CN105970248B - A kind of electrochemical method for synthesizing of isopropyl titanate - Google Patents
A kind of electrochemical method for synthesizing of isopropyl titanate Download PDFInfo
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- CN105970248B CN105970248B CN201610306267.2A CN201610306267A CN105970248B CN 105970248 B CN105970248 B CN 105970248B CN 201610306267 A CN201610306267 A CN 201610306267A CN 105970248 B CN105970248 B CN 105970248B
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- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002848 electrochemical method Methods 0.000 title claims abstract description 17
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000010936 titanium Substances 0.000 claims abstract description 16
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 230000006837 decompression Effects 0.000 claims abstract description 3
- 238000010025 steaming Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- 238000001994 activation Methods 0.000 claims description 14
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 239000010457 zeolite Substances 0.000 claims description 8
- 229910021536 Zeolite Inorganic materials 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- -1 isopropanol Ester Chemical class 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000004381 surface treatment Methods 0.000 claims description 2
- 238000005292 vacuum distillation Methods 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 9
- 230000005518 electrochemistry Effects 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 3
- 229960002163 hydrogen peroxide Drugs 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 230000003213 activating effect Effects 0.000 description 5
- 230000004913 activation Effects 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 5
- 239000010436 fluorite Substances 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- IJMWOMHMDSDKGK-UHFFFAOYSA-N Isopropyl propionate Chemical compound CCC(=O)OC(C)C IJMWOMHMDSDKGK-UHFFFAOYSA-N 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 229940015043 glyoxal Drugs 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/01—Products
- C25B3/13—Organo-metallic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/003—Compounds containing elements of Groups 4 or 14 of the Periodic Table without C-Metal linkages
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The present invention relates to a kind of electrochemical method for synthesizing of isopropyl titanate, belong to titanate esters technical field.Step：1st step, titanium are prepared negative electrode and anode, are installed in electrolytic cell as material；2nd step, using isopropanol as solvent, the aqueous isopropanol of 4-propyl bromide is made, is added into electrolytic cell, and under inert gas conditions, be passed through electric current and reacted；3rd step, after reaction terminates, reaction solution is filtered, filtrate decompression is distilled, isopropyl titanate is obtained after steaming isopropanol.The method of electrochemistry formated isopropyl titanate provided by the invention, there is the advantages of reaction yield is high, product purity is high.
Description
Technical field
The present invention relates to a kind of electrochemical method for synthesizing of isopropyl titanate, belong to titanate esters technical field.
Background technology
Isopropyl titanate（English name：Titanium tetraisopropanolate）Be also known as tetra isopropyl titanate,
Tetraisopropoxy titanium, the isopropyl acetone of metatitanic acid four, titanium tetraisopropylate.Chemical formula is C12H28O4Ti, it is the chemical combination that molecular weight is 284.22
Thing.The ester exchange reaction and the catalyst of condensation reaction being mainly used in organic synthesis.
Traditional chemical synthesis process is that TiCl4 and isopropanol are swapped into reaction, and the method cost of raw material is high, production
Rate is low, and typically 60% or so, and purity is not easy to reach requirement, subsequent step separating-purifying trouble.
Electrochemistry formated is also known as electrosynthesis glyoxal, is to carry out electrode reaction in electrode surface so as to generate newly using electrolysis means
For a kind of green synthesis techniques of material compared with chemical synthesis, the major advantage of electrochemistry formated is as follows：(1) electrochemistry formated is anti-
The reaction reagent that should inherently clean without poisonous or dangerous Oxidizing and Reducing Agents " electronics ".Therefore, in reactant
In system in addition to raw material and product, other reaction reagents are typically free of, therefore synthetic product is easily separated, easily refined, product purity
Height, accessory substance is few, and environmental pollution can be greatly lowered.(2) electrochemistry formated is generally carried out under normal temperature, normal pressure, reaction condition
Gently, energy consumption is low, and equipment manufacturing cost is low.(3) in reaction system, electronics transfer and the two processes that chemically react can be entered simultaneously
OK.Therefore, compared with chemical method, synthesis technique can be shortened, reduce equipment investment, alleviate environmental pollution.(4) in electrochemistry formated
During, can by change electrode potential synthesize it is different have product, while also reaction can be made by pre- by coordination electrode current potential
Fixed target is carried out, so as to obtain the product of high-purity, higher yield and selectivity.
