CN111116315B - Method for removing iron impurities in alkoxy aluminum - Google Patents
Method for removing iron impurities in alkoxy aluminum Download PDFInfo
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- CN111116315B CN111116315B CN201811281921.4A CN201811281921A CN111116315B CN 111116315 B CN111116315 B CN 111116315B CN 201811281921 A CN201811281921 A CN 201811281921A CN 111116315 B CN111116315 B CN 111116315B
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- 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
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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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
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
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Abstract
A method for removing iron impurities in alkoxy aluminum comprises the steps of adding a reducing agent and magnet powder into an alcoholic solution of alkoxy aluminum to fully react, filtering a reaction product to remove solids, and obtaining the alcoholic solution of alkoxy aluminum with iron impurities removed, wherein the reducing agent is selected from one or more of simple substance aluminum, hydroxylamine hydrochloride and ascorbic acid. The method is simple to operate and easy to industrialize, and can effectively remove iron impurities to obtain high-purity alkoxy aluminum.
Description
Technical Field
The invention relates to a method for removing metal impurities in alkoxy aluminum, in particular to a method for filtering and removing iron impurities in alkoxy aluminum.
Background
The alkoxy aluminum is an important chemical intermediate, can be used as a dehydrating agent, a coupling agent, a catalyst, a waterproof agent and the like, and is mainly used as a precursor for preparing high-purity aluminum oxide. The aluminum alkoxide can be prepared by preparing high-purity aluminum hydroxide through thermal decomposition or hydrolysis, and then calcining to prepare high-purity alumina. Since impurities such as silicon, iron, zinc, magnesium and the like in the aluminum alkoxide can be brought into the aluminum hydroxide in the hydrolysis process, namely the purity of the aluminum alkoxide directly determines the purity of the product aluminum oxide, metal impurities need to be removed in the preparation process of the aluminum alkoxide, wherein the iron impurity is one of the metal impurities which are high in content and difficult to remove.
The most common methods for removing iron impurities in the aluminum alkoxide include a reduced pressure distillation method, an extraction method and the like. The conventional methods have good purification effect on the constant iron impurities, but the purification effect and low energy consumption are difficult to be considered simultaneously, and the methods have the defects of high operation difficulty, high equipment investment and the like, and are difficult to produce ultrahigh-purity aluminum oxide or aluminum hydroxide.
CN1085620C discloses a method for preparing high-purity aluminum oxide by an alkoxy aluminum hydrolysis method, wherein the step of purifying the alkoxy aluminum comprises the steps of transferring the alkoxy aluminum into a reduced pressure distillation tower, heating to 120-200 ℃, reducing the pressure to ensure that the vacuum degree reaches 1-10 mmHg, and carrying out reduced pressure distillation purification, wherein the purity of the obtained alkoxy aluminum can reach 99.99-99.999%. The method can obtain high-purity alkoxy aluminum, but the energy consumption for purifying the alkoxy aluminum by reduced pressure distillation is high, and the alkoxy aluminum can be decomposed and polymerized at high temperature, so that the product yield is influenced.
CN1513762A discloses a method for removing trace iron in aluminum alkoxide, which comprises reacting industrial aluminum ingot with alcohol to generate aluminum alkoxide, distilling under reduced pressure to evaporate aluminum alkoxide to obtain primary purified aluminum alkoxide, dissolving in organic solvent, adding complexing agent to form soluble complex of iron and complexing agent, cooling for crystallization, crystallizing aluminum alkoxide, keeping iron complex in solution phase, and removing iron impurity by solid-liquid separation. The method can ensure that the iron content in the aluminum alkoxide is 25-120 ppm (Al) by simple reduced pressure distillation 2 O 3 Calculated) to 6ppm. The distillation operation of the method has high energy consumption and complicated operation steps.
The research on the purification of aluminum isopropoxide by extraction-complexation method (university of general theory, vol.39, no.1, jan.1999, P53-55) by Poplar Yonglai et al discloses a technique for removing iron impurities from aluminum isopropoxide, which comprises dehydrating isopropanol, mixing with industrial aluminum (99.0% by mass, heating and reacting main impurities with mass fractions w (Cu) of less than or equal to 0.05%, w (Fe) of less than or equal to 0.50% and w (Si) of less than or equal to 0.50% in the presence of a catalyst to prepare coarse aluminum isopropoxide, adding a certain extracting agent for liquid-solid extraction, fully stirring, and standing for 12 hours to obtain an extraction clear solution; adding a proper amount of complexing agent (white powdery solid) into a certain amount of the extract, dispersing for 10min under the action of ultrasonic waves, placing on a magnetic stirrer, heating to 60 ℃, stirring for 15min, standing, settling for 12h to obtain high-purity aluminum isopropoxide purified liquid, and evaporating the extracting agent to obtain the high-purity aluminum isopropoxide. DCTA is adopted as a complexing agent, so that the iron content in aluminum isopropoxide can be reduced to 6ppm, but the recovery energy consumption of the extracting agent is too high and the operation steps are complex.
