CN114163557A - Preparation method of organic plastic scintillator - Google Patents
Preparation method of organic plastic scintillator Download PDFInfo
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- CN114163557A CN114163557A CN202111601683.2A CN202111601683A CN114163557A CN 114163557 A CN114163557 A CN 114163557A CN 202111601683 A CN202111601683 A CN 202111601683A CN 114163557 A CN114163557 A CN 114163557A
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers 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
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
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Abstract
The invention discloses a preparation method of an organic plastic scintillator, which comprises the following steps: mixing 2, 5-diphenyl oxazole, styrene, divinylbenzene, azodiisobutyronitrile and a wave-shifting agent according to a certain proportion, carrying out negative-pressure low-temperature ultrasonic dispersion treatment on the mixed solution, and then carrying out supercritical carbon dioxide mixing treatment; carrying out gradient heating on the treated mixed solution, and cooling to obtain an organic plastic scintillator blank; after the organic plastic scintillator is processed at low temperature, the organic plastic scintillator is mechanically cut and polished. The PPO can be dispersed more uniformly by adopting the negative-pressure low-temperature ultrasonic dispersion treatment and the supercritical carbon dioxide mixing treatment; except that PPO is in a spectral grade, all other reagents in the raw materials are analytically pure and can be directly used without purification treatment, so that the possibility of introducing impurities in a complex operation and purification process is avoided; the prepared organic plastic scintillator has the PPO content as high as 50%, and has no bubble, no brittle fracture and good stability.
Description
Technical Field
The invention belongs to the field of preparation of plastic scintillators, and particularly relates to a preparation method of an organic plastic scintillator.
Background
Scintillators are common photoconversion devices for diagnosing rays or particles generated by nuclear reactions, and play a very important role in high-energy particle research. Different requirements are required for the performance of the scintillator according to different application requirements. Some application fields require that the scintillator has better n-gamma resolution capability, so that the precise diagnosis of neutrons is realized; there is a demand for scintillators having a fast response characteristic to pulsed alpha particles.
In the aspect of neutron diagnosis, no solid scintillator commodity capable of realizing n-gamma spectrum shape resolution is sold at home at present. Rivermol reports a first plastic scintillator capable of realizing n-gamma spectrum shape resolution in 2012, and products and preparation methods cannot be obtained in China. A method for preparing an organic plastic scintillator by taking polyvinyl toluene as a matrix material exists in China, but the content of 2, 5-diphenyl oxazole (PPO) in the plastic scintillator is up to 30%, and the plastic scintillator with higher PPO content is not suitable to be prepared. The higher the PPO content in the plastic scintillator, the more excellent the n-gamma resolution performance. Therefore, in order to further increase the content of PPO in the plastic scintillator, the preparation method and formulation of the patent need to be optimized and upgraded.
Based on the reasons, the organic plastic scintillator with high PPO content, high efficiency, high resolution and quick response is developed and used for detecting and diagnosing high-energy particles and rays in the research fields of ICF, nuclear physics, high-energy physics and the like.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing an organic plastic scintillator, comprising the steps of:
mixing 2, 5-diphenyl oxazole, styrene, divinyl benzene, azodiisobutyronitrile and a wave-shifting agent according to a certain proportion, and performing ultrasonic dispersion treatment on the mixed solution;
step two, performing gradient heating on the treated mixed solution, and cooling to obtain an organic plastic scintillator blank;
and step three, carrying out mechanical cutting and polishing treatment on the organic plastic scintillator blank.
Preferably, in the first step, the mass percentages of the 2, 5-diphenyloxazole, the styrene, the divinylbenzene, the azobisisobutyronitrile and the wave-shifting agent in the mixed liquid are 30-50%, 40-70%, 4-20%, 0.2-0.5% and 0-0.5% in sequence.
Preferably, in the first step, the wave-transfer agent is any one of 9, 10-diphenylanthracene, 1, 4-bis (5-phenyl-2-oxazolyl) benzene, 1, 4-bis (2-methylstyrene) benzene and 1, 4-bis (4-methylstyrene) benzene.
Preferably, in the step one, the ultrasonic dispersion treatment process is as follows: and (3) placing the mixed solution in an ultrasonic cleaning machine with the frequency of 40-60 KHz and the power of 200-300W, suspending for 10-20 min after ultrasonic dispersion is carried out for 30-60 min, and then carrying out ultrasonic dispersion for 30-60 min until the mixed solution becomes a clear transparent solution.
