CN108411618A - A kind of preparation method of X, gamma-rays protective fabric - Google Patents

A kind of preparation method of X, gamma-rays protective fabric Download PDF

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CN108411618A
CN108411618A CN201810189538.XA CN201810189538A CN108411618A CN 108411618 A CN108411618 A CN 108411618A CN 201810189538 A CN201810189538 A CN 201810189538A CN 108411618 A CN108411618 A CN 108411618A
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graphene oxide
nitrate
powder
gamma
added
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姚理荣
董莉
石敏
徐思峻
袁国秋
孙启龙
徐山青
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Nantong University
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Nantong University
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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    • D06M10/00Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/02Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
    • D06M10/025Corona discharge or low temperature plasma
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/44Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic System; Zincates; Cadmates
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/48Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters

Abstract

The application is provided in the preparation method of a kind of X, gamma-rays protective fabric, and graphene oxide solution is prepared by raw material of expanded graphite;Using five water bismuth nitrates and sodium tungstate as raw material, in-situ preparation bismuth tungstate obtains the graphene oxide of intercalation sheet bismuth tungstate between graphene oxide layer, and washed, dry, calcining obtains the first graphene oxide powder;The second graphene oxide powder is made as raw material using europium nitrate, gadolinium nitrate, samaric nitrate, barium sulfate;First graphene oxide powder and the second graphene oxide powder are mixed, using the dacron surface for being applied to Corona discharge Treatment in acrylic resin soln after mixing and crossing is added to after silane coupler modified, X is made using hot forming, gamma-rays protects polyester fabric.Prepared polyester fabric not only has good permeability and high temperature resistance, also has X-ray shield rate high, persistence is good, and unleaded light-weighted advantage has good application prospect in terms of X-ray radiation protection.

Description

A kind of preparation method of X, gamma-rays protective fabric
Technical field
This application involves radiation protection field more particularly to the preparation methods of a kind of X, gamma-rays protective fabric.
Background technology
In recent years, with the rapid development of national defence scientific research, Radiation Medicine and atomic energy industry, the use of various rays is increasingly Extensively.X, gamma-rays is its important one kind.Due to Long Term Contact X, gamma-rays, sexual gland, mammary gland, Hematopoietic marrow etc. can all be produced Raw injury is more than that dosage even can be carcinogenic, brings and seriously threaten to human body.Therefore according to X, gamma-ray property and its and substance The mechanism of action, should select and prepare corresponding material and be protected.
Earliest the metal materials such as stereotype, iron plate for X, gamma ray shielding, have developed again later leaded glass, The products such as organic glass and rubber, and be processed into various protective garments, the helmet, protective gloves etc..But these protective articles gas permeabilities Difference, it is heavy, wear uncomfortable, while lead all has serious harm to human body and environment.
The existing related patents about radiation protection fabric have very much, such as Chinese invention patent " a kind of radiation-proof fabric " In (CN 105962502A), a kind of preparation method of radiation-proof fabric is disclosed, which includes surface layer and inner layer, table Layer is formed by silver fiber and gined cotton are blended, and the outer surface on surface layer is uniformly provided with several silver-ion fiber protrusions, and inner layer is by natural cotton Blended fabric fibrous layer and mulberry silk fiber layer is blended forms, is equipped with carbon fiber rod and Sheng-bast fiber block branch between surface layer and inner layer Support layer;In Chinese invention patent " a kind of radiation-proof fabric " (CN 105639788A), a kind of preparation of radiation-proof fabric is disclosed Method, the fabric component include nano-far-infrared ceramic fibre, polysulphonamide fiber, mercerized cotton, alginate fibre, stainless steel wire, glue Stick forms one layer of strict gauze screen using metal layer and achievees the effect that shield ray;" radiation protection is anti-for Chinese invention patent In bacterium fabric " (CN 104354351A), a kind of preparation method of radiation protection antibacterial fabric is disclosed, which uses and receive Rice silver fiber is formed by weaving, and base upper surface is bonded with one layer of aluminum alloy films by adhesive, is provided on aluminum alloy films The antistatic backing being made of the fringe bar with conductive fiber;Its common deficiency is that fabric is multilayered structure, it appears it is heavy, make With, wear off inconvenience, and protection effect is unsatisfactory.
