CN112900155B - Preparation method of non-woven fabric for X and gamma ray protection - Google Patents
Preparation method of non-woven fabric for X and gamma ray protection Download PDFInfo
- Publication number
- CN112900155B CN112900155B CN202110170798.4A CN202110170798A CN112900155B CN 112900155 B CN112900155 B CN 112900155B CN 202110170798 A CN202110170798 A CN 202110170798A CN 112900155 B CN112900155 B CN 112900155B
- Authority
- CN
- China
- Prior art keywords
- preparing
- gamma
- temperature
- ray protection
- ray
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21J—FIBREBOARD; MANUFACTURE OF ARTICLES FROM CELLULOSIC FIBROUS SUSPENSIONS OR FROM PAPIER-MACHE
- D21J3/00—Manufacture of articles by pressing wet fibre pulp, or papier-mâché, between moulds
- D21J3/12—Manufacture of articles by pressing wet fibre pulp, or papier-mâché, between moulds of sheets; of diaphragms
Abstract
The application provides a preparation method of a core-shell structure tungsten/gadolinium oxide PP non-woven fabric for X and gamma ray protection, which comprises the steps of firstly preparing core-shell structure tungsten/gadolinium oxide powder; preparation of W @ Gd from the above powder 2 O 3 a/PP blend melt; then preparing W @ Gd according to the blended melt 2 O 3 a/PP composite fibre; finally preparing W @ Gd according to the composite fiber 2 O 3 the/PP composite non-woven material. The tungsten/gadolinium oxide PP non-woven fabric with the core-shell structure prepared by the method can play a role in cooperative protection in the aspect of radiation protection, eliminates a weak protection area and can effectively absorb secondary radiation generated by radiation. And secondly, the prepared functional non-woven fabric has the characteristics of no lead and light weight, and has good application prospect in the aspect of X-ray and gamma-ray radiation protection.
Description
Technical Field
The application relates to the field of radiation protection, in particular to a preparation method of non-woven fabric for X and gamma ray protection.
Background
The development of nuclear technology brings convenience to people and simultaneously generates a lot of radiation hazards, and the light, flexible and excellent-protection-performance textile for radiation protection is a hot spot of current research. The radiation protection material is mainly divided into a lead material and a lead-free material. Lead is mainly lead, and although the protective effect is good, the lead has toxicity, poor strength and large low-energy X-ray scattering. The lead-free material mainly comprises a composite material prepared from rare earth elements and heavy metal compounds such as tin, tungsten, bismuth and the like, and has excellent protection effect, light weight and safety.
In recent years, micro-nano core-shell materials with special structures attract wide attention of people. The composite particles with different core-shell microstructures have unique physicochemical properties, so that the composite particles have wide application prospects in various fields such as optics, electronics, catalysis, biology, radiation and the like. In the aspect of radiation protection, compared with a single metal physical blending mode, the radiation protection material with the core-shell structure can realize synergistic protection, eliminate a protection weak area and effectively absorb secondary radiation generated by radiation. The preparation method of the core-shell structure mainly comprises a template method, a precipitation method, a hydrothermal synthesis method, a spray drying method, a layer-by-layer self-assembly technology and the like. Li et al prepared gadolinium oxide hollow spheres with controllable shell thickness by using silicon dioxide as a template and adopting a homogeneous precipitation method. However, these methods have disadvantages of many steps and long time, so that it is necessary to specify an effective and simple method to overcome these disadvantages. Mussel secreted adhesion protein has strong adhesion capability, which inspires that the task group of Messer Smith at the northwest university in the United states in 2007 finds that Dopamine (DA) can be oxidized and self-polymerized into polydopamine on the surface of any material under the weak base condition simulating seawater. The polymerization condition is simple and controllable, and the product has excellent adhesiveness, hydrophilicity, stability and biocompatibility. Meanwhile, a large number of phenolic hydroxyl and amino active groups exist on the polydopamine, so that abundant active sites are provided for the complexation of metal ions.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a non-woven fabric for X and gamma ray protection.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a preparation method of a non-woven fabric for X and gamma ray protection, which comprises the following steps:
(1) preparing dopamine salt solution, adding buffer solution to adjust the pH value, then adding tungsten powder, stirring, filtering, washing and drying to obtain W @ PDA;
(2) adding the W @ PDA obtained in the step (1) into a gadolinium nitrate solution, stirring, filtering, and calcining at high temperature to obtain W @ Gd of a core-shell structure 2 O 3 A powder;
(3) enabling the core-shell structure W @ Gd obtained in the step (2) 2 O 3 Sequentially adding the powder and the dried PP master batch into a feed port of a screw extruder to obtain the core-shell structure W @ Gd 2 O 3 /PP blending melt, cooling in air and performing brittle fracture granulation;
(4) adding the dried blended particles obtained in the step (3) into a feed port of a screw extruder, and drawing the extruded melt by a drawing and winding device to prepare composite fibers;
(5) adding paper pulp into a beaker filled with deionized water, and uniformly stirring to obtain a paper pulp suspension;
(6) shearing the composite fiber obtained in the step (4) into short fibers, and adding the short fibers into a wall breaking machine filled with deionized water to break up all the fibers to obtain a fiber suspension;
(7) adding the pulp suspension obtained in the step (5) into the fiber suspension obtained in the step (6), and scattering until the fibers and the pulp are uniformly mixed and dispersed;
(8) pouring the mixed suspension obtained in the step (7) into a vacuum filtration device for filtration to obtain a wet-process formed felt;
(9) putting the felt obtained in the step (8) into a heating type manual tablet press for hot pressing to obtain a pressing sheet material, and drying to obtain a composite non-woven material;
(10) the concentration of the dopamine salt solution in the step (1) is 1.5g/L-2.5 g/L;
(11) the concentration of the gadolinium nitrate solution in the step (2) is 0.3-0.5M/L.
