CN105541600A - A method of producing fatty acid titanium - Google Patents
A method of producing fatty acid titanium Download PDFInfo
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- CN105541600A CN105541600A CN201510706108.7A CN201510706108A CN105541600A CN 105541600 A CN105541600 A CN 105541600A CN 201510706108 A CN201510706108 A CN 201510706108A CN 105541600 A CN105541600 A CN 105541600A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
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Abstract
Through reaction of a fatty acid and a titanium tetraol salt under a certain condition, a low-viscosity and high-titanium-content fatty acid titanium is obtained. The fatty acid titanium is generated through reactions of the titanium tetraol salt composed of monohydric fatty acid having 4-10 carbon atoms and an alkoxide having 1-6 carbon atoms under heating. At the moment, an additive amount of the fatty acid relative to 1mol titanium tetraol salt is 2.0mol to 3.5mol, the reaction temperature is 85 DEG C to 110 DEG C, an alcohol distilled from a reaction system is removed through an amount of more than 0.20 mol/mol totally by weight of the alkoxide contained in the titanium tetraol salt, and the reaction is implemented at the same time.
Description
Technical field
The present invention relates to a kind of preparation method of lipid acid titanium.
Background technology
Titanium oxide demonstrates excellent character as semi-conductor, can be used as the various materials'uses such as photocatalyst, ferroelectrics, piezoelectric element, therefore positive active development thin film of titanium oxide.In the formation method of thin film of titanium oxide, the vacuum vapour deposition, sputtering method, CVD etc. as chemical vapour deposition can be listed.These methods all need large-scale equipment, and need the condition that the high cost such as high vacuum, high temperature, technical difficulty are high.On the other hand, in liquid phase flop-in method, film can be formed with cheaper equipment, the condition that is easy to.
As the method using liquid phase flop-in method to form thin film of titanium oxide, people there will be a known the sol-gel method that make use of Titanium alkoxides hydrolysis.Sol-gel method completes at an easy rate by simple device, but due to the reactivity of used Titanium alkoxides and water high, therefore stability is low, easily causes hydrolysis with moisture in air, produces and precipitates.Now, if raising stability and use long-chain alkoxide, then the titanium content of Titanium alkoxides reduces, and film-forming properties declines.In order to address these problems, be developed and will serve as the coating roasting method of organic acid titanium solution as coating fluid of thin film of titanium oxide formation material.
In coating roasting method, the organic acid titanium being diluted in solvent is coated on substrate, removes solvent by drying, carry out roasting, form thin film of titanium oxide thus.As organic acid titanium, in order to obtain fine and close thin film of titanium oxide, needing high titanium content, in addition, considering from the angle of coating, needing organic acid titanium solution to be low viscosity.In addition, forming material to more easily obtain the high thin film of titanium oxide of manufacturability, it is desirable to by synthesizing organic acid titanium solution in the lump and manufacturing.
As the synthetic method of the organic acid titanium as coating fluid, such as, in Unexamined Patent 7-70155, synthesize organic acid titanium by titanous chloride and organic acid salt.But, in the organic acid titanium synthesized by this replacement(metathesis)reaction, being mixed into of ion not of the same race cannot be avoided, the semiconducting behavior of titanium oxide is reduced.Now, in order to remove ion not of the same race, need to adopt purification process, add process number, manufacturability reduces.Therefore, preferably by direct synthesis organic acid titanium.
As by direct synthesis organic acid titanium, in Unexamined Patent 05-230079, by the back flow reaction synthetic fatty acid titanium of titanium four alkoxide and lipid acid.
Prior art document
Patent documentation
Patent documentation 1: No. 7-70155, Unexamined Patent bulletin
Patent documentation 2: No. 05-230079, Unexamined Patent bulletin
Summary of the invention
The technical problem to be solved in the present invention
But, utilizing in the lipid acid of back flow reaction and the reaction of titanium four alkoxide described, except generating except lipid acid titanium by titanium four alkoxide and lipid acid, also there occurs the esterification of alkoxide and lipid acid.Then, the water generated by esterification is hydrolyzed to titanium four alkoxide, generates titanium hydroxide, there occurs further and generates poly-titanoxane by titanium hydroxide dehydrating condensation.That is, excessively facilitate the generation of ester, generate water, lipid acid titanium polymer is quantized.Thus, the complex structure of lipid acid titanium, lipid acid titanium solution becomes high viscosity, and produces precipitation in synthesis.On the other hand, when reaction is not fully carried out, the titanium content step-down of lipid acid titanium.
