CN104910629A - Flame-retardant flexible lead-free gamma shielding material and preparation method thereof - Google Patents
Flame-retardant flexible lead-free gamma shielding material and preparation method thereof Download PDFInfo
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- CN104910629A CN104910629A CN201510312771.9A CN201510312771A CN104910629A CN 104910629 A CN104910629 A CN 104910629A CN 201510312771 A CN201510312771 A CN 201510312771A CN 104910629 A CN104910629 A CN 104910629A
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Abstract
The invention discloses a flame-retardant flexible lead-free gamma shielding material which comprises the following components in parts by weight: 100 parts of high-temperature vulcanized silicone rubber, 250-400 parts of gamma shielding functional filler, 15.8-48 parts of flame-retardant functional filler, 0.5-1.5 parts of platinum vulcanizing agent component A, 1.5-3 parts of platinum vulcanizing agent component B and 1-5 parts of powder surface modifier. The gamma shielding functional filler is one or mixture of W, WO3, BaO and Gd2O3 in any ratio. The preparation method comprises the following steps: carrying out flexible high-polymer base material plastifying, carrying out functional filler surface modification, compounding with the functional filler powder, and carrying out tabletting and high-temperature normal-pressure molding to finally obtain the product. By using the high-temperature vulcanized silicone rubber as the matrix, the flame-retardant flexible lead-free gamma shielding material has the advantages of favorable flexibility, favorable flame retardancy, favorable mechanical strength and favorable gamma shielding property.
Description
Technical field
The invention belongs to nuclear radiation protection field, Shielding Materials for Nuclear Radiation preparing technical field, particularly relate to a kind of unleaded gamma shielding material of flexibility with flame retardant properties and preparation method thereof.
Background technology
Along with Application of Nuclear Technology plays more and more important effect in radiation processing, medical diagnosis and national defense and military etc., the number of practitioner also rises thereupon.But while bringing convenient and enjoyment, various ray also also brings harm to the mankind to a certain extent, therefore, reduce the occupational exposure level of practitioner in all kinds of radiological operations, ensure that the life and health of radioactivity practitioner is very important.
Tradition gamma-radiation protective material with plumbous rubber for main raw, weight is large, flexible poor, there is bio-toxicity and not there is flame retardant properties, as patent: CN 200510116946.5, CN 201310294900.7 etc., wherein relate to gamma-ray shielding material, and all containing plumbous in these materials, under the gamma shielding material therefore obtained by these methods can not meet nuclear incident condition, emergency personnel is for the requirement of shelter that may occur fire condition; Traditional plumbous rubber shielding material quality relatively firmly arbitrarily can not change, and not possess flame retardant properties with environment size, equipment profile, for nuclear equipment protected working brings certain difficulty and risk simultaneously.Therefore, develop a kind of unleaded gamma shielding material of flexibility with flame retardant properties, become the technical barrier that this area is urgently to be resolved hurrily.
Summary of the invention
For above-mentioned Problems existing, the object of the invention is to provide a kind of unleaded gamma shielding material of flexibility being matrix with high temperature vulcanized silica gel, and it has good snappiness, flame retardant properties, mechanical strength, and has good gamma shielding material.
In order to achieve the above object, the technical solution used in the present invention is as follows: a kind of unleaded gamma shielding material of flexibility with flame retardant properties, in described shielding material, the parts by weight of each component are as follows: 100 parts, high temperature vulcanized silica gel, gamma shielding functional stuffing 250 ~ 400 parts, anti-flaming function filler 15.8 ~ 48 parts, platinum vulcanizing agent A component 0.5 ~ 1.5 part, platinum vulcanizing agent B component 1.5 ~ 3 parts, powder surface modifier 1 ~ 5 part; Described gamma shielding functional stuffing is W, WO
3, BaO, Gd
2o
3in one or more mix with arbitrary proportion.
