CN108411492A - A kind of preparation method of X, gamma-rays protection non-woven fabrics - Google Patents
A kind of preparation method of X, gamma-rays protection non-woven fabrics Download PDFInfo
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- CN108411492A CN108411492A CN201810189536.0A CN201810189536A CN108411492A CN 108411492 A CN108411492 A CN 108411492A CN 201810189536 A CN201810189536 A CN 201810189536A CN 108411492 A CN108411492 A CN 108411492A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/541—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/542—Adhesive fibres
- D04H1/55—Polyesters
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
- G21F1/02—Selection of uniform shielding materials
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F3/00—Shielding characterised by its physical form, e.g. granules, or shape of the material
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- Physics & Mathematics (AREA)
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Abstract
The application is provided in the preparation method of a kind of X, gamma-rays protection non-woven fabrics, prepares 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 graphene oxide powder of intercalation europium oxide, samarium oxide, gadolinium oxide and barium monoxide is prepared according to first graphene oxide powder；The unleaded powder of X ray radiation safeguard functions is prepared according to first graphene oxide powder and the second graphene oxide powder；X, gamma-rays protection non-woven fabrics are prepared according to the unleaded powder of the X ray radiations safeguard function.The additive amount of function powder is improved in prepared PE/PP core-sheath compound fibres, fiber not only has good physical mechanical property, textile process performance kimonos performance, also have X, gamma ray shielding rate high, persistence is good, unleaded light-weighted advantage has good application prospect in terms of X, gamma Rays protection.
Description
Technical field
This application involves radiation protection field more particularly to the preparation methods of a kind of X, gamma-rays protection non-woven fabrics.
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.
It is existing to protect the related patents of fiber to have much about X, gamma-rays, as " one kind carrying X-ray to Chinese invention patent
The preparation method of the quartz fibre of agent coating is penetrated in resistance " in (CN 106316159A), discloses and a kind of penetrating agent painting with X-ray resistance
The preparation method of the quartz fibre of layer, this method coat quartz fibre monofilament surface by penetrating the surface conditioning agent of agent containing resistance
Processing, draws through wire-drawing machine head high speed rotation and is wound into quartz fibre precursor, after drying silk, moving back solution, first twist and twirl
It is produced into resistance and penetrates agent coating quartz fibre；A kind of Chinese invention patent " preparation side of X-ray-preventing rare earth/polypropylene composite materials fiber
In method " (CN 104532381B), a kind of preparation method of X-ray-preventing rare earth/polypropylene composite materials fiber is disclosed, this method is first
Granulation is blended with PP GRANULES point in rare earth oxide particle and obtains rare earth/PP GRANULES, is obtained by melt spinning
To as-spun fibre, then as-spun fibre is cut into staple length it is 3-5 centimeter and tie up, successively spreads even, be made in pressure by film laminator
Thickness is the non-woven cloth of 4-8mm；Chinese invention patent " a kind of X-ray radiation protection cellulose fibre and preparation method thereof " (CN
In 102704023A), a kind of preparation method of X-ray radiation protection cellulose fibre is disclosed, this method is by the sulphur of grain size≤3 μm
Sour barium powder is prepared into barium sulfate emulsion paste in organic dispersion medium miscible with water, then starches the barium sulfate lotion
It is molten that material according to barium sulfate content relative to the weight percent of alpha cellulose 10~30% is added to the dissolved viscose glue of yellow
It is uniformly mixed in liquid, then the X-ray radiation protection cellulose fiber is obtained through spinning coagulation bath spinning moulding, drawing-off and post-processing
Dimension.Its deficiency is that the consistency problem of function powder and polymer causes the additive amount of functional powders in polymer relatively low, from
And lead to lower X-ray shield rate, and agent is penetrated into X-ray resistance and is coated in fiber surface, persistence is poor.
Invention content
In view of this, the embodiment of the present application provides the preparation method of a kind of X, gamma-rays protection non-woven fabrics, to solve
X-ray shield rate in the prior art, and agent is penetrated into X-ray resistance and is coated in fiber surface, the poor problem of persistence.
