CN104525166A - Preparation method of transparent titanium complex - Google Patents
Preparation method of transparent titanium complex Download PDFInfo
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- CN104525166A CN104525166A CN201410755663.4A CN201410755663A CN104525166A CN 104525166 A CN104525166 A CN 104525166A CN 201410755663 A CN201410755663 A CN 201410755663A CN 104525166 A CN104525166 A CN 104525166A
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- preparation
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- titanium complex
- butyl alcohol
- tetraisopropyl titanate
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Abstract
The invention belongs to the technical field of preparation of catalysts, and particularly relates to a preparation method of a transparent titanium complex. Reaction materials are tert-butyl alcohol and tetraisopropyl titanate. The preparation method comprises the following specific steps: (1) adding the tetraisopropyl titanate into a reaction kettle, and adding the tert-butyl alcohol which is 2.5-5 times the mass of the tetraisopropyl titanate into a head tank of the reaction kettle; (2) starting a stirring device, cooling to perform heat dissipation, controlling the reaction temperature to be below 80 DEG C, and dropwisely adding the tert-butyl alcohol into the reaction kettle, wherein the addition of the tert-butyl alcohol needs to be finished within 4 hours; (3) keeping the temperature at 72-75 DEG C, and reacting for 12 hours while keeping the temperature; (4) distilling the completely reacted materials under reduced pressure at 80-85 DEG C for more than 2 hours until no low-boiling-point substance is distilled off; and (5) discharging, and weighing to obtain the required transparent titanium complex. According to the invention, the preparation method is simple in process and easy to operate; the product is colorless, transparent and high in quality; and the product has the advantages of high titanium content, high catalytic activity, long catalyst life, low production cost and the like.
Description
Technical field
The invention belongs to catalyst preparation technical field, be specifically related to a kind of preparation method of transparent titanium complex.
Background technology
Titanate esters is a kind of common and one of organo-metallic catalyst of function admirable, is widely used in coating, ink, high polymer coupling agent or catalyst.But common titanate esters has the reasons such as activity is high, facile hydrolysis, difficult storage due to it and is restricted in suitability for industrialized production application process, is therefore usually made into titanium complex and uses.The reaction raw materials synthesizing basic titanium complex use in prior art roughly has three kinds of materials: titanate ester, dihydroxy base class, beta-dicarbonyl class.Conventional titanate esters has tetraethyl titanate, titanium propanolate, isopropyl titanate etc.; Beta-dicarbonyl class material comprises ethyl acetoacetate, 2,4-pentanediones, 1,3-PD, 2,3-butanediol, Isosorbide-5-Nitrae-ethohexadiol, or polyhydroxy glycerine.
The method of common synthesis titanium complex is: under the protection of inert gas, add titanate esters; preheating; slowly add the beta-dicarbonyl class material of the amount of desired substance at the appointed time; there is exothermic reaction in mixing; system cools, and maintaining reaction temperature is less than 70 DEG C, and temperature is determined according to reactant species; be added dropwise to complete rear continuation stir a period of time make to react completely, decompression distillation.In reactor, dihydroxy radical species is added again with after inert gas vacuum breaker, and strictly to control the addition of dihydroxy radical species, excessively add membership and make to only have a hydroxyl to participate in reaction, unnecessary hydroxyl can cause unnecessary side reaction, even oligomer can be generated, reduce reactivity, after stirring reaction a period of time, slough the alcohol that reaction generates.Although titanium complex catalyst prepared by this technique has higher catalytic activity, existing defects in, product purity high at product heat endurance, product appearance, production cost etc.Therefore along with the continuous change of production technology and the market demand, it is also proposed higher requirement to the quality of titanium complex, researcher constantly improves the synthetic method of titanium complex.
(1) in the building-up process of titanium complex, add toluene solvant, improve reaction system heat conduction efficiency, avoid forming oligomer between unnecessary hydroxyl, simultaneously can also and the alcohols of generation between form azeotropic mixture, take away alcohols material more fully.But the toluene that this method adopts, benzene, dimethylbenzene equal solvent are toxic solvent, toxicity is comparatively strong, and can cause the contraction of glue when the solvent remained in complex compound is used in silicone adhesive.
(2) be alcohols material in thorough removing system after the reaction, improve product purity, inert component can be added in system, the gas do not reacted with titanium complex or liquid, adopt multiple de-low step, first desolvation under little vacuum, promote moving right of reactive chemistry balance simultaneously, re-use large vacuum and slough more low-boiling-point substance, adding the little alcohol of another kind of volatility to being tentatively stripped of in the product after low-boiling-point substance, after reacting completely, sloughing the alcohol in the system of remaining in again.
(3) the titanium complex crystalline temperature prepared is higher, and when there is nucleator, ratio is easier to crystallization, is unfavorable for storage and uses.For preventing this problem from occurring, a small amount of water can be added in titanium complex, making it generate activated dimer, but the addition of water will be controlled well, add, further hydrolysis can be caused, make product lose reactivity.
