Preparation method for tungsten/gadolinium oxide functional fiber having core-shell structure for x and gamma ray protection

Abstract

The present application provides a preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection, comprising: first preparing a core-shell structured tungsten/gadolinium oxide powder; preparing a W@Gd.sub.2O.sub.3/PP blended melt from the powder; and preparing a W@Gd.sub.2O.sub.3/PP composite fiber from the blended melt. The core-shell structured tungsten/gadolinium oxide functional fiber prepared by the method can play a role in synergistic protection in the aspect of radiation protection, eliminate a weak protection area, and effectively absorb secondary radiation generated by radiation. Secondly, the prepared functional fiber has the characteristics of no lead and light weight, and has good application prospects in the aspect of X and ? ray radiation protection.

Claims

1. A preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection, comprising the following steps: (1) preparing a dopamine salt solution, adding a buffer to adjust the pH value, then adding tungsten powder, and stirring, filtering, washing and drying, to obtain W@PDA; (2) adding the W@PDA obtained in the step (1) into a gadolinium nitrate solution, and stirring, filtering, and high-temperature calcining, to obtain a core-shell structured W@Gd.sub.2O.sub.3 powder; (3) adding the core-shell structured W@Gd.sub.2O.sub.3 powder obtained in the step (2) and a dried PP masterbatch sequentially into a feed port of a screw extruder to obtain a core-shell structured W@Gd.sub.2O.sub.3/PP blended melt, which is cooled in air and brittle fractured and granulated, to obtain dried blended particles; and (4) adding the dried blended particles obtained in the step (3) into a feed port of a screw extruder, and passing the extruded melt through a drawing and winding device and stretching the same to form a composite fiber.

2. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the buffer in the step (1) is tris, and the pH value is 8-9.

3. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the tungsten powder in the step (1) is tungsten powder cleaned with ethanol.

4. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the stirring in the step (1) is stirring for 18-24 h with an electric stirrer.

5. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the washing in the step (1) is washing for 2-3 times with deionized water and ethanol respectively.

6. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the dopamine salt solution in the step (1) has a concentration of 1.5 g/L-2.5 g/L.

7. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the high-temperature calcining in the step (2) has a calcining temperature of 800-1000? C., a calcining time of 2-3 h, and a heating rate of 2-4? C./min.

8. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the calcining in the step (2) is carried out in a protective gas, which is nitrogen or an inert gas.

9. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the gadolinium nitrate solution in the step (2) has a concentration of 0.3-0.5 M/L.

10. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the PP masterbatch in the step (3) is dried in an oven at 40-60? C. for 30-60 min.

11. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the screw extruder in the step (3) has an extrusion temperature of 100? C. and a screw rotation speed of 15 r/min.

12. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the blended particles in the step (4) are dried in an oven at 40-60? C. for 30-60 min.

13. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the screw extruder in the step (4) has a screw zone temperature of 100? C., a screw rotation speed of 20 r/min, a spinneret orifice temperature of 85? C., an extrusion speed of 7-8 mm/min, and a spinneret orifice diameter of 2 mm.

14. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the drawing and winding device in the step (4) has a drawing speed of 150 r/min.

15. The preparation method for a core-shell structured tungsten/gadolinium oxide functional fiber for X and ? ray protection of claim 1, wherein the method comprises the following steps: (1) preparing a dopamine salt solution with a concentration of 1.5 g/L-2.5 g/L, adding a tris buffer to adjust the pH to 8-9, then adding tungsten powder cleaned up with ethanol, and stirring with an electric stirrer for 18-24 h, then filtering and separating, and washing for 2-3 times with deionized water and ethanol respectively, and then drying, to obtain W@PDA; (2) adding the W@PDA obtained in the step (1) to a gadolinium nitrate solution with a concentration of 0.3-0.5 M/L, magnetically stirring for a certain period of time, then filtering and separating, and drying, and then high-temperature calcining the prepared sample at 800-1000? C. with charged nitrogen for 2-3 h (with a heating rate of 2-4? C./min), and finally obtaining a core-shell structured W@Gd.sub.2O.sub.3 powder; (3) adding the core-shell structured W@Gd.sub.2O.sub.3 powder obtained in the step (2) and a dried PP masterbatch sequentially into a feed port of a screw extruder with an extrusion temperature of 100? C. and a screw rotation speed of 15 r/min, to obtain a core-shell structured W@Gd.sub.2O.sub.3/PP blended melt, which is cooled in air and brittle fractured and granulated, to obtain dried blended particles; and (4) adding the dried blended particles obtained in the step (3) into a feed port of a screw extruder with a screw zone temperature of 100? C., a screw rotation speed of 20 r/min, a spinneret orifice temperature of 85? C., an extrusion speed of 7-8 mm/min, and a spinneret orifice diameter of 2 mm, and then passing the extruded melt through a drawing and winding device and stretching the same at a drawing speed of 150 r/min to form a composite fiber.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIG. 1s a scanning electron microscope image of a W@Gd.sub.2O.sub.3 powder of a functional fiber for X and ? ray protection prepared in Example 1.

DESCRIPTION OF THE EMBODIMENTS

(2) In order to better illustrate the present application and facilitate understanding of the technical solutions of the present application, some typical but non-limiting embodiments of the present application are given below:

Example 1

(3) The present example provides a preparation method for a functional fiber for X and ? ray protection. The method comprises the following steps:

(4) (1) A dopamine salt solution with a concentration of 2 g/L was prepared, into which a tris buffer was added to adjust the pH value of the solution to 8.5, then a tungsten powder cleaned up with ethanol was added, and stirred with an electric stirrer for 24 h, then the product was filtered and separated, and then washed for 2 times with deionized water and ethanol respectively, and dried at 80? C. for 5 h, to obtain W@PDA.