Invention content
In view of this, the embodiment of the present application provides the preparation method of a kind of X, gamma-rays protective fabric, to prepare one Kind gas permeability height, X, the protective fabric that gamma ray shielding rate is high and persistence is good.
The embodiment of the present application uses following technical proposals:
The embodiment of the present application provides the preparation method of a kind of X, gamma-rays protective fabric, including:Prepare the oxygen containing intermediary water Graphite alkene;
The first graphene oxide powder of intercalation bismuth tungstate is prepared according to the graphene oxide containing intermediary water;
The second of intercalation europium oxide, samarium oxide, gadolinium oxide and barium monoxide is prepared according to first graphene oxide powder Graphene oxide powder;
X-ray radiation safeguard function is prepared according to first graphene oxide powder and the second graphene oxide powder Unleaded powder;
X, gamma-rays protective fabric are prepared according to the unleaded powder of x-ray radiation safeguard function.
Preferably, above-mentioned X, gamma-rays protective fabric preparation method in, prepare the graphene oxide containing intermediary water, Including:
Expanded graphite and the concentrated sulfuric acid are mixed according to a certain percentage, and are sufficiently stirred under ice-water bath;
Potassium permanganate is added until the potassium permanganate total overall reaction finishes;
Hydrogen peroxide is added after mixing in mechanical agitation after deionized water is added, and obtains the first mixed solution;
With including that hydrochloric acid cleans described first with the second mixed solution of deionized water under the conditions of Centrifugal dispersion and mixes Solution obtains graphene oxide to neutrality;
By the graphene oxide in hydrothermal reaction kettle, ultrasonic first preset time, obtains under the first temperature condition Graphene oxide containing intermediary water.
Preferably, above-mentioned X, gamma-rays protective fabric preparation method in, the expanded graphite and concentrated sulfuric acid quality Than being 1:30~1:40, the mass ratio of the expanded graphite and potassium permanganate is 1:1~1:6, the expanded graphite and peroxidating The mass ratio of hydrogen is 1:3~1:10, the volume ratio of hydrochloric acid and deionized water is 1 in second mixed solution:5~1:10;
First temperature is 100~250 DEG C, and first preset time is 1~10 hour.
Preferably, above-mentioned X, gamma-rays protective fabric preparation method in, according to the oxidation stone containing intermediary water Black alkene prepares the first graphene oxide powder of intercalation bismuth tungstate, including:
Bismuth nitrate is dissolved in dust technology, with vigorous stirring, the silver nitrate solution of acquisition is slowly added into wolframic acid In the aqueous solution of sodium;
Graphene oxide solution is added, obtains third mixed solution;
Alkaline solution is added and adjusts the pH value of the third mixed solution to 5~5.5;
Cetyltrimethylammonium bromide and polyethylene glycol are added, after stirring the second preset time, obtains gel;
Then the gel is handled under the first pretreatment condition, obtains first graphene oxide powder.
Preferably, above-mentioned X, gamma-rays protective fabric preparation method in, the quality of the bismuth nitrate and dust technology Than being 1:2~1:5, the mass ratio of the bismuth nitrate and sodium tungstate is 3:1-5:1, the quality of the bismuth nitrate and graphene oxide Than being 1:2~1:5, a concentration of 0.01M~0.1M of the cetyltrimethylammonium bromide, the bismuth nitrate and polyethylene glycol Mass ratio be 1:3~1:5;
The alkaline solution includes sodium hydroxide solution;
Second preset time is 6~10 hours;
First pretreatment condition includes:It is washed with ethyl alcohol, 40~60 DEG C of drying, 300~500 DEG C of calcinings.