Therefore isopropyl titanate is synthesized by electrochemical method and is likely to become a kind of more reliable synthetic route.
The content of the invention
The purpose of the present invention is：A kind of electrochemical method for synthesizing of isopropyl titanate is provided, yin, yang two is done from titanium
Pole, by feature anode process, from 4-propyl bromide as conducting salt, by making titanium anodic solution, negative electrode occurs also
Original is reacted to prepare isopropyl propionate.
Technical scheme is：
A kind of electrochemical method for synthesizing of isopropyl titanate, comprises the following steps：
1st step, titanium are prepared negative electrode and anode, are installed in electrolytic cell as material；
2nd step, using isopropanol as solvent, the aqueous isopropanol of 4-propyl bromide is made, is added into electrolytic cell,
And under inert gas conditions, it is passed through electric current and is reacted；
3rd step, after reaction terminates, reaction solution is filtered, filtrate decompression is distilled, metatitanic acid is obtained after steaming isopropanol
Isopropyl ester.
In the 1st described step, negative electrode and anode are before use, need to polish by surface, oil removing and activation process.
Described activation process refers to by surface treatment of the mixed solution of hydrogen peroxide and hydrofluoric acid to negative electrode and anode.
In the 2nd described step, the concentration of the aqueous isopropanol of 4-propyl bromide is 0.50mol/L.
In the 2nd described step, inert gas is selected from nitrogen or helium.
In the 2nd described step, the current strength scope for the reaction that is powered is 100~500A/m2；50~60 DEG C of reaction temperature；
1~3h of reaction time.
In the 3rd described step, the temperature control of vacuum distillation is at 40~70 DEG C.
In the 2nd described step, in course of reaction, it is also necessary to zeolite is added in electrolytic cell；Distillation filters out solid again after terminating
Body thing.
Described zeolite refers to epidesmine；Described zeolite is to be by modification, method of modifying：By 80~100
Epidesmine between mesh with 10% NH4Digestion 12h at 80 DEG C of Cl solution, soaked 3 days, be washed to 2mol/L HCl solution
Without Cl-, 120 DEG C of drying, according still further to solid-liquid weight than 1：5 dry at concentrated phosphoric acid is soaked 7 days, 100 DEG C, move to porcelain crucible micro-
Ripple stove heat 10min, it is washed with water after taking out cooling, then is dried at 120 DEG C, obtains modified zeolite.
Beneficial effect
The method of electrochemistry formated isopropyl titanate provided by the invention, it is excellent to have that reaction yield is high, product purity is high
Point.
Embodiment
Embodiment 1
The electrochemical method for synthesizing of isopropyl titanate, comprises the following steps：
1st step, titanium prepare negative electrode and anode as material, then are polished by surface, oil removing and activation process；
It is installed in electrolytic cell；Activation can use the conventional method for activating surface of metal titanium, be to use 1% hydrogen in the present embodiment
Fluorspar acid solution and 20% hydrogenperoxide steam generator are according to 1：After 3 mixing, electrode is soaked 1 hour；
2nd step, using isopropanol as solvent, the aqueous isopropanol of 0.50mol/L 4-propyl bromide is made, added
Into electrolytic cell, and under a nitrogen atmosphere, it is passed through electric current and is reacted, the current strength scope for the reaction that is powered is 100A/m2；Instead
Answer temperature 50 C, reaction time 1h；
3rd step, after reaction terminates, reaction solution is filtered, will be evaporated under reduced pressure at 55 DEG C of filtrate, steamed after isopropanol
To isopropyl titanate.