Anti-flaming function filler of the present invention is that one or more in aluminium hydroxide, magnesium hydroxide, zinc borate or red phosphorus mix with arbitrary proportion.Selected aluminium hydroxide, magnesium hydroxide, zinc borate inorganic combustion inhibitor can reduce the heat that flame sends by decomposes water vapour, reduce the production of inflammable gas; Red phosphorus can form phosphoric acid and absorb heat, and forms barrier film blocking-up air, to reach flame retardant effect at polymer surfaces.
Powder surface modifier of the present invention is coupling agent KH-540, aminopropyl trimethoxysilane, coupling agent D-90 wherein one or more mix with arbitrary proportion.Select powder modifier modifying powder surface structure can reduce powder agglomeration, improve the dispersiveness of powder in polymeric matrix.
The hardness of high temperature vulcanized silica gel of the present invention is 10HA.In order to ensure that final specimen material has good flexibility, therefore the silica gel that hardness is lower must be selected.Silica gel hardness value is larger, and final material softness degree is poorer.
Gamma shielding functional stuffing of the present invention, anti-flaming function packing material size are 2um ~ 15um.When the filler particles selected is less, easily form aggregate in process of production, reduce the mechanical property of specimen material, gamma shielding performance and flame retardant properties; When filler particles is larger, the gamma ray shielding performance of film sample can be reduced.
The preparation method with the flexibility unleaded gamma shielding material of flame retardant properties of the present invention: described preparation method comprises: flexible macromolecule body material plasticates → functional stuffing surface modification → with functional stuffing powder mixing → compressing tablet and high-temperature pressure shaping, its detailed preparation method is as follows:
1) the high temperature vulcanized silica gel adding respective quality in two roller mill is plasticated 5-10min, then adds platinum vulcanizing agent B component and to plasticate 10-15min, finally add platinum vulcanizing agent A component and continue the 10-15min that plasticates, obtain product of plasticating;
2) the gamma shielding functional stuffing of respective quality, anti-flaming function filler and powder surface modifier are mixed, obtain filler mixture, then the deionized water of filler mixture total mass 30% ~ 50% and the dehydrated alcohol of filler mixture total mass 5% ~ 10% is added, at 30-50 DEG C of temperature, react 1 ~ 1.5h, filter and obtain modified function filler mixture;
3) by plasticate product and step 2 that step 1) obtains) the modified function filler mixture that obtains adds in vacuum Banbury mixer, and banburying 20-30min at 105-115 DEG C of temperature, obtains silica gel based mixtures;
4) vulcanizing press upper and lower plates temperature is 50-80 DEG C, add the silica gel based mixtures compressing tablet de-bubble together with polyester separatory membrane step 3) obtained, then put into baking oven 150-170 DEG C of heating 8-15min, there is described in namely obtaining after cooling the unleaded gamma shielding material of flexibility of flame retardant properties.
In the operating process of step 1) of the present invention, two roller mill rotating speed is 45rpm, two roller spacing 2mm, working temperature 0-40 DEG C.
The invention has the advantages that: the gamma shielding material that the techniques such as the present invention is plasticated by silica gel and vulcanizing agent, functional stuffing surface modification, silica gel and functional stuffing are mixing, silica gel body material compressing tablet high-temperature pressure is shaping obtain, have good gamma ray shielding performance, the material that 1mm is thick is that the gamma-ray shielding rate of 59.6keV is up to 76.2% to energy;
In formula of the present invention with high temperature vulcanized silica gel for matrix, after the polymer material molding obtained, softness is easily curling; Can decomposition and crystallization water heat absorption or form heat insulation, the starvation of tectum when anti-flaming function filler composition is heated, there is higher flame retardant properties;
In addition, through detecting, this material also has higher mechanical strength and lifeless matter toxicity, can not only meet complex-shaped nuclear instrument equipment perimeter defense, is also good gamma-rays protective clothing core material.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Following examples are several embodiment of the present invention, basis is non-to be limited the scope of the present invention, in concrete operating process, gamma shielding functional stuffing powder can select one or more in W, WO3, BaO, Gd2O3, anti-flaming function filler powder can select aluminium hydroxide, magnesium hydroxide, zinc borate, red phosphorus wherein one or more, powder surface modifier one or more of selecting in coupling agent KH-540, coupling agent KH-550, aminopropyl trimethoxysilane, coupling agent D-90 optional, these change, and all can realize the object of the present invention.
embodiment 1:the unleaded gamma ray shielding material of flexibility with flame retardant properties of the present invention.
