CN107446315A - A kind of preparation method of Composite anti-radiation material - Google Patents
A kind of preparation method of Composite anti-radiation material Download PDFInfo
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- CN107446315A CN107446315A CN201710838074.6A CN201710838074A CN107446315A CN 107446315 A CN107446315 A CN 107446315A CN 201710838074 A CN201710838074 A CN 201710838074A CN 107446315 A CN107446315 A CN 107446315A
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
- C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
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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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention provides a kind of preparation method of Composite anti-radiation material, comprise the following steps：（1）Para aminophenol three glycidyl epoxy resin, bisphenol A type epoxy resin and glycolylurea epoxide resin are mixed, heating water bath obtains mixture A；（2）By nano-cerium oxide, hafnium oxide, nano oxidized samarium, nano barium sulfate and graphene oxide mixing and ball milling；（3）Add ethylene double stearic hard acid amides, Tissuemat E and acetone, ultrasonic disperse；（4）Lecithin, VTES and 3 aminopropyl trimethoxysilanes are added, continue ultrasonic disperse, add mixing A, heating makes acetone volatilization complete；（5）Room temperature is down to, adds methyl tetrahydro phthalic anhydride and the stirring of the monooctyl ester of trimellitic acid three；（6）Mold cured is poured the mixture into produce.The preparation method of this Composite anti-radiation material, prepared material have good mechanical property, while have the shielding property of brilliance, have good protection effect to radiation.
Description
Technical field
The present invention relates to a kind of preparation method of Composite anti-radiation material.
Background technology
With the economic fast development with science and technology, electronic information technology turns into a special kind of skill that people be unable to do without, given people
The life of class brings huge change, there is provided huge facility.But meanwhile radiation also becomes caused by electronic equipment
The mind disease of people, it has also become come the fourth-largest public hazards after atmosphere pollution, water pollution, noise pollution.What radiation referred to
It is that part disengaging field source is distally propagated in the electromagnetic energy gone out by field source, then returns again to the phenomenon of field source, we are usual
" radiation " said is primarily referred to as high-energy electromagnetic radiation and particle radiation.Research shows that electromagnetic radiation causes leukemia of children
One of reason, the reproductive system of people is influenceed, cause children's intelligence incomplete, while the cardiovascular system of people can be influenceed, people is regarded
Feel system produces harmful effect, and can induce human cancer cell's propagation.Therefore, radiation proof material is researched and developed for protecting human body
Health has urgent meaning.
The content of the invention
Technical problems to be solved：It is made it is an object of the invention to provide a kind of preparation method of Composite anti-radiation material
Standby material has good mechanical property, while has the shielding property of brilliance, has good protection effect to radiation.
Technical scheme：A kind of preparation method of Composite anti-radiation material, comprises the following steps：
（1）By 10-15 parts para aminophenol three glycidyl epoxy resin, 10-15 parts bisphenol A type epoxy resin and 20-30
Part glycolylurea epoxide resin mixing, is put into water-bath and is heated to 80-100 DEG C, obtain mixture A；
（2）By 15-25 parts nano-cerium oxide, 5-10 parts hafnium oxide, the nano oxidized samarium of 15-25 parts, 5-10 part nano barium sulfates
Mixed with 1-2 parts graphene oxide, be put into progress ball milling 2-4 hours in ball mill；
（3）1-2 parts ethylene double stearic hard acid amides, 1-2 parts Tissuemat E and 20-40 part acetone are added, ultrasound is carried out with Ultrasound Instrument
Scattered 5-10 minutes；
（4）1-3 parts lecithin, 2-5 parts VTES and 1-2 part 3- aminopropyl trimethoxysilanes are added, after
Continuous ultrasonic disperse 5-10 minutes, mixing A is added, stirring is complete to acetone volatilization at 70-80 DEG C；
（5）Room temperature is down to, adds 0.4-0.7 parts methyl tetrahydro phthalic anhydride and the monooctyl ester of 0.8-1.2 parts trimellitic acid three, stirs 10-
20 minutes；
（6）Pour the mixture into mould, be put into vacuum drying chamber, at 45-55 DEG C of temperature solidification 4-6 hours produce.