Problem of the present invention is, by making lipid acid and titanium four alkoxide react under given conditions, obtains low viscosity, lipid acid titanium that titanium content is high.
The technique means of technical solution problem
Present inventor finds the method by making lipid acid and titanium four alkoxide carry out under given conditions reacting to prepare low viscosity, lipid acid titanium that titanium content is high, thus completes the present invention.
That is, the invention is characterized in, 1 of carbonatoms 4 ~ 10 yuan of lipid acid is reacted under heating with titanium four alkoxide be made up of the alkoxide of carbonatoms 1 ~ 6, when generating lipid acid titanium,
Lipid acid is 2.0 ~ 3.5 moles relative to the addition of 1 mole of titanium four alkoxide, temperature of reaction is 85 ~ 110 DEG C, the amount adding up to more than 0.20 moles/mole with the alkoxide contained in relative to titanium four alkoxide remove in by reaction system distillate the alcohol of (reserving The Ru) while implement above-mentioned reaction.
Invention effect
The titanium content of the lipid acid titanium obtained in preparation method of the present invention is high, viscosity is low, is therefore applicable to the formation material of the thin film of titanium oxide formed by coating roasting method.
Embodiment
Below, further describe.
(lipid acid)
1 yuan of lipid acid that the lipid acid used in the present invention is carbonatoms 4 ~ 10.If carbonatoms is less than 3, then the titanium content of obtained lipid acid titanium is too high, easily produces precipitation, cannot use as coating fluid, if carbonatoms is more than 11, then titanium content reduces.The carbonatoms of this lipid acid is preferably more than 5, is more preferably more than 6.In addition, the carbonatoms of lipid acid is preferably less than 9, and more preferably less than 8.
This lipid acid can be saturated or undersaturated lipid acid arbitrarily, can be used alone, or can two or morely use together.As the example of this lipid acid, butyric acid, isopropylformic acid, valeric acid, isovaleric acid, caproic acid, 2 Ethylbutanoic acid, enanthic acid, sad, 2 ethyl hexanoic acid, n-nonanoic acid, capric acid etc. can be enumerated.
< titanium four alkoxide >
The carbonatoms forming four kinds of alkoxide of titanium four alkoxide used in the present invention is respectively 1 ~ 6.The four kinds of alkoxide forming titanium four alkoxide can be identical each other, also can be mutually different, considers, preferably use identical alkoxide from the angle of easy degree of starting with.The carbonatoms of each alkoxide is preferably more than 2, and more preferably more than 3.In addition, the carbonatoms of each alkoxide is preferably less than 5, and more preferably less than 4.
As the example of this titanium four alkoxide, four methyl alcohol titaniums, titanium tetraethoxide, four n-propyl alcohol titaniums, titanium tetraisopropylate, four n-butyl titaniums, four titanium isobutoxides, four sec-butyl alcohol titaniums, four Pentyl alcohol titaniums, four n-hexyl alcohol titaniums etc. can be listed.
(addition)
Titanium can form 4 keys usually, but due to reasons such as steric hindrances, and with the reaction of lipid acid, 3 keys is main resultant at the most.In addition, if lipid acid relative to the addition of 1 mole of titanium four alkoxide less than 2.0 moles, then the lipid acid owing to reacting with titanium tails off, and the key between titanium and oxygen becomes many and polymer quantizes, and lipid acid titanium becomes high viscosity.If lipid acid is relative to the addition of 1 mole of titanium four alkoxide higher than 3.5 moles, then the lipid acid reacted with titanium becomes many, and the titanium content of lipid acid titanium reduces.
Therefore, lipid acid is set to 2.0 ~ 3.5 moles relative to the addition of 1 mole of titanium four alkoxide.Lipid acid relative to the addition more preferably more than 2.5 of 1 mole of titanium four alkoxide, and more preferably less than 3.0.
(temperature of reaction)
Temperature of reaction is set to 85 ~ 110 DEG C.If this temperature of reaction is less than 85 DEG C, then sluggish, if this temperature of reaction is the high temperature more than 110 DEG C, then lipid acid titanium carries out polymer quantification, generates precipitation.This temperature of reaction more preferably more than 90 DEG C, and more preferably less than 100 DEG C.