In described shielding material, the parts by weight of each component are as follows: high temperature vulcanized silica gel 100g, W powder 250g, the zinc borate powder 48g of hardness 10HA, platinum vulcanizing agent A component is 0.5g, and platinum vulcanizing agent B component is 1.5g, KH-540 coupling agent 1g.
Wherein W powder diameter 2um, zinc borate powder diameter 2.5um.
Preparation method's step with the unleaded gamma ray shielding material of flexibility of flame retardant properties is as follows:
1) high-temperature vulcanized silicon glue body material is plasticated: adjustment mill two roller spacing 2mm, rotating speed 45r/min, and when roller temperature is at 15 DEG C, two roller is rotated in start, is dropped into by high temperature vulcanized for 100g silica gel between two roller and plasticates, plasticate 5 minutes time.1.5g platinum vulcanizing agent B component is added to above-mentioned high temperature vulcanized silica gel relaying is continuous to carry out plasticating 10 minutes, finally add 0.5g platinum vulcanizing agent A component more mixing 10 minutes, period adopts methodology of rolling about to plasticate.
2) functional stuffing surface modification technology: the KH-540 coupling agent getting 90g deionized water, 15g dehydrated alcohol and 1g mixes with functional stuffing powder, and at 30 DEG C of temperature react 1.5 hours and filter obtain powdered mixture.
3) silica gel and functional stuffing powder mixing: the functional powders mixture adding above-mentioned silica gel of having plasticated He reacted in vacuum Banbury mixer, regulate processing temperature 105 DEG C, mixing 30 minutes, fully mix and remove moisture.
4) silica gel base composite material hot-pressed formation: arranging vulcanizing press upper and lower plates temperature is 50 DEG C, the flexible high molecular material based mixtures mixed in vacuum Banbury mixer is put compressing tablet de-bubble together with polyester separatory membrane, then put into 150 DEG C, baking oven heating 15min, there is described in namely obtaining after cooling the unleaded gamma shielding material of flexibility of flame retardant properties.
Material mechanical performance:
Flame Retardancy energy: oxygen index 32.3.
The gamma ray shielding rate of material to the outgoing of 241Am source that gamma ray shielding performance: 1mm is thick is 65.2%.
embodiment 2:the unleaded gamma ray shielding material of flexibility with flame retardant properties of the present invention.
In described shielding material, the parts by weight of each component are as follows: high temperature vulcanized silica gel 100g, W powder 250g, the WO of hardness 10HA
3powder 50g, zinc borate powder 28.3g, platinum vulcanizing agent A component is 1g, and platinum vulcanizing agent B component is 2g, KH-540 coupling agent 3g.
Wherein W powder diameter 2um, WO
3powder diameter 10um, zinc borate powder diameter 2.5um.
Preparation method's step with the unleaded gamma ray shielding material of flexibility of flame retardant properties is as follows:
1) high-temperature vulcanized silicon glue body material is plasticated: adjustment mill two roller spacing 2mm, rotating speed 45r/min, and when roller temperature is at 30 DEG C, two roller is rotated in start, is dropped into by high temperature vulcanized silica gel between two roller and plasticates, plasticate 8 minutes time.2g platinum vulcanizing agent B component is added to above-mentioned high temperature vulcanized silica gel relaying is continuous to carry out plasticating 12 minutes, finally add 1g platinum vulcanizing agent A component more mixing 12 minutes, period adopts methodology of rolling about to plasticate.
