中子照相转换屏用丙烯酸树脂的制备
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摘要
中子照相技术是一项重要的无损检测技术,转化屏的性能极大地影响着中子照相的质量。作为转换屏用的粘接材料,水性丙烯酸树脂不但具备优异的硬度、光泽、耐水性、耐酸碱性及良好的耐候性、耐污染性等有机溶剂型树脂的优点,而且具有价格低、使用安全、节省能源、减少环境污染和公害等特点。
本论文以丙烯酸(AA)、甲基丙烯酸甲酯(MMA)、丙烯酸丁酯(BA)、甲基丙烯酸羟乙酯(HEMA)为单体,以过氧化苯甲酸(BPO)为引发剂,以正丁醇为溶剂,采用溶液聚合法合成了水性丙烯酸树脂。通过研究引发剂用量、丙烯酸用量、溶剂与单体的配比、滴加时间、保温时间以及反应温度等反应条件对树脂水溶性、透光率、固含量、转化率和黏度等性能的影响,确立了制备中子照相转换屏用水性丙烯酸树脂的配方:AA用量为11%,HEMA用量为20%,BPO用量为2.0%,MMA/BA(质量比)为1:1,溶剂:单体(质量比)为1:1,溶剂采用正丁醇;制备工艺条件:单体的滴加时间为3h,保温时间为2.5h,反应温度为110℃左右,中和剂采用氨水,中和度为90%。在上述配方和工艺条件下制得的树脂的性能如下:树脂为淡黄色透明液体,水溶性好,40%水溶液透光率为98%,树脂转化率为96%,10%树脂水溶液的黏度为3.12 mPa·s,树脂玻璃化转变温度为46.1℃,热分解温度360-440℃。
将合成的树脂和反应材料混合均匀,使用丝网印刷的方法制备出中子照相转换屏,测试结果表明采用这种工艺制备的中子照相转换屏具有较好的分辨率和灵敏度。
Neutron radiography is an important technology of non-destruction testing. The quality of neutron radiography is deeply influenced by the property of the converter. As the binders for the converter, the water-soluble acrylic resin posses not only excellent hardness, gloss, resistance of water, acid, alkali and weather which is the advantages of and organic solvent resin, but aslo the low price, the use safety, energy saving and reducing environmental pollution.
The water-soluble acrylic resin is synthesized with the solution polymerization. And it is prepared via solution polymerization which takes acrylic acid, methyl methacrylate, acrylic acid butyl ester and methyl acrylic acid hydroxy ethyl ester as the monomers, takes benzoyl peroxide as the initiator and takes n-butanol as the solvent. By discussing initiator's amount, solvent and monomers' allocated proportion, acrylic acid's amount, instilment time, heat preservation time,neutralization degrees and reaction temperature to the resin's performance influence, such as the water-solubility, the light transmission rate, the content of the firm, the conversion rate and the viscosity, we obtain the formula of synthesis water-soluble acrylic resin for neutron radiography converter: the AA amount used is 11%, the HEMA amount used is 20%, the BPO amount used is 2.0%, the MMA:BA (mass ratio) is 1:1, the solvent: monomer (mass ratio) is 1:1; and the synthesis conditions: the monomer dropping time is 3h, the sintering time is 2.5h, the reaction temperature is 110℃, ammonia is used as the neutralizer and the neutralization degree is 90%.The function of the resin which made under conditions of formula and conditions above-mentioned as follows: It is light yellow transparent liquid, it has good water-solubility, visible light transmittance of its 40% aqueous solution is 98%, its conversion is 96%, viscosity of its 40% aqueous solution is 3.12mPa·s, and its glass transition temperature is 46.1℃, the thermal decomposition temperature is 360-440℃.
Synthetic resin and reaction material are well-mixed, the neutron radiography converter is produced by means of screen printing. The test results showed that this converter exhibits good resolution and sensitivity after radiography.
本论文以丙烯酸(AA)、甲基丙烯酸甲酯(MMA)、丙烯酸丁酯(BA)、甲基丙烯酸羟乙酯(HEMA)为单体,以过氧化苯甲酸(BPO)为引发剂,以正丁醇为溶剂,采用溶液聚合法合成了水性丙烯酸树脂。通过研究引发剂用量、丙烯酸用量、溶剂与单体的配比、滴加时间、保温时间以及反应温度等反应条件对树脂水溶性、透光率、固含量、转化率和黏度等性能的影响,确立了制备中子照相转换屏用水性丙烯酸树脂的配方:AA用量为11%,HEMA用量为20%,BPO用量为2.0%,MMA/BA(质量比)为1:1,溶剂:单体(质量比)为1:1,溶剂采用正丁醇;制备工艺条件:单体的滴加时间为3h,保温时间为2.5h,反应温度为110℃左右,中和剂采用氨水,中和度为90%。在上述配方和工艺条件下制得的树脂的性能如下:树脂为淡黄色透明液体,水溶性好,40%水溶液透光率为98%,树脂转化率为96%,10%树脂水溶液的黏度为3.12 mPa·s,树脂玻璃化转变温度为46.1℃,热分解温度360-440℃。
将合成的树脂和反应材料混合均匀,使用丝网印刷的方法制备出中子照相转换屏,测试结果表明采用这种工艺制备的中子照相转换屏具有较好的分辨率和灵敏度。
Neutron radiography is an important technology of non-destruction testing. The quality of neutron radiography is deeply influenced by the property of the converter. As the binders for the converter, the water-soluble acrylic resin posses not only excellent hardness, gloss, resistance of water, acid, alkali and weather which is the advantages of and organic solvent resin, but aslo the low price, the use safety, energy saving and reducing environmental pollution.
The water-soluble acrylic resin is synthesized with the solution polymerization. And it is prepared via solution polymerization which takes acrylic acid, methyl methacrylate, acrylic acid butyl ester and methyl acrylic acid hydroxy ethyl ester as the monomers, takes benzoyl peroxide as the initiator and takes n-butanol as the solvent. By discussing initiator's amount, solvent and monomers' allocated proportion, acrylic acid's amount, instilment time, heat preservation time,neutralization degrees and reaction temperature to the resin's performance influence, such as the water-solubility, the light transmission rate, the content of the firm, the conversion rate and the viscosity, we obtain the formula of synthesis water-soluble acrylic resin for neutron radiography converter: the AA amount used is 11%, the HEMA amount used is 20%, the BPO amount used is 2.0%, the MMA:BA (mass ratio) is 1:1, the solvent: monomer (mass ratio) is 1:1; and the synthesis conditions: the monomer dropping time is 3h, the sintering time is 2.5h, the reaction temperature is 110℃, ammonia is used as the neutralizer and the neutralization degree is 90%.The function of the resin which made under conditions of formula and conditions above-mentioned as follows: It is light yellow transparent liquid, it has good water-solubility, visible light transmittance of its 40% aqueous solution is 98%, its conversion is 96%, viscosity of its 40% aqueous solution is 3.12mPa·s, and its glass transition temperature is 46.1℃, the thermal decomposition temperature is 360-440℃.
Synthetic resin and reaction material are well-mixed, the neutron radiography converter is produced by means of screen printing. The test results showed that this converter exhibits good resolution and sensitivity after radiography.
引文
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[7]吴洋,唐彬,霍合勇等.LiF-ZnS中子转换屏参数与性能初步理论分析[C].第六届全国核仪器及其应用学术会议论文集,2007,126-130
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[19]李文俊.壳聚糖-聚丙烯酸配合物半互穿聚合物网络膜及其对pH和离子的刺激反应[J].高分子学报,1997(2):106-110
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