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 protection non-woven fabrics, 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 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 protection non-woven fabrics are prepared according to the unleaded powder of the x-ray radiation safeguard function.
Preferably, above-mentioned X, gamma-rays protection non-woven fabrics preparation method in, prepare the oxidation stone containing intermediary water
Black alkene, 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 protection non-woven fabrics preparation method in, the expanded graphite and the 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 expanded graphite and mistake
The mass ratio of hydrogen oxide 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 protection non-woven fabrics preparation method in, according to the oxygen containing intermediary water
Graphite 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 protection non-woven fabrics preparation method in, the bismuth nitrate and dust technology
Mass ratio is 1:2~1:5, the mass ratio of the bismuth nitrate and sodium tungstate is 3:1-5:1, the bismuth nitrate and graphene oxide
Mass ratio is 1:2~1:5, a concentration of 0.01M~0.1M of the cetyltrimethylammonium bromide, the bismuth nitrate and poly- second
The mass ratio of 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.
Preferably, above-mentioned X, gamma-rays protection non-woven fabrics preparation method in, according to first graphite oxide
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 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 protection non-woven fabrics preparation method in, the europium nitrate, gadolinium nitrate, nitre
The mass component ratio of europium nitrate is in sour samarium, barium sulfate mixed solution：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%；
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 protection non-woven fabrics preparation method in, according to first graphite oxide
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 is uniform
Mixing, you can obtain the unleaded powder of x-ray radiation safeguard function.
Preferably, above-mentioned X, gamma-rays protection non-woven fabrics preparation method in, it is anti-according to the x-ray radiation
The unleaded powder of protective function prepares X, gamma-rays protection non-woven fabrics, including：
The unleaded powder of the x-ray radiation safeguard function and silane coupling agent are uniformly mixed, a small amount of water is added dropwise, machinery
Stirring 1~1.5 hour, be added dissaving polymer continue stirring obtain within 1~2 hour modified x-ray radiation safeguard function without
Lead powder body；
The PE components of the x-ray radiation safeguard function unleaded powder modified using addition, PP components are as binder fibre
X, gamma-rays protection non-woven fabrics are prepared with carrier fibre.
Preferably, above-mentioned X, gamma-rays protection non-woven fabrics preparation method in, the PE be fiber Pi Qixiang
Be 2.5~45.0, PP to viscosity be the core of fiber its inherent viscosity not less than the mass ratio shared by powder in 0.64, PP it is 20%
Mass ratio in~40%, PE shared by powder is 20%~40%, and the content of fibre fractionation is：The mass percent of PP be 15~
85%, the mass percent of PE is 85~15%；
When preparing X, gamma-rays protection non-woven fabrics, PE is with 200~230 DEG C, and 5.0~35.0MPa, PP is with 235~265
DEG C, 15~35.0MPa；Cooling wind temperature, humidity, speed is respectively 15~28 DEG C, 75~100%, 0.8~2.5m/s；Spinning
400~1000m/min of speed；Water-bath draft temperature is 70~80 DEG C, and water-bath drafting multiple is 3.5~4.5, then through 90~110
DEG C steam drafting, steam drafting multiple are 1.1~1.5.
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 is added to by the way that silane coupling agent and dissaving polymer are modified in spinning polymer, not only effectively
Ground, which solves, in the prior art directly asks the bad dispersibility of function powder present in function powder addition spinning solution and reunion
Topic, and the compatibility due to improving powder and polymer after modification, to improve function powder in polymer
The unleaded core-skin fibre of additive amount, preparation not only has good physical mechanical property, textile process performance kimonos performance, also
High, the good advantage of persistence with X, gamma ray shielding rate, can be widely applied to make Long Term Contact X, gamma-ray work people
The clothes and Non-Woven Fabric Industry of member, have good economic benefit and social benefit.
