CN116333432A - Anti-radiation protective material and preparation method and application thereof - Google Patents
Anti-radiation protective material and preparation method and application thereof Download PDFInfo
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- CN116333432A CN116333432A CN202310225254.2A CN202310225254A CN116333432A CN 116333432 A CN116333432 A CN 116333432A CN 202310225254 A CN202310225254 A CN 202310225254A CN 116333432 A CN116333432 A CN 116333432A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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Abstract
The invention discloses a radiation protection material and a preparation method and application thereof, wherein lignin is taken as a raw material, firstly, the lignin is subjected to amination modification to obtain amino modified lignin, the amino modified lignin is covalently connected with generated barium sulfate to obtain an amino modified lignin/barium sulfate compound, the problem that barium sulfate particles are easy to agglomerate is solved, then the amino modified lignin/barium sulfate compound is utilized to chelate lanthanum ions, the loss of the lanthanum ions is effectively avoided through the chelation of functional groups, meanwhile, lanthanum ions are dispersed more uniformly, meanwhile, through the modification of basalt fibers, the modified basalt fibers and the modified lignin distributed around are connected into a network structure, radiation protection shielding bodies are formed inside the material, the radiation resistance of the material is greatly improved, and meanwhile, the modified basalt fibers and the modified lignin play a role in enhancing the mechanical properties of the material.
Description
Technical Field
The invention relates to the technical field of engineering materials, in particular to a radiation protection material and a preparation method and application thereof.
Background
In the medical inspection and treatment technology, radioactive instruments are used for inspecting and treating certain malignant diseases, the use of the radioactive instruments improves the diagnosis rate and the treatment rate of the diseases, but various rays are generated, the radiation of the rays can harm normal tissues, the incidence rate of various diseases such as malignant tumors, leukemia, degenerative nervous system diseases, cardiovascular diseases, genital system diseases and the like can be increased, and diseases such as organism cell mutation, hematopoietic function deficiency, cancer and the like can be caused, so that the radiation-proof material attracts great attention.
The existing radiation-proof materials can be divided into penetration-proof radiation materials and surface radiation-proof protective materials, and heavy metal materials such as lead, cadmium, steel and the like have good protective performance, but are difficult to be used for preparing radiation-proof products due to poor plasticity and high processing difficulty, and particularly have higher application difficulty in the field of flexible radiation-proof products; the surface radiation protection material is generally formed by coating or compounding a radiation protection layer on the surface of a product by a processing method, the processing method has complex process, and the radiation protection layer has the risk of wearing, falling and losing the radiation protection function; the existing radiation-proof material has poor compatibility with a matrix polymer material, and has great influence on the processing performance of products.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a radiation protection material, a preparation method and application thereof, and solves the technical problems that the existing radiation protection material has poor compatibility with a matrix polymer material and is difficult to process and mold.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the radiation protection material consists of the following raw materials in parts by weight: 40-60 parts of polyvinyl chloride, 10-20 parts of polystyrene, 15-25 parts of polyimide, 10-15 parts of modified lignin, 5-10 parts of modified basalt fiber, 0.5-1.5 parts of amino silicone oil and 1-2 parts of microcrystalline wax.
Preferably, the preparation method of the modified lignin comprises the following steps:
(1) Adding alkali lignin into deionized water, stirring uniformly, adding polyethyleneimine and epichlorohydrin, heating and stirring at 60-90 ℃ for reaction for 2-3h, and washing, drying and grinding reaction products after the reaction is completed to obtain amino modified lignin;
(2) Preparing barium chloride ethanol aqueous solution, adding amino modified lignin and stearic acid, performing ultrasonic dispersion uniformly, dropwise adding sodium sulfate aqueous solution into the solution under magnetic stirring, continuously stirring for 30-45min at 40-50 ℃, and then centrifuging, washing and drying the reaction product to obtain an amino modified lignin/barium sulfate compound;
(3) And (3) ultrasonically dispersing the amino modified lignin/barium sulfate compound in a lanthanum nitrate solution, oscillating and adsorbing for 3-5h at room temperature, and then filtering, washing and drying to obtain the modified lignin.
Preferably, in the step (1), the mass ratio of the alkali lignin, the polyethyleneimine and the epichlorohydrin is 6-12:5-8:3-6.
Preferably, in the step (2), the dosage ratio of the barium chloride ethanol aqueous solution, the amino modified lignin and the stearic acid is 100-150mL:8-12g:0.5-1g.
Preferably, in the step (2), the concentration of the barium chloride ethanol aqueous solution is 0.1-0.2mol/L.
Preferably, in step (2), the molar ratio of barium chloride to sodium sulfate is 1:1.
Preferably, in the step (3), the mass ratio of the amino modified lignin/barium sulfate compound to the lanthanum nitrate solution is 5-8:100, and the mass fraction of the lanthanum nitrate solution is 2-4%.
