CN111039758A - Liquid mixed alkoxy aluminum and synthetic method thereof - Google Patents
Liquid mixed alkoxy aluminum and synthetic method thereof Download PDFInfo
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- CN111039758A CN111039758A CN201911406332.9A CN201911406332A CN111039758A CN 111039758 A CN111039758 A CN 111039758A CN 201911406332 A CN201911406332 A CN 201911406332A CN 111039758 A CN111039758 A CN 111039758A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/68—Preparation of metal alcoholates
- C07C29/70—Preparation of metal alcoholates by converting hydroxy groups to O-metal groups
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Abstract
The invention provides a liquid mixed alkoxy aluminum and a synthesis method thereof, the melting point of the mixed alkoxy aluminum is lower than 25 ℃, and the molecular formula of the mixed alkoxy aluminum can be expressed as Al (OR)1)x(OR2)y(OR3)3‑x‑y，(0≤x<3,0≤y<3,0≤3‑x‑y<3) Wherein OR is1Is isopropoxy, R2And R3Has a molecular formula of CnH2n+1N is a natural number, and n is not less than 4. The preparation method is that the aluminium isopropoxide is used as raw material, at least one monohydric alcohol with more than C3 is mixed and heated for reflux to form solution, then the formed solution is heated and distilled, and the obtained product is a liquid mixed alkoxy aluminium after distillation is finished. The invention mainly provides a suitable raw material for high-purity aluminum oxide or high-purity aluminum hydroxide.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and relates to liquid mixed alkoxy aluminum and a synthetic method thereof.
Background
The alkoxy aluminum is also called aluminum alkoxide or aluminum alkoxide, is a very important chemical intermediate, is an important raw material for preparing high-purity aluminum oxide, high-purity aluminum hydroxide, high-purity aluminum nitride and superfine aluminum oxide, and can also be used as a dehydrating agent, a catalyst and the like. The preparation of aluminum alkoxides has been studied in a large number of ways since the last century. Such as:
USP2579251 discloses a process for the preparation of an aluminum alkoxide using a catalyst comprising HgCl2，CuCl2，FeCl3,SnCl4And BCl3The method is that the metallic aluminum and the catalyst are ground into fine powder and react with ethanol under the heating state to prepare the aluminum ethoxide.
EP0248195A2The preparation method of alkoxy aluminium is characterized by that it adopts alcohol containing 5-10 carbon atoms and uses gallium or gallium alloy as catalyst, and the system activity of said catalyst is higher.
CN1046526C proposes a preparation method of low-carbon alkoxy aluminum, which is characterized in that 30-50% of excessive C is added1～C4Reacting low-carbon alcohol and metal aluminum at 80-180 ℃ for 4-24 h in the presence of aluminum chloride, mercury chloride or a low-carbon alkyl aluminum catalyst, evaporating excessive low-carbon alcohol, and filtering while keeping the reactant in a liquid state, so that the problems of long-term stable production, low product yield and the like caused by a distillation method are solved.
CN101935326B proposes a method for preparing an aluminum alkoxide by reacting C in the presence of a titanium halide catalyst5～C10The fatty alcohol and the metal aluminum are fully reacted at the temperature of 90-180 ℃. The method has the advantages of reaction at a lower temperature, reduction of side reaction and improvement of the yield of the product.
CN102050700B proposes a method for preparing alkoxy aluminum, which comprises placing aluminum powder and/or aluminum wire and aluminum ingot into a reaction vessel, and reacting C in an inert environment3～C10Of fatty alcohols intoAnd two parts, wherein the first part is 10-35 wt.% of the total amount of alcohol, the first part is added into a reaction container firstly, the first part and aluminum powder or aluminum wires are subjected to initiation reaction, and the remaining second part of alcohol is continuously added into the reactor after the initiation of the reaction. The method does not use a catalyst, and has simple preparation method and complete reaction.
CN104355967B discloses a method for synthesizing aluminum isopropoxide by autocatalysis in one step, which adopts aluminum isopropoxide as a catalyst to synthesize high-purity aluminum isopropoxide by autocatalysis. High-purity aluminum isopropoxide is used as a catalyst, so that autocatalysis in the aluminum isopropoxide synthesis process is realized, and HgCl is replaced2、AlCl3、I2、CuCl2And the impurity elements are not introduced, the purity of the aluminum isopropoxide is improved, and a reliable raw material is provided for producing related high-purity materials by utilizing the aluminum isopropoxide subsequently.
In the process of synthesizing the aluminum alkoxide by aluminum, only aluminum isopropoxide can be used as a self-catalyst or no catalyst is used in the synthesis of the aluminum alkoxide, and a halogen-containing or mercury-containing catalyst is needed in most cases, so that the halogen-containing or mercury-containing catalyst can remain in products to influence the purity and is not suitable for raw materials of high-purity aluminum oxide or high-purity aluminum hydroxide; in addition, the reactor can be corroded or the reactor can enter the environment, so that the human health is endangered. The content of metal impurities in the aluminum isopropoxide is low due to the advantages of the catalyst, but the aluminum isopropoxide is easy to form a massive solid with a four-conglomerate structure, and is very inconvenient to use, ship and transport as a raw material of high-purity aluminum oxide and high-purity aluminum hydroxide.