According to the invention, the concentration of the prepared dopamine salt solution in the step (1) is controlled to be 1.5-2.5 g/L. Mainly because only a small amount of PDA particles were deposited on the surface of W when the DA concentration was below 1.5g/L, and a PDA film was formed on the surface of W powder when the DA concentration was 1.5-2.5 g/L. When the concentration of DA is higher than 2.5g/L, larger PDA particles are formed on the surface of W powder through self-polymerization due to the fact that the concentration of DA is too high, and the subsequent adsorption of gadolinium ions is not facilitated.
It is worth noting that in the step (1), after the dopamine salt solution is prepared, tris buffer solution is added into the system to adjust the pH value of the solution to be 8-9, because dopamine can be polymerized into polydopamine in the presence of weak base and oxygen, the polydopamine on the surfaces of different substances has extraordinary surface activity and adhesiveness, and a platform can be provided for secondary functionalization of materials.
Further, the stirring in the step (1) needs to be carried out for 18-24 hours under an electric stirrer.
In addition, for the washing in step (1), washing with water and ethanol is required 2 to 3 times, respectively.
The specific conditions for the drying in the step (1) are not particularly limited as long as the object of drying the sample can be achieved.
According to the invention, the concentration of the gadolinium nitrate solution in the step (2) should be controlled to be 0.3-0.5M/L. Because when Gd is present + At a concentration of 0.02M/L, the surface of W is coated with a small amount of sparse nano-dotted Gd 2 O 3 And (3) granules. When Gd is present + Gd on the W surface increased to 0.1M/L 2 O 3 The nanoparticles become larger and larger due to Gd + Increased concentration of Gd 2 O 3 The nanoparticles combine with each other to form larger Gd 2 O 3 And (3) granules. When Gd is present + Gd on the W surface increased to 0.2M/L 2 O 3 The nanoparticles become larger and more dense. With Gd + Gd increased in concentration to 0.3M/L, W surface 2 O 3 W @ Gd with core-shell structure formed by mutually combining nano particles 2 O 3 . Continued increase in Gd + Gd on the W surface after concentration to 0.4M/L 2 O 3 Nanoparticles compared to Gd + The concentration of 0.3M/L did not change much, due to poly-dopamine on the W surface to Gd + Chelating agents for Gd + The concentration of 0.3M/L is saturated, and the waste is caused by the excessively high concentration.
Further, the stirring in the step (2) is not particularly limited, and only magnetic stirring is needed for a certain time.
In addition, the high-temperature calcination in the step (2) needs to be carried out for 2-3h under the conditions of 800-1000 ℃ in a muffle furnace, and the temperature rise is 2-4 ℃/min. In order to avoid the formation of impurities during the reaction, the calcination in step (2) of the present invention is performed in a protective gas, wherein the protective gas includes nitrogen or an inert gas, and the inert gas may be argon, helium, etc., and the present invention is not particularly limited in this respect.
According to the invention, the PP master batch in the step (3) needs to be dried in an oven at 40-60 ℃ for 30-60 min.
In addition, the screw extruder in the step (3) has the extrusion temperature of 100 ℃ and the screw rotation speed of 15 r/min.
According to the invention, the blended particles in the step (4) are dried in an oven at 40-60 ℃ for 30-60 min.
It is noted that in the screw extruder described in the step (4), the temperature of the screw zone is 100 ℃, the rotation speed of the screw is 20r/min, the temperature of the spinneret orifice is 85 ℃, and the extrusion speed is as follows: 7-8 mm/min, and the aperture of a spinneret orifice is 2 mm.
In addition, the drafting and winding device in the step (4) has a drafting speed of 150 r/min.
According to the invention, the pulp of step (5) was 50ml of deionized water, with a pulp addition of 3 wt.%.
In addition, after the magnetic stirring is carried out for 5min at the stirring speed of 80r/min in the step (5), the stirring is carried out for 20min at the stirring speed of 40 r/min.
According to the invention, the short fibers in the step (6) have a length of 1-3 mm.