Preferably, the preparation method of the modified basalt fiber comprises the following steps: immersing basalt fiber into ethanol water solution containing silane coupling agent, stirring and reacting for 2-3h at 40-60 ℃, and then washing and drying to obtain modified basalt fiber.
The invention provides a preparation method of the radiation protection material, which comprises the following steps: uniformly mixing polyvinyl chloride, polystyrene, polyimide, modified lignin, modified basalt fiber, amino silicone oil and microcrystalline wax in a high-speed mixer according to parts by weight to obtain a mixed material, and adding the mixed material into a double-screw extruder for extrusion granulation to obtain the radiation protection material.
The invention also provides application of the radiation protection material in protective clothing, protective gloves and protective plates.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, lignin is taken as a raw material, the lignin is subjected to amination modification to obtain amino modified lignin, the amino modified lignin is covalently connected with generated barium sulfate to obtain an amino modified lignin/barium sulfate compound, the problem that barium sulfate particles are easy to agglomerate is solved, and then the amino modified lignin/barium sulfate compound is utilized to chelate lanthanum ions, so that the loss of the lanthanum ions is effectively avoided through the chelation of functional groups on the lanthanum ions, and meanwhile, the lanthanum ions are dispersed more uniformly.
(2) According to the invention, the basalt fiber is modified, the modified basalt fiber and the modified lignin distributed around are connected into a network structure, and the radiation-proof shielding body is formed in the material, so that the radiation resistance of the material is greatly improved, and meanwhile, the modified basalt fiber and the modified lignin play a role in enhancing the mechanical property of the material.
(3) The radiation protection material provided by the invention is easy to process and form, and has excellent radiation protection performance, mechanical property and plasticity.
Detailed Description
The present invention will be described in further detail with reference to the following preferred examples, but the present invention is not limited to the following examples.
Unless otherwise specified, the chemical reagents involved in the present invention are all commercially available.
The polyvinyl chloride used in the invention is purchased from Wuhan Xin dynamic benefit chemical industry Co., ltd;
polystyrene was purchased from Dongguan double-arm plastic limited, model: GP525;
polyimide is purchased from Dongguan medical super Rong plastic raw materials Co., ltd., trade mark: JGN3030;
alkali lignin is purchased from Nantong Runfeng petrochemical Co., ltd;
basalt fiber was purchased from the new technical institute of seven stars in martial arts with a fiber length of 6mm.
Example 1
A preparation method of a radiation protection material comprises the following steps:
mixing 40 parts of polyvinyl chloride, 10 parts of polystyrene, 15 parts of polyimide, 10 parts of modified lignin, 5 parts of modified basalt fiber, 0.5 part of amino silicone oil and 1 part of microcrystalline wax in a high-speed mixer for 30min to obtain a mixed material, and then adding the mixed material into a double-screw extruder for extrusion granulation to obtain the radiation protection material;
the preparation method of the modified lignin comprises the following steps:
(1) Adding 6g of alkali lignin into 250mL of deionized water, uniformly stirring, adding 5g of polyethyleneimine and 3g of epichlorohydrin, heating and stirring at 60 ℃ for reaction for 3 hours, and washing, drying and grinding a reaction product after the reaction is completed to obtain amino modified lignin;
(2) Preparing 100mL of 0.1mol/L barium chloride ethanol water solution, wherein the volume ratio of ethanol to water in the solution is 1:1, adding 8g of amino modified lignin and 0.5g of stearic acid, uniformly dispersing by ultrasonic, dropwise adding 100mL of 0.1mol/L sodium sulfate water solution under magnetic stirring, continuously stirring for 30min at 40 ℃, and centrifuging, washing and drying the reaction product to obtain an amino modified lignin/barium sulfate compound;
(3) Dispersing 5g of amino modified lignin/barium sulfate compound in 100g of 2wt% lanthanum nitrate solution by ultrasonic, oscillating and adsorbing for 3 hours at room temperature, and then filtering, washing and drying to obtain modified lignin;
the preparation method of the modified basalt fiber comprises the following steps: 10g basalt fiber is immersed into 150g of 2wt% silane coupling agent KH560 solution, the mass ratio of ethanol to water in the solution is 1:1, stirred and reacted for 3 hours at 40 ℃, and then washed and dried, thus obtaining the modified basalt fiber.