Preferably, in the step one, the ultrasonic dispersion treatment process is as follows: placing the mixed solution under the conditions of 100-800 Pa of pressure and 0-10 ℃ for ultrasonic treatment; wherein the ultrasonic frequency is 30-60 kHz, the ultrasonic treatment is suspended for 3-6 min after 3-6 min, and the ultrasonic dispersion treatment is performed for 1-3 h by taking the ultrasonic treatment as a circulation.
Preferably, in the step one, after the mixed solution is subjected to ultrasonic dispersion treatment, supercritical carbon dioxide mixing treatment is performed, and the process is as follows: placing the mixed solution subjected to the ultrasonic dispersion treatment in a supercritical reaction kettle, introducing carbon dioxide, controlling the temperature in the reaction kettle to be 30-40 ℃, the pressure to be 6-24 MPa, and the magnetic stirring speed to be 1000-1500 rpm, and stirring for 1-3 hours; stopping heating, controlling the pressure relief rate to be 0.1-5 MPa/s when the temperature in the reaction kettle is 20-30 ℃, and discharging carbon dioxide gas to obtain the treated mixed solution.
Preferably, in the second step, the gradient temperature-raising heating process is as follows: heating the temperature from the room temperature to 80-90 ℃ in 1-2 h, preserving the heat for 24-48 h, heating the temperature from 80-90 ℃ to 90-100 ℃ in 1-2 h, preserving the heat for 24-48 h, heating the temperature from 90-100 ℃ to 100-110 ℃ in 1-2 h, and preserving the heat for 24-48 h; and finally, in 1-2 h, raising the temperature from 100-110 ℃ to 110-120 ℃, and preserving the heat for 48-72 h.
Preferably, in the second step, the cooling process is as follows: in 12-24 h, the temperature is reduced from 110-120 ℃ to 20-25 ℃.
Preferably, in the third step, before mechanically cutting the organic plastic scintillator blank, the organic plastic scintillator blank needs to be processed at a low temperature of-10 to 20 ℃ for 12 to 24 hours
The invention at least comprises the following beneficial effects: the preparation method of the organic plastic scintillator is simple to operate and implement, and the whole reaction process does not need vacuum protection, so that bubbles are avoided. The PPO can be dispersed more uniformly by negative pressure low temperature ultrasonic dispersion treatment and supercritical carbon dioxide mixing treatment. Except that PPO is in a spectrum level, all other reagents are analytically pure and can be directly used without purification treatment, so that the possibility of introducing impurities in a complex operation and purification process is avoided. And no organic solvent is used in the preparation process, so that the possible harm of the organic solvent to the environment is avoided. The prepared organic plastic scintillator has the PPO content as high as 50%, and has no bubble, no brittle fracture and good stability. The scintillator can be used for diagnosis and resolution of n-gamma rays.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 is an organic plastic scintillator having a 30% PPO content of 2 inches by 2 inches prepared in example 1 of the present invention;
FIG. 2 is an organic plastic scintillator having a 50% PPO content of 2 inches by 2 inches prepared in example 3 of the present invention;
FIG. 3 is an n-gamma ray resolution spectrum of an organic plastic scintillator with 30% PPO content prepared in example 1 of the present invention;
FIG. 4 is an n-gamma ray resolution spectrum of an organic plastic scintillator with a PPO content of 40% prepared in example 2 of the present invention;
FIG. 5 is an n-gamma ray resolution spectrum of an organic plastic scintillator with a PPO content of 50% prepared in example 3 of the present invention;
FIG. 6 is an n- γ ray resolution spectrum of an organic scintillator 1 having a PPO content of 1% prepared in comparative example 1 of the present invention;
FIG. 7 is an n- γ ray resolution spectrum of an organic scintillator 2 of 20% PPO content prepared in comparative example 2 of the present invention;
FIG. 8 is an n- γ ray-resolved spectrum of an organic scintillator 3 of the present invention prepared in comparative example 3 having a PPO content of 25%;
FIG. 9 is an n-gamma ray resolved spectrum of an inlet liquid scintillator according to comparative example 4 of the present invention.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
< example 1>
The invention relates to a preparation method of an organic plastic scintillator, which comprises the following steps:
step one, mixing 112.5g of 2, 5-diphenyloxazole, 247.5g of styrene, 15g of divinylbenzene, 0.75g of azobisisobutyronitrile and 0.75g of 9, 10-diphenylanthracene, putting the mixed solution in a 40KHz 200W ultrasonic cleaning machine, performing ultrasonic dispersion for 30min, then pausing for 10min, and performing ultrasonic treatment for 30min until the mixed solution becomes a clear transparent solution.