In addition to the above methods, the filtration method has been applied to the synthesis of metal alkoxide compounds because of its simple operation and high energy utilization efficiency.
CN102120598A discloses a preparation method of high-purity hydrated alumina, which comprises the steps of reacting metal aluminum with C5-C8 alcohol in the presence of an aluminum trichloride catalyst, filtering while the reaction is hot to obtain alkoxy aluminum, removing impurities in the alkoxy aluminum, and then adding water into the alkoxy aluminum for hydrolysis to obtain the high-purity hydrated alumina. The content of iron impurities in the high-purity hydrated alumina obtained by the method is less than 50ppm, but the method can not remove soluble impurities in the aluminum alkoxide, the aluminum alkoxide is not treated, the content of the impurities in the aluminum alkoxide is completely dependent on the content of the impurities in the raw materials, the product property is difficult to control, and the method is difficult to industrially apply.
GB825972A discloses an improved process for the preparation of high purity alumina by reacting aluminium with an alcohol to form an alcoholic solution of an aluminium alkoxide, adding a hydrocarbon or mixture of liquid hydrocarbons, settling out some of the impurities, separating out the impurities and hydrolysing the aluminium alkoxide. The hydrocarbon is pentane, hexane, benzene, toluene or xylene, and also mixtures of hydrocarbons, such as petroleum ether. The method uses a large amount of solvent, so that the energy consumption required by the rectification and recovery of the solvent is increased, and soluble impurities cannot be removed.
CN106673959A discloses a preparation method of high-purity aluminum alkoxide. The method takes anhydrous aluminum chloride as a catalyst, and makes materials contact with stainless steel filler in the process of generating the alkoxy aluminum by reacting alcohol and aluminum, preferably, the alcohol and aluminum are reacted under the condition of an external magnetic field, and after the reaction is finished, the high-purity alkoxy aluminum can be obtained by filtering.
CN106673960A discloses a preparation method of high-purity aluminum alkoxide, which takes anhydrous aluminum chloride as a catalyst, and adds crystalline Fe into a material obtained by the reaction of alcohol and aluminum 3 O 4 Solid particles, preferably, the reaction of the alcohol and aluminum is carried out in the presence of an externally applied magnetic field. In order to ensure that the filtration is rapid, trimethylbenzene is added into the reaction raw materials, and the high-purity alkoxy aluminum can be obtained by filtration after the reaction is finished.
Disclosure of Invention
The invention aims to provide a method for removing iron impurities in aluminum alkoxide. The method removes iron impurities in the alkoxy aluminum by adding a reducing agent and magnet powder to react and then filtering, and has the advantages of simple operation and good effect.
The method for removing the iron impurities in the alkoxy aluminum comprises the steps of adding a reducing agent and magnet powder into an alcoholic solution of the alkoxy aluminum for full reaction, filtering a reaction product to remove solids, and obtaining the alcoholic solution of the alkoxy aluminum with the iron impurities removed, wherein the reducing agent is selected from one or more of simple substance aluminum, hydroxylamine hydrochloride and ascorbic acid.
The method of the invention adds a reducing agent and magnet powder into an alcoholic solution of alkoxy aluminum for reaction, and then filters to remove iron impurities. The method is simple to operate and easy to industrialize, and can effectively remove iron impurities to obtain high-purity alkoxy aluminum.
Detailed Description
According to the method, a reducing agent and magnet powder are added into an alkoxy aluminum alcohol solution to react, the reducing agent reduces iron impurities into simple substance iron, the magnet powder in the system adsorbs the reduced iron and plays a role in filter aid in the subsequent filtering process, so that the filtering is easy to carry out, the alkoxy aluminum alcohol solution after reaction is filtered, the impurity iron is removed by filtering along with the magnet powder, and the obtained filtrate is the high-purity alkoxy aluminum after iron removal.