Preferably, above-mentioned X, gamma-rays protective fabric preparation method in, according to the first graphene oxide powder Body prepares the second graphene oxide powder of intercalation europium oxide, samarium oxide, gadolinium oxide and barium monoxide, including:
Europium nitrate, gadolinium nitrate, samaric nitrate, barium sulfate mixed solution are added in graphene oxide solution, ammonium hydroxide is added After being ultrasonically treated third preset time, it is transferred to hydrothermal reaction kettle, the 4th preset time of hydro-thermal reaction under the conditions of second temperature, Obtain the 4th mixed solution;
4th mixed solution is handled under the second pretreatment condition, obtains second graphene oxide powder.
Preferably, above-mentioned X, gamma-rays protective fabric preparation method in, the europium nitrate, gadolinium nitrate, samaric nitrate, The mass component ratio of europium nitrate is in barium sulfate mixed solution:30%~40%;The mass component ratio of gadolinium nitrate be 30%~ 40%;The mass component ratio of the samaric nitrate is 10%~20%;The mass component ratio of the barium sulfate is 10%~20%;
The 1 of the europium nitrate, gadolinium nitrate, samaric nitrate, barium sulfate mixed solution and graphene oxide:3~1:5, the nitre Sour europium, gadolinium nitrate, samaric nitrate, barium sulfate mixed solution and ammonium hydroxide mass ratio be 1:3~1:6;
The second temperature is 100~300 DEG C, and the third preset time is 2-4 hours;4th preset time is 1~48 hour;
Second pretreatment condition is:It is washed with ethyl alcohol, 40~60 DEG C of drying, is calcined using 900~1200 DEG C.
Preferably, above-mentioned X, gamma-rays protective fabric preparation method in, according to the first graphene oxide powder Body and the second graphene oxide powder prepare the unleaded powder of x-ray radiation safeguard function, including:
By first graphene oxide powder and the second graphene oxide powder according to 3:1~5:1 molar ratio is uniform Mixing, you can obtain the unleaded powder of x-ray radiation safeguard function.
Preferably, above-mentioned X, gamma-rays protective fabric preparation method in, according to x-ray radiation safeguard function without Lead powder body prepares X, gamma-rays protective fabric, including:
A small amount of acetone is added in silane coupling agent, and after being uniformly mixed, the unleaded powder of x-ray radiation safeguard function is added, The 4th preset time is handled in supersonic generator, acrylic resin is added, continues to stir evenly, and it is de- to be warming up to third temperature Except acetone, it is continuously heating to the 4th temperature after the 5th preset time, is coated in through corona under 15-18KV voltages under certain viscosity Pre-irradiation handles the dacron surface after 4-7min, X is made after elevated cure, gamma-rays protects polyester fabric.
Preferably, above-mentioned X, gamma-rays protective fabric preparation method in, the x-ray radiation safeguard function without The mass ratio of lead powder body and silane coupling agent is 1:2~1:5, the unleaded powder of the x-ray radiation safeguard function and epoxy resin Mass ratio be 1:6~1:8, viscosity 5000-14000mPa.s;
The dacron specification is:80~165/cm of warp count, 20~45/cm of weft count, grammes per square metre 50~ 200g/m2;
4th preset time is:30~50 minutes, the third temperature was 70~80 DEG C, the 5th preset time It it is 20~30 minutes, the 4th temperature is 110~130 DEG C.
Above-mentioned at least one technical solution that the embodiment of the present application uses can reach following advantageous effect:By X, gamma-rays Screener-nano-powder, which is added in acrylic resin, is coated in polyester fabric surface, and sided corona treatment improves the work of terylene surface Property group to have a stronger adhesion strength to slurry, prepared polyester fabric not only has good permeability, also has X, gamma ray shielding rate is high, and persistence is good, and unleaded light-weighted advantage has good application in terms of X, gamma Rays protection Foreground.