(distillating alcohol)
In reaction through time the alcohol that distillates to come from relative to titanium four alkoxide of raw material be the alkoxide of 4 equivalent.Distillate alcohol to remove with the amount adding up to more than 0.2 moles/mole relative to this alkoxide.If this removal amount is less than 0.2 moles/mole, then produce water in the system of carrying out in esterification, because of the hydrolysis of titanium four alkoxide and dehydrating condensation, polymer quantizes, and produces precipitation.
The removal amount of this alcohol more preferably adds up to more than 0.25 moles/mole relative to alkoxide.
In addition, the removal amount distillating alcohol preferably amounts to below 0.5 moles/mole relative to alkoxide.In addition, also whole removals of alcohol essence will can be distillated to outside reaction system.
In addition, distillating the unit " moles/mole " of the removal amount of alcohol, is the mole number of alcohol removed from reaction system relative to 1 mole of alkoxide.
There is no particular limitation to remove the method distillating alcohol, preferably in the inactive gas such as nitrogen or argon gas, carries out bubbling to reaction solution, or reduce pressure to reaction system.
The removal speed the distillating alcohol preferably quantity of distillate of every 1 hour is 0.005 ~ 0.2 moles/mole, more preferably 0.008 ~ 0.12 moles/mole.If this speed is slow, then in reaction system, produce water because of the carrying out of esterification, there is hydrolysis and the dehydrating condensation because of titanium four alkoxide and polymer quantizes, the tendency that generation precipitates.But by the removal amount of every 1 hour is set to more than 0.01 moles/mole, then such precipitation is easier to suppress.In addition, if the quantity of distillate of every 1 hour is greater than 0.2 moles/mole, then the water generated because of esterification reduces, and the hydrolysis of titanium four alkoxide, by extra-inhibitory, has lipid acid titanium low molecule and quantizes, the tendency that titanium content reduces.The removal speed distillating alcohol is all passable to what terminate as certain or change from reaction, preferably removes with certain speed after obtaining starting fraction.
In the present invention, when carrying out heating to the reaction system containing titanium four alkoxide and lipid acid and making it react, remove from reaction system and distillate alcohol.Even if remove alcohol after completion of the reaction, also above-mentioned precipitation cannot be prevented.
(ester)
In this preparation method, while generation lipid acid titanium, generate fatty acid ester by raw fatty acid and alkoxide, therefore, it is possible to obtain the fatty acid ester solution of lipid acid titanium.This fatty acid ester makes the titanium stabilized dissolving of lipid acid, and further, this soltion viscosity is low, is therefore suitable for being used as thin film of titanium oxide formation coating fluid.
On the other hand, the lipid acid titanium obtained by preparation method of the present invention can change the kind of solvent or the concentration of lipid acid titanium according to the substrate of formation thin film of titanium oxide or device etc.Lipid acid titanium is dissolved in toluene, tetrahydrofuran (THF), other fatty acid ester equal solvents, therefore can prepare coating fluid using them as solvent, forms material as thin film of titanium oxide.
As the solvent of the lipid acid titanium obtained in this preparation method, particularly preferably fatty acid ester.
The weight ratio (both gross weights are set to 100) of lipid acid titanium and solvent is preferably 1:99 ~ 70:30.By the weight ratio of lipid acid titanium is set to more than 1, the titanium composition in solution is high, easily obtains sufficient film forming.Consider from this angle, the weight ratio of lipid acid titanium and solvent is preferably set to more than 10 and less than 90.In addition by the weight ratio of lipid acid titanium is set to less than 70, the viscosity of solution can be reduced, easily carry out uniform film forming, and due to titanium composition not too high, therefore thickness not easily increases.Consider from this angle, the preferred weight ratio by lipid acid titanium and solvent is set to less than 60 and more than 40 further.
Embodiment
Below, by embodiment, the present invention is described in more detail, but the present invention is not limited to following embodiment.
(embodiment 1)
Sad (the 0.94mol of 135.4g is added in the four-hole boiling flask being configured with thermometer, nitrogen ingress pipe, the water and basis weight receptor of band cooling tube, agitating vane, NAA-82, Japan Oil Co), while carry out nitrogen bubble, while add 106.6g tetra-n-butyl titanium (0.32mol, OrgatixTA-25, MatsumotoFineChemical Co., Ltd.), 100mmHg is forced into, heated and stirred at 95 DEG C with vacuum pump.The n-butyl alcohol quantity of distillate of every 1 hour is 0.100mol/molh, and quantity of distillate adds up to 0.390mol/mol, and overhead product disappears, and obtains the lipid acid titanium solution of brown.