And (4) breaking the wall of the step (6), wherein the wall breaking machine is filled with 800ml of deionized water, pausing for 30s every 1min of breaking at a low speed, and repeating for 10 times.
According to the invention, the wall breaking machine in the step (7) breaks up, pauses for 30s every 1min at low speed, and repeats for 10 times.
According to the invention, the felt of step (8) has a diameter of 15 cm.
According to the hot press in the step (9), the rolling temperature of the upper plate and the lower plate is set to be 60 ℃, and the hot press is firstly carried out at 15000Pa for 1min, then at 20000Pa for 1min, then at 25000Pa for 30s and finally at 27500Pa for 30 s.
In addition, the drying in the step (9) needs to be carried out in an oven at 40-60 ℃ for 30-60 min.
As a preferable technical scheme, the preparation method of the non-woven fabric for X and gamma ray protection comprises the following steps:
(1) preparing a dopamine salt solution with the concentration range of 1.5-2.5g/L, adding tris buffer solution to adjust the pH value to 8-9, then adding tungsten powder cleaned by ethanol, stirring for 18-24h by using an electric stirrer, filtering and separating, washing for 2-3 times by using deionized water and ethanol respectively, and drying to obtain W @ PDA:
(2) adding the W @ PDA obtained in the step (1) into a gadolinium nitrate solution with the concentration range of 0.3-0.5M/L, magnetically stirring for a certain time, filtering, separating, drying, introducing nitrogen into the prepared sample at the temperature of 800- 2 O 3 And (3) powder.
(3) Enabling the core-shell structure W @ Gd obtained in the step (2) 2 O 3 Sequentially adding the powder and the dried PP master batch into a feed port of a screw extruder, wherein the extrusion temperature is 100 ℃, and the screw rotation speed is 15r/min, so as to obtain the core-shell structure W @ Gd 2 O 3 the/PP is blended with the melt and cooled in the air for brittle fracture granulation.
(4) Adding the dried blended particles obtained in the step (3) into a feed inlet of a screw extruder, wherein the temperature of a screw zone is 100 ℃, the rotating speed of the screw is 20r/min, the temperature of a spinneret orifice is 85 ℃, and the extrusion speed is as follows: 7-8 mm/min, the diameter of a spinneret orifice is 2mm, and then the extruded melt is drawn by a drawing and winding device at a drawing speed of 150r/min to prepare the composite fiber.
(5) Adding the paper pulp into a beaker filled with 50ml of deionized water, keeping the paper pulp addition amount of 3 wt.%, magnetically stirring for 5min at the speed of 80r/min, and then stirring for 20min at the speed of 40r/min to obtain a uniform paper pulp suspension.
(6) And (5) cutting the composite fiber obtained in the step (4) into short fibers with the length of 1-3 mm, adding the short fibers into a wall breaking machine filled with 800mL of deionized water, pausing for 30s every 1min at a low speed, and repeating for 10 times until all the fibers are broken up to obtain a fiber suspension.
(7) And (3) adding the pulp suspension obtained in the step (5) into the fiber suspension obtained in the step (6), pausing for 30s every 1min of scattering at a low speed, and repeating for 10 times until the fibers and the pulp are uniformly mixed and dispersed.
(8) And (4) pouring the mixed suspension obtained in the step (7) into a vacuum filtration device for filtration to obtain the wet-process formed felt with the diameter of 15 cm.
(9) Putting the felt obtained in the step (8) into a heating type manual tablet press for hot pressing, wherein the calendering temperature of the upper plate and the lower plate of the hot press is set as follows: and (3) when the temperatures of the upper plate and the lower plate are stabilized at 60 ℃, putting the felt between two heating and pressurizing plates of the heating type manual tablet press. Firstly carrying out 15000Pa hot pressing for 1min, then carrying out 20000Pa hot pressing for 1min, then carrying out 25000Pa hot pressing for 30s, finally carrying out 27500Pa hot pressing for 30s, and then placing the obtained pressing sheet material in an oven at 40 ℃ for drying for 30min to obtain the composite non-woven material.
The core-shell structure W @ Gd prepared by adopting the preferred technical scheme 2 O 3 Compared with tungsten and gadolinium oxide blended powder, the core-shell structure can play a synergistic protection role in radiation protection, and secondary radiation generated by radiation is effectively absorbed while a protection weak area is eliminated.
Compared with the prior art, the invention at least has the following beneficial effects:
the method comprises the steps of firstly utilizing that dopamine can be polymerized into polydopamine in the presence of weak base and oxygen, and the polydopamine has extraordinary adhesion on the surfaces of different substances, and can successfully coat tungsten to obtain W @ PDA.