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 a kind of X, gamma-rays protection non-woven fabrics 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 of the preparation method of gamma-rays protection non-woven fabrics is illustrated
Figure.The method can be as follows.The method includes：The graphene oxide containing intermediary water is prepared, such as the step in Fig. 1
Shown in S101；The first graphene oxide powder of intercalation bismuth tungstate, such as Fig. 1 are prepared according to the graphene oxide containing intermediary water
In step S103 shown in；Intercalation europium oxide, samarium oxide, gadolinium oxide and oxidation are prepared according to first graphene oxide powder
Step S105 in the second graphene oxide powder such as Fig. 1 of barium；It is aoxidized according to first graphene oxide powder and second
Graphene powder prepares the unleaded powder of x-ray radiation safeguard function, such as the step S107 in Fig. 1；And it is penetrated according to the X-
The unleaded powder of beta radiation safeguard function prepares X, gamma-rays protection non-woven fabrics, as shown in 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 protection non-woven fabrics according to the unleaded powder of the x-ray radiation safeguard function.
Specifically, the unleaded powder of the x-ray radiation safeguard function and silane coupling agent are uniformly mixed, it is added dropwise a small amount of
Water, mechanical agitation 1~1.5 hour are added dissaving polymer and continue stirring to obtain within 1~2 hour modified x-ray radiation anti-
The unleaded powder of protective function；
The PE components of the x-ray radiation safeguard function unleaded powder modified using addition, PP components are as binder fibre
X, gamma-rays protection non-woven fabrics are prepared with carrier fibre.
Wherein, it be 2.5~45.0, PP is that the core of fiber its inherent viscosity is not low that the PE, which is the skin of fiber its relative viscosity,
Mass ratio in 0.64, PP shared by powder is that the mass ratio in 20%~40%, PE shared by powder is 20%~40%, fiber
The content of component is：The mass percent of PP is 15~85%, the mass percent of PE is 85~15%；
When preparing X, gamma-rays protection non-woven fabrics, PE is with 200~230 DEG C, and 5.0~35.0MPa, PP is with 235~265
DEG C, 15~35.0MPa；Cooling wind temperature, humidity, speed is respectively 15~28 DEG C, 75~100%, 0.8~2.5m/s；Spinning
400~1000m/min of speed；Water-bath draft temperature is 70~80 DEG C, and water-bath drafting multiple is 3.5~4.5, then through 90~110
DEG C steam drafting, steam drafting multiple are 1.1~1.5.
Next, being illustrated with a specific embodiment.
First, it takes a certain amount of expanded graphite and suitable concentrated sulfuric acid to be placed in glass container, is sufficiently stirred under ice-water bath；
A certain amount of potassium permanganate is slowly added to until potassium permanganate total overall reaction, adds a certain amount of deionized water in certain temperature
Lower mechanical agitation, is added a certain amount of hydrogen peroxide after mixing, and solution becomes glassy yellow by brownish black；With hydrochloric acid and go from
Cleaning solution obtains graphene oxide to neutrality under the conditions of sub- water Centrifugal dispersion.
Secondly, take the graphene oxide of above-mentioned preparation in hydrothermal reaction kettle, ultrasound, which is made, under the conditions of certain temperature contains layer
Between water graphene oxide.
Then, a certain amount of five water bismuth nitrate is dissolved in a certain amount of dust technology, with vigorous stirring, by nitrate
Solution is slowly added into the aqueous solution of a certain amount of sodium tungstate, adds a certain amount of graphene oxide solution, and hydrogen-oxygen is added
Change sodium solution and adjust PH to 5~5.5, polyethylene glycol is added and stirs 6~10 hours, obtained gel washs with ethyl alcohol, 40~60
DEG C drying, 300~500 DEG C calcining, obtain the first graphene oxide powder of intercalation bismuth tungstate.
Next, it is a certain amount of to have a certain amount of europium nitrate, gadolinium nitrate, samaric nitrate, barium sulfate mixed solution to be added to
In graphene oxide solution, a certain amount of ammonium hydroxide strength ultrasound is added 2~4 hours, is transferred to 100~300 in hydrothermal reaction kettle
DEG C temperature condition under 1~48h of hydro-thermal reaction, obtained solution washs with ethyl alcohol, 40~60 DEG C of drying, using 900~
1200 DEG C of calcinings, obtain the 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 3：1~5：1 molar ratio is uniform
It mixes up to x-ray radiation safeguard function powder.
