CN106179300A - For improveing nano titanium oxide of 3D printing consumables performance and preparation method thereof - Google Patents
For improveing nano titanium oxide of 3D printing consumables performance and preparation method thereof Download PDFInfo
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- CN106179300A CN106179300A CN201610510085.7A CN201610510085A CN106179300A CN 106179300 A CN106179300 A CN 106179300A CN 201610510085 A CN201610510085 A CN 201610510085A CN 106179300 A CN106179300 A CN 106179300A
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- printing consumables
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- 238000010146 3D printing Methods 0.000 title claims abstract description 28
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229960000583 acetic acid Drugs 0.000 claims abstract description 14
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 14
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 9
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 8
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 8
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008187 granular material Substances 0.000 claims abstract description 8
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims abstract description 8
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 4
- 238000003763 carbonization Methods 0.000 claims abstract description 4
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000029087 digestion Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 229920000747 poly(lactic acid) Polymers 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 206010008190 Cerebrovascular accident Diseases 0.000 description 1
- 206010058467 Lung neoplasm malignant Diseases 0.000 description 1
- 208000006011 Stroke Diseases 0.000 description 1
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004500 asepsis Methods 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002790 naphthalenes Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002685 pulmonary effect Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
- B01J37/0036—Grinding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0072—Preparation of particles, e.g. dispersion of droplets in an oil bath
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Ink Jet Recording Methods And Recording Media Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention provides a kind of nano titanium oxide for improveing 3D printing consumables performance and preparation method thereof.The method of the present invention comprises the steps: that (1) prepares solution A: instills in dehydrated alcohol by butyl titanate while stirring, is subsequently adding glacial acetic acid, stirs 0.5 1 hours；(2) preparation B solution: while stirring the chloride of gadolinium, praseodymium is respectively dropped in dehydrated alcohol, is subsequently adding glacial acetic acid, stir 0.5 1 hours；(3) solution B is poured slowly in solution A, makes gel；(4) the gel ageing that will be formed；(5) gel after ageing is put into drying in baking oven, form granule；(6) gained granule after drying is put in mortar and grind, then be placed in chamber type electric resistance furnace, carbonization half an hour, be continuously heating to 600～800 DEG C of roastings, obtain the nano titanium dioxide powder for improveing 3D printing consumables performance.The present invention crosses TiO2The Photocatalytic Degradation Property of material improves the properties of product of 3D printing consumables, reduces the harmful gas produced in its print procedure.
Description
Technical field:
The present invention relates to a kind of nano titanium oxide for improveing 3D printing consumables performance and preparation method thereof, belong to inorganization
Learn field of material technology.
Background technology:
All using ABS and PLA as matrix close to 95% for FDM consumptive material at present, its print temperature is generally on 220 DEG C of left sides
The right side, belongs to middle temperature FDM consumptive material.The current research of Illinois Polytechnics of the U.S. finds, uses ABS and PLA polymer to make
Printer ultra-fine grain (UFP) discharge capacity for plastic raw materials is higher, and emission index connects with using laser printer or burning cigarette
Closely.Owing to volume is small, UFP can be deposited on pulmonary and directly be absorbed in blood.UFP concentration is higher with pulmonary carcinoma, apoplexy
Development with symptoms of asthma is relevant, is not particularly pointed out the chemical composition of ABS and PLA emission in report, but existing before this
Prove that display ABS is poisonous, and PLA is the polymer with biocompatibility, is widely used in making medicament capsule.This just promotees
Make the improvement raw material of the 3D printed material that we develop a kind of low melting point, environment-protecting asepsis is harmful, shrinkage factor is little.
In in the past few decades, due to its potential using value in solving problem of environmental pollution, nanometer titanium dioxide
Titanium photocatalyst has attracted a lot of concern.But, pure nano titanium dioxide photocatalyst powder is also deposited in actual application
In many defects.
Summary of the invention:
It is an object of the invention to a kind of nano titanium oxide for improveing 3D printing consumables performance of the problem for above-mentioned existence
And preparation method thereof, pass through TiO2The Photocatalytic Degradation Property of material improves the properties of product of 3D printing consumables, such as ABS and PLA
Deng, reduce the harmful gas produced in its print procedure, simultaneously improvement shrinkage factor and toughness.