It is further preferred that step（1）In be heated to 90 DEG C.
It is further preferred that step（2）Middle Ball-milling Time is 3-3.5 hours.
It is further preferred that step（3）Middle ultrasonic time is 6-9 minutes.
It is further preferred that step（4）Middle ultrasonic time is 6-9 minutes, and temperature is 75 DEG C.
It is further preferred that step（5）Middle mixing time is 15 minutes.
It is further preferred that step（6）Middle temperature is 50 DEG C, and hardening time is 4.5-5.5 hours.
Beneficial effect：With the Composite anti-radiation material prepared by the present invention, there is good mechanical property, its tensile strength
53.2MPa and 35.1MPa have been respectively reached with bending strength highest, while there is the shielding property of brilliance, to 79.9keV's
Gamma-ray protection ratio has been up to -99.6%, and linear attenuation coefficient has also reached 6.65cm2/ g, have to radiation fine
Protection effect.
Embodiment
Embodiment 1
A kind of preparation method of Composite anti-radiation material, comprises the following steps：
（1）By 10 parts of para aminophenol three glycidyl epoxy resins, 10 parts of bisphenol A type epoxy resins and 20 parts of glycolylurea rings
Oxygen tree fat mixes, and is put into water-bath and is heated to 80 DEG C, obtains mixture A；
（2）By 15 parts of nano-cerium oxides, 5 parts of hafnium oxides, 15 parts of nano oxidized samariums, 5 parts of nano barium sulfates and 1 part of oxidation stone
Black alkene mixing, it is put into ball mill and carries out ball milling 2 hours；
（3）1 part of ethylene double stearic hard acid amides, 1 part of Tissuemat E and 20 parts of acetone are added, ultrasonic disperse 5 is carried out with Ultrasound Instrument and divides
Clock；
（4）1 part of lecithin, 2 parts of VTESs and 1 part of 3- aminopropyl trimethoxysilane are added, continues ultrasound
It is scattered 5 minutes, mixing A is added, stirring is complete to acetone volatilization at 70 DEG C；
（5）Room temperature is down to, adds 0.4 part of methyl tetrahydro phthalic anhydride and 0.8 part of monooctyl ester of trimellitic acid three, is stirred 10 minutes；
（6）Mould is poured the mixture into, is put into vacuum drying chamber, solidifies 6 hours under temperature 45 C and produces.
Embodiment 2
A kind of preparation method of Composite anti-radiation material, comprises the following steps：
（1）By 11 parts of para aminophenol three glycidyl epoxy resins, 11 parts of bisphenol A type epoxy resins and 22 parts of glycolylurea rings
Oxygen tree fat mixes, and is put into water-bath and is heated to 85 DEG C, obtains mixture A；
（2）By 17 parts of nano-cerium oxides, 6 parts of hafnium oxides, 18 parts of nano oxidized samariums, 6 parts of nano barium sulfates and 1.5 parts of oxidations
Graphene mixes, and is put into ball mill and carries out ball milling 2.5 hours；
（3）1.5 parts of ethylenes double stearic hard acid amides, 1.5 parts of Tissuemat Es and 25 parts of acetone are added, ultrasound point is carried out with Ultrasound Instrument
Dissipate 6 minutes；
（4）1.5 parts of lecithin, 3 parts of VTESs and 1.5 parts of 3- aminopropyl trimethoxysilanes are added, are continued
Ultrasonic disperse 7 minutes, mixing A is added, stirring is complete to acetone volatilization at 75 DEG C；
（5）Room temperature is down to, adds 0.5 part of methyl tetrahydro phthalic anhydride and 0.9 part of monooctyl ester of trimellitic acid three, is stirred 13 minutes；
（6）Mould is poured the mixture into, is put into vacuum drying chamber, solidifies 5.5 hours under temperature 50 C and produces.