Next, x-ray radiation safeguard function powder and silane coupling agent are uniformly mixed, a small amount of water is added dropwise, machinery stirs
It mixes 1~1.5 hour, addition dissaving polymer continues stirring and obtains within 1~2 hour modified x-ray radiation safeguard function powder
Body.
Finally, using the PE components of the modified x-ray radiation safeguard function powder powder of addition, PP components as viscous
Condensating fiber and carrier fibre prepare PE/PP core-sheath compound fibres.
A kind of X provided by the embodiments of the present application, gamma-rays protection non-woven fabrics preparation method in, be with expanded graphite
Raw material prepares graphene oxide solution；Using five water bismuth nitrates and sodium tungstate as raw material, the in-situ preparation between graphene oxide layer
Bismuth tungstate obtains the graphene oxide of intercalation sheet bismuth tungstate, and washed, dry, calcining obtains the first oxidation of intercalation bismuth tungstate
Graphene powder；Using europium nitrate, gadolinium nitrate, samaric nitrate, barium sulfate as raw material be made intercalation europium oxide, samarium oxide, gadolinium oxide and
Second graphene oxide powder of barium monoxide；First graphene oxide powder and the second graphene oxide powder are mixed, utilized
Silane coupling agent and modified be added in PE components, PP components of dissaving polymer are prepared with anti-X, gamma Rays work(
The PE/PP core-sheath compound fibres of energy.The additive amount of function powder is carried in prepared PE/PP core-sheath compound fibres
Height, fiber not only have good physical mechanical property, textile process performance kimonos performance, also have X, gamma ray shielding rate
Height, persistence is good, and unleaded light-weighted advantage has good application prospect in terms of X, gamma Rays protection.
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.
Above is only an example of the present application, it is not intended to limit this application.For those skilled in the art
For, the application can have various modifications and variations.It is all within spirit herein and principle made by any modification, equivalent
Replace, improve etc., it should be included within the scope of claims hereof.
Claims (10)
1. the preparation method of a kind of X, gamma-rays protection non-woven fabrics, 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 protection non-woven fabrics are prepared according to the unleaded powder of the x-ray radiation safeguard function.
2. the preparation method of X according to claim 1, gamma-rays protection non-woven fabrics, which is characterized in that prepare and contain interlayer
The graphene oxide of 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 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 protection non-woven fabrics, which is characterized in that the puffing stone
Ink is 1 with concentrated sulfuric acid mass ratio:30~1:40, the mass ratio of the expanded graphite and potassium permanganate is 1:1~1:6, it is described swollen
The mass ratio of graphite and hydrogen peroxide is 1:3~1:10, the volume ratio of hydrochloric acid and deionized water in second mixed solution
It is 1:5~1:10；
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 protection non-woven fabrics, which is characterized in that contained according to described
The graphene oxide of intermediary 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 protection non-woven fabrics, which is characterized in that the bismuth nitrate
Mass ratio with dust technology is 1:2~1:5, the mass ratio of the bismuth nitrate and sodium tungstate is 3:1-5:1, the bismuth nitrate and oxygen
The mass ratio of graphite alkene is 1:2~1:5, a concentration of 0.01M~0.1M of the cetyltrimethylammonium bromide, the nitre
The mass ratio of sour bismuth and 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 protection non-woven fabrics, which is characterized in that according to described
One graphene oxide powder prepares the second graphene oxide powder of intercalation europium oxide, samarium oxide, gadolinium oxide and barium monoxide, packet
It includes：
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 protection non-woven fabrics, which is characterized in that the nitric acid
The mass component ratio of europium nitrate is in europium, gadolinium nitrate, samaric nitrate, barium sulfate mixed solution：30%~40%；The quality of gadolinium nitrate
Ingredient ratio is 30%~40%；The mass component ratio of the samaric nitrate is 10%~20%；The mass component ratio of the barium sulfate
It 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 protection non-woven fabrics, which is characterized in that according to described
One graphene oxide 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 protection non-woven fabrics, which is characterized in that according to the X-
The unleaded powder of ray radiation safeguard function prepares X, gamma-rays protection non-woven fabrics, including：
The unleaded powder of the x-ray radiation safeguard function and silane coupling agent are uniformly mixed, a small amount of water, mechanical agitation 1 is added dropwise
~1.5 hours, addition dissaving polymer continued stirring and obtains within 1~2 hour modified x-ray radiation safeguard function without lead powder
Body；
The PE components of the x-ray radiation safeguard function unleaded powder modified using addition, PP components are as binder fibre and load
Body fiber prepares X, gamma-rays protection non-woven fabrics.