Description of the drawings
Attached drawing described herein is used for providing further understanding of the present application, constitutes part of this application, this Shen Illustrative embodiments and their description please do not constitute the improper restriction to the application for explaining the application.In the accompanying drawings:
Fig. 1 is the flow chart of the preparation method of X, gamma-rays protective fabric in the embodiment of the present application.
Specific implementation mode
To keep the purpose, technical scheme and advantage of the application clearer, below in conjunction with the application specific embodiment and Technical scheme is clearly and completely described in corresponding attached drawing.Obviously, described embodiment is only the application one Section Example, instead of all the embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not doing Go out the every other embodiment obtained under the premise of creative work, shall fall in the protection scope of this application.
Below in conjunction with attached drawing, the technical solution that each embodiment of the application provides is described in detail.
Fig. 1 is a kind of X provided by the embodiments of the present application, the flow diagram of the preparation method of gamma-rays protective fabric.Institute The method of stating can be as follows.The method includes:The graphene oxide containing intermediary water is prepared, such as the step S101 institutes in Fig. 1 Show;The first graphene oxide powder that intercalation bismuth tungstate is prepared according to the graphene oxide containing intermediary water, such as the step in Fig. 1 Shown in rapid S103;The of intercalation europium oxide, samarium oxide, gadolinium oxide and barium monoxide is prepared according to first graphene oxide powder Step S105 in titanium dioxide graphene powder such as Fig. 1;According to first graphene oxide powder and the second graphene oxide Powder prepares the unleaded powder of x-ray radiation safeguard function, such as the step S107 in Fig. 1;According to x-ray radiation safeguard function without Lead powder body prepares X, gamma-rays protective fabric, such as the step S109 in Fig. 1.
Step S101 prepares the graphene oxide containing intermediary water.
Specifically, first, expanded graphite and the concentrated sulfuric acid are mixed according to a certain percentage, and under ice-water bath fully Stirring.The expanded graphite is 1 with concentrated sulfuric acid mass ratio:30~1:40.
Then, add potassium permanganate until the potassium permanganate total overall reaction finish, the expanded graphite and permanganic acid The mass ratio of potassium is 1:1~1:6.
Next, mechanical agitation after deionized water is added, after mixing, hydrogen peroxide is added, obtains the first mixing The mass ratio of solution, the expanded graphite and hydrogen peroxide is 1:3~1:10.
With including that hydrochloric acid cleans described first with the second mixed solution of deionized water under the conditions of Centrifugal dispersion and mixes Solution obtains graphene oxide to neutrality.Wherein, the volume ratio of hydrochloric acid and deionized water is 1 in second mixed solution:5 ~1:10.
By the graphene oxide in hydrothermal reaction kettle, ultrasonic first preset time, obtains under the first temperature condition Graphene oxide containing intermediary water.Wherein, first temperature is 100~250 DEG C, and first preset time is 1~10 small When.
Step S103 prepares the first graphene oxide powder of intercalation bismuth tungstate according to the graphene oxide containing intermediary water Body.
Specifically, bismuth nitrate is dissolved in dust technology, with vigorous stirring, the nitrate solution of acquisition is slowly added to Into the aqueous solution of sodium tungstate, the mass ratio of the bismuth nitrate and dust technology is 1:2~1:5, the bismuth nitrate and sodium tungstate Mass ratio is 3:1-5:1.
Graphene oxide solution is added, obtains third mixed solution, wherein the quality of the bismuth nitrate and graphene oxide Than being 1:2~1:5.
It adds alkaline solution and adjusts the pH value of the third mixed solution to 5~5.5, the alkaline solution includes But it is not limited to sodium hydroxide solution.
Cetyltrimethylammonium bromide and polyethylene glycol are added, after stirring the second preset time, obtains gel. Wherein, a concentration of 0.01M~0.1M of the cetyltrimethylammonium bromide, the mass ratio of the bismuth nitrate and polyethylene glycol It is 1:3~1:5, second preset time is 6~10 hours.