Embodiment 3
A kind of preparation method of Composite anti-radiation material, comprises the following steps：
（1）By 12.5 parts of para aminophenol three glycidyl epoxy resins, 12.5 parts of bisphenol A type epoxy resins and 25 parts of seas
Because epoxy resin mixes, it is put into water-bath and is heated to 90 DEG C, obtain mixture A；
（2）By 20 parts of nano-cerium oxides, 7.5 parts of hafnium oxides, 20 parts of nano oxidized samariums, 7.5 parts of nano barium sulfates and 1.5 parts
Graphene oxide mixes, and is put into ball mill and carries out ball milling 3 hours；
（3）1.5 parts of ethylenes double stearic hard acid amides, 1.5 parts of Tissuemat Es and 30 parts of acetone are added, ultrasound point is carried out with Ultrasound Instrument
Dissipate 7 minutes；
（4）2 parts of lecithin, 3.5 parts of VTESs and 1.5 parts of 3- aminopropyl trimethoxysilanes are added, are continued
Ultrasonic disperse 7 minutes, mixing A is added, stirring is complete to acetone volatilization at 75 DEG C；
（5）Room temperature is down to, adds 0.55 part of methyl tetrahydro phthalic anhydride and 1 part of monooctyl ester of trimellitic acid three, is stirred 15 minutes；
（6）Mould is poured the mixture into, is put into vacuum drying chamber, solidifies 5 hours under temperature 50 C and produces.
Embodiment 4
A kind of preparation method of Composite anti-radiation material, comprises the following steps：
（1）By 14 parts of para aminophenol three glycidyl epoxy resins, 14 parts of bisphenol A type epoxy resins and 28 parts of glycolylurea rings
Oxygen tree fat mixes, and is put into water-bath and is heated to 95 DEG C, obtains mixture A；
（2）By 22 parts of nano-cerium oxides, 9 parts of hafnium oxides, 22 parts of nano oxidized samariums, 8 parts of nano barium sulfates and 1.5 parts of oxidations
Graphene mixes, and is put into ball mill and carries out ball milling 3.5 hours；
（3）1.5 parts of ethylenes double stearic hard acid amides, 1.5 parts of Tissuemat Es and 35 parts of acetone are added, ultrasound point is carried out with Ultrasound Instrument
Dissipate 9 minutes；
（4）2.5 parts of lecithin, 4 parts of VTESs and 1.5 parts of 3- aminopropyl trimethoxysilanes are added, are continued
Ultrasonic disperse 9 minutes, mixing A is added, stirring is complete to acetone volatilization at 75 DEG C；
（5）Room temperature is down to, adds 0.6 part of methyl tetrahydro phthalic anhydride and 1.1 parts of monooctyl esters of trimellitic acid three, is stirred 18 minutes；
（6）Mould is poured the mixture into, is put into vacuum drying chamber, solidifies 5 hours under temperature 50 C and produces.
Embodiment 5
A kind of preparation method of Composite anti-radiation material, comprises the following steps：
（1）By 15 parts of para aminophenol three glycidyl epoxy resins, 15 parts of bisphenol A type epoxy resins and 30 parts of glycolylurea rings
Oxygen tree fat mixes, and is put into water-bath and is heated to 100 DEG C, obtains mixture A；
（2）By 25 parts of nano-cerium oxides, 10 parts of hafnium oxides, 25 parts of nano oxidized samariums, 10 parts of nano barium sulfates and 2 parts of oxidations
Graphene mixes, and is put into ball mill and carries out ball milling 4 hours；
（3）2 parts of ethylenes double stearic hard acid amides, 2 parts of Tissuemat Es and 40 parts of acetone are added, ultrasonic disperse 10 is carried out with Ultrasound Instrument
Minute；
（4）3 parts of lecithin, 5 parts of VTESs and 2 parts of 3- aminopropyl trimethoxysilanes are added, continue ultrasound
It is scattered 10 minutes, mixing A is added, stirring is complete to acetone volatilization at 80 DEG C；
（5）Room temperature is down to, adds 0.7 part of methyl tetrahydro phthalic anhydride and 1.2 parts of monooctyl esters of trimellitic acid three, is stirred 20 minutes；
（6）Mould is poured the mixture into, is put into vacuum drying chamber, solidifies 4 hours at 55 DEG C of temperature and produces.