Example 2
A preparation method of a radiation protection material comprises the following steps:
60 parts of polyvinyl chloride, 20 parts of polystyrene, 25 parts of polyimide, 15 parts of modified lignin, 10 parts of modified basalt fiber, 1.5 parts of amino silicone oil and 2 parts of microcrystalline wax are mixed in a high-speed mixer for 30min to obtain a mixed material, and then the mixed material is added into a double-screw extruder for extrusion granulation to obtain the radiation protection material;
the preparation method of the modified lignin comprises the following steps:
(1) Adding 12g of alkali lignin into 250mL of deionized water, uniformly stirring, adding 8g of polyethyleneimine and 6g of epichlorohydrin, heating and stirring at 90 ℃ for reaction for 2 hours, and washing, drying and grinding a reaction product after the reaction is completed to obtain amino modified lignin;
(2) Preparing 150mL of 0.1mol/L barium chloride ethanol water solution, wherein the volume ratio of ethanol to water in the solution is 1:1, adding 12g of amino modified lignin and 1g of stearic acid, uniformly dispersing by ultrasonic, dropwise adding 150mL of 0.1mol/L sodium sulfate water solution under magnetic stirring, continuously stirring for 30min at 50 ℃, and centrifuging, washing and drying the reaction product to obtain an amino modified lignin/barium sulfate compound;
(3) Dispersing 8g of amino modified lignin/barium sulfate compound in 100g of 4wt% lanthanum nitrate solution by ultrasonic, oscillating and adsorbing for 5 hours at room temperature, and then filtering, washing and drying to obtain modified lignin;
the preparation method of the modified basalt fiber comprises the following steps: 10g basalt fiber is immersed into 150g of 3wt% silane coupling agent KH560 solution, the mass ratio of ethanol to water in the solution is 1:1, stirred and reacted for 2 hours at 60 ℃, and then washed and dried, thus obtaining the modified basalt fiber.
Example 3
A preparation method of a radiation protection material comprises the following steps:
mixing 50 parts of polyvinyl chloride, 15 parts of polystyrene, 20 parts of polyimide, 12 parts of modified lignin, 8 parts of modified basalt fiber, 1 part of amino silicone oil and 2 parts of microcrystalline wax in a high-speed mixer for 30min to obtain a mixed material, and then adding the mixed material into a double-screw extruder for extrusion granulation to obtain the radiation protection material;
the preparation method of the modified lignin comprises the following steps:
(1) Adding 10g of alkali lignin into 250mL of deionized water, uniformly stirring, adding 6g of polyethyleneimine and 5g of epichlorohydrin, heating and stirring at 80 ℃ for reaction for 3 hours, and washing, drying and grinding a reaction product after the reaction is completed to obtain amino modified lignin;
(2) Preparing 100mL of 0.1mol/L barium chloride ethanol water solution, wherein the volume ratio of ethanol to water in the solution is 1:1, adding 10g of amino modified lignin and 0.8g of stearic acid, uniformly dispersing by ultrasonic, dropwise adding 100mL of 0.1mol/L sodium sulfate water solution under magnetic stirring, continuously stirring for 45min at 40 ℃, and centrifuging, washing and drying the reaction product to obtain an amino modified lignin/barium sulfate compound;
(3) Dispersing 6g of amino modified lignin/barium sulfate compound in 100g of 3wt% lanthanum nitrate solution by ultrasonic, oscillating and adsorbing for 5 hours at room temperature, and then filtering, washing and drying to obtain modified lignin;
the preparation method of the modified basalt fiber comprises the following steps: 10g basalt fiber is immersed into 150g of 2wt% silane coupling agent KH560 solution, the mass ratio of ethanol to water in the solution is 1:1, stirred and reacted for 2 hours at 60 ℃, and then washed and dried, thus obtaining the modified basalt fiber.
Comparative example 1
A preparation method of a radiation protection material comprises the following steps:
50 parts of polyvinyl chloride, 15 parts of polystyrene, 20 parts of polyimide, 10 parts of lignin, 1.5 parts of barium sulfate, 0.5 part of lanthanum oxide, 8 parts of basalt fiber, 1 part of amino silicone oil and 2 parts of microcrystalline wax are mixed in a high-speed mixer for 30min to obtain a mixed material, and then the mixed material is added into a double-screw extruder to be extruded and granulated to obtain the radiation protection material.
Comparative example 2
A preparation method of a radiation protection material comprises the following steps:
50 parts of polyvinyl chloride, 15 parts of polystyrene, 20 parts of polyimide, 11.5 parts of modified lignin, 0.5 part of lanthanum oxide, 8 parts of modified basalt fiber, 1 part of amino silicone oil and 2 parts of microcrystalline wax are mixed in a high-speed mixer for 30min to obtain a mixed material, and then the mixed material is added into a double-screw extruder to be extruded and granulated to obtain the radiation protection material;
the preparation method of the modified lignin comprises the following steps:
(1) Adding 10g of alkali lignin into 250mL of deionized water, uniformly stirring, adding 6g of polyethyleneimine and 5g of epichlorohydrin, heating and stirring at 80 ℃ for reaction for 3 hours, and washing, drying and grinding a reaction product after the reaction is completed to obtain amino modified lignin;
(2) Preparing 100mL of 0.1mol/L barium chloride ethanol water solution, wherein the volume ratio of ethanol to water in the solution is 1:1, adding 10g of amino modified lignin and 0.8g of stearic acid, uniformly dispersing by ultrasonic, dropwise adding 100mL of 0.1mol/L sodium sulfate water solution under magnetic stirring, continuously stirring for 45min at 40 ℃, and centrifuging, washing and drying the reaction product to obtain modified lignin;
the preparation method of the modified basalt fiber comprises the following steps: 10g basalt fiber is immersed into 150g of 2wt% silane coupling agent KH560 solution, the mass ratio of ethanol to water in the solution is 1:1, stirred and reacted for 2 hours at 60 ℃, and then washed and dried, thus obtaining the modified basalt fiber.