Above-mentioned purpose is realized by following technical scheme:
The preparation method of a kind of nano titanium oxide for improveing 3D printing consumables performance, the method comprises the steps:
(1) preparation solution A: instill in dehydrated alcohol by butyl titanate while stirring, is subsequently adding glacial acetic acid, and 0.5-1 is little in stirring
Time, wherein in butyl titanate, dehydrated alcohol, the mol ratio of glacial acetic acid be 1:6:2；
(2) preparation B solution: while stirring the chloride of gadolinium, praseodymium is respectively dropped in dehydrated alcohol, is subsequently adding glacial acetic acid, stir
Mix 0.5-1 hour, wherein in gadolinium, praseodymium, dehydrated alcohol, the mol ratio of glacial acetic acid be 1:0.5:3:1；
(3) solution B is poured slowly in solution A, instilling hydrochloric acid solution regulation pH value and be equal to 4, continuing stirring, until becoming solidifying
Glue, stops stirring；
(4) the gel filter paper formed is sealed rear chamber temperature still aging；
(5) gel after ageing is put into drying in baking oven, form granule；
(6) gained granule after drying is put in mortar and grinds, then be placed in chamber type electric resistance furnace, in stove, ensure have air to enter,
It is to slowly warm up to 250 DEG C with the heating rate of 10～20 DEG C/min, carbonization half an hour, is continuously heating to 600～800 DEG C of roastings,
Obtain the nano titanium dioxide powder for improveing 3D printing consumables performance.
The preparation method of the described nano titanium oxide for improveing 3D printing consumables performance, dries described in step (5)
Dry temperature is 77～82 DEG C.
The preparation method of the described nano titanium oxide for improveing 3D printing consumables performance, roasts described in step (6)
The burning time is 3～5 hours.
The preparation method of the described nano titanium oxide for improveing 3D printing consumables performance, old described in step (4)
The change time is 1～2 day.
The preparation method of the described nano titanium oxide for improveing 3D printing consumables performance, fast described in step (1)
The mixing speed of speed stirring is 300～500r/min.
A kind of nano titanium dioxide powder for improveing 3D printing consumables performance prepared in aforementioned manners.
Beneficial effect:
1. the present inventor shows through test of many times research, owing to gadolinium, praseodymium have the 4f track and portion not exclusively occupied
Divide the 5d track with sky, can be at TiO2Introducing defect in lattice, stop crystal growth, (table is compared in increase to the size of reduction crystal
Area), hinder the recombination rate of electronics and hole, thus improve TiO2Photocatalysis performance.Simultaneously because the structure of methyl orange has
Phenyl ring, naphthalene nucleus, exist with the structure of azo and quinoid respectively under the conditions of alkalescence acid, be the agent structure of dyestuff, public
Think a kind of representational water solublity refractory organic compounds.TiO2 can this pollutant of catalytic degradation.
2. the nano-TiO of the present invention2Nontoxic, harmless, non-secondary pollution, is green catalyst.Doped with rare-earth elements has
Hope the service life improving catalyst.Existing TiO2Utilize ultraviolet light, available visible ray after doped with rare-earth elements, and light
Utilization rate higher.Several factors of photocatalysis methyl orange, more exchange premium practical situation is affected as light source, research with natural light.
Detailed description of the invention:
Embodiment 1:
The preparation method of a kind of nano titanium oxide for improveing 3D printing consumables performance, the method comprises the steps:
(1) preparation solution A: instill in dehydrated alcohol by butyl titanate while stirring, is subsequently adding glacial acetic acid, and 0.5-1 is little in stirring
Time, wherein in butyl titanate, dehydrated alcohol, the mol ratio of glacial acetic acid be 1:6:2；
(2) preparation B solution: while stirring the chloride of gadolinium, praseodymium is respectively dropped in dehydrated alcohol, is subsequently adding glacial acetic acid, stir
Mix 0.5-1 hour, wherein in gadolinium, praseodymium, dehydrated alcohol, the mol ratio of glacial acetic acid be 1:0.5:3:1；
(3) solution B is poured slowly in solution A, instilling hydrochloric acid solution regulation pH value and be equal to 4, continuing stirring, until becoming solidifying
Glue, stops stirring；
(4) the gel filter paper formed is sealed rear chamber temperature still aging；
(5) gel after ageing is put into drying in baking oven, form granule；
(6) gained granule after drying is put in mortar and grinds, then be placed in chamber type electric resistance furnace, in stove, ensure have air to enter,
It is to slowly warm up to 250 DEG C with the heating rate of 10～20 DEG C/min, carbonization half an hour, is continuously heating to 600～800 DEG C of roastings,
Obtain the nano titanium dioxide powder for improveing 3D printing consumables performance.