Comparative example 1
A kind of preparation method of Composite anti-radiation material, comprises the following steps：
（1）By 10 parts of para aminophenol three glycidyl epoxy resins, 10 parts of bisphenol A type epoxy resins and 20 parts of glycolylurea rings
Oxygen tree fat mixes, and is put into water-bath and is heated to 80 DEG C, obtains mixture A；
（2）20 parts of nano-cerium oxides, 20 parts of nano oxidized samariums and 1 part of graphene oxide are mixed, is put into ball mill and carries out ball
Mill 2 hours；
（3）1 part of ethylene double stearic hard acid amides, 1 part of Tissuemat E and 20 parts of acetone are added, ultrasonic disperse 5 is carried out with Ultrasound Instrument and divides
Clock；
（4）1 part of lecithin, 2 parts of VTESs and 1 part of 3- aminopropyl trimethoxysilane are added, continues ultrasound
It is scattered 5 minutes, mixing A is added, stirring is complete to acetone volatilization at 70 DEG C；
（5）Room temperature is down to, adds 0.4 part of methyl tetrahydro phthalic anhydride and 0.8 part of monooctyl ester of trimellitic acid three, is stirred 10 minutes；
（6）Mould is poured the mixture into, is put into vacuum drying chamber, solidifies 6 hours under temperature 45 C and produces.
Comparative example 2
A kind of preparation method of Composite anti-radiation material, comprises the following steps：
（1）20 parts of para aminophenol three glycidyl epoxy resins and 20 parts of bisphenol A type epoxy resins are mixed, are put into water
80 DEG C are heated in bath, obtains mixture A；
（2）By 15 parts of nano-cerium oxides, 5 parts of hafnium oxides, 15 parts of nano oxidized samariums, 5 parts of nano barium sulfates and 1 part of oxidation stone
Black alkene mixing, it is put into ball mill and carries out ball milling 2 hours；
（3）1 part of ethylene double stearic hard acid amides, 1 part of Tissuemat E and 20 parts of acetone are added, ultrasonic disperse 5 is carried out with Ultrasound Instrument and divides
Clock；
（4）1 part of lecithin, 2 parts of VTESs and 1 part of 3- aminopropyl trimethoxysilane are added, continues ultrasound
It is scattered 5 minutes, mixing A is added, stirring is complete to acetone volatilization at 70 DEG C；
（5）Room temperature is down to, adds 0.4 part of methyl tetrahydro phthalic anhydride and 0.8 part of monooctyl ester of trimellitic acid three, is stirred 10 minutes；
（6）Mould is poured the mixture into, is put into vacuum drying chamber, solidifies 6 hours under temperature 45 C and produces.
Tensile strength is measured using GB/T 9340-92 standards.
Bending strength is measured using national standard GB/T 19885-2005.
Protection ratio and linear attenuation coefficient are determined on NaI gamma ray spectrometers.
Each embodiment is compared with comparative example, comparing result is as shown in the table, it may be seen that the present invention thick 1cm
Material has good mechanical property, and its tensile strength and bending strength highest have respectively reached 53.2MPa and 35.1MPa, together
When with brilliance shielding property, -99.6% has been up to 79.9keV gamma-ray protection ratio, linear attenuation system
Number has also reached 6.65cm2/ g, there is good protection effect to radiation.