The content of the aluminum alkoxide in the alcohol solution of the aluminum alkoxide in the method of the present invention may be 60 to 99.9 mass%, preferably 70 to 97 mass%.
The carbon number of the alkoxy group in the aluminum alkoxide of the present invention is 2 to 12, preferably 3 to 10. The carbon number of the alcohol in the alkoxy aluminum alcohol solution can be the same as or different from that of the alkoxy in the alkoxy aluminum. The alcohol may be C 2 ～C 12 The fatty alcohol of (1).
The alcohol solution of the aluminum alkoxide can be a fresh solution prepared by reacting aluminum with excessive alcohol, and can also be a solution prepared by adding alcohol into the aluminum alkoxide.
The magnet powder used in the method is used for adsorbing the reduced simple substance iron and has the function of filter aid. The particle size of the magnet powder is preferably 50 to 1000. Mu.m, more preferably 50 to 900. Mu.m. The magnetic material content in the magnet powder is preferably 90 to 100 mass%, more preferably 98 to 100 mass%.
The mass ratio of the magnet powder to the alcohol solution of the aluminum alkoxide added in the present invention is 0.02 to 0.8, and more preferably 0.04 to 0.6. The mass ratio of the reducing agent to the alcoholic solution of aluminum alkoxide added is 0.01 to 0.5, more preferably 0.02 to 0.4. If the reducing agent is added as a mixture of two or three substances, the amount of reducing agent added is the total amount of substances contained in the mixture. When the reducing agent is hydroxylamine hydrochloride and/or ascorbic acid, the mass ratio of the added reducing agent to the alcoholic solution of the aluminum alkoxide is preferably 0.02 to 0.2.
When the reducing agent is elemental aluminum, the purity is not less than 99.99 mass%, and before use, the aluminum is preferably treated with hydrochloric acid having a concentration of 1 to 8 mass%, and then washed with water to remove surface oxides and impurities. The mass ratio of the added simple substance aluminum to the alkoxy aluminum alcohol solution is preferably 0.1-0.4.
In the method, the temperature for adding the reducing agent and the magnet powder into the alkoxy aluminum alcohol solution to react is 5-100 ℃ higher than the condensation point of the alkoxy aluminum alcohol solution, so that the reaction is carried out in a liquid phase. In general, the higher the number of carbons in the alkoxy group of the aluminum alkoxide, the higher the condensation point of the aluminum alkoxide alcohol solution, and the higher the reaction temperature. Preferably, the reducing agent and the magnet powder are added to the alkoxy aluminum alcohol solution to react at a temperature of 50 to 230 ℃, preferably 50 to 200 ℃, for 0.5 to 6 hours, preferably 0.5 to 2 hours.
According to the method, after a reducing agent and magnet powder are added into an alkoxy aluminum alcohol solution for reaction, a filtering method is adopted to remove solids in a reaction product, and the filtering can adopt one of pressure filtering, reduced pressure filtering and centrifugal filtering or a combination of the filtering methods. The temperature for filtering the reaction product is 5-100 ℃ higher than the condensation point of the alcohol solution of the aluminum alkoxide, and is preferably the same as the reaction temperature.
The magnet powder obtained by filtering can be reused after impurities are removed by washing.
The fresh alkoxy aluminum alcohol solution prepared by the reaction of aluminum and excessive alcohol can be prepared by a two-step feeding method, and comprises the following steps:
(1) Adding aluminum and alcohol into a reaction kettle, initiating reaction at a reaction temperature of 5-50 ℃ lower than the boiling point of the alcohol until the reaction is stable,
(2) And adding aluminum and alcohol into the reaction kettle, and continuing to react until the aluminum is completely dissolved.
The aluminum used for preparing the alkoxy aluminum in the above method may be at least one of aluminum wire, aluminum sheet, aluminum ingot, aluminum bean and aluminum powder, and the purity of the aluminum is not less than 97.0 mass%, preferably not less than 97.5 mass%. Preferably, the purity of the aluminum used for the initiation reaction in the step (1) is higher than that of the aluminum used for the preparation of the aluminum alkoxide in the step (2).
The alcohol may be C 2 ～C 12 Fatty alcohols of (2), preferably C 3 ～C 10 Such as ethanol, n-propanol, isopropanol, n-butanol, isobutanol, n-pentanol, isopentanol, n-hexanol, isohexanol, n-heptanol, isoheptanol, n-octanol, isooctanol. The purity of the alcohol is not less than 99.5 mass%, preferably not less than 99.8 mass%.