Step two, carrying out gradient heating on the treated mixed solution, wherein the process is as follows: raising the temperature from room temperature to 80 ℃ in 1 hour, and keeping the temperature for 24 hours; then, the temperature is increased from 80 ℃ to 90 ℃ in 1 hour, and the temperature is kept for 24 hours; then, the temperature is increased from 90 ℃ to 100 ℃ in 1 hour, and the temperature is kept for 24 hours; the temperature was then raised from 100 ℃ to 110 ℃ over 1 hour and held for 48 hours. Finally, the temperature was reduced from 110 ℃ to 25 ℃ over 12 hours. And obtaining an organic plastic scintillator blank.
And step three, treating the organic plastic scintillator blank at the low temperature of-10 ℃ for 12h, and then mechanically cutting and polishing the organic plastic scintillator blank to obtain an organic plastic scintillator sample with the PPO content of 30%.
< example 2>
The invention relates to a preparation method of an organic plastic scintillator, which comprises the following steps:
step one, 150g of 2, 5-diphenyl oxazole, 150g of styrene, 75g of divinylbenzene, 0.75g of azodiisobutyronitrile and 0.75g of 9, 10-diphenyl anthracene are mixed, the mixed solution is placed in a 40KHz and 200W ultrasonic cleaning machine, ultrasonic dispersion is carried out for 30min, the mixed solution is suspended for 10min, and ultrasonic treatment is carried out for 30min until the mixed solution becomes a clear transparent solution.
Step two, carrying out gradient heating on the treated mixed solution, wherein the process is as follows: raising the temperature from room temperature to 80 ℃ in 1 hour, and keeping the temperature for 24 hours; then, the temperature is increased from 80 ℃ to 90 ℃ in 1 hour, and the temperature is kept for 24 hours; then, the temperature is increased from 90 ℃ to 100 ℃ in 1 hour, and the temperature is kept for 24 hours; the temperature was then raised from 100 ℃ to 110 ℃ over 1 hour and held for 48 hours. Finally, the temperature was reduced from 110 ℃ to 25 ℃ over 12 hours. And obtaining an organic plastic scintillator blank.
And step three, treating the organic plastic scintillator blank at the low temperature of-10 ℃ for 12h, and then mechanically cutting and polishing the organic plastic scintillator blank to obtain an organic plastic scintillator sample with the PPO content of 40%.
< example 3>
The invention relates to a preparation method of an organic plastic scintillator, which comprises the following steps:
step one, 187.5g of 2, 5-diphenyloxazole, 157.5g of styrene, 30g of divinylbenzene, 0.75g of azobisisobutyronitrile and 0.75g of 9, 10-diphenylanthracene are mixed, the mixed solution is placed in a 40KHz and 200W ultrasonic cleaning machine, ultrasonic dispersion is carried out for 30min, the mixed solution is suspended for 10min, and ultrasonic treatment is carried out for 30min until the mixed solution becomes clear and transparent solution.
Step two, carrying out gradient heating on the treated mixed solution, wherein the process is as follows: raising the temperature from room temperature to 80 ℃ in 1 hour, and keeping the temperature for 24 hours; then, the temperature is increased from 80 ℃ to 90 ℃ in 1 hour, and the temperature is kept for 24 hours; then, the temperature is increased from 90 ℃ to 100 ℃ in 1 hour, and the temperature is kept for 24 hours; the temperature was then raised from 100 ℃ to 110 ℃ over 1 hour and held for 48 hours. Finally, the temperature was reduced from 110 ℃ to 25 ℃ over 12 hours. And obtaining an organic plastic scintillator blank.
And step three, treating the organic plastic scintillator blank at the low temperature of-10 ℃ for 12h, and then mechanically cutting and polishing the organic plastic scintillator blank to obtain an organic plastic scintillator sample with the PPO content of 50%.