Though above-mentioned improvement can solve some problems existed in titanium complex preparation process, new defect can be introduced in process simultaneously, further limit its application.
Summary of the invention
For solving above-mentioned the problems of the prior art, the present invention aims to provide a kind of preparation method of titanium complex, and that process of the method technique is simple, and raw material applied amount easily controls, and product is colourless, the complexes preparation method of stable in properties.The present invention is achieved through the following technical solutions:
A preparation method for transparent titanium complex, reaction raw materials is the tert-butyl alcohol and tetraisopropyl titanate.
Wherein said concrete preparation process is: tetraisopropyl titanate adds in reactor by (1), adds the tert-butyl alcohol of tetraisopropyl titanate 2.5-5 times quality in reactor head tank;
(2) open agitating device, cooling heat dissipation, controlling reaction temperature is less than 80 DEG C, is added dropwise to by the tert-butyl alcohol in reactor, adds in 4h;
(3) temperature 72-75 DEG C, insulation reaction 12h is kept;
(4) the material decompression distillation will reacted completely, vapo(u)rizing temperature 80-85 DEG C, distillation more than 2h, until distillate without low-boiling-point substance;
(5) blowing, required transparent titanium complex of weighing to obtain.
Concrete, described preparation method is with argon gas or nitrogen for protection gas, and the described tert-butyl alcohol is chemical pure.
Preferably, the described tert-butyl alcohol and tetraisopropyl titanate mass ratio are 3: 1.
The present invention only adopts the tert-butyl alcohol and tetraisopropyl titanate two kinds of raw materials to prepare titanium complex, and raw material is few, and reinforced simple, production cost is low.Adopt the tert-butyl alcohol to ensure that product has more shallow color and luster, the final titanium complex color of production is water white transparency shape.For ensureing that product purity adds Excess t-butanol and ensures that tetraisopropyl titanate can complete reaction in production process, distillating low-boiling-point substance by decompression distillation afterwards, ensureing product titanium final mass mark.Present invention process is simple, and operation CCP is few, reinforced process without the need to strictly needed for chemical reaction quality strictly control the quality of adding the tert-butyl alcohol, only need to ensure that the tert-butyl alcohol is excessive and at utmost can meet product chemistry reaction needed.Therefore to have technique simple, easy to operate in the present invention; Product water white transparency, quality is good; Ti content is high, and product catalytic activity is strong, long catalytic life, the advantages such as production cost is low.
Detailed description of the invention
In the mode exemplified, the present invention will be further described below; but protection scope of the present invention is not limited in this; described embodiment is only the indicative explaination that the mode that exemplifies is done the present invention; all those skilled in the art, with the change of spirit of the present invention to the equivalence that the present invention makes, all fall into protection scope of the present invention.
Embodiment 1
A preparation method for transparent titanium complex, adopts Excess t-butanol and tetraisopropyl titanate to react.
Its concrete preparation process is: 300g tetraisopropyl titanate adds in reactor by (1), adds the 750g chemical pure tert-butyl alcohol in reactor head tank;
(2) open agitating device, cooling heat dissipation, controlling reaction temperature is 75 DEG C, is slowly added dropwise in reactor by the tert-butyl alcohol, adds in 4h;
(3) temperature 72-75 DEG C, insulation reaction 12h is kept;
(4) the material decompression distillation will reacted completely, vapo(u)rizing temperature 80-85 DEG C, distillation 2.5h, until distillate without low-boiling-point substance;
(5) blowing, required transparent titanium complex of weighing to obtain.
Whole course of reaction adopts argon gas to do reaction protective gas.
Embodiment 2
A preparation method for transparent titanium complex, reaction raw materials is Excess t-butanol and tetraisopropyl titanate.
Wherein said concrete preparation process is: 300g tetraisopropyl titanate adds in reactor by (1), adds the 900g chemical pure tert-butyl alcohol in reactor head tank;
(2) open agitating device, cooling heat dissipation, controlling reaction temperature is 70 DEG C, is slowly added dropwise in reactor by the tert-butyl alcohol, adds in 4h;
(3) temperature 75 DEG C is kept, insulation reaction 12h;
(4) the material decompression distillation will reacted completely, vapo(u)rizing temperature 80 DEG C, distillation 4h, until distillate without low-boiling-point substance;
(5) blowing, required transparent titanium complex of weighing to obtain.
Whole course of reaction adopts nitrogen to be protective gas.
Embodiment 3
A preparation method for transparent titanium complex, reaction raw materials is Excess t-butanol and tetraisopropyl titanate.