(embodiment 2)
Use reaction unit described in embodiment 1 and reaction raw materials, carry out nitrogen bubble with 300ml/min, in normal pressure, heated and stirred at 95 DEG C.The n-butyl alcohol quantity of distillate of every 1 hour is 0.026mol/molh, and quantity of distillate adds up to 0.320mol/mol, and overhead product disappears, and obtains the lipid acid titanium solution of brown.
(embodiment 3)
Use reaction unit described in embodiment 1 and reaction raw materials, carry out nitrogen bubble with 100ml/min, in normal pressure, heated and stirred at 95 DEG C.The n-butyl alcohol quantity of distillate of every 1 hour is 0.020mol/molh, and quantity of distillate adds up to 0.320mol/mol, and overhead product disappears, and obtains the lipid acid titanium solution of brown.
(embodiment 4)
Use reaction unit described in embodiment 1 and reaction raw materials, carry out nitrogen bubble with 100ml/min, in normal pressure, heated and stirred at 95 DEG C.The n-butyl alcohol quantity of distillate of every 1 hour is 0.012mol/molh, and quantity of distillate adds up to 0.300mol/mol, and overhead product disappears, and obtains the lipid acid titanium solution of brown.
(embodiment 5)
Use reaction unit described in embodiment 1 and reaction raw materials, carry out nitrogen bubble with 100ml/min, in normal pressure, heated and stirred at 95 DEG C.The n-butyl alcohol quantity of distillate of every 1 hour is 0.011mol/molh, and quantity of distillate adds up to 0.260mol/mol, and overhead product disappears, and obtains the lipid acid titanium solution of brown.
(embodiment 6)
Use reaction unit described in embodiment 1 and reaction raw materials, carry out nitrogen bubble with 100ml/min, in normal pressure, heated and stirred at 95 DEG C.The n-butyl alcohol quantity of distillate of every 1 hour is 0.008mol/molh, and quantity of distillate adds up to 0.210mol/mol, and overhead product disappears, and obtains the lipid acid titanium solution of brown.
(comparative example 1)
Use reaction unit described in embodiment 1 and reaction raw materials, carry out nitrogen bubble with 10ml/min, in normal pressure, heated and stirred at 95 DEG C.The n-butyl alcohol quantity of distillate of every 1 hour is 0.006mol/molh, generates white precipitate in the reaction.
(comparative example 2)
Use reaction unit described in embodiment 1 and reaction raw materials, carry out nitrogen bubble with 10ml/min, in normal pressure, heated and stirred at 95 DEG C.The n-butyl alcohol quantity of distillate of every 1 hour is 0.004mol/molh, generates white precipitate in the reaction.
(comparative example 3)
Sad (the 0.94mol of 135.4g is added in the four-hole boiling flask being configured with thermometer, nitrogen ingress pipe, cooling tube, agitating vane, NAA-82, day is oily), while carry out nitrogen bubble, while add 106.6g tetra-n-butyl titanium (0.32mol, OrgatixTA-25, MatsumotoFineChemical), at 95 DEG C, heated and stirred 2 hours, carries out back flow reaction.Afterwards n-butyl alcohol is distillated outside system, obtain the lipid acid titanium solution of brown.
(comparative example 4)
Use reaction unit described in comparative example 2 and reaction raw materials, carry out nitrogen bubble, while at 95 DEG C heated and stirred 14 hours, after carrying out back flow reaction, generate white precipitate in the reaction.
(embodiment 7)
Except with 111.2g sad (0.78mol), 128.8g tetra-n-butyl titanium (0.39mol) for except raw material, react in the same way as in example 2.The n-butyl alcohol quantity of distillate of every 1 hour is 0.027mol/molh, and quantity of distillate adds up to 0.410mol/mol, and overhead product disappears, and obtains the lipid acid titanium solution of brown.
(comparative example 5)
Except with 152.4g sad (1.08mol), 88.4g tetra-n-butyl titanium (0.27mol) for except raw material, react in the same way as in example 2.The n-butyl alcohol quantity of distillate of every 1 hour is 0.026mol/molh, and quantity of distillate adds up to 0.350mol/mol, and overhead product disappears, and obtains the lipid acid titanium solution of brown.
(separation of lipid acid titanium)
By the lipid acid titanium solution underpressure distillation removing at 150 DEG C obtained in embodiment 1 ~ 7 and comparative example 3,5, isolate the lipid acid titanium as brown oil.
