monomers containing active groups, wherein the matrix monomers are one or a mixture of two or more of styrene, vinyl toluene or methyl methacrylate;
the first scintillation substance is one or a mixture of two or more of 2, 5-diphenyl oxazole (PPO), p-terphenyl (p-TP), 2- (4 '-tert-butylphenyl) -5- (4' -biphenyl) -1,3, 4-oxadiazole (b-PBD) and 2- (4-biphenyl) -5-phenyl oxadiazole (PBD);
the wave-shifting agent is one or a mixture of two or more of 1, 4-Bis (5-phenyl-2-oxazolyl) benzene (POPOPOP), 1, 4-Bis (2-methylstyrene) benzene (Bis-MSB), 1, 4-Bis (4-methylstyrene) benzene (Me-MSB) and 9, 10-Diphenylanthracene (DPA).
The initiator-free preparation method of the plastic scintillator comprises the following steps:
a. putting an unsaturated matrix monomer containing an active group into a container, and dissolving a first scintillation substance and a wave-shifting agent into the matrix monomer to obtain a uniform solution system;
b. vacuumizing the container, introducing nitrogen, circulating for three times, heating the homogeneous solution system to 70-80 ℃, preserving heat for 48-72 hours, heating to 110-120 ℃ at a speed of 5 ℃/hour, preserving heat for 120 hours, completing primary curing of the homogeneous solution system, and slowly cooling to room temperature to obtain a cured product I; preserving the temperature of the cured product I at 0.09MPa and 60 ℃ for 48 hours to finish secondary curing to obtain a cured product II; and taking the cured product II out of the container, and grinding and polishing to obtain the required plastic scintillator.
And (b) putting the container into an ultrasonic machine for ultrasonic treatment to accelerate the dissolution of the first scintillation substance and the wave-transfer agent in the matrix monomer.
The plastic scintillator has large light yield and short fast decay time, and both indexes are superior to those of the plastic scintillator which is doped with the first scintillating substance and the wave-shifting agent with the same concentration and contains the initiator; the initiator-free preparation method of the plastic scintillator has the advantages of simple process and high yield, and is suitable for industrial popularization.
Detailed Description
The present invention will be described in detail with reference to examples.
The following examples are intended to illustrate the invention, but not to limit it. Various changes, substitutions and alterations can be made herein by those skilled in the relevant art without departing from the spirit and scope of the invention, and it is intended that all such equivalent arrangements fall within the scope of the invention.
In the following examples, different plastic scintillators with different physicochemical properties can be obtained by selecting different first scintillating substances and wave-shifting agents and different concentrations.
Example 1
2, 5-Diphenyloxazole (PPO) and 1, 4-bis (5-phenyl-2-oxazolyl) benzene (POPOPOP) were dissolved in the styrene system in weight percentages of 1% and 0.02%, respectively. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 75 ℃, preserving heat for 60 hours, heating to 115 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MP and 45 ℃. And grinding and polishing to obtain the plastic scintillator material-I.
Plastic scintillator material
The light yield of (a) was 83.49% of the EJ-200 of the standard sample, and the fast decay time was 1.80 ns.
Example 2
P-terphenyl (p-TP) and 1, 4-Bis (2-methylstyrene-based) benzene (Bis-MSB) were dissolved in the styrene system at 2.5% and 0.03%, respectively, by weight. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 75 ℃, preserving heat for 72 hours, heating to 120 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MPa and 45 ℃. And grinding and polishing to obtain the plastic scintillator material-II.
The light yield of the plastic scintillator material-II was 82.45% of the EJ-200 of the standard sample, and the fast decay time was 1.95 ns.
Example 3
2- (4 '-tert-butylphenyl) -5- (4' -biphenyl) -1,3, 4-oxadiazole (b-PBD) and 1, 4-bis (4-methylstyrene) benzene (Me-MSB) were dissolved in the styrene system in percentages by weight of 2% and 0.03%, respectively. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 75 ℃, preserving heat for 60 hours, heating to 115 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MPa and 45 ℃. And grinding and polishing to obtain the plastic scintillator material-III.
The light yield of the plastic scintillator material-III was 81.37% of the EJ-200 of the standard sample, with a fast decay time of 2.01 ns.
Example 4
2- (4-Biphenyl) -5-phenyl oxadiazole (PBD) and 9, 10-Diphenylanthracene (DPA) were dissolved in the styrene system at 2 and 0.02 weight percent, respectively. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 75 ℃, preserving heat for 60 hours, heating to 115 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MPa and 45 ℃. And grinding and polishing to obtain the plastic scintillator material-IV.