Wherein said concrete preparation process is: 300g tetraisopropyl titanate adds in reactor by (1), adds the 1050g chemical pure tert-butyl alcohol in reactor head tank;
(2) open agitating device, cooling heat dissipation, controlling reaction temperature is 65 DEG C, is slowly added dropwise in reactor by the tert-butyl alcohol, adds in 4h;
(3) temperature 72 DEG C is kept, insulation reaction 12h;
(4) the material decompression distillation will reacted completely, vapo(u)rizing temperature 85 DEG C, distillation 3h, until distillate without low-boiling-point substance;
(5) blowing, required transparent titanium complex of weighing to obtain.
Whole course of reaction adopts nitrogen to be protective gas.
Embodiment 4
A preparation method for transparent titanium complex, reaction raw materials is Excess t-butanol and tetraisopropyl titanate.
Wherein said concrete preparation process is: 300g tetraisopropyl titanate adds in reactor by (1), adds the 1500g chemical pure tert-butyl alcohol in reactor head tank;
(2) open agitating device, cooling heat dissipation, controlling reaction temperature is 65 DEG C, is slowly added dropwise in reactor by the tert-butyl alcohol, adds in 4h;
(3) temperature 72 DEG C is kept, insulation reaction 12h;
(4) the material decompression distillation will reacted completely, vapo(u)rizing temperature 85 DEG C, distillation 3h, until distillate without low-boiling-point substance;
(5) blowing, required transparent titanium complex of weighing to obtain.
Whole course of reaction adopts nitrogen to be protective gas.
Embodiment 5
A preparation method for transparent titanium complex, adopts Excess t-butanol and tetraisopropyl titanate to react.
Its concrete preparation process is: 300g tetraisopropyl titanate adds in reactor by (1), adds the 1200g chemical pure tert-butyl alcohol in reactor head tank;
(2) open agitating device, cooling heat dissipation, controlling reaction temperature is 66 DEG C, is slowly added dropwise in reactor by the tert-butyl alcohol, adds in 4h;
(3) temperature 74 DEG C is kept, insulation reaction 12h;
(4) the material decompression distillation will reacted completely, vapo(u)rizing temperature 82 DEG C, distillation 5h, until distillate without low-boiling-point substance;
(5) blowing, required transparent titanium complex of weighing to obtain.
Whole course of reaction adopts argon gas to do reaction protective gas.
Claims (5)
1. a preparation method for transparent titanium complex, is characterized in that: reaction raw materials is the tert-butyl alcohol and tetraisopropyl titanate.
2. the preparation method of a kind of transparent titanium complex as claimed in claim 1, it is characterized in that: the transparent titanium complex concrete steps of described preparation are: tetraisopropyl titanate adds in reactor by (1), adds the tert-butyl alcohol of tetraisopropyl titanate 2.5-5 times quality in reactor head tank; (2) open agitating device, cooling heat dissipation, controlling reaction temperature is less than 80 DEG C, is added dropwise to by the tert-butyl alcohol in reactor, adds in 4h; (3) temperature 72-75 DEG C, insulation reaction 12h is kept; (4) the material decompression distillation will reacted completely, vapo(u)rizing temperature 80-85 DEG C, distillation more than 2h, until distillate without low-boiling-point substance; (5) blowing, required transparent titanium complex of weighing to obtain.
3. the preparation method of a kind of transparent titanium complex as claimed in claim 1, is characterized in that: described preparation method with argon gas or nitrogen for protection gas.
4. the preparation method of a kind of transparent titanium complex as claimed in claim 2, is characterized in that: the described tert-butyl alcohol is chemical pure.
5. the preparation method of a kind of transparent titanium complex as claimed in claim 2, is characterized in that: the described tert-butyl alcohol and tetraisopropyl titanate mass ratio are 3: 1.
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| CN201410755663.4A CN104525166A (en) | 2014-12-05 | 2014-12-05 | Preparation method of transparent titanium complex |
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| CN201410755663.4A CN104525166A (en) | 2014-12-05 | 2014-12-05 | Preparation method of transparent titanium complex |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0853101A1 (en) * | 1997-01-10 | 1998-07-15 | Dow Corning Corporation | Alkoxy-functional sealants with rapid development of green strength |
| CN102513156A (en) * | 2011-11-23 | 2012-06-27 | 湖北新蓝天新材料股份有限公司 | Preparation method of titanium complex with high catalytic activity |
| CN102875591A (en) * | 2012-09-25 | 2013-01-16 | 湖北新蓝天新材料股份有限公司 | Method for preparing tetra-tert-butyl orthotitanate composite |
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2014
- 2014-12-05 CN CN201410755663.4A patent/CN104525166A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0853101A1 (en) * | 1997-01-10 | 1998-07-15 | Dow Corning Corporation | Alkoxy-functional sealants with rapid development of green strength |
| CN102513156A (en) * | 2011-11-23 | 2012-06-27 | 湖北新蓝天新材料股份有限公司 | Preparation method of titanium complex with high catalytic activity |
| CN102875591A (en) * | 2012-09-25 | 2013-01-16 | 湖北新蓝天新材料股份有限公司 | Method for preparing tetra-tert-butyl orthotitanate composite |
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Application publication date: 20150422 |
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