(lipid acid titanium solution A)
Relative to the above-mentioned lipid acid titanium obtained, the mode being 15.0% with titanium composition adds butyl caprylate (Tokyo HuaCheng Industry Co., Ltd), as lipid acid titanium solution A.
< analyzes >
(viscosity)
For the lipid acid titanium solution obtained in embodiment 1 ~ 7 and comparative example 3,5 and lipid acid titanium solution A, use rheometer (rheometer, AntonPaar MCR302), measure the shear viscosity of 25 DEG C.
(titanium composition)
For the lipid acid titanium solution obtained in embodiment 1 ~ 7 and comparative example 3,5, separated lipid acid titanium, lipid acid titanium solution A, following method is used to measure titanium composition.
Porcelain crucible adds the sample of weighing, electricradiator heats, light a fire, make it burn.Then, heat 3 hours in atmosphere with the electric furnaces of 650 DEG C, make sample burn cinder.The ashes that weighing obtains, according to the titanium composition of following formulae discovery sample.
Titanium composition (%)=(ash weight/example weight) × (formula weight of the nucleidic mass/titanium dioxide of titanium) × 100
[table 1]
[table 2]
" precipitation " project in table 1,2 is as described below.
"○": without precipitation, can prepare
"×": produce precipitation in preparation
The lipid acid titanium obtained in embodiment 1 ~ 7 and lipid acid titanium solution are low viscosity, and the titanium composition of contained lipid acid titanium demonstrates high level.
In comparative example 1,2 and 3, in synthesis, create white precipitate.
The lipid acid titanium obtained in comparative example 3 and lipid acid titanium solution viscosity high, the titanium composition of contained lipid acid titanium demonstrates low value.
The lipid acid titanium viscosity obtained in comparative example 5 is low, but the viscosity of lipid acid titanium solution is high, and the titanium composition of contained lipid acid titanium demonstrates low value.
Claims (1)
1. the preparation method of a lipid acid titanium, it is characterized in that, react under heating making 1 yuan of lipid acid of titanium four alkoxide and carbonatoms 4 ~ 10, when generating lipid acid titanium, the carbonatoms forming each alkoxide of described titanium four alkoxide is 1 ~ 6, described lipid acid is 2.0 ~ 3.5 moles relative to the addition of 1 mole of titanium four alkoxide, temperature of reaction is 85 ~ 110 DEG C, while the amount adding up to more than 0.20 moles/mole with the alkoxide contained in relative to titanium four alkoxide removes in by reaction system the alcohol distillated, implement described reaction.
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| Application Number | Priority Date | Filing Date | Title |
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| JP2014-219145 | 2014-10-28 | ||
| JP2014219145 | 2014-10-28 |
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| CN105541600A true CN105541600A (en) | 2016-05-04 |
| CN105541600B CN105541600B (en) | 2020-06-05 |
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| JP (1) | JP6590294B2 (en) |
| KR (1) | KR102344230B1 (en) |
| CN (1) | CN105541600B (en) |
| TW (1) | TWI654197B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108250063A (en) * | 2018-02-11 | 2018-07-06 | 广州新驰化工科技有限公司 | A kind of isooctyl acid titanium preparation method |
| CN109734744A (en) * | 2018-12-26 | 2019-05-10 | 佛山市天宇安贝尔新材料有限公司 | A kind of preparation method of 2- base caproic acid titanium |
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- 2015-10-20 JP JP2015206014A patent/JP6590294B2/en active Active
- 2015-10-27 KR KR1020150149386A patent/KR102344230B1/en active IP Right Grant
- 2015-10-27 CN CN201510706108.7A patent/CN105541600B/en active Active
- 2015-10-27 TW TW104135170A patent/TWI654197B/en active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108250063A (en) * | 2018-02-11 | 2018-07-06 | 广州新驰化工科技有限公司 | A kind of isooctyl acid titanium preparation method |
| CN109734744A (en) * | 2018-12-26 | 2019-05-10 | 佛山市天宇安贝尔新材料有限公司 | A kind of preparation method of 2- base caproic acid titanium |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105541600B (en) | 2020-06-05 |
| JP6590294B2 (en) | 2019-10-16 |
| KR102344230B1 (en) | 2021-12-27 |
| TWI654197B (en) | 2019-03-21 |
| TW201615649A (en) | 2016-05-01 |
| KR20160049991A (en) | 2016-05-10 |
| JP2016084339A (en) | 2016-05-19 |
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