(5) (2) The W@PDA obtained in the step (1) was added into a gadolinium nitrate solution with a concentration of 0.3 M/L, magnetically stirred for 2 h, then the product was filtered and separated, and dried at 80? C. for 5 h, and then the prepared sample was high-temperature calcined at 800? C. with charged nitrogen for 2 h (with a heating rate of 2? C./min), and finally a core-shell structured W@Gd.sub.2O.sub.3 powder was obtained.

(6) (3) The core-shell structured W@Gd.sub.2O.sub.3 powder obtained in the step (2) and a dried PP masterbatch were sequentially added into a feed port of a screw extruder with an extrusion temperature of 100? C. and a screw rotation speed of 15 r/min, to obtain a core-shell structured W@Gd.sub.2O.sub.3/PP blended melt, which was cooled in air and brittle fractured and granulated.

(7) (4) The dried blended particles obtained in the step (3) were added into a feed port of a screw extruder with a screw zone temperature of 100? C., a screw rotation speed of 20 r/min, a spinneret orifice temperature of 85? C., an extrusion speed of 7 mm/min, and a spinneret orifice diameter of 2 mm, and then the extruded melt was passed through a drawing and winding device and stretched at a drawing speed of 150 r/min to form a composite fiber.

(8) The W@Gd.sub.2O.sub.3 powder prepared in this example was scanned by SEM, and the resulting photograph is shown in FIGURE. It can be seen from the figure that a PDA film is formed on the surface of the W powder.

Example 2

(9) The present example provides a preparation method for a functional fiber for X and ? ray protection. The method comprises the following steps:

(10) (1) A dopamine salt solution with a concentration of 1.5 g/L was prepared, into which a tris buffer was added to adjust the pH value of the solution to 8, then a tungsten powder cleaned up with ethanol was added, and stirred with an electric stirrer for 20 h, then the product was filtered and separated, and then washed for 3 times with deionized water and ethanol respectively, and dried at 60? C. for 8 h, to obtain W@PDA.

(11) (2) The W@PDA obtained in the step (1) was added into a gadolinium nitrate solution with a concentration of 0.35 M/L, magnetically stirred for 3 h, then the product was filtered and separated, and dried at 60? C. for 8 h, and then the prepared sample was high-temperature calcined at 900? C. with charged nitrogen for 2.5 h (with a heating rate of 3? C./min), and finally a core-shell structured W@Gd.sub.2O.sub.3 powder was obtained.

(12) (3) The core-shell structured W@Gd.sub.2O.sub.3 powder obtained in the step (2) and a dried PP masterbatch were sequentially added into a feed port of a screw extruder with an extrusion temperature of 100? C. and a screw rotation speed of 15 r/min, to obtain a core-shell structured W@Gd.sub.2O.sub.3/PP blended melt, which was cooled in air and brittle fractured and granulated.

(13) (4) The dried blended particles obtained in the step (3) were added into a feed port of a screw extruder with a screw zone temperature of 100? C., a screw rotation speed of 20 r/min, a spinneret orifice temperature of 85? C., an extrusion speed of 7.5 mm/min, and a spinneret orifice diameter of 2 mm, and then the extruded melt was passed through a drawing and winding device and stretched at a drawing speed of 150 r/min to form a composite fiber.

Example 3

(14) The present example provides a preparation method for a functional fiber for X and ? ray protection. The method comprises the following steps:

(15) (1) A dopamine salt solution with a concentration of 2.5 g/L was prepared, into which a tris buffer was added to adjust the pH value of the solution to 9, then a tungsten powder cleaned up with ethanol was added, and stirred with an electric stirrer for 18 h, then the product was filtered and separated, and then washed for 2 times with deionized water and ethanol respectively, and dried at 70? C. for 6 h, to obtain W@PDA.

(16) (2) The W@PDA obtained in the step (1) was added into a gadolinium nitrate solution with a concentration of 0.4 M/L, magnetically stirred for 2.5 h, then the product was filtered and separated, and dried at 70? C. for 6 h, and then the prepared sample was high-temperature calcined at 1000? C. with charged nitrogen for 3 h (with a heating rate of 4? C./min), and finally a core-shell structured W@Gd.sub.2O.sub.3 powder was obtained.

(17) (3) The core-shell structured W@Gd.sub.2O.sub.3 powder obtained in the step (2) and a dried PP masterbatch were sequentially added into a feed port of a screw extruder with an extrusion temperature of 100? C. and a screw rotation speed of 15 r/min, to obtain a core-shell structured W@Gd.sub.2O.sub.3/PP blended melt, which was cooled in air and brittle fractured and granulated.

(18) (4) The dried blended particles obtained in the step (3) were added into a feed port of a screw extruder with a screw zone temperature of 100? C., a screw rotation speed of 20 r/min, a spinneret orifice temperature of 85? C., an extrusion speed of 8 mm/min, and a spinneret orifice diameter of 2 mm, and then the extruded melt was passed through a drawing and winding device and stretched at a drawing speed of 150 r/min to form a composite fiber.

(19) The above description of the embodiments is intended to facilitate those of ordinary skill in the technical art to understand and use the invention. It is obvious that those skilled in the art can easily make various modifications to these embodiments, and apply the general principles described herein to other embodiments without creative effort. Therefore, the present application is not limited to the above embodiments. All improvements and modifications made by those skilled in the art from the disclosure of the present application without departing from the scope of the present application should fall within the protection scope of the present application.