The surface of PDA contains a large amount of polar groups such as phenolic hydroxyl, amido and the like, provides rich active sites for complexing various metal ions, and can effectively react with Gd in gadolinium nitrate solution + Chelation was performed. After high-temperature calcination, the PDA forms a nitrogen-doped carbon layer which is attached to the surface of tungsten and is connected with Gd + Conversion of chelating W @ PDA to W @ Gd 2 O 3 。
Drawings
FIG. 1 is a scanning electron microscope image of an X, gamma ray protective functional material prepared in example 1.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a preparation method of a non-woven fabric for X and gamma ray protection, which comprises the following steps:
(1) preparing a dopamine salt solution with the concentration of 2g/L, adding tris buffer solution to adjust the pH value of the solution to 8.5, then adding tungsten powder cleaned by ethanol, stirring for 24 hours by using an electric stirrer, filtering and separating, washing for 2 times by using deionized water and ethanol respectively, and drying for 5 hours at 80 ℃ to obtain W @ PDA;
(2) adding the W @ PDA obtained in the step (1) into a gadolinium nitrate solution with the concentration of 0.3M/L, magnetically stirring for 2 hours, filtering and separating, drying for 5 hours at 80 ℃, introducing nitrogen into the prepared sample at 800 ℃ to calcine for 2 hours at high temperature, and finally obtaining the W @ Gd of the core-shell structure 2 O 3 And (3) powder.
(3) Enabling the core-shell structure W @ Gd obtained in the step (2) 2 O 3 Sequentially adding the powder and the dried PP master batch into a feed port of a screw extruder, wherein the extrusion temperature is 100 ℃, and the screw rotating speed is 15r/min, so as to obtain the core-shell structure W @ Gd 2 O 3 The melt is blended with PP and then cooled in air to form brittle fracture granules.
(4) Adding the dried blended particles obtained in the step (3) into a feeding port of a screw extruder, wherein the temperature of a screw zone is 100 ℃, the rotating speed of the screw is 20r/min, the temperature of a spinneret orifice is 85 ℃, and the extrusion speed is as follows: mm/min, the pore diameter of a spinneret orifice is 2mm, and then the extruded melt is drawn by a drawing and winding device under the condition of the drawing speed of 150r/min to prepare the composite fiber.
(5) Adding the pulp into a beaker filled with 50ml of deionized water, keeping the adding amount of the pulp at 3 wt.%, carrying out magnetic stirring at the speed of 80r/min for 5min, and then stirring at the speed of 40r/min for 20min to obtain a uniform pulp suspension.
(6) And (3) shearing the composite fiber obtained in the step (4) into short fibers with the length of 1mm, adding the short fibers into a wall breaking machine filled with 800mL of deionized water, pausing for 30s at low speed every 1min for breaking, and repeating for 10 times until the fibers are completely broken to obtain a fiber suspension.
(7) And (3) adding the pulp suspension obtained in the step (5) into the fiber suspension obtained in the step (6), pausing for 30s every 1min of scattering at a low speed, and repeating for 10 times until the fibers and the pulp are uniformly mixed and dispersed.
(8) And (5) pouring the mixed suspension obtained in the step (7) into a vacuum filtration device for filtration to obtain a wet-process formed felt with the diameter of 15 cm.
(9) Putting the felt obtained in the step (8) into a heating type manual tablet press for hot pressing, wherein the calendering temperature of the upper plate and the lower plate of the hot press is set as follows: and (3) when the temperatures of the upper plate and the lower plate are stabilized at 60 ℃, putting the felt between two heating and pressurizing plates of the heating type manual tablet press. Firstly carrying out hot pressing at 15000Pa for 1min, then carrying out hot pressing at 20000Pa for 1min, then carrying out hot pressing at 25000Pa for 30s, finally carrying out hot pressing at 27500Pa for 30s, and then placing the obtained pressing sheet material in an oven at 40 ℃ for drying for 30min to obtain the composite non-woven material.
W @ Gd prepared in this example 2 O 3 The powder was SEM-scanned, and the photograph is shown in FIG. 1, in which it was found that a PDA film was formed on the surface of the W powder.
Example 2
The embodiment provides a preparation method of a non-woven fabric for X and gamma ray protection, which comprises the following steps:
(1) preparing 1.5g/L dopamine salt solution, adding tris buffer solution to adjust the pH value of the solution to 8, then adding tungsten powder cleaned by ethanol, stirring for 20 hours by using an electric stirrer, filtering and separating, washing for 3 times by using deionized water and ethanol respectively, and drying for 8 hours at 60 ℃ to obtain W @ PDA;
(2) adding the W @ PDA obtained in the step (1) into a gadolinium nitrate solution with the concentration of 0.35M/L, magnetically stirring for 3 hours, filtering and separating, drying for 8 hours at the temperature of 60 ℃, introducing nitrogen into the prepared sample at the temperature of 900 ℃, and calcining for 2.5 hours at high temperature to obtain the W @ Gd core-shell structure 2 O 3 And (3) powder.
(3) Enabling the core-shell structure W @ Gd obtained in the step (2) 2 O 3 Sequentially adding the powder and the dried PP master batch into a feed port of a screw extruder, wherein the extrusion temperature is 100 ℃, and the screw rotation speed is 15r/min, so as to obtain the core-shell structure W @ Gd 2 O 3 the/PP is blended with the melt and cooled in the air for brittle fracture granulation.