Disclosure of Invention
The invention aims to overcome the defect of high melting point of alkoxy aluminum used by the existing high-purity aluminum oxide and high-purity aluminum hydroxide, and provides liquid mixed alkoxy aluminum and a synthesis method thereof.
The technical scheme of the invention is as follows:
a liquid mixed aluminum alkoxide having a melting point below 25 ℃ and a formula expressed as Al (OR)1)x(OR2)y(OR3)3-x-yWherein 0 is less than or equal to x<3,0≤y<3,0≤3-x-y<3, wherein OR1Is isopropoxy, R2And R3Has a molecular formula of CnH2n+1N is a natural number, and n is not less than 4.
A method for synthesizing liquid mixed alkoxy aluminum comprises the following steps:
step 1, mixing aluminum isopropoxide and at least one alcohol, and heating and refluxing to form a solution;
and 2, distilling the solution obtained in the step 1, controlling the temperature of the material to be not higher than 230 ℃, and obtaining a liquid mixed alkoxy aluminum product after the distillation is finished.
The molecular formula of the alcohol is CnH2n+1OH, n is a natural number, and n is more than or equal to 4 and less than or equal to 10.
The mass ratio of the alcohol to the aluminum isopropoxide is 1:3 to 6: 1.
The invention has the beneficial effects that: the easily obtained aluminium isopropoxide is used as a raw material and reacts with alcohol to generate liquid mixed alkoxy aluminium, the problems that the original aluminium isopropoxide is easy to cure and is difficult to package and transport and mercury-containing or halogen-containing catalysts are used in the synthesis of other alkoxy aluminium are solved, and the requirements of high-purity alumina and high-purity aluminium hydroxide on high purity and good fluidity of the alkoxy aluminium are met.
Detailed Description
The following detailed description of the invention will be made in conjunction with the accompanying drawings
Example 1
Putting 204g (1mol) of aluminium isopropoxide into a three-neck flask with the volume of 0.5L, adding 74g (1mol) of sec-butyl alcohol into the three-neck flask, heating and refluxing until a transparent solution is formed, and then carrying out normal pressure distillation to control the temperature of a distillate to be 82-83 ℃; when the temperature of the materials in the three-neck flask reaches 150 ℃ and no fraction flows out, carrying out reduced pressure distillation on the system (the absolute pressure is not higher than 0.01MPa), and controlling the temperature of the materials in the three-neck flask to be not higher than 150 ℃; when no fraction below 100 deg.C flows out, stopping heating and reducing pressure, cooling the product in three-neck flask to room temperature to obtain Al (C) as molecular formula3H7O)2(C4H9O) of a liquid mixed aluminum alkoxide.
Example 2
204g (1mol) of aluminum isopropoxide is taken and put into a containerAdding 148g (2mol) of sec-butyl alcohol into a 1L three-neck flask, heating and refluxing until a transparent solution is formed, and then carrying out atmospheric distillation to control the temperature of a distillate to be 82-83 ℃; when the temperature of the materials in the three-neck flask reaches 150 ℃ and no fraction flows out, carrying out reduced pressure distillation on the system (the absolute pressure is not higher than 0.01Mpa), and controlling the temperature of the materials in the three-neck flask to be not higher than 150 ℃; when no fraction below 100 deg.C flows out, stopping heating and reducing pressure, cooling the product in three-neck flask to room temperature to obtain Al (C) as molecular formula3H7O)(C4H9O)2The liquid mixed aluminum alkoxide of (2).
Example 3
Putting 204g (1mol) of aluminium isopropoxide into a three-neck flask with the volume of 1L, then adding 260g (2mol) of isooctanol into the three-neck flask, heating and refluxing until a transparent solution is formed, and then carrying out atmospheric distillation to control the temperature of a distillate to be 82-83 ℃; when the temperature of the materials in the three-neck flask reaches 190 ℃ and no fraction flows out, carrying out reduced pressure distillation on the system (the absolute pressure is not higher than 0.01MPa), and controlling the temperature of the materials in the three-neck flask to be not higher than 190 ℃; when no fraction below 100 deg.C flows out, stopping heating and reducing pressure, cooling the product in three-neck flask to room temperature to obtain Al (C) as molecular formula3H7O)(C8H17O)2The liquid mixed aluminum alkoxide of (2).
