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In this paper, a large number of hydrogen bonds were constructed between B4C particles and poly(vinyl alcohol) (PVA) matrix by means of surface modification to enhance the interaction between the two phases, and highly filled B4C/PVA fibers and their fabrics were successfully prepared by wet spinning technology, which provided both neutron protection and air- and moisture-permeability. The results show that cetyltrimethylammonium bromide (CTAB) is uniformly coated on the surface of B4C particles and alkyl tail entanglement with OP-10, which makes the high-filled B4C particles stable in suspension in PVA spinning solution and stable in spinning process, and the B4C/PVA fibers and their textile fabrics are obtained with up to 50% filling capacity. Neutron protection and air permeability and moisture permeability of textile fabrics need to be provided 50% wt% B4C-CTAB-OP-10/PVA fabrics with a single-layer neutron shielding rate of 49.43%. The present work provides a new solution for wearing comfort and radiation protection safety of the products. [ABSTRACT FROM AUTHOR]