(4) Adding the dried blended particles obtained in the step (3) into a feed inlet of a screw extruder, wherein the temperature of a screw zone is 100 ℃, the rotating speed of the screw is 20r/min, the temperature of a spinneret orifice is 85 ℃, and the extrusion speed is as follows: 7.5mm/min, the pore diameter of a spinneret orifice is 2mm, and then the extruded melt is drawn by a drawing and winding device under the condition of the drawing speed of 150r/min to prepare the composite fiber.
(5) Adding the pulp into a beaker filled with 50ml of deionized water, keeping the adding amount of the pulp at 3 wt.%, carrying out magnetic stirring at the speed of 80r/min for 5min, and then stirring at the speed of 40r/min for 20min to obtain a uniform pulp suspension.
(6) And (3) shearing the composite fiber obtained in the step (4) into short fibers with the length of 2mm, adding the short fibers into a wall breaking machine filled with 800mL of deionized water, pausing for 30s at low speed every 1min for breaking, and repeating for 10 times until the fibers are completely broken to obtain a fiber suspension.
(7) And (3) adding the pulp suspension obtained in the step (5) into the fiber suspension obtained in the step (6), pausing for 30s every 1min of scattering at a low speed, and repeating for 10 times until the fibers and the pulp are uniformly mixed and dispersed.
(8) And (4) pouring the mixed suspension obtained in the step (7) into a vacuum filtration device for filtration to obtain the wet-process formed felt with the diameter of 15 cm.
(9) Putting the felt obtained in the step (8) into a heating type manual tablet press for hot pressing, wherein the calendering temperature of the upper plate and the lower plate of the hot press is set as follows: and (3) when the temperatures of the upper plate and the lower plate are stabilized at 60 ℃, putting the felt between two heating and pressurizing plates of the heating type manual tablet press. Firstly carrying out hot pressing at 15000Pa for 1min, then carrying out hot pressing at 20000Pa for 1min, then carrying out hot pressing at 25000Pa for 30s, finally carrying out hot pressing at 27500Pa for 30s, and then placing the obtained pressing sheet material in an oven at 40 ℃ for drying for 30min to obtain the composite non-woven material.
Example 3
The embodiment provides a preparation method of a non-woven fabric for X and gamma ray protection, which comprises the following steps:
(1) preparing a dopamine salt solution with the concentration of 2.5g/L, adding tris buffer solution to adjust the pH value of the solution to 9, then adding tungsten powder cleaned by ethanol, stirring for 18 hours by using an electric stirrer, filtering and separating, washing for 2 times by using deionized water and ethanol respectively, and drying for 6 hours at 70 ℃ to obtain W @ PDA;
(2) adding the W @ PDA obtained in the step (1) into a gadolinium nitrate solution with the concentration of 0.4M/L, magnetically stirring for 2.5h, filtering and separating, drying at 70 ℃ for 6h, introducing nitrogen into the prepared sample at 1000 ℃ and calcining at high temperature for 3h to finally obtain the W @ Gd of the core-shell structure 2 O 3 And (3) powder.
(3) The core-shell structure W @ Gd obtained in the step (2) 2 O 3 Sequentially adding the powder and the dried PP master batch into a feed port of a screw extruder, wherein the extrusion temperature is 100 ℃, and the screw rotation speed is 15r/min, so as to obtain the core-shell structure W @ Gd 2 O 3 the/PP is blended with the melt and cooled in the air for brittle fracture granulation.
(4) Adding the dried blended particles obtained in the step (3) into a feeding port of a screw extruder, wherein the temperature of a screw zone is 100 ℃, the rotating speed of the screw is 20r/min, the temperature of a spinneret orifice is 85 ℃, and the extrusion speed is as follows: 8mm/min, the pore diameter of a spinneret orifice is 2mm, and then the extruded melt is drawn by a drawing and winding device under the condition of the drawing speed of 150r/min to prepare the composite fiber.
(5) Adding the pulp into a beaker filled with 50ml of deionized water, keeping the adding amount of the pulp at 3 wt.%, carrying out magnetic stirring at the speed of 80r/min for 5min, and then stirring at the speed of 40r/min for 20min to obtain a uniform pulp suspension.
(6) And (3) shearing the composite fiber obtained in the step (4) into short fibers with the length of 3mm, adding the short fibers into a wall breaking machine filled with 800mL of deionized water, pausing for 30s at low speed every 1min for breaking, and repeating for 10 times until the fibers are completely broken to obtain a fiber suspension.
(7) And (4) adding the pulp suspension obtained in the step (5) into the fiber suspension obtained in the step (6), pausing for 30s every 1min at a low speed, and repeating for 10 times until the fibers and the pulp are uniformly mixed and dispersed.
(8) And (4) pouring the mixed suspension obtained in the step (7) into a vacuum filtration device for filtration to obtain the wet-process formed felt with the diameter of 15 cm.