10. the preparation method of X according to claim 9, gamma-rays protection non-woven fabrics, which is characterized in that the PE is
It is the core of fiber its inherent viscosity not less than shared by powder in 0.64, PP that its relative viscosity of the skin of fiber, which is 2.5~45.0, PP,
Mass ratio is that the mass ratio in 20%~40%, PE shared by powder is 20%~40%, and the content of fibre fractionation is：The quality of PP
Percentage is 15~85%, the mass percent of PE is 85~15%；
When preparing X, gamma-rays protection non-woven fabrics, PE with 200~230 DEG C, 5.0~35.0MPa, PP with 235~265 DEG C,
15~35.0MPa；Cooling wind temperature, humidity, speed is respectively 15~28 DEG C, 75~100%, 0.8~2.5m/s；Spinning speed
400~1000m/min；Water-bath draft temperature is 70~80 DEG C, and water-bath drafting multiple is 3.5~4.5, then is steamed through 90~110 DEG C
Vapour drawing-off, steam drafting multiple are 1.1~1.5.
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| CN110565205A (en) * | 2019-09-08 | 2019-12-13 | 中山市蝶安芬内衣有限公司 | preparation method and application of fat-reducing functional fiber |
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| CN114038602A (en) * | 2021-09-16 | 2022-02-11 | 武汉市莎卡娜尔科技有限公司 | Radiation protection material for inorganic fiber one-dimensional multi-element nano-micron composite crystal |
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| CN110565205A (en) * | 2019-09-08 | 2019-12-13 | 中山市蝶安芬内衣有限公司 | preparation method and application of fat-reducing functional fiber |
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| CN111235694A (en) * | 2020-03-23 | 2020-06-05 | 旷达纤维科技有限公司 | Graphene composite negative ion polyester fiber |
| CN112900155A (en) * | 2021-02-08 | 2021-06-04 | 南通大学 | Preparation method of non-woven fabric for X and gamma ray protection |
| CN114038602A (en) * | 2021-09-16 | 2022-02-11 | 武汉市莎卡娜尔科技有限公司 | Radiation protection material for inorganic fiber one-dimensional multi-element nano-micron composite crystal |
| CN115305598A (en) * | 2022-08-23 | 2022-11-08 | 中国核动力研究设计院 | Core-shell structure shielding material and preparation method thereof |
| CN115785585A (en) * | 2023-02-09 | 2023-03-14 | 中星(广州)纳米材料有限公司 | Neutron and gamma ray shielding material, preparation method and application |
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Effective date of registration: 20201211 Address after: 213000 No.23 Lingxiang Road, Wujin economic development zone, Changzhou City, Jiangsu Province Patentee after: Changzhou Jinxinda fiber new material Co.,Ltd. Address before: 226019 Jiangsu city of Nantong province sik Road No. 9 Patentee before: NANTONG University |
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Address after: 213000 No.23 Lingxiang Road, Wujin economic development zone, Changzhou City, Jiangsu Province Patentee after: Jiangsu Jinxinda fiber new material Technology Group Co.,Ltd. Address before: 213000 No.23 Lingxiang Road, Wujin economic development zone, Changzhou City, Jiangsu Province Patentee before: Changzhou Jinxinda fiber new material Co.,Ltd. |