Then the gel is handled under the first pretreatment condition, obtains first graphene oxide powder.It is described First pretreatment condition includes:It is washed with ethyl alcohol, 40~60 DEG C of drying, 300~500 DEG C of calcinings.
Step S105 prepares intercalation europium oxide, samarium oxide, gadolinium oxide and oxidation according to first graphene oxide powder Second graphene oxide powder of barium.
Specifically, europium nitrate, gadolinium nitrate, samaric nitrate, barium sulfate mixed solution are added in graphene oxide solution, add After entering ammonium hydroxide supersound process third preset time, it is transferred to hydrothermal reaction kettle, hydro-thermal reaction the 4th is pre- under the conditions of second temperature If the time, the 4th mixed solution is obtained.The quality of europium nitrate in the europium nitrate, gadolinium nitrate, samaric nitrate, barium sulfate mixed solution Ingredient ratio is:30%~40%;The mass component ratio of gadolinium nitrate is 30%~40%;The mass component ratio of the samaric nitrate is 10%~20%;The mass component ratio of the barium sulfate is 10%~20%, and the second temperature is 100~300 DEG C, described the Three preset times are 2-4 hours;4th preset time is 1~48 hour.
4th mixed solution is handled under the second pretreatment condition, obtains second graphene oxide powder. Second pretreatment condition is:It is washed with ethyl alcohol, 40~60 DEG C of drying, is calcined using 900~1200 DEG C.
Step S107 prepares x-ray radiation according to first graphene oxide powder and the second graphene oxide powder The unleaded powder of safeguard function.
Specifically, by first graphene oxide powder and the second graphene oxide powder according to 3:1~5:1 mole Than uniformly mixing, you can obtain the unleaded powder of x-ray radiation safeguard function.
Step S109 prepares X, gamma-rays protective fabric according to the unleaded powder of x-ray radiation safeguard function.
Specifically, a small amount of acetone is added in silane coupling agent, after being uniformly mixed, x-ray radiation safeguard function is added Unleaded powder handles the 4th preset time in supersonic generator, and acrylic resin is added, continues to stir evenly, be warming up to Third temperature removes acetone, and the 4th temperature is continuously heating to after the 5th preset time, is coated in through 15-18KV under certain viscosity Corona pre-irradiation handles the dacron surface after 4-7min under voltage, and X, gamma-rays protection terylene face are made after elevated cure Material.
Wherein, the mass ratio of the unleaded powder of the x-ray radiation safeguard function and silane coupling agent is 1:2~1:5, institute The mass ratio for stating the unleaded powder of x-ray radiation safeguard function and epoxy resin is 1:6~1:8, viscosity 5000- 14000mPa.s;Dacron specification is:80~165/cm of warp count, 20~45/cm of weft count, grammes per square metre 50 ~200g/m2;4th preset time is:30~50 minutes, the third temperature be 70~80 DEG C, it is described 5th it is default when Between be 20~30 minutes, the 4th temperature be 110~130 DEG C.
Next, being illustrated with a specific embodiment.
First, it takes 4g expanded graphites and the 184ml concentrated sulfuric acids to be placed in glass container, is sufficiently stirred under ice-water bath;Slowly add Enter 3g potassium permanganate up to potassium permanganate total overall reaction, add 200ml deionized waters mechanical agitation at a certain temperature, mixes The hydrogen peroxide of 20ml is added after uniformly, solution becomes glassy yellow by brownish black;With 300ml hydrochloric acid and deionized water (dilute hydrochloric acid Ratio with deionized water is 1:9) cleaning solution obtains graphene oxide to neutrality under the conditions of Centrifugal dispersion.
Secondly, take the graphene oxide of above-mentioned preparation in hydrothermal reaction kettle, ultrasound is made for 2 hours at 135 DEG C contains interlayer The graphene oxide of water.