(9) Putting the felt obtained in the step (8) into a heating type manual tablet press for hot pressing, wherein the calendering temperature of the upper plate and the lower plate of the hot press is set as follows: and (3) when the temperatures of the upper plate and the lower plate are stabilized at 60 ℃, putting the felt between two heating and pressurizing plates of the heating type manual tablet press. Firstly carrying out hot pressing at 15000Pa for 1min, then carrying out hot pressing at 20000Pa for 1min, then carrying out hot pressing at 25000Pa for 30s, finally carrying out hot pressing at 27500Pa for 30s, and then placing the obtained pressing sheet material in an oven at 40 ℃ for drying for 30min to obtain the composite non-woven material.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (21)
1. A preparation method of non-woven fabric for X and gamma ray protection is characterized by comprising the following steps:
(1) preparing dopamine salt solution, adding buffer solution to adjust the pH value, then adding tungsten powder, stirring, filtering, washing and drying to obtain W @ PDA;
(2) adding the W @ PDA obtained in the step (1) into a gadolinium nitrate solution, stirring, filtering, and calcining at high temperature to obtain W @ Gd of a core-shell structure 2 O 3 Powder;
(3) enabling the core-shell structure W @ Gd obtained in the step (2) 2 O 3 Sequentially adding the powder and the dried PP master batch into a feed port of a screw extruder to obtain the core-shell structure W @ Gd 2 O 3 /PP blending melt, cooling in air and performing brittle fracture granulation;
(4) adding the dried blended particles obtained in the step (3) into a feed port of a screw extruder, and drawing the extruded melt by a drawing and winding device to prepare composite fibers;
(5) adding paper pulp into a beaker filled with deionized water, and uniformly stirring to obtain a paper pulp suspension;
(6) shearing the composite fiber obtained in the step (4) into short fibers, and adding the short fibers into a wall breaking machine filled with deionized water to break up all the fibers to obtain a fiber suspension;
(7) adding the pulp suspension obtained in the step (5) into the fiber suspension obtained in the step (6), and scattering until the fibers and the pulp are uniformly mixed and dispersed;
(8) pouring the mixed suspension obtained in the step (7) into a vacuum filtration device for filtration to obtain a wet-process formed felt;
(9) putting the felt obtained in the step (8) into a heating type manual tablet press for hot pressing to obtain a pressed sheet material, and drying to obtain a composite non-woven material;
(10) the concentration of the dopamine salt solution in the step (1) is 1.5g/L-2.5 g/L;
(11) the concentration of the gadolinium nitrate solution in the step (2) is 0.3-0.5M/L.
2. The method for preparing a nonwoven fabric for X-and y-ray protection according to claim 1, wherein the buffer is added to adjust the pH in step (1), wherein the buffer is tris and the pH is 8 to 9.
3. The method of claim 1, wherein the tungsten powder in step (1) is tungsten powder cleaned with ethanol.
4. The method for preparing a nonwoven fabric for X-and gamma-ray protection according to claim 1, wherein the stirring in step (1) is carried out with an electric stirrer for 18 to 24 hours.
5. The method for preparing a nonwoven fabric for X-and y-ray protection according to claim 1, wherein the washing in step (1) is performed by washing with deionized water and ethanol 2 to 3 times, respectively.
6. The method for preparing the non-woven fabric for X and gamma ray protection as claimed in claim 1, wherein in the step (2), the high temperature calcination temperature is 800-1000 ℃, the time is 2-3h, and the temperature rise rate is 2-4 ℃/min.
7. The method for producing a nonwoven fabric for X-ray and gamma-ray protection according to claim 1, wherein the calcination in the step (2) is carried out in a protective gas which is an inert gas.
8. The method for preparing the non-woven fabric for X-ray and gamma-ray protection according to claim 1, wherein the PP master batch in the step (3) is dried in an oven at 40-60 ℃ for 30-60 min.
9. The method for preparing a nonwoven fabric for X-and gamma-ray protection according to claim 1, wherein the screw extruder in the step (3) has an extrusion temperature of 100 ℃ and a screw rotation speed of 15 r/min.
10. The method for preparing a nonwoven fabric for X-and gamma-ray protection according to claim 1, wherein the blended particles in step (4) are dried in an oven at 40-60 ℃ for 30-60 min.
11. The method for preparing a nonwoven fabric for X, γ ray protection according to claim 1, wherein in the screw extruder of step (4), the temperature of the screw zone is 100 ℃, the screw rotation speed is 20r/min, the temperature of the spinneret orifice is 85 ℃, the extrusion speed is as follows: 7-8 mm/min, and the aperture of a spinneret orifice is 2 mm.
12. The method for preparing a nonwoven fabric for X-ray and gamma-ray protection according to claim 1, wherein the drawing speed of the drawing and winding device in the step (4) is 150 r/min.
13. The method of claim 1, wherein the pulp in step (5) is 50ml of deionized water, and the amount of pulp added is 3 wt.%.
