CN107349967A - A kind of preparation method of the organic titanium dioxide hollow ball of photocatalysis - Google Patents
A kind of preparation method of the organic titanium dioxide hollow ball of photocatalysis Download PDFInfo
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- CN107349967A CN107349967A CN201710793805.XA CN201710793805A CN107349967A CN 107349967 A CN107349967 A CN 107349967A CN 201710793805 A CN201710793805 A CN 201710793805A CN 107349967 A CN107349967 A CN 107349967A
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- titanium dioxide
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 23
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 14
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229920000728 polyester Polymers 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 6
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 5
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000004359 castor oil Substances 0.000 claims description 4
- 235000019438 castor oil Nutrition 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 4
- 229940117958 vinyl acetate Drugs 0.000 claims description 4
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 235000019359 magnesium stearate Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 5
- 239000011368 organic material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000945 filler Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000003911 water pollution Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 8
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- 239000000126 substance Substances 0.000 description 3
- LEVWYRKDKASIDU-QWWZWVQMSA-N D-cystine Chemical compound OC(=O)[C@H](N)CSSC[C@@H](N)C(O)=O LEVWYRKDKASIDU-QWWZWVQMSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229960003067 cystine Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
Classifications
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- B01J35/39—
-
- B01J35/51—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a kind of preparation method of the organic titanium dioxide hollow ball of photocatalysis, the titanium dioxide hollow ball of the present invention is by that can be used as the filler of organic material after organic-treating, it is and good with the compatibility of organic material, improve the stability of organic material, the titanium dioxide hollow ball light weight of the present invention, has good photocatalysis effect, particularly suitable as water pollution material, high recycling rate, it is not easily damaged.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of the organic titanium dioxide hollow ball of photocatalysis.
Background technology
Catalyst, the chemical reaction rate (can improve can also reduce) of reactant can be changed in chemical reaction without changing
Become chemical balance, and the material that the quality of itself and chemical property all do not change before and after chemical reaction is catalyst
(solid catalyst is also catalyst).According to statistics, there are about using catalyst in more than 90% industrial process, such as chemical industry, petrochemical industry, life
Change, environmental protection etc..
Application number：201510428408.3 open is a kind of new modified titanium dioxide optical catalyst, according to mass fraction
Meter includes following components：Absolute ethyl alcohol 45-60 parts, nitric acid 12-18 parts, cystine 5-10 parts, titanium dioxide 25-35 parts, second two
Amine 3-9 parts, sodium borohydride 11-15 parts, sodium oxalate 8-13 parts, calgon 3.6-5.4 parts, deionized water 80-110 parts.Adopt
After above-mentioned formula, photochemical catalyst of the invention can be applied in photocatalysis oxidation technique, effectively can remove in water environment
Organic pollution；In addition, the photochemical catalyst of the present invention improves the absorbability to visible ray, can effectively improve to organic
The photocatalytic degradation efficiency of pollutant.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of organic titanium dioxide of photocatalysis is empty
The preparation method of bulbus cordis.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of the organic titanium dioxide hollow ball of photocatalysis, comprises the following steps：
（1）The magnesium stearate of 0.7-1 parts by weight is taken, is added in the tetrahydrofuran of 10-17 times of its weight, stirs, is added
Vinylacetate, the castor oil acid of 1-2 parts by weight of 20-30 parts by weight, nitrogen is passed through, rise temperature is 60-70 DEG C, is added
The azodiisobutyronitrile of 0.7-1 parts by weight, insulated and stirred 3-4 hours, obtain acid doping polyester dispersion；
（2）The butyl titanate of 46-50 parts by weight is taken, is added in the deionized water of 30-40 times of its weight, stirs, is dripped
Add 10-12% ammoniacal liquor, regulation pH is 10-11, stirring reaction 2-3 hours, adds the pentaerythrite of 3-4 parts by weight, raises temperature
For 70-80 DEG C, insulated and stirred 20-30 minutes, alcoholization colloidal sol is obtained；
（3）Above-mentioned acid doping polyester dispersion, alcoholization colloidal sol mixing are taken, is stirred, rise temperature is 90-95 DEG C, and insulation is stirred
Mix 1-2 hours, add the dimethyl suflfate of 1-2 parts by weight, it is 40-45 DEG C to reduce temperature, adds the hydrogen-oxygen of 0.1-0.2 parts by weight
Change lithium, insulated and stirred 3-4 hours, filtering, precipitation is washed, air drying, must methylate polyester colloidal sol；
（4）The above-mentioned polyester colloidal sol that methylates is taken, is added in the acetone of 3.5-4 times of its weight, the insulated and stirred 2- at 70-80 DEG C
3 hours, filtering, precipitation is washed, 1-2 hours are dried at 110-120 DEG C of vacuum, must methylate titanium dioxide hollow ball；
（5）The above-mentioned titanium dioxide hollow ball that methylates is taken, is added in the pentaerythrite of 5-7 times of its weight, stirs, is added
The silane coupler kh550 of 0.6-1 parts by weight, rise temperature are 60-65 DEG C, insulated and stirred 2-3 hours, filtering, will precipitate water
Wash, air drying, produce the organic titanium dioxide hollow ball of the photocatalysis.