Embodiment 2
The electrochemical method for synthesizing of isopropyl titanate, comprises the following steps：
1st step, titanium prepare negative electrode and anode as material, then are polished by surface, oil removing and activation process；
It is installed in electrolytic cell；Activation can use the conventional method for activating surface of metal titanium, be to use 1% hydrogen in the present embodiment
Fluorspar acid solution and 20% hydrogenperoxide steam generator are according to 1：After 3 mixing, electrode is soaked 1 hour；
2nd step, using isopropanol as solvent, the aqueous isopropanol of 0.50mol/L 4-propyl bromide is made, added
Into electrolytic cell, and under a nitrogen atmosphere, it is passed through electric current and is reacted, the current strength scope 500A/m for the reaction that is powered2；Reaction
Temperature 60 C, reaction time 2h；
3rd step, after reaction terminates, reaction solution is filtered, will be evaporated under reduced pressure at 55 DEG C of filtrate, steamed after isopropanol
To isopropyl titanate.
Embodiment 3
The electrochemical method for synthesizing of isopropyl titanate, comprises the following steps：
1st step, titanium prepare negative electrode and anode as material, then are polished by surface, oil removing and activation process；
It is installed in electrolytic cell；Activation can use the conventional method for activating surface of metal titanium, be to use 1% hydrogen in the present embodiment
Fluorspar acid solution and 20% hydrogenperoxide steam generator are according to 1：After 3 mixing, electrode is soaked 1 hour；
2nd step, using isopropanol as solvent, the aqueous isopropanol of 0.50mol/L 4-propyl bromide is made, added
Into electrolytic cell, and under a nitrogen atmosphere, it is passed through electric current and is reacted, the current strength scope for the reaction that is powered is 200A/m2；Instead
Answer 55 DEG C of temperature, reaction time 2h；
3rd step, after reaction terminates, reaction solution is filtered, will be evaporated under reduced pressure at 55 DEG C of filtrate, steamed after isopropanol
To isopropyl titanate.
Embodiment 4
Difference with embodiment 3 is, in the 2nd described step, in course of reaction, it is also necessary to granularity is added in electrolytic cell
Epidesmine between 80~100 mesh, the weight of epidesmine are the 1/20 of aqueous isopropanol weight.
1st step, titanium prepare negative electrode and anode as material, then are polished by surface, oil removing and activation process；
It is installed in electrolytic cell；Activation can use the conventional method for activating surface of metal titanium, be to use 1% hydrogen in the present embodiment
Fluorspar acid solution and 20% hydrogenperoxide steam generator are according to 1：After 3 mixing, electrode is soaked 1 hour；
2nd step, using isopropanol as solvent, the aqueous isopropanol of 0.50mol/L 4-propyl bromide is made, added
Into electrolytic cell, 80~100 mesh epidesmines of isopropanol weight 1/20 are added, and under a nitrogen atmosphere, is passed through electric current and enters
Row reaction, the current strength scope for the reaction that is powered is 200A/m2；55 DEG C of reaction temperature, reaction time 2h；
3rd step, after reaction terminates, reaction solution is filtered, will be evaporated under reduced pressure at 55 DEG C of filtrate, steamed after isopropanol again
Filter out solids and obtain isopropyl titanate.
Embodiment 5
Difference with embodiment 4 is：Described epidesmine passes through modification, and method of modifying is by 80~100 mesh
Between epidesmine with 10% NH4Digestion 12h at 80 DEG C of Cl solution, soaked 3 days with 2mol/L HCl solution, be washed to nothing
Cl-, 120 DEG C of drying, according still further to solid-liquid weight than 1：5 in concentrated phosphoric acid（16.03mol/L）Immersion is dried at 7 days, 100 DEG C, is moved to
Porcelain crucible is in micro-wave oven（220V, 2450MHz）Moderate heat heats 10min, is washed with water after taking out cooling, then is dried at 120 DEG C, obtains
To modified zeolite.
1st step, titanium prepare negative electrode and anode as material, then are polished by surface, oil removing and activation process；
It is installed in electrolytic cell；Activation can use the conventional method for activating surface of metal titanium, be to use 1% hydrogen in the present embodiment
Fluorspar acid solution and 20% hydrogenperoxide steam generator are according to 1：After 3 mixing, electrode is soaked 1 hour；
2nd step, using isopropanol as solvent, the aqueous isopropanol of 0.50mol/L 4-propyl bromide is made, added
Into electrolytic cell, 80~100 mesh modified zeolites of isopropanol weight 1/20 are added, and under a nitrogen atmosphere, is passed through electric current and enters
Row reaction, the current strength scope for the reaction that is powered is 200A/m2；55 DEG C of reaction temperature, reaction time 2h；
3rd step, after reaction terminates, reaction solution is filtered, will be evaporated under reduced pressure at 55 DEG C of filtrate, steamed after isopropanol again
Filter out solids and obtain isopropyl titanate.