14. The method of claim 1, wherein the magnetic stirring is performed at 80r/min for 5min, and then the stirring is performed at 40r/min for 20 min.
15. The method of claim 1, wherein the short fibers in step (6) have a length of 1 to 3 mm.
16. The method for preparing the nonwoven fabric for X and gamma ray protection as claimed in claim 1, wherein the breaking machine is broken up in step (6), the breaking machine is filled with 800ml of deionized water, and the breaking is suspended for 30s at a low speed every 1min, and repeated 10 times.
17. The method for preparing nonwoven fabric for X, γ ray protection as claimed in claim 1, wherein the breaking machine breaks up in step (7), pauses for 30s for 1min at low speed, repeats 10 times.
18. The method of claim 1, wherein the felt in step (8) has a diameter of 15 cm.
19. The method of preparing a non-woven fabric for X-ray and gamma-ray protection according to claim 1, wherein in the step (9) of the heating type manual tablet press, the calendering temperature of the upper and lower plates is set to 60 ℃, and the upper and lower plates are hot-pressed at 15000Pa for 1min, then at 20000Pa for 1min, then at 25000Pa for 30s, and finally at 27500Pa for 30 s.
20. The method for preparing a nonwoven fabric for X-and gamma-ray protection according to claim 1, wherein the drying in step (9) is carried out in an oven at 40-60 ℃ for 30-60 min.
21. The method for producing a nonwoven fabric for X-ray and gamma-ray protection according to any one of claims 1 to 20, comprising the steps of:
(1) preparing 1.5g/L-2.5g/L dopamine salt solution, adding tris buffer solution to adjust the pH value to 8-9, then adding tungsten powder cleaned by ethanol, stirring for 18-24h by using an electric stirrer, filtering and separating, washing for 2-3 times by using deionized water and ethanol respectively, and drying to obtain W @ PDA;
(2) adding the W @ PDA obtained in the step (1) into gadolinium nitrate solution with the concentration of 0.3-0.5M/L, magnetically stirring for a certain time, filtering, separating, drying, introducing nitrogen into the prepared sample at the temperature of 800- 2 O 3 Powder;
(3) enabling the core-shell structure W @ Gd obtained in the step (2) 2 O 3 Sequentially adding the powder and the dried PP master batch into a feed port of a screw extruder, wherein the extrusion temperature is 100 ℃, and the screw rotation speed is 15r/min, so as to obtain the core-shell structure W @ Gd 2 O 3 the/PP blending melt is cooled in the air and subjected to brittle fracture granulation;
(4) adding the dried blended particles obtained in the step (3) into a feed inlet of a screw extruder, wherein the temperature of a screw zone is 100 ℃, the rotating speed of the screw is 20r/min, the temperature of a spinneret orifice is 85 ℃, and the extrusion speed is as follows: 7-8 mm/min, the aperture of a spinneret orifice is 2mm, and then the extruded melt is drawn by a drawing and winding device at a drawing speed of 150r/min to prepare composite fibers;
(5) adding paper pulp into a beaker filled with 50ml of deionized water, keeping the adding amount of the paper pulp of 3 wt.%, magnetically stirring for 5min at the speed of 80r/min, and then stirring for 20min at the speed of 40r/min to obtain uniform paper pulp suspension;
(6) shearing the composite fiber obtained in the step (4) into short fibers with the length of 1-3 mm, adding the short fibers into a wall breaking machine filled with 800mL of deionized water, pausing for 30s every 1min at low speed, and repeating for 10 times until all the fibers are broken up to obtain a fiber suspension;
(7) adding the pulp suspension obtained in the step (5) into the fiber suspension obtained in the step (6), pausing for 30s at low speed every 1min, and repeating for 10 times until the fibers and the pulp are uniformly mixed and dispersed;
(8) pouring the mixed suspension obtained in the step (7) into a vacuum filtration device for filtration to obtain a wet-process formed felt with the diameter of 15 cm;
(9) putting the felt obtained in the step (8) into a heating type manual tablet press for hot pressing, wherein the calendering temperature of the upper plate and the lower plate of the hot press is set as follows: and (2) when the temperature of the upper plate and the lower plate is stabilized at 60 ℃, putting the felt between two heating and pressurizing plates of a heating type manual tablet press, carrying out hot pressing at 15000Pa for 1min, then carrying out hot pressing at 20000Pa for 1min, then carrying out hot pressing at 25000Pa for 30s, finally carrying out hot pressing at 27500Pa for 30s, and then putting the obtained pressing sheet material in an oven at 40-60 ℃ for drying for 30-60min to obtain the composite non-woven material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110170798.4A CN112900155B (en) | 2021-02-08 | 2021-02-08 | Preparation method of non-woven fabric for X and gamma ray protection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110170798.4A CN112900155B (en) | 2021-02-08 | 2021-02-08 | Preparation method of non-woven fabric for X and gamma ray protection |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112900155A CN112900155A (en) | 2021-06-04 |
