CN109399639A - A kind of preparation method of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle - Google Patents
A kind of preparation method of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle Download PDFInfo
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Abstract
The invention belongs to new method fields prepared by medication chemistry nano material, and in particular to a kind of preparation method of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle.This method uses fatty acid salt for the first time and cationic surfactant forms mixed surfactant and as template molecule, it is the polymer of silica by adjusting the adjustable preparation dispersibility of usage amount and the good spherical mesoporous silicon nanoparticle (less than 100 nanometers) of roundness and ball shaped nano silicon particle (about 200 nanometers or more), chemical nature of silicon precursor agent.Preparation method mild condition of the invention, environmental protection, is easy to amplify production, and obtained product structure is stablized, favorable dispersibility, and the carrier that can be used as slightly solubility and biopharmaceutical macromolecular drug uses.
Description
Technical field
The invention belongs to new method fields prepared by medication chemistry nano material, and in particular to a kind of regulation ball shaped nano
The preparation method of silicon particle and spherical mesoporous silicon nanoparticle.
Background technique
Nanometer material (particle size is less than 500 nanometers) has more technological merit, such as higher compares table
Area and pore volume, good colloidal stability, excellent biocompatibility etc..In addition, the size of particle, mesoporous pore size and shape
Looks are adjustable, can also make its functionalization inside particle surface and hole by chemical modification, thus field of biomedicine (at
As diagnosis, bioprobe, biocatalysis, Bone Defect Repari, bracket engineering, pharmaceutical carrier etc.) there is extensive and important application prospect.
The good adsorption delivered payload capability of meso-porous nano silicon materials has become the candidate of catalyst and drug molecule carrier
Person causes extensive interest in relevant application field.Common meso-porous nano silicon materials, such as MCM-41, duct are whole
It is arranged in parallel structure of hexagonal crystal, about 2-3 nanometers of aperture, is suitble to absorption small molecule compound.But exploitation can adjust difference
Size, different pore size and dispersibility and the preparation method of the good silicon nanoparticle of roundness are still challenging.Therefore
The preparation method for meeting requirements above is developed as project urgently to be resolved at present.
Summary of the invention
The existing reported method for preparing mesoporous nano silicon mostly uses the alkali in template molecule (mostly surfactant)
Property solution in be added silicon precursor agent reaction method, granule roundness is not good enough, it is difficult to relatively largely regulate and control preparation received having a size of 100
Rice or particle below.Ball shaped nano silicon particle is only then in alkaline solution (such as alcohol water mixed solution containing ammonium hydroxide)
Silicon precursor agent reaction preparation is added, particle size is larger (can reach micron order).In view of the existing technical defect, of the invention
Be designed to provide it is a kind of regulate and control prepare spherical mesoporous silicon nanoparticle and ball shaped nano silicon particle method, this method is for the first time
Using fatty acid salt and cationic surfactant formation mixed surfactant and as template molecule, by adjusting silicon precursor
The usage amount of agent adjustable preparation dispersibility and the good spherical mesoporous silicon nanoparticle of roundness (are less than or close to 100
Nanometer) and ball shaped nano silicon particle (150 nanometers or more than), chemical nature for silica polymer.
To achieve the goals above, the present invention adopts the following technical scheme that.
A method of adjusting preparation has mesoporous ball shaped nano silicon particle and ball shaped nano silicon particle, and this method utilizes
Cetyl trimethyl ammonium halide, positive esters of silicon acis, fatty acid salt and deionized water prepare surface and contain Jie as reaction raw materials
The molar ratio of hole or non-porous ball shaped nano silicon particle, the fatty acid salt and cetyl trimethyl ammonium halide is 0. 25:
1 - 4:1。
A method of it prepares with mesoporous ball shaped nano silicon particle and ball shaped nano silicon particle, specific preparation method is such as
Under.
Step 1 mixes cetyl trimethyl ammonium halide, fatty acid salt with deionized water in proportion, and heating, constant temperature are permanent
Fast magnetic agitation makes it completely dissolved.
Pasc reaction precursor agent is added in step 2.
Step 3, reaction time are 2-16 hours；12000 revs/min or more are centrifuged at least 5 minutes, abandon supernatant；With water or
Methanol or ethyl alcohol disperse again, are centrifuged, repeated washing 2-3 times, dry, obtain product.
Fatty acid salt (the C of the step 1nH2n-1O2-) whether mesoporous be divided into: mesoporous sphere nano-silicon is contained according to product
The single-stranded fatty acid salt that particle requirement carbon number is two to ten；It is two to four single-stranded rouge that ball shaped nano silicon particle, which requires carbon number,
Fat hydrochlorate.
The fatty acid salt of the step 1 is the salt containing lithium, sodium, potassium, caesium, magnesium, calcium, strontium, barium, manganese, zinc or aluminium.
The cetyl trimethyl ammonium halide of the step 1 is cetyl trimethylammonium bromide (CTAB) or cetyl
Trimethyl ammonium chloride (CTAC).
The pasc reaction precursor agent of the step 2 is ethyl orthosilicate, methyl orthosilicate, 1,2- bis- (triethoxysilicane) ethane
Etc. inorganic or organic silicon source.
Whether the volume ratio (v:v) of the step 2 pasc reaction precursor agent and deionized water contains mesoporous be divided into according to product:
Mesoporous sphere silicon nanoparticle is 1:100 ~ 1:50.
Ball shaped nano silicon particle be 1:16.6 or more than.
The reaction temperature is 95 DEG C ± 5 DEG C.
Existing meso-porous nano silicon particle is mainly prepared by template, i.e., with surfactant (such as cetyl front three
Base ammonium halide, P123 etc.) with silicon precursor agent be added under alkaline condition react preparation after water mixing, different pore size and grain can be obtained
The spherical mesoporous nano-silicon of diameter.Present invention uses the hybrid template molecular fat hydrochlorate different from reported method,
Contain hydrophobic carbochain in molecular structure, is in aqueous solution alkalescent, can be adjusted according to the dosage of silicon precursor agent and be catalyzed life
At spherical nanometer particle and ball shaped nano silicon particle.The present invention has following technical advantage.
(1) production cost is low, and environmental protection easy to operate, easy expanding production: the present invention is prepared in water phase, and the original used
Material includes that fatty acid salt, cetyl trimethyl ammonium halide, silicon precursor agent etc. are relatively environment-friendly reaction reagent.Prepare item
Part can be amplified in proportion by embodiment.
(2) product has good dispersibility, and particle diameter distribution is uniform, and roundness is good and pore structure is uniform.
(3) carrier or filler that can be used as drug, catalyst molecule of medicine or chemical field etc. use.
Detailed description of the invention
Fig. 1 is spherical mesoporous nano-silicon transmission electron microscope photo prepared by embodiment 1.
Fig. 2 is spherical mesoporous nano-silicon transmission electron microscope photo prepared by embodiment 2.
Fig. 3 is spherical mesoporous nano-silicon transmission electron microscope photo prepared by embodiment 3.
Fig. 4 is ball shaped nano silicon transmission electron microscope photo prepared by embodiment 4.
Fig. 5 is spherical mesoporous nano-silicon transmission electron microscope photo prepared by embodiment 5.
Fig. 6 is spherical mesoporous nano-silicon transmission electron microscope photo prepared by embodiment 6.
Fig. 7 is the spherical mesoporous nano-silicon transmission electron microscope photo that reaction temperature is 80 DEG C of preparations.
Fig. 8 be sodium acetate and cetyl trimethyl ammonium halide molar ratio be 1:1 preparation spherical mesoporous nano-silicon it is saturating
Penetrate electromicroscopic photograph.
Fig. 9 be sodium acetate and cetyl trimethyl ammonium halide molar ratio be 2:1 preparation spherical mesoporous nano-silicon it is saturating
Penetrate electromicroscopic photograph.
Figure 10 is the spherical mesoporous nano-silicon transmission electricity that the molar ratio of sodium acetate and cetyl trimethyl ammonium halide is 4:1
Mirror photo.
Figure 11 is the dendroid nano-silicon transmission electron microscope that the molar ratio of Sodium Caprylate and cetyl trimethyl ammonium halide is 1:1
Photo.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and examples, but following embodiments are not intended to limit right model of the invention
It encloses.
Embodiment 1.
1.5 grams of cetyl trimethylammonium bromides and 0.17 gram of sodium acetate (molar ratio 1:0.5) are added to 100 milliliters
In deionized water, stirring and dissolving 30 minutes at 95 DEG C, 2 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, and 12000
Rev/min centrifugation 20 minutes, abandon supernatant；With 20 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times is dry, obtains grain
The spherical mesoporous silicon silicon nanoparticle (Fig. 1) that diameter is 76 ± 5 nanometers.
Embodiment 2.
1.5 grams of cetyl trimethylammonium bromides and 0.17 gram of sodium acetate (molar ratio 1:0.5) are added to 100 milliliters
In deionized water, stirring and dissolving 30 minutes at 95 DEG C, 4 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, and 12000
Rev/min centrifugation 20 minutes, abandon supernatant；With 20 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times is dry, obtains grain
The spherical mesoporous silicon nanoparticle (Fig. 2) that diameter is 97 ± 4 nanometers.
Embodiment 3.
1.5 grams of cetyl trimethylammonium bromides and 0.23 gram of sodium butyrate (molar ratio 1:0.5) be added to 100 milliliters go from
In sub- water, stirring and dissolving 30 minutes at 95 DEG C, 2 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, and 12000 revs/min
Supernatant is abandoned in centrifugation 20 minutes；With 20 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, obtains partial size and received for 89 ± 5
The spherical mesoporous silicon nanoparticle (Fig. 3) of rice.
Embodiment 4.
1.5 grams of cetyl trimethylammonium bromides and 0.23 gram of sodium butyrate (molar ratio 1:0.5) be added to 100 milliliters go from
In sub- water, stirring and dissolving 30 minutes at 95 DEG C, 10 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, 12000 turns/
Supernatant is abandoned in the separation heart 10 minutes；With 20 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 time, obtain partial size for 164 ±
9 nanometers of ball shaped nano silicon particle (Fig. 4).
Embodiment 5.
1.5 grams of cetyl trimethylammonium bromides and 0.29 gram of sodium n-caproate (molar ratio 1:0.5) be added to 100 milliliters go from
In sub- water, stirring and dissolving 30 minutes at 95 DEG C, 2 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, and 12000 revs/min
Supernatant is abandoned in centrifugation 20 minutes；With 20 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, dry, obtaining partial size is
107 ± 7 nanometers of spherical mesoporous silicon nanoparticle (Fig. 5).
Embodiment 6.
1.5 grams of cetyl trimethylammonium bromides are added to 100 milliliters with 0.3457 gram of Sodium Caprylate (molar ratio 1:0.5) and go
In ionized water, stirring and dissolving 30 minutes at 95 DEG C, 2 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, 12000 turns/
Supernatant is abandoned in the separation heart 10 minutes；With 20 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, dry, obtaining partial size is
111 ± 6 nanometers of dendroid silicon nanoparticle (Fig. 6).
The screening experiment of reaction condition.
1) screening of reaction temperature.
Differential responses temperature has a significant impact the dispersibility of nano-particle product, and ideal temperature is 95 DEG C ± 5 DEG C, reduces
Temperature can lead to product dispersibility variation, be the product electromicroscopic photograph (Fig. 7) at 80 DEG C below.
1.5 grams of cetyl trimethylammonium bromides and 0.17 gram of sodium acetate (molar ratio 1:0.5) are added to 100 milliliters
In deionized water, stirring and dissolving 30 minutes at 80 DEG C, 2 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, and 12000
Rev/min centrifugation 20 minutes, abandon supernatant；With 20 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times is dry, is divided
Dissipate the poor product (Fig. 7) of property.
As seen from Figure 7, when reaction temperature is reduced to 80 DEG C (Fig. 7), silicon nanoparticle each other produce compared with
The dispersibility of more adhesions, particle is obviously identical not as good as 1 other conditions of embodiment, the preparation result (Fig. 1) that temperature is 95 DEG C.
2) screening of sodium soap and cetyl trimethylammonium bromide molar ratio.
1.5 grams of cetyl trimethylammonium bromides are added to 100 milliliters with 0.34 gram of sodium acetate (molar ratio 1:1) and go
In ionized water, stirring and dissolving 30 minutes at 95 DEG C, 2 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, 12000 turns/
Supernatant is abandoned in the separation heart 20 minutes；With 20 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, dry, obtaining partial size is
79 ± 5 nanometers of spherical mesoporous silicon silicon nanoparticle (Fig. 8).
1.5 grams of cetyl trimethylammonium bromides are added to 100 milliliters with 0.68 gram of sodium acetate (molar ratio 1:2) and go
In ionized water, stirring and dissolving 30 minutes at 95 DEG C, 2 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, 12000 turns/
Supernatant is abandoned in the separation heart 10 minutes；With 20 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, dry, obtaining partial size is
77 ± 6 nanometers of spherical mesoporous silicon silicon nanoparticle (Fig. 9).
1.5 grams of cetyl trimethylammonium bromides are added to 100 milliliters with 1.36 grams of sodium acetates (molar ratio 1:4) and go
In ionized water, stirring and dissolving 30 minutes at 95 DEG C, 2 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, 12000 turns/
Supernatant is abandoned in the separation heart 10 minutes；With 20 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times, dry, obtaining partial size is
88 ± 9 nanometers of spherical mesoporous silicon silicon nanoparticle (Figure 10).
It is this model of 0.5:1 ~ 4:1 that the present invention, which tests fatty acid salt and the molar ratio of cetyl trimethyl ammonium halide,
Enclose the influence to product.Fatty acid salt has alkalescent, while having the function of adjusting product and catalysis reaction, the too low meeting of dosage
Lead to reaction not exclusively (such as ratio is lower than 0.25:1).As shown in Fig. 8, Fig. 9 and Figure 10, compares and (implement together with embodiment 1
The molar ratio of 1 result figure 1 of example, sodium acetate and cetyl trimethyl ammonium halide is respectively 0.5:1) as can be seen that fixing other
Reaction condition, when increasing to 4:1 with the molar ratio of sodium acetate and cetyl trimethyl ammonium halide, the partial size of product nano silicon
Slightly increase (88 ± 9 nanometers), dispersibility and roundness have little effect, and the ratio for continuing growing fatty acid salt must not then
It wants.This conclusion is only limitted to the case where sodium acetate and sodium butyrate, and the influence about fatty acid salt carbon chain lengths is as detailed below.
3) screening of silicon precursor agent dosage.
Whether the volume ratio (v:v) of pasc reaction precursor agent and deionized water contains mesoporous be divided into according to product: containing mesoporous
Ball shaped nano silicon particle be 1:100 ~ 1:50；Ball shaped nano silicon particle is 1:16.6 or more.
The dosage for increasing silicon precursor agent in the preparation of spherical mesoporous silicon nanoparticle can increase particle size, such as implement
Example 1 and embodiment 2, increasing silicon precursor agent dosage can make particle size increase to 97 ± 4 nanometers from 76 ± 5 nanometers to 2 times.After
The continuous dosage for increasing silicon precursor agent can then be such that partial size further increases, and surface pore further reduces, and generate ball shaped nano silicon
Grain (such as embodiment 4, partial size are 164 ± 9 nanometers).
4) screening of the fatty acid salt of different carbon chain lengths.
The fatty acid salt of different carbon chain lengths has larger impact to the pattern of product nano silicon.In higher silicon precursor agent
Under dosage, carbochain, which increases to six carbon or more, will lead to the dendritic silicon nanoparticle of generation.Such as shown in Figure 11, reaction condition is
1.5 grams of cetyl trimethylammonium bromides and 0.7 gram of Sodium Caprylate (molar ratio 1:1) are added into 100 ml deionized waters, in 95
Stirring and dissolving 30 minutes at DEG C, 6 milliliters of ethyl orthosilicates, which are added, and are stirred to react 2 hours terminates, and 6000 revs/min are centrifuged 10 minutes,
Abandon supernatant；With 20 milliliters of water or ethyl alcohol dispersion, centrifugation, repeated washing 2-3 times is dry, and obtaining partial size is 175 ± 14 nanometers
Dendroid silicon nanoparticle (Figure 11).
5) investigation of speed of agitator and centrifugal rotational speed time.
Experiments have shown that speed of agitator influences less the property of product, the constant range of speeds can from 100 revs/min to
700 revs/min.The magnetic agitation rotating speed of the reaction influences less product characteristics, appropriate.
Centrifugation step system after the reaction precipitates solid product from liquid, and the revolving speed time does not have
Rigid requirement.
Claims (8)
1. a kind of preparation method of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle, which is characterized in that this method
Using cetyl trimethyl ammonium halide, positive esters of silicon acis, fatty acid salt and deionized water as reaction raw materials, synthesize surface texture
For the ball shaped nano silicon particle of meso-hole structure, the molar ratio of the fatty acid salt and cetyl trimethyl ammonium halide is 0. 5:1
- 4:1。
2. a kind of preparation method of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle, which is characterized in that the preparation
Method the following steps are included:
Step 1 mixes cetyl trimethyl ammonium halide, fatty acid salt with deionized water in proportion, heating, constant temperature constant speed magnetic
Power stirring makes it completely dissolved；
Pasc reaction precursor agent is added in step 2；
Step 3, reaction time are 2-4 hours；12000 revs/min or more are centrifuged at least 5 minutes, abandon supernatant；With methanol or ethyl alcohol weight
New dispersion, centrifugation, repeated washing 2-3 times is dry, obtains product.
3. the preparation side of a kind of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle according to claim 2
Method, which is characterized in that the fatty acid salt (CnH of the step 12n-1O2-) whether mesoporous be divided into is contained according to product: containing mesoporous
It is two to ten two single-stranded fatty acid salt that the ball shaped nano silicon particle of carbon, which requires carbon number,；Ball shaped nano silicon particle requires carbon number
For two to four single-stranded fatty acid salt.
4. the preparation side of a kind of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle according to claim 2
Method, which is characterized in that the fatty acid salt of the step 1 is the salt containing lithium, sodium, potassium, caesium, magnesium, calcium, strontium, barium, manganese, zinc or aluminium.
5. the preparation side of a kind of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle according to claim 2
Method, which is characterized in that the cetyl trimethyl bromine ammonium halide of the step 1 is cetyl trimethylammonium bromide CTAB or ten
Six alkyl trimethyl ammonium chloride CTAC.
6. the preparation side of a kind of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle according to claim 2
Method, which is characterized in that the pasc reaction precursor agent of the step 2 is ethyl orthosilicate, methyl orthosilicate, 1,2- bis- (three
Ethyoxyl silicon) the inorganic or organic silicon source such as ethane.
7. the preparation side of a kind of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle according to claim 2
Method, which is characterized in that whether the volume ratio (v:v) of the step 2 pasc reaction precursor agent and deionized water contains Jie according to product
Hole is divided into: the ball shaped nano silicon particle containing mesoporous carbon is 1:100 ~ 1:50；Ball shaped nano silicon particle is 1:16.6 or more.
8. the preparation side of a kind of regulation ball shaped nano silicon particle and spherical mesoporous silicon nanoparticle according to claim 2
Method, which is characterized in that it is 95 DEG C ± 5 DEG C that reaction temperature is heated in the step 1.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865137A (en) * | 2005-05-18 | 2006-11-22 | 中国石油化工股份有限公司 | Nano silicon dioxide preparation method |
| CN101214965A (en) * | 2008-01-11 | 2008-07-09 | 北京化工大学 | Preparation method and application of macropore-mesoporous silicon dioxide hollow micro-sphere |
| CN101935044A (en) * | 2010-08-31 | 2011-01-05 | 浙江工业大学 | Method for preparing silicon oxide mesoporous material with green template agent |
| WO2011127218A2 (en) * | 2010-04-06 | 2011-10-13 | Ndsu Research Foundation | Liquid silane-based compositions and methods for producing silicon-based materials |
| CN103663478A (en) * | 2013-11-20 | 2014-03-26 | 华东师范大学 | Preparation method of mesoporous silica spherical nano particles with dendritic pore structure |
| CN104891511A (en) * | 2015-05-25 | 2015-09-09 | 华东师范大学 | Method for synthesizing mesoporous silicon dioxide nanoparticles by using alkali-free method |
| US20160251227A1 (en) * | 2013-09-13 | 2016-09-01 | Ndsu Research Foundation | Synthesis of si-based nano-materials using liquid silanes |
-
2019
- 2019-01-08 CN CN201910016304.XA patent/CN109399638A/en active Pending
- 2019-01-08 CN CN201910016879.1A patent/CN109399639A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865137A (en) * | 2005-05-18 | 2006-11-22 | 中国石油化工股份有限公司 | Nano silicon dioxide preparation method |
| CN101214965A (en) * | 2008-01-11 | 2008-07-09 | 北京化工大学 | Preparation method and application of macropore-mesoporous silicon dioxide hollow micro-sphere |
| WO2011127218A2 (en) * | 2010-04-06 | 2011-10-13 | Ndsu Research Foundation | Liquid silane-based compositions and methods for producing silicon-based materials |
| CN101935044A (en) * | 2010-08-31 | 2011-01-05 | 浙江工业大学 | Method for preparing silicon oxide mesoporous material with green template agent |
| US20160251227A1 (en) * | 2013-09-13 | 2016-09-01 | Ndsu Research Foundation | Synthesis of si-based nano-materials using liquid silanes |
| CN103663478A (en) * | 2013-11-20 | 2014-03-26 | 华东师范大学 | Preparation method of mesoporous silica spherical nano particles with dendritic pore structure |
| CN104891511A (en) * | 2015-05-25 | 2015-09-09 | 华东师范大学 | Method for synthesizing mesoporous silicon dioxide nanoparticles by using alkali-free method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113526515A (en) * | 2021-08-29 | 2021-10-22 | 浙江华飞电子基材有限公司 | Nano spherical silicon micro powder separation and extraction method |
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Application publication date: 20190301 |