Then, five water bismuth nitrates of 3g are dissolved in 6g dust technologies, with vigorous stirring, nitrate solution is slowly added to Into the aqueous solution containing 1g sodium tungstates, graphene oxide solutions of the 6g containing intermediary water is added, sodium hydroxide solution tune is added PH to 5~5.5 is saved, 2.5g0.01M cetyltrimethylammonium bromide is then added, it is small that the stirring 6~10 of 9g polyethylene glycol is added When, obtained gel washs with ethyl alcohol, 40~60 DEG C of drying, and 300~500 DEG C of calcinings obtain the first oxidation of intercalation bismuth tungstate Graphene powder.
Next, the mixed solution of 1g europium nitrates, gadolinium nitrate, samaric nitrate, barium sulfate is added to oxygen of the 2g containing intermediary water In graphite alkene solution (europium nitrate, gadolinium nitrate, samaric nitrate, the mass component shared by barium sulfate than be respectively 30%, 30%, 20% and 20%), 3g ammonium hydroxide strengths ultrasound is added 2-4 hours, is transferred to 100~300 DEG C in hydrothermal reaction kettle of temperature condition 1~48h of lower hydro-thermal reaction, obtained solution is washed with ethyl alcohol, 40~60 DEG C of drying are obtained using 900~1200 DEG C of calcinings Second graphene oxide powder of intercalation europium oxide, samarium oxide, gadolinium oxide and barium monoxide.
Subsequently, the first graphene oxide powder and the second graphene oxide powder are pressed 4:1 molar ratio uniformly mixes Obtain X, the unleaded powder of gamma Rays safeguard function.
Finally, a small amount of acetone is added in 2g silane coupling agents, be uniformly mixed, 1gX is added, gamma Rays protect work( The unleaded powder of energy, handles 30min in supersonic generator, and 6g acrylic resins are added, continues to stir evenly, is warming up to 70 DEG C Acetone is removed, 110 DEG C are continuously heating to after 20min, is coated in through the pre- spoke of corona under 15KV voltages under 13000mPa.s viscosity According to the dacron surface after processing 4min, X, gamma-rays protection polyester fabric are made after elevated cure, wherein dacron is advised Lattice are 165/cm of warp count, weft count 45/cm, grammes per square metre 160g/m2.
A kind of X provided by the embodiments of the present application, gamma-rays protective fabric preparation method in, using expanded graphite as raw material Prepare graphene oxide solution;Using five water bismuth nitrates and sodium tungstate as raw material, the in-situ preparation wolframic acid between graphene oxide layer Bismuth obtains the graphene oxide of intercalation sheet bismuth tungstate, and washed, dry, calcining obtains the first graphite oxide of intercalation bismuth tungstate Alkene powder;Intercalation europium oxide, samarium oxide, gadolinium oxide and oxidation is made as raw material using europium nitrate, gadolinium nitrate, samaric nitrate, barium sulfate Second graphene oxide powder of barium;First graphene oxide powder and the second graphene oxide powder are mixed, silane is utilized It is added to after coupling agent modified and is applied to the dacron surface that Corona discharge Treatment is crossed in acrylic resin soln after mixing, X is made using hot forming, gamma-rays protects polyester fabric.Prepared polyester fabric not only have good permeability and High temperature resistance also has X-ray shield rate high, and persistence is good, unleaded light-weighted advantage, in terms of X-ray radiation protection There is good application prospect.
Each embodiment in this specification is described in a progressive manner, identical similar portion between each embodiment Point just to refer each other, and each embodiment focuses on the differences from other embodiments.The foregoing is merely this The embodiment of application, is not intended to limit this application.To those skilled in the art, the application can have it is various more Change and changes.All any modification, equivalent replacement, improvement and so within spirit herein and principle, should be included in Within the scope of claims hereof.

Claims (10)

1. the preparation method of a kind of X, gamma-rays protective fabric, which is characterized in that including:
Prepare the graphene oxide containing intermediary water;
The first graphene oxide powder of intercalation bismuth tungstate is prepared according to the graphene oxide containing intermediary water;
The second oxidation of intercalation europium oxide, samarium oxide, gadolinium oxide and barium monoxide is prepared according to first graphene oxide powder Graphene powder;
It is unleaded that x-ray radiation safeguard function is prepared according to first graphene oxide powder and the second graphene oxide powder Powder;
X, gamma-rays protective fabric are prepared according to the unleaded powder of x-ray radiation safeguard function.