The preparation method of the described nano titanium oxide for improveing 3D printing consumables performance, dries described in step (5)
Dry temperature is 77～82 DEG C.
The preparation method of the described nano titanium oxide for improveing 3D printing consumables performance, roasts described in step (6)
The burning time is 3～5 hours.
The preparation method of the described nano titanium oxide for improveing 3D printing consumables performance, old described in step (4)
The change time is 1～2 day.
The preparation method of the described nano titanium oxide for improveing 3D printing consumables performance, fast described in step (1)
The mixing speed of speed stirring is 300～500r/min.
Below being only highly preferred embodiment of the present invention, the method for the present invention includes but not limited to above-described embodiment, the present invention
Unaccomplished matter, belong to the common knowledge of those skilled in the art.
Claims (6)
1., for improveing a preparation method for the nano titanium oxide of 3D printing consumables performance, it is characterized in that: the method includes
Following steps:
(1) preparation solution A: instill in dehydrated alcohol by butyl titanate while stirring, is subsequently adding glacial acetic acid, and 0.5-1 is little in stirring
Time, wherein in butyl titanate, dehydrated alcohol, the mol ratio of glacial acetic acid be 1:6:2；
(2) preparation B solution: while stirring the chloride of gadolinium, praseodymium is respectively dropped in dehydrated alcohol, is subsequently adding glacial acetic acid, stir
Mix 0.5-1 hour, wherein in gadolinium, praseodymium, dehydrated alcohol, the mol ratio of glacial acetic acid be 1:0.5:3:1；
(3) solution B is poured slowly in solution A, instilling hydrochloric acid solution regulation pH value and be equal to 4, continuing stirring, until becoming solidifying
Glue, stops stirring；
(4) the gel filter paper formed is sealed rear chamber temperature still aging；
(5) gel after ageing is put into drying in baking oven, form granule；
(6) gained granule after drying is put in mortar and grinds, then be placed in chamber type electric resistance furnace, in stove, ensure have air to enter,
It is to slowly warm up to 250 DEG C with the heating rate of 10～20 DEG C/min, carbonization half an hour, is continuously heating to 600～800 DEG C of roastings,
Obtain the nano titanium dioxide powder for improveing 3D printing consumables performance.
The preparation method of the nano titanium oxide for improveing 3D printing consumables performance the most according to claim 1, it is special
Levy and be: drying temperature described in step (5) is 77～82 DEG C.
The preparation method of the nano titanium oxide for improveing 3D printing consumables performance the most according to claim 1, it is special
Levy and be: roasting time described in step (6) is 3～5 hours.
The preparation method of the nano titanium oxide for improveing 3D printing consumables performance the most according to claim 1, it is special
Levy and be: described in step (4), digestion time is 1～2 day.
The preparation method of the nano titanium oxide for improveing 3D printing consumables performance the most according to claim 1, it is special
Levy and be: described in step (1), the mixing speed of quickly stirring is 300～500r/min.
6. the nano titanium dioxide powder for improveing 3D printing consumables performance prepared in aforementioned manners.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610510085.7A CN106179300A (en) | 2016-07-03 | 2016-07-03 | For improveing nano titanium oxide of 3D printing consumables performance and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610510085.7A CN106179300A (en) | 2016-07-03 | 2016-07-03 | For improveing nano titanium oxide of 3D printing consumables performance and preparation method thereof |
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| Publication Number | Publication Date |
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| CN106179300A true CN106179300A (en) | 2016-12-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610510085.7A Pending CN106179300A (en) | 2016-07-03 | 2016-07-03 | For improveing nano titanium oxide of 3D printing consumables performance and preparation method thereof |
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| Country | Link |
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| CN (1) | CN106179300A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109174203A (en) * | 2018-07-09 | 2019-01-11 | 福建师范大学 | A kind of skin-core structure 3D printing wire rod and preparation method thereof with photo-catalysis function |
-
2016
- 2016-07-03 CN CN201610510085.7A patent/CN106179300A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109174203A (en) * | 2018-07-09 | 2019-01-11 | 福建师范大学 | A kind of skin-core structure 3D printing wire rod and preparation method thereof with photo-catalysis function |
| CN109174203B (en) * | 2018-07-09 | 2021-09-28 | 福建师范大学 | Skin-core structure 3D printing wire with photocatalysis function and preparation method thereof |
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Application publication date: 20161207 |