| CN112900155B true CN112900155B (en) | 2022-08-30 |
Family
ID=76123976
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110170798.4A Active CN112900155B (en) | 2021-02-08 | 2021-02-08 | Preparation method of non-woven fabric for X and gamma ray protection |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112900155B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112831855B (en) * | 2021-02-08 | 2022-05-31 | 南通大学 | Preparation method of core-shell structure tungsten/gadolinium oxide functional fiber for X, gamma ray protection |
| CN112831078B (en) * | 2021-02-08 | 2022-08-16 | 南通大学 | Preparation method of core-shell structure tungsten/gadolinium oxide PVC (polyvinyl chloride) calendered material for X and gamma ray protection |
| CN112846173A (en) * | 2021-02-08 | 2021-05-28 | 南通大学 | Preparation method of core-shell structure tungsten/gadolinium oxide powder for X, gamma ray protection |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6608319B2 (en) * | 2001-06-08 | 2003-08-19 | Adrian Joseph | Flexible amorphous composition for high level radiation and environmental protection |
| DE10340124A1 (en) * | 2002-12-17 | 2004-07-01 | Bayer Ag | Lead-free mixture as a radiation protection additive |
| KR20100047510A (en) * | 2008-10-29 | 2010-05-10 | 한국원자력연구원 | Radiation shielding members including nano-particles as a radiation shielding materials and preparation method thereof |
| CN104532381B (en) * | 2014-12-21 | 2016-11-23 | 北京服装学院 | A kind of preparation method of X-ray-preventing rare earth/polypropylene composite materials fiber |
| CN108411492B (en) * | 2018-03-08 | 2020-06-30 | 南通大学 | Preparation method of non-woven fabric for X and gamma ray protection |
| CN111250697B (en) * | 2020-02-18 | 2022-03-29 | 太原理工大学 | Preparation method of gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material |
| CN111469506A (en) * | 2020-03-17 | 2020-07-31 | 江苏丽洋新材料股份有限公司 | Novel nuclear radiation protection material and preparation method thereof |
-
2021
- 2021-02-08 CN CN202110170798.4A patent/CN112900155B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN112900155A (en) | 2021-06-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112900155B (en) | Preparation method of non-woven fabric for X and gamma ray protection | |
| CN112831855B (en) | Preparation method of core-shell structure tungsten/gadolinium oxide functional fiber for X, gamma ray protection | |
| WO2022166142A1 (en) | PREPARATION METHOD FOR CORE-SHELL STRUCTURE TUNGSTEN/GADOLINIUM OXIDE PVC CALENDERED MATERIAL FOR X-RAY AND γ-RAY PROTECTION | |
| CN112900110B (en) | Preparation method of core-shell structure tungsten/gadolinium oxide PU coating fabric for X, gamma ray protection | |
| CN110936676A (en) | Filter layer body for efficient dust mask | |
| WO2022166152A1 (en) | PREPARATION METHOD FOR CORE-SHELL STRUCTURED TUNGSTEN/GADOLINIUM OXIDE POWDER FOR X AND γ RAY PROTECTION | |
| CN108411492B (en) | Preparation method of non-woven fabric for X and gamma ray protection | |
| CN108147457A (en) | Prepare the application of the method and bismuth system oxide nanometer sheet of bismuth system oxide nanometer sheet | |
| CN109428035A (en) | Battery diaphragm and preparation method thereof and lithium ion battery | |
| CN104120501A (en) | Production method of negative ion BCF fiber and application of fiber to carpets | |
| CN107349681A (en) | A kind of water process environment-friendly antibacterial fire-resistant antistatic filter cloth | |
| JPS6130045B2 (en) | ||
| CN108771981A (en) | Graphene composite material and its preparation method and application, graphene-carbon nano-fiber film and preparation method thereof | |
| CN102242407B (en) | Method for preparing silicon oxide/silver nano composite fibers | |
| CN112756617A (en) | Preparation method of flake silver powder for conductive silver adhesive | |
| CN104064783A (en) | Preparation method of magnetic conductive nanofiber membrane for anode of microbial fuel cell | |
| CN104872865B (en) | A kind of production method of biodegradable environmental protection anti-dust respirator nanometer filter core | |
| CN104087777B (en) | Method for preparing particle dispersion reinforced metal matrix composite material | |
| CN112647189A (en) | Antibacterial melt-blown fabric and preparation process thereof | |
| CN110257957A (en) | A kind of molybdic acid vanadium sodium nanofiber and preparation method thereof | |
| CN112920508B (en) | Polypropylene electret master batch with high dielectric constant and preparation method thereof | |
| CN108505388B (en) | Adjustable mixed nano-fibril filter paper and preparation method and application thereof | |
| CN107162038A (en) | A kind of cuprous oxide powder and preparation method thereof | |
| CN109133822A (en) | A kind of combined oxidation magnesium-based curing agent, preparation method and application | |
| CN115467091B (en) | Bismuth oxide/gadolinium oxide nanofiber membrane alternately-stacked composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |