CN105273190A - Polysulfide rubber nanoparticles and preparing method and application thereof - Google Patents
Polysulfide rubber nanoparticles and preparing method and application thereof Download PDFInfo
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- CN105273190A CN105273190A CN201510776808.3A CN201510776808A CN105273190A CN 105273190 A CN105273190 A CN 105273190A CN 201510776808 A CN201510776808 A CN 201510776808A CN 105273190 A CN105273190 A CN 105273190A
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- thiorubber
- nano microsphere
- polysulfide
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- photonic crystal
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Abstract
The invention discloses polysulfide rubber nanoparticles and a preparing method and application thereof. The molecular chain of the polysulfide rubber nanoparticles is of a macromolecular structure obtained through polycondensation of alkali metal polysulfide and polychloroalkanes, and the alkali metal polysulfide is of the structure M2Sx as shown in formula (I). The polysulfide rubber nanoparticles are prepared by adding water to an alkali metal polysulfide solution for dilution, then adding an organic solvent and a surfactant, adding stoichiometric polychloroalkanes, conducting stirring reaction to obtain polysulfide rubber nanoparticle original emulsion, conducting centrifugal separation and deionized water washing on the polysulfide rubber nanoparticle original emulsion, and conducting ternary cycle. The preparing method is simple, equipment is simple, operation is convenient, conditions are mild, the solvent is environmentally friendly and nontoxic, the prepared nanoparticles are high in monodispersity, photonic crystals can be prepared through self-assembly, the color of a photonic crystal structural color film can be controlled through the particle size of the nanoparticles, and the polysulfide rubber nanoparticles have realistic and potential application prospects in enriching the sources of materials for preparing photonic crystals and developing materials with special properties.
Description
Technical field
The present invention relates to a kind of thiorubber microballoon and preparation method thereof, and the method for photonic crystal structure color film is prepared in self-assembly.
Background technology
Photonic crystal is the periodic structure of the optics yardstick be arranged in by the material of different refractivity, similar with semiconductor crystal (electron crystal) modulation to electron wave function, can modulate the hertzian wave of respective wavelength owing to there is Bragg scattering formation photon band gap, making manipulation and control photon Design and manufacture photonic crystal and device thereof reach the dream controlling photon motion becomes possibility.Photonic crystal has a wide range of applications, as being used as to manufacture photonic crystal fiber, photon crystal wave-guide, photon crystal laser, photonic crystal sensors etc.Manually prepare photonic crystal method and have dielectric rod accumulation, precision optical machinery boring, colloidal solid self-assembled growth, colloidal solution self-assembled growth and semiconductor technology etc.Wherein relying on the self-assembly of colloidal solid to prepare photonic crystal is the easiest the most frequently used method at present.
Photonic crystal is generally by the 1-D photon crystal of the film preparation of inorganic (silicon-dioxide, titanium dioxide), organic or polymer material (polymethylmethacrylate, polystyrene) or the structure being self-assembled into two dimension or three-dimensional by its monodispersed microballoon.
At present, the material that photonic crystal is prepared in self-assembly mainly concentrates on a few materials such as silicon-dioxide, titanium dioxide, polymethylmethacrylate, polystyrene, urgently expands the scope of available materials.Macromolecular material is due to the diversity of its kind, and the controllability of structure properties and becoming prepares the selection of photonic crystal more heated door.But the macromolecular material being successfully used for preparing photonic crystal is at present only the several of the minority such as polymethylmethacrylate, polystyrene, urgently explores the method for the homogeneous microballoon of preparation of more how suitable macromolecule resin material and correspondence and assemble the method preparing photonic crystal.
Summary of the invention
The object of this invention is to provide a kind of thiorubber Nano microsphere and preparation method thereof.
Technical scheme of the present invention is as follows:
A kind of thiorubber Nano microsphere, its molecular chain is the macromolecular structure obtained through polycondensation by alkali metals polysulfide and polyhalogenide, and wherein said alkali metals polysulfide has the structure shown in formula I:
M
2S
x......(Ⅰ)
In formula I, M is Na
+, K
+, Li
+or Rb
+in one, x is the integer of 1 ~ 6;
Described polyhalogenide is C
1~ C
10the many chloroparaffins of straight chain, C
1~ C
10the many brominated alkanes of straight chain, C
1~ C
10the many chloroparaffins of side chain, C
1~ C
10the many brominated alkanes of side chain, dichloroethyl ether, 2,2'-bis-chloro-dimethylbenzene, 2,5-dichloromethyl thiophene, 2,2'-Dichloroethyl formal or xylylene dichlorides, the halo atom of described polyhalogenide is at least containing two.