2) functional stuffing surface modification technology: the KH-550 getting 160g deionized water, 31.8g dehydrated alcohol and 3g mixes with functional stuffing powder, and react 1.2 hours at 40 DEG C of temperature.
3) silica gel and functional stuffing powder mixing: the functional powders mixture adding above-mentioned silica gel of having plasticated He reacted in vacuum Banbury mixer, regulate processing temperature 110 DEG C, mixing 25 minutes, fully mix and remove moisture.
4) silica gel base composite material hot-pressed formation: arranging vulcanizing press upper and lower plates temperature is 70 DEG C, the flexible high molecular material based mixtures mixed in vacuum Banbury mixer is put compressing tablet de-bubble together with polyester separatory membrane, then put into 160 DEG C, baking oven heating 11min, there is described in namely obtaining after cooling the unleaded gamma shielding material of flexibility of flame retardant properties.
Material mechanical performance:
Flame Retardancy energy: oxygen index 27.7.
The gamma ray shielding rate of material to the outgoing of 241Am source that gamma ray shielding performance: 1mm is thick is 70.7%.
embodiment 3:the unleaded gamma ray shielding material of flexibility with flame retardant properties of the present invention.
In described shielding material, the parts by weight of each component are as follows: high temperature vulcanized silica gel 100g, W powder 300g, the Gd of hardness 10HA
2o
3powder 100g, zinc borate powder 15.8g, platinum vulcanizing agent A component is 1.5g, and platinum vulcanizing agent B component is 3g, aminopropyl trimethoxysilane 5g.
Wherein W powder diameter 2um, Gd
2o
3particle diameter 15um, zinc borate powder diameter 2.5um.
Preparation method's step with the unleaded gamma ray shielding material of flexibility of flame retardant properties is as follows:
1) high-temperature vulcanized silicon glue body material is plasticated: the two roller spacing 2mm of adjustment mill, rotating speed 45r/min, when roller temperature is at 50 DEG C, two roller is rotated in start, 3g platinum vulcanizing agent B component is added to above-mentioned high temperature vulcanized silica gel relaying is continuous to carry out plasticating 15 minutes, finally add 1.5g platinum vulcanizing agent A component more mixing 15 minutes, period adopts methodology of rolling about to plasticate.
2) functional stuffing surface modification technology: get 208g deionized water, 41.6g dehydrated alcohol and 5g aminopropyl trimethoxysilane and mix with functional stuffing powder, and react 1 hour at 50 DEG C of temperature.
3) silica gel and functional stuffing powder mixing: the functional powders mixture adding above-mentioned silica gel of having plasticated He reacted in vacuum Banbury mixer, regulate processing temperature 115 DEG C, mixing 20 minutes, fully mix and remove moisture.
4) silica gel matrix composite is hot-forming: arranging vulcanizing press upper and lower plates temperature is 80 DEG C, the flexible high molecular material based mixtures mixed in vacuum Banbury mixer is put compressing tablet de-bubble together with polyester separatory membrane, then put into 170 DEG C, baking oven heating 8min, there is described in namely obtaining after cooling the unleaded gamma shielding material of flexibility of flame retardant properties.
Material mechanical performance:
Flame Retardancy energy: oxygen index 24.5.
The gamma ray shielding rate of material to the outgoing of 241Am source that gamma ray shielding performance: 1mm is thick is 76.2%.
embodiment 4:formulation content simultaneous test: the content of each component in formula in embodiment of the present invention 1-3 is carried out simultaneous test under the same conditions, and its result is as shown in the table:
Can be drawn by upper table, when gamma shielding functional stuffing in formula of the present invention 250 ~ 400 parts, anti-flaming function filler 15.8 ~ 48 parts, during powder surface modifier 1 ~ 5 part, the gamma ray shielding performance of specimen material can be improved when gamma shielding functional stuffing is excessive, but specimen material mechanical property can be reduced simultaneously; When gamma shielding functional stuffing is very few, specimen material gamma ray shielding performance obviously reduces.The flame retardant properties of specimen material can be improved when anti-flaming function filler is excessive, but specimen material mechanical property can be reduced simultaneously; Significantly specimen material flame retardant properties can be reduced when anti-flaming function filler is very few.Can reagent be wasted when powder surface modifier is excessive, substantially can not have an impact to material property; Powder dispersity can be made when powder surface modifier is very few and reduce with body material caking ability, reducing specimen material mechanical property.
