Neutron radiation protection fiber and preparation and application thereof
A radiation protection and neutron technology, which is applied in the field of neutron radiation-resistant polymer materials, can solve the problems of complex spinning equipment and process, insufficient boron content, and degradation of polymer mechanical properties, so as to improve the neutron shielding performance and mechanical properties, expanding the application range, improving heat resistance and processing performance
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Embodiment 1
[0053] Carborane dicarboxylic acid-containing monomer: 5-(o-carborane-1'-methyleneoxy) dimethyl isophthalate (BDMI) is used as a comonomer, and its structural formula is:
[0054]
[0055] The synthetic route of 5-(o-carborane-1'-methyleneoxy) dimethyl isophthalate (BDMI) is as follows:
[0056]
[0057] In a three-neck flask, add 0.22mol of 5-hydroxyisophthalic acid, 300ml of methanol and 12ml of concentrated sulfuric acid in sequence, and react under reflux in an oil bath at 70°C, monitored by TLC, and cool naturally to room temperature after the reaction. The reaction solution was slowly added to distilled water, and a large amount of white precipitates precipitated out. They were suction filtered and vacuum-dried to obtain a white powder with a yield of 96.8%. The product was methyl 5-hydroxyisophthalate with a melting point of 169°C.
[0058] In the three-necked flask, 0.22mol of dimethyl 5-hydroxyisophthalate, 0.48mol of anhydrous potassium carbonate and solvent DM...
Embodiment 2
[0068] In embodiment 2, the synthetic route of 5-(o-carborane-1'-methyleneoxy) dimethyl isophthalate (BDMI) is the same as embodiment 1, and the concrete steps are:
[0069] In the three-necked flask, 0.22mol dimethyl 5-hydroxyisophthalate, 0.48mol anhydrous potassium carbonate and solvent DMAC were sequentially added. Oil bath at 65°C, stir for 1 hour, cool to room temperature, slowly add 0.24mol 3-bromopropyne dropwise, keep warm at 25°C for reaction, TLC monitoring until the reaction is complete, the reaction solution is slowly added to distilled water, a large amount of white precipitate precipitates, and suction filtered , and dried to obtain dimethyl 5-propargyloxyisophthalate.
[0070] In a three-necked flask, add 0.40mol 5-propargyloxyisophthalate dimethyl ester, 0.42mol decaborane, 0.40mol N,N dimethylaniline and anhydrous toluene in sequence, reflux reaction at 110°C, TLC monitoring, reaction At the end, add dilute hydrochloric acid solution, filter while it is hot,...
Embodiment 3~5
[0073] The synthesis of BDMI is the same as in Example 1, and the preparation method of boron-containing polyester is the same as in Example 1, except for the ratio of raw materials, see Table 1 for details. The products prepared in Examples 1-5 are marked as B-PBT-2, B-PBT-3, B-PBT-4, B-PBT-5.
[0074] Table 1 Raw material components and mass ratio of boron-containing polyester B-PBT
[0075]
[0076] Table 2 Properties of boron-containing polyester B-PBT
[0077]
[0078] The molecular weight of the product is determined to be above 10,000 by intrinsic viscosity, and the range of n and m is known to be in the range of 60-100 in combination with the comonomer ratio.
[0079] The fiber is tested for tensile strength, and polyester PBT is used as a comparison, and the results are shown in figure 1 and Table 3. figure 1 The abscissa is the strain ε, and the ordinate is the stress, the unit is MPa. figure 1 The strain ε value of the bottom curve B-PBT-4 is 0.
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