The partial properties index of the Composite anti-radiation material of table 1
| Name of product | Tensile strength（MPa） | Bending strength（MPa） | Protection ratio（%） | Linear attenuation coefficient（cm2/g） |
| Embodiment 1 | 52.3 | 34.5 | -98.7 | 6.52 |
| Embodiment 2 | 52.8 | 34.7 | -98.9 | 6.55 |
| Embodiment 3 | 52.6 | 35.1 | -99.4 | 6.59 |
| Embodiment 4 | 53.2 | 34.5 | -99.6 | 6.65 |
| Embodiment 5 | 53.1 | 34.8 | -98.9 | 6.61 |
| Comparative example 1 | 52.3 | 32.8 | -98.6 | 5.14 |
| Comparative example 2 | 45.6 | 31.6 | -93.8 | 5.38 |
Claims (7)
- A kind of 1. preparation method of Composite anti-radiation material, it is characterised in that：Comprise the following steps：（1）By 10-15 parts para aminophenol three glycidyl epoxy resin, 10-15 parts bisphenol A type epoxy resin and 20-30 Part glycolylurea epoxide resin mixing, is put into water-bath and is heated to 80-100 DEG C, obtain mixture A；（2）By 15-25 parts nano-cerium oxide, 5-10 parts hafnium oxide, the nano oxidized samarium of 15-25 parts, 5-10 part nano barium sulfates Mixed with 1-2 parts graphene oxide, be put into progress ball milling 2-4 hours in ball mill；（3）1-2 parts ethylene double stearic hard acid amides, 1-2 parts Tissuemat E and 20-40 part acetone are added, ultrasound is carried out with Ultrasound Instrument Scattered 5-10 minutes；（4）1-3 parts lecithin, 2-5 parts VTES and 1-2 part 3- aminopropyl trimethoxysilanes are added, after Continuous ultrasonic disperse 5-10 minutes, mixing A is added, stirring is complete to acetone volatilization at 70-80 DEG C；（5）Room temperature is down to, adds 0.4-0.7 parts methyl tetrahydro phthalic anhydride and the monooctyl ester of 0.8-1.2 parts trimellitic acid three, stirs 10- 20 minutes；（6）Pour the mixture into mould, be put into vacuum drying chamber, at 45-55 DEG C of temperature solidification 4-6 hours produce.
- A kind of 2. preparation method of Composite anti-radiation material according to claim 1, it is characterised in that：The step（1） In be heated to 90 DEG C.
- A kind of 3. preparation method of Composite anti-radiation material according to claim 1, it is characterised in that：The step（2） Middle Ball-milling Time is 3-3.5 hours.
- A kind of 4. preparation method of Composite anti-radiation material according to claim 1, it is characterised in that：The step（3） Middle ultrasonic time is 6-9 minutes.
- A kind of 5. preparation method of Composite anti-radiation material according to claim 1, it is characterised in that：The step（4） Middle ultrasonic time is 6-9 minutes, and temperature is 75 DEG C.
- A kind of 6. preparation method of Composite anti-radiation material according to claim 1, it is characterised in that：The step（5） Middle mixing time is 15 minutes.
- A kind of 7. preparation method of Composite anti-radiation material according to claim 1, it is characterised in that：The step（6） Middle temperature is 50 DEG C, and hardening time is 4.5-5.5 hours.
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| CN108178900A (en) * | 2017-12-22 | 2018-06-19 | 中航复合材料有限责任公司 | It can collapse and be unfolded the preparation method of composite material support bar epoxy resin-base |
| CN108411492A (en) * | 2018-03-08 | 2018-08-17 | 南通大学 | A kind of preparation method of X, gamma-rays protection non-woven fabrics |
| CN108411618A (en) * | 2018-03-08 | 2018-08-17 | 南通大学 | A kind of preparation method of X, gamma-rays protective fabric |
| CN109401206A (en) * | 2018-12-24 | 2019-03-01 | 张冬生 | A kind of Epocryl base shielding material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108178900A (en) * | 2017-12-22 | 2018-06-19 | 中航复合材料有限责任公司 | It can collapse and be unfolded the preparation method of composite material support bar epoxy resin-base |
| CN108411492A (en) * | 2018-03-08 | 2018-08-17 | 南通大学 | A kind of preparation method of X, gamma-rays protection non-woven fabrics |
| CN108411618A (en) * | 2018-03-08 | 2018-08-17 | 南通大学 | A kind of preparation method of X, gamma-rays protective fabric |
| CN108411492B (en) * | 2018-03-08 | 2020-06-30 | 南通大学 | Preparation method of non-woven fabric for X and gamma ray protection |
| CN109401206A (en) * | 2018-12-24 | 2019-03-01 | 张冬生 | A kind of Epocryl base shielding material |
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Application publication date: 20171208 |