The light yield of the plastic scintillator material-IV was 82.34% of the EJ-200 of the standard sample, with a fast decay time of 1.88 ns.
Example 5
2, 5-Diphenyloxazole (PPO) and 1, 4-bis (5-phenyl-2-oxazolyl) benzene (POPOPOP) were dissolved in the vinyltoluene system at 1% and 0.01% by weight, respectively. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 70 ℃, preserving heat for 48 hours, heating to 110 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MPa and 45 ℃. And grinding and polishing to obtain the plastic scintillator material-V.
The light yield of the plastic scintillator material-V was 85.07% of the EJ-200 of the standard sample, with a fast decay time of 1.74 ns.
Example 6
P-terphenyl (p-TP) and 1, 4-Bis (2-methylstyrene) benzene (Bis-MSB) were dissolved in the vinyltoluene system at 1.5% and 0.02% by weight, respectively. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 70 ℃, preserving heat for 48 hours, heating to 110 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MPa and 45 ℃. And grinding and polishing to obtain the plastic scintillator material-VI.
The light yield of the plastic scintillator material-VI was 84.12% of the EJ-200 of the standard sample, and the fast decay time was 1.78 ns.
Example 7
2- (4 '-tert-butylphenyl) -5- (4' -biphenyl) -1,3, 4-oxadiazole (b-PBD) and 1, 4-bis (4-methylstyrene) benzene (Me-MSB) were dissolved in the vinyltoluene system in percentages by weight of 2% and 0.02%, respectively. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 70 ℃, preserving heat for 48 hours, heating to 110 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MPa and 45 ℃. And grinding and polishing to obtain the plastic scintillator material-VII.
The light yield of the plastic scintillator material-VII was 84.76% of the EJ-200 of the standard sample, with a fast decay time of 1.87 ns.
Example 8
2- (4-Biphenyl) -5-phenyl oxadiazole (PBD) and 9, 10-Diphenylanthracene (DPA) were dissolved in the vinyltoluene system at 1.5 and 0.02 weight percent, respectively. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 70 ℃, preserving heat for 48 hours, heating to 110 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MPa and 45 ℃. And grinding and polishing to obtain the plastic scintillator material-VIII.
The light yield of the plastic scintillator material-VIII was 84.85% of the EJ-200 of the standard sample, with a fast decay time of 1.82 ns.
Example 9
2, 5-Diphenyloxazole (PPO) and 1, 4-bis (5-phenyl-2-oxazolyl) benzene (POPOPOP) were dissolved in the methyl methacrylate system in weight percentages of 2% and 0.03%, respectively. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 80 ℃, preserving heat for 72 hours, heating to 120 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MPa and 45 ℃. Grinding and polishing to obtain the plastic scintillator material-IX.
The light yield of the plastic scintillator material-IX was 76.85% of that of EJ-200 of the standard sample, and the fast decay time was 2.12 ns.
Example 10
P-terphenyl (p-TP) and 1, 4-Bis (2-methylstyrene-based) benzene (Bis-MSB) were dissolved in the methyl methacrylate system at 2% and 0.04% by weight, respectively. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 80 ℃, preserving heat for 72 hours, heating to 120 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MPa and 45 ℃. And grinding and polishing to obtain the plastic scintillator material-X.
The light yield of plastic scintillator material-X was 75.18% of the EJ-200 of the standard sample, with a fast decay time of 2.21 ns.
Example 11
2- (4 '-tert-butylphenyl) -5- (4' -biphenyl) -1,3, 4-oxadiazole (b-PBD) and 1, 4-bis (4-methylstyrene) benzene (Me-MSB) were dissolved in the methyl methacrylate system in percentages by weight of 3% and 0.04%, respectively. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 80 ℃, preserving heat for 72 hours, heating to 120 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MPa and 45 ℃. And grinding and polishing to obtain the plastic scintillator material-XI.
The light yield of the plastic scintillator material-XI was 75.78% of the EJ-200 of the standard sample, and the fast decay time was 2.25 ns.
Example 12
2- (4-Biphenyl) -5-phenyl oxadiazole (PBD) and 9, 10-Diphenylanthracene (DPA) were dissolved in the vinyltoluene system at 2 and 0.04 weight percent, respectively. Vacuumizing, introducing nitrogen, circulating for three times, heating the system to 80 ℃, preserving heat for 72 hours, heating to 120 ℃ at the speed of 5 ℃/hour, preserving heat for 120 hours, slowly cooling to room temperature, and finally preserving heat for 48 hours at the temperature of 0.09MPa and 45 ℃. And grinding and polishing to obtain the plastic scintillator material XII.
The light yield of the plastic scintillator material-XII was 75.92% of the EJ-200 of the standard sample, with a fast decay time of 2.33 ns.