Example 4
Putting 204g (1mol) of aluminium isopropoxide into a three-neck flask with the volume of 1L, then adding 222g (3mol) of sec-butyl alcohol and 65g (0.5mol) of isooctyl alcohol into the three-neck flask, heating and refluxing until a transparent solution is formed, and then carrying out atmospheric distillation to control the temperature of a distillate to be 82-83 ℃; when the temperature of the materials in the three-neck flask reaches 160 ℃ and no fraction flows out, carrying out reduced pressure distillation on the system (the absolute pressure is not higher than 0.01MPa), and controlling the temperature of the materials in the three-neck flask to be not higher than 180 ℃; when no fraction below 100 deg.C flows out, stopping heating and reducing pressure, cooling the product in three-neck flask to room temperature to obtain Al (C) as molecular formula4H9O)2.5(C8H17O)0.5Of a liquid stateAluminum alkoxides are synthesized.
Example 5
204g (1mol) of aluminium isopropoxide is taken and put into a three-neck flask with the volume of 1L, then 144g (2mol) of sec-butyl alcohol and 65g (0.5mol) of isooctyl alcohol are added into the three-neck flask, heating and refluxing are carried out until a transparent solution is formed, and then atmospheric distillation is carried out to control the temperature of the distillate to be 82-83 ℃; when the temperature of the materials in the three-neck flask reaches 190 ℃ and no fraction flows out, carrying out reduced pressure distillation on the system (the absolute pressure is not higher than 0.01MPa), and controlling the temperature of the materials in the three-neck flask to be not higher than 190 ℃; stopping heating and reducing pressure when no fraction below 100 deg.C flows out, cooling the product in three-neck flask to room temperature to obtain liquid mixed alkoxy aluminum with molecular formula of Al (C)3H7O)0.5(C4H9O)2(C8H17O)0.5。
Claims (4)
1. A liquid mixed aluminum alkoxide, wherein the liquid mixed aluminum alkoxide has a melting point of less than 25 ℃ and a formula of Al (OR)1)x(OR2)y(OR3)3-x-yWherein 0 is less than or equal to x<3,0≤y<3,0≤3-x-y<3, wherein OR1Is isopropoxy, R2And R3Has a molecular formula of CnH2n+1N is a natural number, and n is not less than 4.
2. A method for synthesizing liquid mixed alkoxy aluminum is characterized by comprising the following steps:
step 1, mixing aluminum isopropoxide and at least one alcohol, and heating and refluxing to form a solution;
and 2, distilling the solution obtained in the step 1, controlling the temperature of the material to be not higher than 230 ℃, and obtaining a liquid mixed alkoxy aluminum product after the distillation is finished.
3. The method of claim 2, wherein the alcohol has the formula CnH2n+1OH, n is a natural number, and n is more than or equal to 4 and less than or equal to 10.
4. The method according to claim 2 or 3, wherein the ratio of the amount of the alcohol to the amount of the aluminum isopropoxide is 1:3 to 6: 1.
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|---|---|---|---|---|
| US3905936A (en) * | 1972-08-25 | 1975-09-16 | Commw Scient Ind Res Org | Coating particulates |
| US4525307A (en) * | 1983-08-02 | 1985-06-25 | Joseph Ayers, Inc. | Modified aluminum tri-alkoxide compounds |
| US4567030A (en) * | 1981-12-23 | 1986-01-28 | Tokuyama Soda Kabushiki Kaisha | Amorphous, spherical inorganic compound and process for preparation thereof |
| JP2001214268A (en) * | 2000-01-31 | 2001-08-07 | Asahi Denka Kogyo Kk | Aluminum raw material for chemical vapor growth and method for producing thin film using the same |
| CN101045805A (en) * | 2007-04-17 | 2007-10-03 | 广州市合诚化学有限公司 | Polypropylene resin composite for filling hollow shaping product and preparation method thereof |
| CN101250302A (en) * | 2008-04-02 | 2008-08-27 | 广州市合诚化学有限公司 | Anti-static polyolefin ventilated membrane composition and method for preparing the same |
| CN104355967A (en) * | 2014-11-12 | 2015-02-18 | 山东恒通晶体材料有限公司 | Self-catalyzed one-step synthesis method of high-purity aluminum isopropoxide |
| CN105246683A (en) * | 2013-05-28 | 2016-01-13 | 柯尼卡美能达株式会社 | Gas-barrier film and process for producing the same |
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| US4567030A (en) * | 1981-12-23 | 1986-01-28 | Tokuyama Soda Kabushiki Kaisha | Amorphous, spherical inorganic compound and process for preparation thereof |
| US4525307A (en) * | 1983-08-02 | 1985-06-25 | Joseph Ayers, Inc. | Modified aluminum tri-alkoxide compounds |
| JP2001214268A (en) * | 2000-01-31 | 2001-08-07 | Asahi Denka Kogyo Kk | Aluminum raw material for chemical vapor growth and method for producing thin film using the same |
| CN101045805A (en) * | 2007-04-17 | 2007-10-03 | 广州市合诚化学有限公司 | Polypropylene resin composite for filling hollow shaping product and preparation method thereof |
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