Above example be prepared isopropyl titanate yield and purity it is as follows：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Purity | 97.4% | 97.8% | 97.5% | 98.0% | 98.5% |
| Yield | 67% | 65% | 68% | 68% | 71% |
As can be seen from the above table, technique of the invention has the advantages of synthesis yield is high, product purity is good；Pass through addition
After zeolite, the impurity that 4-propyl bromide can be avoided to go out in heat resolve resides in isopropyl titanate in still-process
In, product purity can be improved.
Claims (7)
1. a kind of electrochemical method for synthesizing of isopropyl titanate, it is characterised in that comprise the following steps：
1st step, titanium are prepared negative electrode and anode, are installed in electrolytic cell as material；
2nd step, using isopropanol as solvent, the aqueous isopropanol of 4-propyl bromide is made, is added into electrolytic cell, and
Under inert gas conditions, it is passed through electric current and is reacted；
3rd step, after reaction terminates, reaction solution is filtered, filtrate decompression is distilled, metatitanic acid isopropyl is obtained after steaming isopropanol
Ester；
In the 2nd described step, in course of reaction, it is also necessary to zeolite is added in electrolytic cell；Distillation filters out solids again after terminating；
Described zeolite refers to epidesmine；Described zeolite is to be by modification, method of modifying：By 80~100 mesh it
Between epidesmine with 10% NH4Digestion 12h at 80 DEG C of Cl solution, soaked 3 days with 2mol/L HCl solution, be washed to nothing
Cl-, 120 DEG C of drying, according still further to solid-liquid weight than 1：5 dry at concentrated phosphoric acid is soaked 7 days, 100 DEG C, move to porcelain crucible in microwave
Stove heat 10min, it is washed with water after taking out cooling, then is dried at 120 DEG C, obtains modified zeolite.
2. the electrochemical method for synthesizing of isopropyl titanate according to claim 1, it is characterised in that：In the 1st described step,
Negative electrode and anode are before use, need to polish by surface, oil removing and activation process.
3. the electrochemical method for synthesizing of isopropyl titanate according to claim 2, it is characterised in that：Described activation process
Refer to by surface treatment of the mixed solution of hydrogen peroxide and hydrofluoric acid to negative electrode and anode.
4. the electrochemical method for synthesizing of isopropyl titanate according to claim 1, it is characterised in that：In the 2nd described step,
The concentration of the aqueous isopropanol of 4-propyl bromide is 0.50mol/L.
5. the electrochemical method for synthesizing of isopropyl titanate according to claim 1, it is characterised in that：In the 2nd described step,
Inert gas is selected from nitrogen or helium.
6. the electrochemical method for synthesizing of isopropyl titanate according to claim 1, it is characterised in that：In the 2nd described step,
The current strength scope reacted that is powered is 100~500A/m2；50~60 DEG C of reaction temperature；1~3h of reaction time.
7. the electrochemical method for synthesizing of isopropyl titanate according to claim 1, it is characterised in that：In the 3rd described step,
The temperature control of vacuum distillation is at 40~70 DEG C.
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| CN107475661A (en) * | 2017-07-12 | 2017-12-15 | 江苏科技大学 | A kind of pure titanium surface TiAlN thin film and its in-situ self-grown method |
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Effective date of registration: 20200622 Address after: 215500 No.13, Caotang Road, Changshu, Suzhou, Jiangsu Province Patentee after: Changshu intellectual property operation center Co.,Ltd. Address before: 350200 No. 27, Wu Hang Liberation Road, Changle city, Fujian Province Patentee before: Feng Jinwen |
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Address after: 215500 5th floor, building 4, 68 Lianfeng Road, Changfu street, Changshu City, Suzhou City, Jiangsu Province Patentee after: Changshu intellectual property operation center Co.,Ltd. Address before: No.13 caodang Road, Changshu City, Suzhou City, Jiangsu Province Patentee before: Changshu intellectual property operation center Co.,Ltd. |
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