2. the preparation method of X according to claim 1, gamma-rays protective fabric, which is characterized in that prepare containing intermediary water Graphene oxide, including:
Expanded graphite and the concentrated sulfuric acid are mixed according to a certain percentage, and are sufficiently stirred under ice-water bath;
Potassium permanganate is added until the potassium permanganate total overall reaction finishes;
Hydrogen peroxide is added after mixing in mechanical agitation after deionized water is added, and obtains the first mixed solution;
With including that the second mixed solution of hydrochloric acid and deionized water cleans first mixed solution under the conditions of Centrifugal dispersion To neutrality, graphene oxide is obtained;
By the graphene oxide in hydrothermal reaction kettle, ultrasonic first preset time, obtains and contains layer under the first temperature condition Between water graphene oxide.
3. the preparation method of X according to claim 2, gamma-rays protective fabric, which is characterized in that the expanded graphite with Concentrated sulfuric acid mass ratio is 1:30~1:40, the mass ratio of the expanded graphite and potassium permanganate is 1:1~1:6, the puffing stone The mass ratio of ink and hydrogen peroxide is 1:3~1:10, the volume ratio of hydrochloric acid and deionized water is 1 in second mixed solution:5 ~1:10;
First temperature is 100~250 DEG C, and first preset time is 1~10 hour.
4. the preparation method of X according to claim 1, gamma-rays protective fabric, which is characterized in that contain interlayer according to described The graphene oxide of water prepares the first graphene oxide powder of intercalation bismuth tungstate, including:
Bismuth nitrate is dissolved in dust technology, with vigorous stirring, the silver nitrate solution of acquisition is slowly added into sodium tungstate In aqueous solution;
Graphene oxide solution is added, obtains third mixed solution;
Alkaline solution is added and adjusts the pH value of the third mixed solution to 5~5.5;
Cetyltrimethylammonium bromide and polyethylene glycol are added, after stirring the second preset time, obtains gel;
Then the gel is handled under the first pretreatment condition, obtains first graphene oxide powder.
5. the preparation method of X according to claim 4, gamma-rays protective fabric, which is characterized in that the bismuth nitrate with it is dilute The mass ratio of nitric acid is 1:2~1:5, the mass ratio of the bismuth nitrate and sodium tungstate is 3:1-5:1, the bismuth nitrate with oxidation stone The mass ratio of black alkene is 1:2~1:5, a concentration of 0.01M~0.1M of the cetyltrimethylammonium bromide, the bismuth nitrate Mass ratio with polyethylene glycol is 1:3~1:5;
The alkaline solution includes sodium hydroxide solution;
Second preset time is 6~10 hours;
First pretreatment condition includes:It is washed with ethyl alcohol, 40~60 DEG C of drying, 300~500 DEG C of calcinings.
6. the preparation method of X according to claim 1, gamma-rays protective fabric, which is characterized in that according to first oxygen Graphite alkene powder prepares the second graphene oxide powder of intercalation europium oxide, samarium oxide, gadolinium oxide and barium monoxide, including:
Europium nitrate, gadolinium nitrate, samaric nitrate, barium sulfate mixed solution are added in graphene oxide solution, ammonium hydroxide ultrasound is added After handling third preset time, it is transferred to hydrothermal reaction kettle, the 4th preset time of hydro-thermal reaction, obtains under the conditions of second temperature 4th mixed solution;
4th mixed solution is handled under the second pretreatment condition, obtains second graphene oxide powder.