Advantages of the present invention：
For the present invention first using vinylacetate as monomer, azodiisobutyronitrile is initiator, is adulterated by castor oil acid, obtains acid
Polyester dispersion is adulterated, then using butyl titanate as presoma, obtains refining colloidal sol under the catalyzing hydrolysis effect of ammoniacal liquor；So
Acid doping polyester dispersion, alcoholization colloidal sol are blended afterwards, are esterified under high temperature, then using dimethyl suflfate as the examination that methylates
Agent, lithium hydroxide are catalyst, and must methylate polyester colloidal sol, be then dispersed in acetone, polyvinyl acetate is dissolved,
Obtain organic titanium dioxide hollow ball；
The titanium dioxide hollow ball of the present invention is by that can be used as the filler of organic material, and and organic matter after organic-treating
The compatibility of material is good, improves the stability of organic material, titanium dioxide hollow ball light weight of the invention, has good
Photocatalysis effect, it is not easily damaged particularly suitable as water pollution material, high recycling rate.
Embodiment
Embodiment 1
A kind of preparation method of the organic titanium dioxide hollow ball of photocatalysis, comprises the following steps：
（1）The magnesium stearate of 0.7 parts by weight is taken, is added in the tetrahydrofuran of 10 times of its weight, stirs, adds 20 weight
The vinylacetate, the castor oil acid of 1 parts by weight of part, nitrogen is passed through, rise temperature is 60 DEG C, adds the azo of 0.7 parts by weight
Bis-isobutyronitrile, insulated and stirred 3 hours, obtains acid doping polyester dispersion；
（2）The butyl titanate of 46 parts by weight is taken, is added in the deionized water of 30 times of its weight, is stirred, be added dropwise 10%
Ammoniacal liquor, regulation pH are 10, stirring reaction 2 hours, add the pentaerythrite of 3 parts by weight, and rise temperature is 70 DEG C, insulated and stirred 20
Minute, obtain alcoholization colloidal sol；
（3）Above-mentioned acid doping polyester dispersion, alcoholization colloidal sol mixing are taken, is stirred, rise temperature is 90 DEG C, insulated and stirred 1
Hour, the dimethyl suflfate of 1 parts by weight is added, it is 40 DEG C to reduce temperature, adds the lithium hydroxide of 0.1 parts by weight, insulated and stirred 3
Hour, filtering, precipitation is washed, air drying, must methylate polyester colloidal sol；
（4）The above-mentioned polyester colloidal sol that methylates is taken, is added in the acetone of 3.5 times of its weight, insulated and stirred 2 hours at 70 DEG C,
Filtering, precipitation is washed, dried 1 hour at 110 DEG C of vacuum, must methylate titanium dioxide hollow ball；
（5）The above-mentioned titanium dioxide hollow ball that methylates is taken, is added in the pentaerythrite of 5 times of its weight, stirs, is added
The silane coupler kh550 of 0.6 parts by weight, rise temperature are 60 DEG C, insulated and stirred 2 hours, filtering, precipitation are washed, normal temperature
Dry, produce the organic titanium dioxide hollow ball of the photocatalysis.