Further, in technique scheme, state the x described in formula I and be preferably 2.
Further, in technique scheme, the particle diameter of described thiorubber Nano microsphere is 100nm ~ 2000nm, and be preferably 150 ~ 400nm, be more preferably 150 ~ 270nm, size distribution PDI is below 0.1.
The present invention also provides the preparation method of above-mentioned thiorubber Nano microsphere, comprises the steps:
(1) alkali metal hydroxide or alkali metalsulphide soluble in water, under agitation add stoichiometric sulphur powder, stirring reaction 0.5 ~ 2h at 50 DEG C ~ 100 DEG C, obtains the alkali metals polysulfide aqueous solution;
(2) the alkali metals polysulfide aqueous solution in step (1) adds water dilution, add organic solvent and tensio-active agent again, add stoichiometric polyhalogenide, 40 ~ 100 DEG C, 300 ~ 1500rpm/min stir under reaction 0.5 ~ 6h, obtain thiorubber Nano microsphere original emulsion, described organic solvent is ethanol, ethylene glycol or Diethylene Glycol;
(3) the thiorubber Nano microsphere original emulsion of step (2) is through centrifugation and deionized water wash, circulates three times, obtains thiorubber Nano microsphere.
In above-mentioned preparation method, alkali metal hydroxide or alkali metalsulphide and stoichiometric sulphur powder react and generate alkali metals polysulfide, the structure had as formula I of described alkali metals polysulfide, i.e. M in step (1)
2s
x.The method of the sulphur powder adding different chemical metering is adopted in the reaction system of step (1), can prepare different alkali metals polysulfide, the stoichiometric sulphur powder described in step (1) calculates according to formula (a) or formula (b):
6MOH+(2x+2)S→2M
2S
x+M
2S
2O
3+3H
2O(a)
M
2S+(x-1)S→M
2S
x(b)
Wherein, in formula (a) and formula (b), M is Na
+, K
+, Li
+or Rb
+in one; In formula (a) and formula (b), x is the integer of 1 ~ 6, and preferably x is 2.
Further, in above-mentioned preparation method, alkali metal hydroxide described in step (1) is the one in sodium hydroxide (NaOH), potassium hydroxide (KOH), lithium hydroxide (LiOH) or rubidium hydroxide (RbOH), preferred sodium hydroxide; Described alkali metalsulphide is sodium sulphite (Na
2s), potassium sulphide (Ka
2s), lithium sulfide (Li
2or rubidium sulfide (Rb S)
2s) one in, preferred sodium sulphite.
Further, in above-mentioned preparation method, described in step (1), temperature of reaction is preferably 100 DEG C, and the reaction times is preferably 1h.
Further, in above-mentioned preparation method, in stirring reaction described in step (2), stirring velocity is preferably 500 ~ 1000rpm/min, and temperature of reaction is preferably 70 DEG C, and the reaction times is preferably 6h.
Further, in above-mentioned preparation method, in step (2), the mol ratio of described alkali metals polysulfide and alkyl polyhalides is 1:1 ~ 1:0.1, is preferably 1:0.5; The concentration of described alkali metals polysulfide in reaction system is 0.01 ~ 1mol/L, is preferably 0.1mol/L.
Further, in above-mentioned preparation method, the ratio of solution total amount that in step (2), the add-on of described water forms with water and organic solvent is by volume 0.1 ~ 1.Namely water used and ethanol or, ethylene glycol, the cumulative volume of Diethylene Glycol is VmL, and the cumulative volume of water is V ' mL, and 0.1 < (V '/V) < 1, and described organic solvent is preferably ethanol.
Further, in above-mentioned preparation method, described polyhalogenide is C
1~ C
10the many chloroparaffins of straight chain, C
1~ C
10the many brominated alkanes of straight chain, C
1~ C
10the many chloroparaffins of side chain, C
1~ C
10the many brominated alkanes of side chain, dichloroethyl ether, 2,2'-bis-chloro-dimethylbenzene, 2,5-dichloromethyl thiophene, 2,2'-Dichloroethyl formals, one in xylylene dichlorides, preferred glyceryl trichloride, the halo atom of polyhalogenide is at least containing two; Described xylylene dichlorides comprise neighbour, or contraposition xylylene dichlorides.