< example 4>
The invention relates to a preparation method of an organic plastic scintillator, which comprises the following steps:
mixing 187.5g of 2, 5-diphenyloxazole, 157.5g of styrene, 30g of divinylbenzene, 0.75g of azobisisobutyronitrile and 0.75g of 9, 10-diphenylanthracene, and carrying out ultrasonic treatment on the mixed solution under the conditions of pressure of 100Pa and temperature of 10 ℃; wherein the ultrasonic frequency is 30kHz, the ultrasonic treatment is suspended for 3min after 3min, and the ultrasonic dispersion treatment is carried out for 2h by taking the ultrasonic treatment as a circulation.
Step two, carrying out gradient heating on the treated mixed solution, wherein the process is as follows: raising the temperature from room temperature to 80 ℃ in 1 hour, and keeping the temperature for 24 hours; then, the temperature is increased from 80 ℃ to 90 ℃ in 1 hour, and the temperature is kept for 24 hours; then, the temperature is increased from 90 ℃ to 100 ℃ in 1 hour, and the temperature is kept for 24 hours; the temperature was then raised from 100 ℃ to 110 ℃ over 1 hour and held for 48 hours. Finally, the temperature was reduced from 110 ℃ to 25 ℃ over 12 hours. And obtaining an organic plastic scintillator blank.
And step three, treating the organic plastic scintillator blank at the low temperature of-10 ℃ for 12h, and then mechanically cutting and polishing the organic plastic scintillator blank to obtain an organic plastic scintillator sample with the PPO content of 50%.
In this example, a mixed solution of 2, 5-diphenyloxazole, styrene, divinylbenzene, azobisisobutyronitrile, and 9, 10-diphenylanthracene was subjected to negative pressure low temperature ultrasonic dispersion treatment. Under the low temperature condition, the styrene can be prevented from being overheated under the action of ultrasonic waves, so that the styrene is slowly polymerized and oxidized, and the PPO is dispersed unevenly; under the negative pressure condition, the vacuole that the mixed liquid of ultrasonic vibration produced can spill over the mixed liquid sooner, makes the mixture more even, makes follow-up reaction more thorough. Compared with the embodiment 3, the prepared organic plastic scintillator PPO has better dispersion effect and stronger detection and diagnosis capability on high-energy particles and rays.
< example 5>
The invention relates to a preparation method of an organic plastic scintillator, which comprises the following steps:
mixing 187.5g of 2, 5-diphenyloxazole, 157.5g of styrene, 30g of divinylbenzene, 0.75g of azobisisobutyronitrile and 0.75g of 9, 10-diphenylanthracene, placing the mixed solution in a 40KHz 200W ultrasonic cleaning machine, ultrasonically dispersing for 30min, then pausing for 10min, and further ultrasonically treating for 30min until the mixed solution becomes clear transparent solution; placing the mixed solution subjected to the ultrasonic dispersion treatment in a supercritical reaction kettle, introducing carbon dioxide, controlling the temperature in the reaction kettle to be 32 ℃, the pressure to be 7.2MPa, and the magnetic stirring speed to be 1000rpm, and stirring for 2 hours; stopping heating, controlling the pressure relief rate to be 0.2MPa/s when the temperature in the reaction kettle is 25 ℃, and discharging carbon dioxide gas to obtain the treated mixed solution.
Step two, carrying out gradient heating on the treated mixed solution, wherein the process is as follows: raising the temperature from room temperature to 80 ℃ in 1 hour, and keeping the temperature for 24 hours; then, the temperature is increased from 80 ℃ to 90 ℃ in 1 hour, and the temperature is kept for 24 hours; then, the temperature is increased from 90 ℃ to 100 ℃ in 1 hour, and the temperature is kept for 24 hours; the temperature was then raised from 100 ℃ to 110 ℃ over 1 hour and held for 48 hours. Finally, the temperature was reduced from 110 ℃ to 25 ℃ over 12 hours. And obtaining an organic plastic scintillator blank.
And step three, treating the organic plastic scintillator blank at the low temperature of-10 ℃ for 12h, and then mechanically cutting and polishing the organic plastic scintillator blank to obtain an organic plastic scintillator sample with the PPO content of 50%.