7. the preparation method of X according to claim 6, gamma-rays protective fabric, which is characterized in that the europium nitrate, nitre The mass component ratio of europium nitrate is in sour gadolinium, samaric nitrate, barium sulfate mixed solution:30%~40%;The mass component of gadolinium nitrate Than being 30%~40%;The mass component ratio of the samaric nitrate is 10%~20%;The mass component ratio of the barium sulfate is 10%~20%;
The 1 of the europium nitrate, gadolinium nitrate, samaric nitrate, barium sulfate mixed solution and graphene oxide:3~1:5, the europium nitrate, Gadolinium nitrate, samaric nitrate, barium sulfate mixed solution and ammonium hydroxide mass ratio be 1:3~1:6;
The second temperature is 100~300 DEG C, and the third preset time is 2-4 hours;4th preset time be 1~ 48 hours;
Second pretreatment condition is:It is washed with ethyl alcohol, 40~60 DEG C of drying, is calcined using 900~1200 DEG C.
8. the preparation method of X according to claim 1, gamma-rays protective fabric, which is characterized in that according to first oxygen Graphite alkene powder and the second graphene oxide powder prepare the unleaded powder of x-ray radiation safeguard function, including:
By first graphene oxide powder and the second graphene oxide powder according to 3:1~5:1 molar ratio uniformly mixes, It can be obtained the unleaded powder of x-ray radiation safeguard function.
9. the preparation method of X according to claim 1, gamma-rays protective fabric, which is characterized in that according to x-ray radiation The unleaded powder of safeguard function prepares X, gamma-rays protective fabric, including:
A small amount of acetone is added in silane coupling agent, after being uniformly mixed, the unleaded powder of x-ray radiation safeguard function is added, The 4th preset time is handled in supersonic generator, acrylic resin is added, continues to stir evenly, and is warming up to the removing of third temperature Acetone is continuously heating to the 4th temperature after the 5th preset time, is coated under certain viscosity pre- through corona under 15-18KV voltages X is made after elevated cure for dacron surface after radiation treatment 4-7min, gamma-rays protects polyester fabric.
10. the preparation method of X according to claim 9, gamma-rays protective fabric, which is characterized in that the X-ray spoke The mass ratio for penetrating the unleaded powder of safeguard function and silane coupling agent is 1:2~1:5, the x-ray radiation safeguard function is without lead powder The mass ratio of body and epoxy resin is 1:6~1:8, viscosity 5000-14000mPa.s;
The dacron specification is:80~165/cm of warp count, weft count 20~45/cm, 50~200g/ of grammes per square metre m2;
4th preset time is:30~50 minutes, the third temperature was 70~80 DEG C, and the 5th preset time is 20 ~30 minutes, the 4th temperature was 110~130 DEG C.
CN201810189538.XA 2018-03-08 2018-03-08 A kind of preparation method of X, gamma-rays protective fabric Pending CN108411618A (en)

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CN109679422A (en) * 2018-12-05 2019-04-26 上海六晶科技股份有限公司 A kind of Lead free coating and preparation method thereof for shielding X-ray
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CN112900110A (en) * 2021-02-08 2021-06-04 南通大学 Preparation method of core-shell structure tungsten/gadolinium oxide PU coating fabric for X, gamma ray protection
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CN113334878A (en) * 2021-05-27 2021-09-03 中国辐射防护研究院 Sandwich-like structure ionizing radiation flexible shielding material and preparation method thereof
CN113600132A (en) * 2021-08-31 2021-11-05 南通大学 Preparation method of intercalated graphene blended polyurethane open-cell sponge for adsorption
CN113600132B (en) * 2021-08-31 2023-09-15 南通大学 Preparation method of intercalation graphene blended polyurethane open-cell sponge for adsorption
CN115787289A (en) * 2022-10-11 2023-03-14 无锡市圣华盾医疗科技有限公司 Light nuclear radiation protection fabric and preparation process thereof
CN115787289B (en) * 2022-10-11 2023-10-10 无锡市圣华盾医疗科技有限公司 Light nuclear radiation protection fabric and preparation process thereof

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Application publication date: 20180817