Further, in above-mentioned preparation method, described tensio-active agent is the one in poloxamer, polyoxyethylene glycol phenyl ether, Sorbitan carboxylic ester, polyoxyethylene sorbitan acid esters, sodium alkyl benzene sulfonate, sodium alkyl naphthalene sulfonate; Wherein poloxamer preferably adopts as the one in PluronicF127, PluronicP123, PluronicF68, PLURONICS F87, poloxamer188, polyoxyethylene glycol phenyl ether preferably adopts as OP10 ~ 60, and Sorbitan carboxylic ester adopts as Span20 ~ 85, polyoxyethylene sorbitan acid esters preferably adopt as Tween20 ~ 85.
Further, in above-mentioned preparation method, institute's thiorubber Nano microsphere original emulsion is after three circulations of centrifugation and deionized water wash step in described step (3), ultrasonic disperse is prepared into the thiorubber Nano microsphere that concentration is 10 ~ 200g/L in the deionized water of certain volume, and concentration is preferably 50g/L.
Another object of the present invention is to provide photonic crystal of a kind of thiorubber Nano microsphere assembling and preparation method thereof.
A kind of photonic crystal, by particle diameter between 150nm ~ 500nm and the photonic crystal with periodically ordered structure that is self-assembled into of the single dispersing thiorubber Nano microsphere that size distribution PDI is less than 0.1.
A preparation method for photonic crystal, utilize heating volatilization assemble method to prepare photon crystal material, the temperature of wherein heating volatilization assembling is 25 DEG C ~ 80 DEG C.
Preparation method's preferred technical scheme of photonic crystal of the present invention is: be spread on substrate by the microballoon emulsion of 50g/L, heated substrate, and Heating temperature is 25 DEG C ~ 80 DEG C.
Preparation method's preferred substrate of photonic crystal of the present invention is glass substrate.
Beneficial effect of the present invention is: thiorubber Nano microsphere provided by the present invention is expanding greatly of applying traditional thiorubber, prepare microballoon method therefor simple, device is simple, easy to operate, the advantage that solvent is green non-poisonous, ratio simultaneously by regulating, the ratio of water and ethanol, temperature of reaction, surfactant concentration, sulphur contents etc. regulate the particle diameter of microballoon, the microballoon monodispersity of preparation is good, the method simple practical of photonic crystal is prepared in self-assembly, schemochrome film color can be regulated and controled by particle diameter, development for the abundant material source and property material of preparing photonic crystal has the application prospect of reality and potentiality.
Accompanying drawing explanation
The scanning electron microscope (SEM) photograph of Fig. 1 thiorubber Nano microsphere prepared by embodiment 41;
The infrared spectrogram of Fig. 2 thiorubber prepared by embodiment 41;
The scanning electron microscope (SEM) photograph of Fig. 3 thiorubber Nano microsphere prepared by embodiment 43;
Fig. 4 is the digital photograph that embodiment 103 assembling obtains photonic crystal structure color film;
Fig. 5 is the reflected light spectrogram that embodiment 103 assembling obtains photonic crystal structure color film;
Fig. 6 is the scanning electron microscope (SEM) photograph that embodiment 103 assembling obtains photonic crystal structure color film.
Embodiment
The following examples can make the present invention of those of ordinary skill in the art's comprehend, but do not limit the present invention in any way.In following embodiment, if no special instructions, the experimental technique used is ordinary method, and material therefor, reagent etc. all can be bought by chemical reagents corporation.
Embodiment 1
Sodium hydroxide method prepares sodium disulfide (Na
2s
2) solution: reaction unit is 250ml there-necked flask, with mechanical stirring, reflux condensing tube, thermometer and oil bath heating unit; Taking 4.0g sodium hydroxide is dissolved in the deionized water of 100ml, pours there-necked flask into and is heated to 100 DEG C, then takes 3.2g sublimed sulphur powder and add under violent mechanical stirring, reacts and obtains light brown sodium disulfide solution after 1 hour.
Embodiment 2 ~ 5
Sodium hydroxide method prepares other sodium polysulfide solution: reaction unit is 250ml there-necked flask, with mechanical stirring, reflux condensing tube, thermometer and oil bath heating unit; Taking 4.0g sodium hydroxide is dissolved in the deionized water of 100ml, pour there-necked flask into and be heated to 100 DEG C, take 4.26g, 5.33g, 6.4g, 7.46g sublimed sulphur powder more respectively to add under violent mechanical stirring, react and obtain the trisulfides sodium of deep mixed brown, sodium tetrasulfide, sodium pentosulfide, six sodium sulfide solutions respectively after 1 hour.