Claims (1)
1. a kind of preparation method of the organic titanium dioxide hollow ball of photocatalysis, it is characterised in that comprise the following steps：
（1）The magnesium stearate of 0.7-1 parts by weight is taken, is added in the tetrahydrofuran of 10-17 times of its weight, stirs, is added
Vinylacetate, the castor oil acid of 1-2 parts by weight of 20-30 parts by weight, nitrogen is passed through, rise temperature is 60-70 DEG C, is added
The azodiisobutyronitrile of 0.7-1 parts by weight, insulated and stirred 3-4 hours, obtain acid doping polyester dispersion；
（2）The butyl titanate of 46-50 parts by weight is taken, is added in the deionized water of 30-40 times of its weight, stirs, is dripped
Add 10-12% ammoniacal liquor, regulation pH is 10-11, stirring reaction 2-3 hours, adds the pentaerythrite of 3-4 parts by weight, raises temperature
For 70-80 DEG C, insulated and stirred 20-30 minutes, alcoholization colloidal sol is obtained；
（3）Above-mentioned acid doping polyester dispersion, alcoholization colloidal sol mixing are taken, is stirred, rise temperature is 90-95 DEG C, and insulation is stirred
Mix 1-2 hours, add the dimethyl suflfate of 1-2 parts by weight, it is 40-45 DEG C to reduce temperature, adds the hydrogen-oxygen of 0.1-0.2 parts by weight
Change lithium, insulated and stirred 3-4 hours, filtering, precipitation is washed, air drying, must methylate polyester colloidal sol；
（4）The above-mentioned polyester colloidal sol that methylates is taken, is added in the acetone of 3.5-4 times of its weight, the insulated and stirred 2- at 70-80 DEG C
3 hours, filtering, precipitation is washed, 1-2 hours are dried at 110-120 DEG C of vacuum, must methylate titanium dioxide hollow ball；
（5）The above-mentioned titanium dioxide hollow ball that methylates is taken, is added in the pentaerythrite of 5-7 times of its weight, stirs, is added
The silane coupler kh550 of 0.6-1 parts by weight, rise temperature are 60-65 DEG C, insulated and stirred 2-3 hours, filtering, will precipitate water
Wash, air drying, produce the organic titanium dioxide hollow ball of the photocatalysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710793805.XA CN107349967A (en) | 2017-09-06 | 2017-09-06 | A kind of preparation method of the organic titanium dioxide hollow ball of photocatalysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710793805.XA CN107349967A (en) | 2017-09-06 | 2017-09-06 | A kind of preparation method of the organic titanium dioxide hollow ball of photocatalysis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107349967A true CN107349967A (en) | 2017-11-17 |
Family
ID=60290749
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710793805.XA Pending CN107349967A (en) | 2017-09-06 | 2017-09-06 | A kind of preparation method of the organic titanium dioxide hollow ball of photocatalysis |
Country Status (1)
| Country | Link |
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| CN (1) | CN107349967A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031022A (en) * | 2010-10-27 | 2011-04-27 | 华南理工大学 | Method for modifying nano titanium dioxide sol by utilizing silane coupling agent |
| CN102631951A (en) * | 2012-04-10 | 2012-08-15 | 同济大学 | Method for preparing organic-inorganic hybrid nano-titania hollow ball with high catalytic performance |
| CN103304979A (en) * | 2013-07-26 | 2013-09-18 | 天津大学 | Phosphorylation titanium dioxide hollow sphere-filled sulfonated polyether ether ketone film as well as preparation and application |
| CN103359782A (en) * | 2013-07-24 | 2013-10-23 | 南京理工大学 | Preparation method of hollow titanium dioxide microspheres |
| CN103936599A (en) * | 2014-05-09 | 2014-07-23 | 上海晋鲁医药科技有限公司 | Preparation method of 2-methoxy ethylamine |
-
2017
- 2017-09-06 CN CN201710793805.XA patent/CN107349967A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031022A (en) * | 2010-10-27 | 2011-04-27 | 华南理工大学 | Method for modifying nano titanium dioxide sol by utilizing silane coupling agent |
| CN102631951A (en) * | 2012-04-10 | 2012-08-15 | 同济大学 | Method for preparing organic-inorganic hybrid nano-titania hollow ball with high catalytic performance |
| CN103359782A (en) * | 2013-07-24 | 2013-10-23 | 南京理工大学 | Preparation method of hollow titanium dioxide microspheres |
| CN103304979A (en) * | 2013-07-26 | 2013-09-18 | 天津大学 | Phosphorylation titanium dioxide hollow sphere-filled sulfonated polyether ether ketone film as well as preparation and application |
| CN103936599A (en) * | 2014-05-09 | 2014-07-23 | 上海晋鲁医药科技有限公司 | Preparation method of 2-methoxy ethylamine |
Non-Patent Citations (1)
| Title |
|---|
| 徐惠等: ""硅烷偶联剂对纳米TiO2表面改性的研究"", 《涂料工业》 * |
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Application publication date: 20171117 |