In this example, a mixed solution of 2, 5-diphenyloxazole, styrene, divinylbenzene, azobisisobutyronitrile, and 9, 10-diphenylanthracene is subjected to ultrasonic dispersion treatment, and then subjected to supercritical carbon dioxide mixing treatment. In this treatment method, carbon dioxide is in a supercritical state between a gas and a liquid at a specific pressure and temperature, and is a solvent having a very strong dissolving power. The mixed solution is magnetically stirred at high speed in the system, so that PPO can be dispersed more uniformly. The carbon dioxide is inactive and has strong inertia, and the temperature in the reaction kettle is low, thus having no influence on the raw materials in the mixed liquid. Compared with the embodiment 3, the prepared organic plastic scintillator PPO has better dispersion effect and stronger detection and diagnosis capability on high-energy particles and rays.
< example 6>
The invention relates to a preparation method of an organic plastic scintillator, which comprises the following steps:
mixing 187.5g of 2, 5-diphenyloxazole, 157.5g of styrene, 30g of divinylbenzene, 0.75g of azobisisobutyronitrile and 0.75g of 9, 10-diphenylanthracene, and carrying out ultrasonic treatment on the mixed solution under the conditions of pressure of 100Pa and temperature of 10 ℃; wherein the ultrasonic frequency is 30kHz, the ultrasonic treatment is suspended for 3min after 3min, and the ultrasonic dispersion treatment is carried out for 2h by taking the ultrasonic treatment as a circulation; placing the mixed solution subjected to the ultrasonic dispersion treatment in a supercritical reaction kettle, introducing carbon dioxide, controlling the temperature in the reaction kettle to be 32 ℃, the pressure to be 7.2MPa, and the magnetic stirring speed to be 1000rpm, and stirring for 2 hours; stopping heating, controlling the pressure relief rate to be 0.2MPa/s when the temperature in the reaction kettle is 25 ℃, and discharging carbon dioxide gas to obtain the treated mixed solution.
Step two, carrying out gradient heating on the treated mixed solution, wherein the process is as follows: raising the temperature from room temperature to 80 ℃ in 1 hour, and keeping the temperature for 24 hours; then, the temperature is increased from 80 ℃ to 90 ℃ in 1 hour, and the temperature is kept for 24 hours; then, the temperature is increased from 90 ℃ to 100 ℃ in 1 hour, and the temperature is kept for 24 hours; the temperature was then raised from 100 ℃ to 110 ℃ over 1 hour and held for 48 hours. Finally, the temperature was reduced from 110 ℃ to 25 ℃ over 12 hours. And obtaining an organic plastic scintillator blank.
And step three, treating the organic plastic scintillator blank at the low temperature of-10 ℃ for 12h, and then mechanically cutting and polishing the organic plastic scintillator blank to obtain an organic plastic scintillator sample with the PPO content of 50%.
In this embodiment, a mixed solution of 2, 5-diphenyloxazole, styrene, divinylbenzene, azobisisobutyronitrile, and 9, 10-diphenylanthracene is subjected to negative pressure low temperature ultrasonic dispersion treatment, and then subjected to supercritical carbon dioxide mixing treatment. In the process of negative pressure low temperature ultrasonic dispersion treatment, under the low temperature condition, the styrene can be prevented from overheating due to the action of ultrasonic waves, so that the styrene is slowly polymerized and oxidized, and the 2, 5-diphenyl oxazole (PPO) is not uniformly dispersed; under the negative pressure condition, the vacuole that the mixed liquid produced of ultrasonic vibration can spill over the mixed liquid sooner, lets mix more evenly. In the magnetic stirring treatment process of the supercritical carbon dioxide, the carbon dioxide is in a supercritical state between gas and liquid at a specific pressure and temperature and is a solvent with extremely strong dissolving capacity; the mixed solution is magnetically stirred at high speed in the system, so that PPO can be dispersed more uniformly. The carbon dioxide is inactive and has strong inertia, and the temperature in the reaction kettle is low, thus having no influence on the raw materials in the mixed liquid. Compared with the embodiment 3, the prepared organic plastic scintillator PPO has better dispersion effect and stronger detection and diagnosis capability on high-energy particles and rays.
< comparative example 1>
Step one, mixing 2.7g of 2, 5-diphenyloxazole, 247.5g of styrene, 15g of divinylbenzene, 0.75g of azobisisobutyronitrile and 0.75g of 9, 10-diphenylanthracene, putting the mixed solution in a 40KHz 200W ultrasonic cleaning machine, ultrasonically dispersing for 30min, then pausing for 10min, and then ultrasonically treating for 30min until the mixed solution becomes a clear transparent solution.