Embodiment 6 ~ 20
The preparation of other polysulfide solution: implementation method and synthesis condition are all identical with embodiment 1 ~ 5, just use the sodium hydroxide in the potassium hydroxide of equimolar amount, lithium hydroxide, rubidium hydroxide replacement embodiment 1 ~ 5, obtain corresponding potassium polysulfide, many lithium sulfides, many rubidium sulfides solution respectively.
Embodiment 21
Sodium sulfide method prepares sodium disulfide (Na
2s
2) solution: reaction unit is 250ml there-necked flask, with mechanical stirring, reflux condensing tube, thermometer and oil bath heating unit; Taking 2.6g sodium sulphite is dissolved in the deionized water of 100ml, pours there-necked flask into and is heated to 100 DEG C, then takes 1.07g sublimed sulphur powder and add under violent mechanical stirring, reacts and obtains sodium disulfide solution after 1 hour.
Embodiment 22 ~ 25
Sodium sulfide method prepares other sodium polysulfide solution: reaction unit is 250ml there-necked flask, with mechanical stirring, reflux condensing tube, thermometer and oil bath heating unit; Taking 2.6g sodium sulphite is dissolved in the deionized water of 100ml, pour there-necked flask into and be heated to 100 DEG C, take 2.13g, 3.2g, 4.27g, 5.33g sublimed sulphur powder more respectively to add under violent mechanical stirring, to react after 1 hour respectively trisulfides sodium, sodium tetrasulfide, sodium pentosulfide, six sodium sulfide solutions.
Embodiment 26 ~ 40
The preparation of other polysulfide solution: implementation method and synthesis condition are all identical with embodiment 21 ~ 25, just use the sodium sulphite in the potassium sulphide of equimolar amount, lithium sulfide, rubidium sulfide replacement embodiment 21 ~ 25, obtain corresponding potassium polysulfide, many lithium sulfides, many rubidium sulfides solution respectively.
Embodiment 41
The preparation of thiorubber Nano microsphere: reaction unit is be equipped with reflux condensing tube, the 500ml there-necked flask of thermometer and the heating kettle with magnetic agitation, 50ml sodium disulfide solution freshly prepd in embodiment 1 is transferred in there-necked flask reactor while hot, under stable magnetic agitation (800r/min), add 180ml deionized water and 70ml ethanol and be heated to 70 DEG C in advance, take 0.5gPluronicF127 and add reaction system, stir 10min, separately take 1.25g1, 2, 3-trichloropropane to add in reaction system at 70 DEG C and continues reaction 6h, after finally the original emulsion obtained being carried out " centrifugal-dispensing laundry-centrifugal-redispersion washing " circulation three times, be dispersed in 30ml deionized water, obtain stable aqueous microsphere to fall apart emulsion.
Prepared microballoon emulsion is carried out to the sign (Fig. 1) of particle diameter (Size), current potential (Zeta) and scanning electron microscope, the hydration particle diameter determining to have prepared thiorubber Nano microsphere is 232.9nm, PDI is 0.015, current potential is-23mv, and microballoon is regular monodisperse spherical.
By infrared spectra (Fig. 2), structural characterization is carried out to thiorubber.
Embodiment 42 ~ 45
The preparation of thiorubber Nano microsphere: implementation method and synthesis condition are all identical with embodiment 41, just change the consumption of wherein ethanol into 50ml, 60ml, 80ml, 90ml, other condition is identical with embodiment 41, prepares the particle diameter of microballoon, PDI sees the following form 1 and Fig. 3; The scanning electron microscope (SEM) photograph that Fig. 3 is ethanol consumption when being 60ml.
The particle diameter of the thiorubber microballoon prepared in table 1 embodiment 42 ~ 46 and size distribution
Embodiment 47 ~ 55
The preparation of thiorubber Nano microsphere: implementation method and synthesis condition are all identical with embodiment 41, just change tensio-active agent PluronicF127 used into PluronicP123, PluronicF68, PLURONICS F87, poloxamer188, OP-10, Span-80, Tween-80, Sodium dodecylbenzene sulfonate, sodium methylene bis-naphthalene sulfonate, other condition is identical with embodiment 41.
Embodiment 56 ~ 63
The preparation of thiorubber Nano microsphere: implementation method and synthesis condition are all identical with embodiment 41, just by used 1,2,3-trichloropropane changes ethylene dichloride, dichloroethyl ether, 2 respectively into, the chloro-dimethylbenzene of 2'-bis-, 2,5-dichloromethyl thiophene, 2,2'-Dichloroethyl formal, neighbour, or contraposition-xylylene dichlorides, other condition is identical with embodiment 41.