The first scintillating substance in the above embodiment may be two or a mixture of two or more of 2, 5-diphenyloxazole (PPO), p-terphenyl (p-TP), 2- (4 '-tert-butylphenyl) -5- (4' -biphenyl) -1,3, 4-oxadiazole (b-PBD), and 2- (4-biphenyl) -5-Phenyloxadiazole (PBD).
The wave-shifting agent in the above embodiment may be two or more of 1, 4-Bis (5-phenyl-2-oxazolyl) benzene (POPOPOP), 1, 4-Bis (2-methylstyrene) benzene (Bis-MSB), 1, 4-Bis (4-methylstyrene) benzene (Me-MSB), 9, 10-Diphenylanthracene (DPA), and mixtures of two or more thereof.
Claims (3)
1. An initiator-free plastic scintillator, characterized in that the components of the plastic scintillator comprise a base material, a first scintillating substance and a wave-shifting agent;
the matrix material is formed by polymerizing unsaturated matrix monomers containing active groups, wherein the matrix monomers are one or a mixture of two or more of styrene, vinyl toluene or methyl methacrylate;
the first scintillation substance is one or a mixture of two or more of 2, 5-diphenyl oxazole, p-terphenyl, 2- (4 '-tert-butylphenyl) -5- (4' -biphenyl) -1,3, 4-oxadiazole and 2- (4-biphenyl) -5-phenyl oxadiazole;
the wave-shifting agent is one or a mixture of two or more of 1, 4-bis (5-phenyl-2-oxazolyl) benzene, 1, 4-bis (2-methyl styryl) benzene, 1, 4-bis (4-methyl styryl) benzene and 9, 10-diphenyl anthracene.
2. An initiator-free preparation method based on the plastic scintillator according to claim 1, wherein the initiator-free preparation method comprises the following steps:
a. putting an unsaturated matrix monomer containing an active group into a container, and dissolving a first scintillation substance and a wave-shifting agent into the matrix monomer to obtain a uniform solution system;
b. vacuumizing the container, introducing nitrogen, circulating for three times, heating the homogeneous solution system to 70-80 ℃, preserving heat for 48-72 hours, heating to 110-120 ℃ at a speed of 5 ℃/hour, preserving heat for 120 hours, finishing primary curing of the homogeneous solution system, and slowly cooling to room temperature to obtain a cured product I; preserving the temperature of the cured product I at 0.09MPa and 60 ℃ for 48 hours to finish secondary curing to obtain a cured product II; and taking the cured product II out of the container, and grinding and polishing to obtain the required plastic scintillator.
3. The initiator-free preparation method of a plastic scintillator according to claim 2, wherein the container is placed in an ultrasonic machine to be subjected to ultrasonic treatment in the step a, so as to accelerate the dissolution of the first scintillating substance and the wave-transfer agent in the matrix monomer.
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| CN113970780A (en) * | 2020-07-23 | 2022-01-25 | 固安县朝阳生物科技有限公司 | Novel plastic scintillator for nuclear detection |
| CN114085430B (en) * | 2020-08-24 | 2022-08-16 | 中国科学院上海硅酸盐研究所 | Organic/inorganic composite scintillator and preparation method thereof |
| CN112239667B (en) * | 2020-10-15 | 2022-11-01 | 湘潭大学 | Red light plastic scintillator and preparation method and application thereof |
| CN112441871B (en) * | 2020-11-05 | 2022-12-09 | 河北科技大学 | Modification method and application of organic photoelectric material |
| CN112745416A (en) * | 2020-12-29 | 2021-05-04 | 苏州昊唐兴核高新材料有限公司 | Plastic scintillator sheet, preparation method and preparation device thereof |
| CN113671555B (en) * | 2021-08-20 | 2023-10-20 | 兰州大学 | Plastic scintillator microsphere, preparation method and application |
| CN114163557B (en) * | 2021-12-24 | 2023-05-09 | 中国工程物理研究院激光聚变研究中心 | Preparation method of organic plastic scintillator |
| CN114672103A (en) * | 2022-03-16 | 2022-06-28 | 中国辐射防护研究院 | Plastic scintillation microsphere and preparation method thereof |
| CN114671969B (en) * | 2022-03-16 | 2024-04-12 | 中国辐射防护研究院 | Polystyrene scintillating particles and preparation method thereof |
| CN114721030B (en) * | 2022-05-05 | 2023-04-18 | 四川大学 | Preparation method of wave-shifting optical fiber |
| CN114891138A (en) * | 2022-06-20 | 2022-08-12 | 中国科学院近代物理研究所 | Pouring method for large-volume plastic flash preparation |
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