Step two, carrying out gradient heating on the treated mixed solution, wherein the process is as follows: raising the temperature from room temperature to 80 ℃ in 1 hour, and keeping the temperature for 24 hours; then, the temperature is increased from 80 ℃ to 90 ℃ in 1 hour, and the temperature is kept for 24 hours; then, the temperature is increased from 90 ℃ to 100 ℃ in 1 hour, and the temperature is kept for 24 hours; the temperature was then raised from 100 ℃ to 110 ℃ over 1 hour and held for 48 hours. Finally, the temperature was reduced from 110 ℃ to 25 ℃ over 12 hours. And obtaining an organic plastic scintillator blank.
And step three, treating the organic plastic scintillator blank at the low temperature of-10 ℃ for 12h, and then mechanically cutting and polishing the organic plastic scintillator blank to obtain an organic scintillator 1 sample with the PPO content of 1%.
< comparative example 2>
Step one, 66g of 2, 5-diphenyloxazole, 247.5g of styrene, 15g of divinylbenzene, 0.75g of azobisisobutyronitrile and 0.75g of 9, 10-diphenylanthracene are mixed, the mixed solution is placed in a 40KHz and 200W ultrasonic cleaning machine, ultrasonic dispersion is carried out for 30min, then the mixture is suspended for 10min, and ultrasonic treatment is carried out for 30min until the mixed solution becomes a clear transparent solution.
Step two, carrying out gradient heating on the treated mixed solution, wherein the process is as follows: raising the temperature from room temperature to 80 ℃ in 1 hour, and keeping the temperature for 24 hours; then, the temperature is increased from 80 ℃ to 90 ℃ in 1 hour, and the temperature is kept for 24 hours; then, the temperature is increased from 90 ℃ to 100 ℃ in 1 hour, and the temperature is kept for 24 hours; the temperature was then raised from 100 ℃ to 110 ℃ over 1 hour and held for 48 hours. Finally, the temperature was reduced from 110 ℃ to 25 ℃ over 12 hours. And obtaining an organic plastic scintillator blank.
And step three, treating the organic plastic scintillator blank at the low temperature of-10 ℃ for 12h, and then mechanically cutting and polishing the organic plastic scintillator blank to obtain an organic scintillator 2 sample with the PPO content of 20%.
< comparative example 3>
Step one, 87.9g of 2, 5-diphenyl oxazole, 247.5g of styrene, 15g of divinylbenzene, 0.75g of azobisisobutyronitrile and 0.75g of 9, 10-diphenyl anthracene are mixed, the mixed solution is placed in a 40KHz and 200W ultrasonic cleaning machine, ultrasonic dispersion is carried out for 30min, the mixed solution is suspended for 10min, and ultrasonic treatment is carried out for 30min until the mixed solution becomes clear and transparent solution.
Step two, carrying out gradient heating on the treated mixed solution, wherein the process is as follows: raising the temperature from room temperature to 80 ℃ in 1 hour, and keeping the temperature for 24 hours; then, the temperature is increased from 80 ℃ to 90 ℃ in 1 hour, and the temperature is kept for 24 hours; then, the temperature is increased from 90 ℃ to 100 ℃ in 1 hour, and the temperature is kept for 24 hours; the temperature was then raised from 100 ℃ to 110 ℃ over 1 hour and held for 48 hours. Finally, the temperature was reduced from 110 ℃ to 25 ℃ over 12 hours. And obtaining an organic plastic scintillator blank.
And step three, treating the organic plastic scintillator blank at the low temperature of-10 ℃ for 12h, and then mechanically cutting and polishing the organic plastic scintillator blank to obtain an organic plastic scintillator sample with the PPO content of 25%.
< comparative example 4>
An n-gamma ray resolution test was performed on the inlet liquid scintillator.
FIGS. 3 to 5 are graphs sequentially showing n-gamma ray resolution spectra of organic plastic scintillators with 30%, 40% and 50% PPO content prepared in examples 1 to 3. The upper and lower point groups in the figure are neutrons and gamma rays respectively, the n-gamma resolution can be observed at the positions indicated by the white long arrows, and the weaker the resolution is, the more the positions indicated by the white long arrows are separated, the more fuzzy the resolution is.