Embodiment 64 ~ 67
The preparation of thiorubber Nano microsphere: implementation method and synthesis condition are all identical with embodiment 41, just sodium disulfide solution in embodiment 1 used is changed into trisulfides sodium, sodium tetrasulfide, sodium pentosulfide, six sodium sulfide solutions prepared by embodiment 2 ~ 5, other condition is identical with embodiment 41.
Embodiment 68 ~ 102
The preparation of thiorubber Nano microsphere: implementation method and synthesis condition are all identical with embodiment 41, just sodium disulfide solution in embodiment 1 used is changed into polysulfide solution prepared by embodiment 6 ~ 40, other condition is identical with embodiment 41.
Embodiment 103
Thiorubber Nano microsphere photonic crystal is prepared in assembling: carried out heating assembling experiment, namely the particle diameter sprawling preparation in above-described embodiment 41 ~ 46 on clean sheet glass is respectively the microballoon emulsion of 175nm, 232nm and 280nm, volatilization assembling at 50 DEG C, wherein 280nm particle diameter emulsion assembling effect is as Fig. 4.The digital optical photograph of Fig. 4 to be 280nm particle diameter emulsion through heating assemble photonic crystal prepared, Fig. 5 and Fig. 6 is respectively reflected light spectrogram under 10 ° of input angles of the schemochrome film that obtains and film surface scanning electron microscope (SEM) photo.Result shows, the microballoon emulsion of 280nm particle diameter obtains red schemochrome film after adding assembling, reflection spectrum shows has obvious and sharp-pointed reflection peak at 645nm place, corresponding when this and red schemochrome film, simultaneously scanning electron microscope display microballoon be arranged as regular ordered structure.
Embodiment 104 ~ 162
Thiorubber Nano microsphere photonic crystal is prepared in assembling: identical with embodiment 102, employ heating construction from part, corresponding operational condition is also identical with embodiment 102, just to have selected in embodiment 46 ~ 101 the suitable microballoon emulsion of the particle diameter of preparation to carry out assembling to test, the microballoon emulsion that wherein size meets the requirement of light photon crystal all obtains the photonic crystal structure color film of corresponding different colours.
The particle diameter of the thiorubber Nano microsphere that the method for above-described embodiment 47-102 prepares is all within the scope of 100 ~ 2000nm, and PDI is in 0.1 ~ 0.001 scope.
Claims (9)
1. a thiorubber Nano microsphere, its molecular chain is the macromolecular structure obtained through polycondensation by alkali metals polysulfide and polyhalogenide, and wherein said alkali metals polysulfide has the structure shown in formula I:
M
2S
x(Ⅰ)
In formula I, M is Na
+, K
+, Li
+or Rb
+in one, x is the integer of 1 ~ 6;
Described polyhalogenide is C
1~ C
10the many chloroparaffins of straight chain, C
1~ C
10the many brominated alkanes of straight chain, C
1~ C
10the many chloroparaffins of side chain, C
1~ C
10the many brominated alkanes of side chain, dichloroethyl ether, 2,2'-bis-chloro-dimethylbenzene, 2,5-dichloromethyl thiophene, 2,2'-Dichloroethyl formal or xylylene dichlorides, the halo atom of described polyhalogenide is at least containing two.
2. thiorubber Nano microsphere according to claim 1, is characterized in that, the particle diameter of described thiorubber Nano microsphere is 100nm ~ 2000nm, and size distribution PDI is below 0.1.
3. the preparation method of thiorubber Nano microsphere as claimed in claim 1, is characterized in that, comprise the following steps:
(1) alkali metal hydroxide or alkali metalsulphide soluble in water, under agitation add stoichiometric sulphur powder, stirring reaction 0.5 ~ 2h at 50 DEG C ~ 100 DEG C, obtains the alkali metals polysulfide aqueous solution;
(2) the alkali metals polysulfide aqueous solution in step (1) adds water dilution, add organic solvent and tensio-active agent again, add stoichiometric polyhalogenide, 40 ~ 100 DEG C, 300 ~ 1500rpm/min stir under reaction 0.5 ~ 6h, obtain thiorubber Nano microsphere original emulsion, described organic solvent is ethanol, ethylene glycol or Diethylene Glycol;
(3) the thiorubber Nano microsphere original emulsion of step (2) is through centrifugation and deionized water wash, circulates three times, obtains thiorubber Nano microsphere.