There is excessive situation in the part material in comparative example 1 and comparative example 2, although its flame retardant properties and shielding properties are relative to close in technical scheme of the present invention, but because the mechanical property of two embodiment the finished product is all poor, cause the range of application of bi-material less, be not suitable for the actual demand of custom IC.
It should be noted that, above-mentioned is only preferred embodiment of the present invention, is not used for limiting protection scope of the present invention, and equivalents done on the basis of above-described embodiment all belongs to protection scope of the present invention.
Claims (7)
1. one kind has the unleaded gamma shielding material of flexibility of flame retardant properties, it is characterized in that, in described shielding material, the parts by weight of each component are as follows: 100 parts, high temperature vulcanized silica gel, gamma shielding functional stuffing 250 ~ 400 parts, anti-flaming function filler 15.8 ~ 48 parts, platinum vulcanizing agent A component 0.5 ~ 1.5 part, platinum vulcanizing agent B component 1.5 ~ 3 parts, powder surface modifier 1 ~ 5 part; Described gamma shielding functional stuffing is W, WO
3, BaO, Gd
2o
3in one or more mix with arbitrary proportion.
2. the unleaded gamma shielding material of flexibility with flame retardant properties according to claim 1, is characterized in that, described anti-flaming function filler is that one or more in aluminium hydroxide, magnesium hydroxide, zinc borate or red phosphorus mix with arbitrary proportion.
3. the unleaded gamma shielding material of flexibility with flame retardant properties according to claim 1, it is characterized in that, described powder surface modifier is coupling agent KH-540, aminopropyl trimethoxysilane, coupling agent D-90 wherein one or more mix with arbitrary proportion.
4. the unleaded gamma shielding material of flexibility with flame retardant properties according to claim 1, it is characterized in that, the hardness of described high temperature vulcanized silica gel is 10HA.
5. according to the unleaded gamma shielding material of the flexibility with flame retardant properties described in claim 1 or 2, it is characterized in that, described gamma shielding functional stuffing, anti-flaming function packing material size are 2um ~ 15um.
6. the preparation method of the unleaded gamma shielding material of the flexibility with flame retardant properties described in a claim 1, it is characterized in that, described preparation method comprises: flexible macromolecule body material plasticates → functional stuffing surface modification → with functional stuffing powder mixing → compressing tablet and high-temperature pressure shaping, its detailed preparation method is as follows:
1) the high temperature vulcanized silica gel adding respective quality in two roller mill is plasticated 5-10min, then adds platinum vulcanizing agent B component and to plasticate 10-15min, finally add platinum vulcanizing agent A component and continue the 10-15min that plasticates, obtain product of plasticating;
2) the gamma shielding functional stuffing of respective quality, anti-flaming function filler and powder surface modifier are mixed, obtain filler mixture, then the deionized water of filler mixture total mass 30% ~ 50% and the dehydrated alcohol of filler mixture total mass 5% ~ 10% is added, at 30-50 DEG C of temperature, react 1 ~ 1.5h, filter and obtain modified function filler mixture;
3) by plasticate product and step 2 that step 1) obtains) the modified function filler mixture that obtains adds in vacuum Banbury mixer, and banburying 20-30min at 105-115 DEG C of temperature, obtains silica gel based mixtures;
4) vulcanizing press upper and lower plates temperature is 50-80 DEG C, add the silica gel based mixtures compressing tablet de-bubble together with polyester separatory membrane step 3) obtained, then put into baking oven 150-170 DEG C of heating 8-15min, there is described in namely obtaining after cooling the unleaded gamma shielding material of flexibility of flame retardant properties.