The composites prepared in examples 1-3 and comparative examples 1-2 were subjected to performance testing as follows:
tensile strength test: testing according to GB/T1040-2006 standard;
bending strength test: testing according to GB/T9341-2008 standard;
x-ray shielding test: the thickness of the sample is 8mm, the voltage of the X-ray tube is 120kV, a 2.5mm aluminum sheet is adopted for filtration, and the result is characterized by lead millimeter equivalent; the test results are shown in the following table:
| example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| Tensile Strength (MPa) | 88 | 93 | 89 | 62 | 74 |
| Flexural Strength (MPa) | 93 | 97 | 96 | 71 | 80 |
| Specific lead equivalent (mmPb/mm) | 0.14 | 0.15 | 0.14 | 0.07 | 0.09 |
Finally, it should be noted that: the above examples are not intended to limit the present invention in any way. Modifications and improvements will readily occur to those skilled in the art upon the basis of the present invention. Accordingly, any modification or improvement made without departing from the spirit of the invention is within the scope of the invention as claimed.
Claims (10)
1. The radiation protection material is characterized by comprising the following raw materials in parts by weight: 40-60 parts of polyvinyl chloride, 10-20 parts of polystyrene, 15-25 parts of polyimide, 10-15 parts of modified lignin, 5-10 parts of modified basalt fiber, 0.5-1.5 parts of amino silicone oil and 1-2 parts of microcrystalline wax.
2. The radiation protection material of claim 1, wherein the method for preparing the modified lignin comprises the following steps:
(1) Adding alkali lignin into deionized water, stirring uniformly, adding polyethyleneimine and epichlorohydrin, heating and stirring at 60-90 ℃ for reaction for 2-3h, and washing, drying and grinding reaction products after the reaction is completed to obtain amino modified lignin;
(2) Preparing barium chloride ethanol aqueous solution, adding amino modified lignin and stearic acid, performing ultrasonic dispersion uniformly, dropwise adding sodium sulfate aqueous solution into the solution under magnetic stirring, continuously stirring for 30-45min at 40-50 ℃, and then centrifuging, washing and drying the reaction product to obtain an amino modified lignin/barium sulfate compound;
(3) And (3) ultrasonically dispersing the amino modified lignin/barium sulfate compound in a lanthanum nitrate solution, oscillating and adsorbing for 3-5h at room temperature, and then filtering, washing and drying to obtain the modified lignin.
3. The radiation protection material according to claim 2, wherein in the step (1), the mass ratio of the alkali lignin, the polyethyleneimine and the epichlorohydrin is 6-12:5-8:3-6.
4. The radiation protection material according to claim 2, wherein in the step (2), the dosage ratio of the barium chloride ethanol aqueous solution, the amino modified lignin and the stearic acid is 100-150mL:8-12g:0.5-1g.
5. The radiation protective material according to claim 2, wherein in the step (2), the concentration of the barium chloride ethanol aqueous solution is 0.1-0.2mol/L.
6. The radiation protective material according to claim 2, wherein in step (2), the molar ratio of barium chloride to sodium sulfate is 1:1.
7. The radiation protection material according to claim 2, wherein in the step (3), the mass ratio of the amino modified lignin/barium sulfate composite to the lanthanum nitrate solution is 5-8:100, and the mass fraction of the lanthanum nitrate solution is 2-4%.
8. The radiation protection material according to claim 1, wherein the preparation method of the modified basalt fiber comprises the following steps: immersing basalt fiber into ethanol water solution containing silane coupling agent, stirring and reacting for 2-3h at 40-60 ℃, and then washing and drying to obtain modified basalt fiber.
9. The method for preparing the radiation protection material according to any one of claims 1 to 8, comprising the steps of: uniformly mixing polyvinyl chloride, polystyrene, polyimide, modified lignin, modified basalt fiber, amino silicone oil and microcrystalline wax in a high-speed mixer according to parts by weight to obtain a mixed material, and adding the mixed material into a double-screw extruder for extrusion granulation to obtain the radiation protection material.
10. Use of the radiation protection material according to any one of claims 1-8 in protective clothing, gloves, panels.
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