4. the preparation method of thiorubber Nano microsphere according to claim 3, is characterized in that, described alkali metal hydroxide is the one in sodium hydroxide, potassium hydroxide, lithium hydroxide or rubidium hydroxide; Described alkali metalsulphide is the one in sodium sulphite, potassium sulphide, lithium sulfide or rubidium sulfide.
5. the preparation method of thiorubber Nano microsphere according to claim 3, is characterized in that, in step (2), the mol ratio of described alkali metals polysulfide and alkyl polyhalides is 1:1 ~ 1:0.1; The concentration of described alkali metals polysulfide in reaction system is 0.01 ~ 1mol/L.
6. the preparation method of thiorubber Nano microsphere according to claim 3, is characterized in that, the ratio of solution total amount that in step (2), the add-on of described water forms with water and organic solvent is by volume 0.1 ~ 1.
7. the preparation method of thiorubber Nano microsphere according to claim 3, it is characterized in that, described tensio-active agent is the one in poloxamer, polyoxyethylene glycol phenyl ether, Sorbitan carboxylic ester, polyoxyethylene sorbitan acid esters, sodium alkyl benzene sulfonate, sodium alkyl naphthalene sulfonate.
8. the photonic crystal based on thiorubber Nano microsphere as claimed in claim 1, it is characterized in that, by particle diameter between 150nm ~ 500nm and size distribution PDI is less than the photonic crystal with periodically ordered structure that the single dispersing thiorubber Nano microsphere of 0.1 is self-assembled into.
9. a preparation method for photonic crystal as claimed in claim 8., is characterized in that, utilize heating volatilization assemble method to prepare photonic crystal, the temperature of wherein heating volatilization assembling is 25 DEG C ~ 80 DEG C.
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Cited By (7)
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| CN109216668A (en) * | 2018-08-03 | 2019-01-15 | 河南师范大学 | A kind of spherical tio2 package lithium sulfide/sulphur composite material preparation method |
| CN109244383A (en) * | 2018-08-03 | 2019-01-18 | 河南师范大学 | A kind of preparation method of ant nest shape sulphur package lithium sulfide composite material |
| CN109400878A (en) * | 2018-11-08 | 2019-03-01 | 锦西化工研究院有限公司 | A kind of method for sulfur content of dissociating in reduction polysulfide rubber |
| CN110128887A (en) * | 2019-05-15 | 2019-08-16 | 安徽华文塑胶科技有限公司 | A kind of schemochrome membrane stabilizer and preparation method thereof |
| CN112159492A (en) * | 2020-08-29 | 2021-01-01 | 浙江理工大学 | Heat-resistant photonic crystal element nano-microsphere and preparation method thereof |
| CN112442213A (en) * | 2019-08-28 | 2021-03-05 | 广东广山新材料股份有限公司 | Phosphorus-containing flame retardant with halogen atoms and preparation method and application thereof |
| WO2024061218A1 (en) * | 2022-09-22 | 2024-03-28 | Jiangsu Cheeshine Performance Materials Co., Ltd. | Organic polysulfide, preparation method and use thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109216668A (en) * | 2018-08-03 | 2019-01-15 | 河南师范大学 | A kind of spherical tio2 package lithium sulfide/sulphur composite material preparation method |
| CN109244383A (en) * | 2018-08-03 | 2019-01-18 | 河南师范大学 | A kind of preparation method of ant nest shape sulphur package lithium sulfide composite material |
| CN109400878A (en) * | 2018-11-08 | 2019-03-01 | 锦西化工研究院有限公司 | A kind of method for sulfur content of dissociating in reduction polysulfide rubber |
| CN110128887A (en) * | 2019-05-15 | 2019-08-16 | 安徽华文塑胶科技有限公司 | A kind of schemochrome membrane stabilizer and preparation method thereof |
| CN112442213A (en) * | 2019-08-28 | 2021-03-05 | 广东广山新材料股份有限公司 | Phosphorus-containing flame retardant with halogen atoms and preparation method and application thereof |
| CN112159492A (en) * | 2020-08-29 | 2021-01-01 | 浙江理工大学 | Heat-resistant photonic crystal element nano-microsphere and preparation method thereof |
| WO2024061218A1 (en) * | 2022-09-22 | 2024-03-28 | Jiangsu Cheeshine Performance Materials Co., Ltd. | Organic polysulfide, preparation method and use thereof |
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