7. the preparation method with the unleaded gamma shielding material of flexibility of flame retardant properties according to claim 6, is characterized in that, in the operating process of described step 1), two roller mill rotating speed is 45rpm, two roller spacing 2mm, working temperature 0 ~ 40 DEG C.
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106098127A (en) * | 2016-06-06 | 2016-11-09 | 南京航空航天大学 | There is flexible radiation protection material radiating warning and temp regulating function and preparation method thereof |
CN109133081A (en) * | 2018-10-25 | 2019-01-04 | 青岛科技大学 | Heavy metals removal technique in zinc borate preparation process |
CN110828019A (en) * | 2019-11-29 | 2020-02-21 | 西安交通大学 | Silica gel-based flexible shielding material for gamma ray shielding and preparation method thereof |
CN111111080A (en) * | 2019-12-12 | 2020-05-08 | 山东科技大学 | Surface-modified aggregate-enhanced fire prevention and extinguishing foam gel and preparation method thereof |
CN111849175A (en) * | 2020-07-16 | 2020-10-30 | 成都盛帮密封件股份有限公司 | Irradiation-resistant lead-free radiation shielding flexible material, and preparation method and application thereof |
CN112280308A (en) * | 2020-11-10 | 2021-01-29 | 四川全息新材料有限公司 | High-elasticity lead-free silicic acid gel ionizing radiation shielding flexible body, and manufacturing method and application thereof |
CN113696369A (en) * | 2021-09-08 | 2021-11-26 | 西安工程大学 | Preparation method of X-ray and gamma-ray protective body based on thermoplastic elastomer |
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JPS6212896A (en) * | 1985-07-10 | 1987-01-21 | 東芝シリコ−ン株式会社 | Gamma-ray shielding material |
CN101717583A (en) * | 2009-11-03 | 2010-06-02 | 山东大学 | Additional hot vulcanized silicon rubber with radiation resistant property and preparation method thereof |
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2015
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Patent Citations (2)
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JPS6212896A (en) * | 1985-07-10 | 1987-01-21 | 東芝シリコ−ン株式会社 | Gamma-ray shielding material |
CN101717583A (en) * | 2009-11-03 | 2010-06-02 | 山东大学 | Additional hot vulcanized silicon rubber with radiation resistant property and preparation method thereof |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106098127A (en) * | 2016-06-06 | 2016-11-09 | 南京航空航天大学 | There is flexible radiation protection material radiating warning and temp regulating function and preparation method thereof |
CN109133081A (en) * | 2018-10-25 | 2019-01-04 | 青岛科技大学 | Heavy metals removal technique in zinc borate preparation process |
CN110828019A (en) * | 2019-11-29 | 2020-02-21 | 西安交通大学 | Silica gel-based flexible shielding material for gamma ray shielding and preparation method thereof |
CN111111080A (en) * | 2019-12-12 | 2020-05-08 | 山东科技大学 | Surface-modified aggregate-enhanced fire prevention and extinguishing foam gel and preparation method thereof |
CN111111080B (en) * | 2019-12-12 | 2021-12-28 | 山东科技大学 | Surface-modified aggregate-enhanced fire prevention and extinguishing foam gel and preparation method thereof |
CN111849175A (en) * | 2020-07-16 | 2020-10-30 | 成都盛帮密封件股份有限公司 | Irradiation-resistant lead-free radiation shielding flexible material, and preparation method and application thereof |
CN112280308A (en) * | 2020-11-10 | 2021-01-29 | 四川全息新材料有限公司 | High-elasticity lead-free silicic acid gel ionizing radiation shielding flexible body, and manufacturing method and application thereof |
CN113696369A (en) * | 2021-09-08 | 2021-11-26 | 西安工程大学 | Preparation method of X-ray and gamma-ray protective body based on thermoplastic elastomer |
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Application publication date: 20150916 |