FIGS. 6 to 8 are n-gamma ray resolution spectrograms of organic scintillators with PPO contents of 1%, 20% and 25% prepared in comparative examples 1 to 3 in sequence. The weight PPO content of the organic scintillator in the graph of FIG. 6 is 1%, only one dot group is needed, and the discrimination of n-gamma cannot be realized; fig. 7 shows a PPO content of 20% and fig. 8 shows a PPO content of 25%, although the discrimination of n- γ can be achieved, the discrimination is poor at the low energy end, i.e., near the ordinate region.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A preparation method of an organic plastic scintillator is characterized by comprising the following steps:
mixing 2, 5-diphenyl oxazole, styrene, divinyl benzene, azodiisobutyronitrile and a wave-shifting agent according to a certain proportion, and performing ultrasonic dispersion treatment on the mixed solution;
step two, performing gradient heating on the treated mixed solution, and cooling to obtain an organic plastic scintillator blank;
and step three, carrying out mechanical cutting and polishing treatment on the organic plastic scintillator blank.
2. The method for preparing an organic plastic scintillator according to claim 1, wherein in the first step, the 2, 5-diphenyloxazole, the styrene, the divinylbenzene, the azobisisobutyronitrile and the wave-shifting agent account for 30 to 50%, 40 to 70%, 4 to 20%, 0.2 to 0.5%, and 0 to 0.5% by mass of the mixed solution in this order.
3. The method for preparing an organic plastic scintillator according to claim 1, wherein the wave-shifting agent in the first step is any one of 9, 10-diphenylanthracene, 1, 4-bis (5-phenyl-2-oxazolyl) benzene, 1, 4-bis (2-methylstyrene) benzene, and 1, 4-bis (4-methylstyrene) benzene.
4. The method for preparing an organic plastic scintillator according to claim 1, wherein the ultrasonic dispersion treatment in the first step is carried out by: and (3) placing the mixed solution in an ultrasonic cleaning machine with the frequency of 40-60 KHz and the power of 200-300W, suspending for 10-20 min after ultrasonic dispersion is carried out for 30-60 min, and then carrying out ultrasonic dispersion for 30-60 min until the mixed solution becomes a clear transparent solution.
5. The method for preparing an organic plastic scintillator according to claim 1, wherein the ultrasonic dispersion treatment in the first step is carried out by: placing the mixed solution under the conditions of 100-800 Pa of pressure and 0-10 ℃ for ultrasonic treatment; wherein the ultrasonic frequency is 30-60 kHz, the ultrasonic treatment is suspended for 3-6 min after 3-6 min, and the ultrasonic dispersion treatment is performed for 1-3 h by taking the ultrasonic treatment as a circulation.
6. The method for preparing an organic plastic scintillator according to claim 1, wherein the mixed solution is subjected to ultrasonic dispersion treatment and then to supercritical carbon dioxide mixing treatment in the first step, and the process is as follows: placing the mixed solution subjected to the ultrasonic dispersion treatment in a supercritical reaction kettle, introducing carbon dioxide, controlling the temperature in the reaction kettle to be 30-40 ℃, the pressure to be 6-24 MPa, and the magnetic stirring speed to be 1000-1500 rpm, and stirring for 1-3 hours; stopping heating, controlling the pressure relief rate to be 0.1-5 MPa/s when the temperature in the reaction kettle is 20-30 ℃, and discharging carbon dioxide gas to obtain the treated mixed solution.
7. The method for preparing an organic plastic scintillator according to claim 1, wherein the step two, the step of heating with a gradient temperature rise, comprises: heating the temperature from the room temperature to 80-90 ℃ in 1-2 h, preserving the heat for 24-48 h, heating the temperature from 80-90 ℃ to 90-100 ℃ in 1-2 h, preserving the heat for 24-48 h, heating the temperature from 90-100 ℃ to 100-110 ℃ in 1-2 h, and preserving the heat for 24-48 h; and finally, in 1-2 h, raising the temperature from 100-110 ℃ to 110-120 ℃, and preserving the heat for 48-72 h.
8. The method for preparing an organic plastic scintillator as claimed in claim 1, wherein the temperature reduction process in the second step is: in 12-24 h, the temperature is reduced from 110-120 ℃ to 20-25 ℃.
9. The method for preparing an organic plastic scintillator according to claim 1, wherein the organic plastic scintillator blank is subjected to a low temperature treatment at-10 to 20 ℃ for 12 to 24 hours before the mechanical cutting of the organic plastic scintillator blank in the third step.
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