The amount of aluminum used in the step (1) of the above process is 30 to 60 mass%, preferably 40 to 55 mass%, based on the total amount of aluminum required for the whole reaction. The amount of the alcohol to be used is 5 to 40% by mass, preferably 10 to 35% by mass, based on the total amount of the alcohol required for the entire reaction.
In the whole reaction of the method, the molar ratio of the alcohol to the aluminum is 3-10: 1. preferably 4 to 6:1.
in the above step (2), it is preferable to control the reaction temperature within. + -. 20 ℃ from the boiling point of the alcohol in order to make the reaction proceed smoothly.
The present invention is described in further detail below by way of examples, but the present invention is not limited thereto.
In the examples and comparative examples, the iron content of the alkoxy aluminium alcohol solution was determined by means of an iCAP 6000 inductively coupled plasma spectrometer from Thermo corporation, USA, and the analytical method is GB/T20975.25-2008.
Example 1
(1) Preparation of AlkoxyAlcoholic solutions
Taking 2.25 kg (37.46 mol) of isopropanol with the purity of 99.8 mass percent, adding 450 g (16.62 mol) of monoblock aluminum ingot with the purity of 99.7 mass percent, slowly heating to 70 ℃, initiating reaction after 8 minutes, maintaining the temperature at 68-72 ℃ until the reaction is stable, adding 450 g (16.62 mol) of aluminum ingot with the purity of 99.7 mass percent, continuously dropwise adding 5.25 kg (87.41 mol) of isopropanol for 1 hour, then reacting at 70 ℃ for 4 hours, and cooling to 25 ℃; an isopropyl alcohol solution of aluminum isopropoxide was obtained, in which the content of aluminum isopropoxide was 80.54 mass%, and the content of iron impurities was as shown in Table 1.
(2) Removing iron impurities
Taking 50ml (40 g) of the isopropoxy aluminum alcohol solution (the boiling point of which is 135 ℃ and the condensation point of which is 12 ℃) prepared in the step (1), heating to 70 ℃, adding 2g of hydroxylamine hydrochloride and 2g of magnet powder (the brand name of which is Titd, manufactured by Nangongkao gold welding materials Co., ltd.) with the granularity of 70-150 mu m and the magnetic substance content of 99.9 mass percent, stirring and reacting for 1 hour, and filtering by using a filter funnel at reduced pressure and 65 ℃, wherein the obtained filtrate is the iron-removed isopropoxy aluminum alcohol solution, and the iron impurity content of the solution is shown in Table 1.
Example 2
(1) Preparation of Alkoxyal solutions
An alkoxyaluminum alcohol solution was prepared by the method of the step (1) in example 1, except that isopropanol was replaced with an equimolar amount of n-hexylalcohol, the reaction temperature was initiated at 110 ℃ for 25 minutes, the reaction temperature was 140 to 169 ℃ and the n-hexyloxy aluminum solution obtained had an n-hexyloxy aluminum content of 79.75% by mass and an iron impurity content as shown in Table 1.
(2) Removing iron impurities
40g of an alcoholic solution of n-hexyloxy aluminum (boiling point: 161 ℃ C., condensation point: 46 ℃ C.) was taken, and iron impurities were removed by the procedure of example 1 (2), the reaction temperature was 110 ℃ C., and the filtration temperature was 100 ℃ C., and the iron content of the obtained iron impurity-removed n-hexyloxy aluminum alcoholic solution was shown in Table 1.
Example 3
The iron impurity in the aluminum isopropoxide alcohol solution was removed in the same manner as in example 1, except that 6g of hydroxylamine hydrochloride was added in the step (2), and the iron content in the iron impurity-removed aluminum isopropoxide alcohol solution was obtained as shown in Table 1.
Example 4
The iron impurity in the aluminum isopropoxide alcohol solution was removed in the same manner as in example 1, except that 1g of hydroxylamine hydrochloride and 1g of ascorbic acid were added as reducing agents in the step (2), and the iron content in the iron impurity-removed aluminum isopropoxide alcohol solution was obtained as shown in Table 1.
Example 5
The iron impurity in the aluminum isopropoxide alcohol solution was removed as in example 1, except that 2g of ascorbic acid was used in place of hydroxylamine hydrochloride in the step (2), and the iron content in the iron impurity-removed aluminum isopropoxide alcohol solution was obtained as shown in Table 1.
Example 6
Iron impurities were removed from the aluminum isopropoxide alcohol solution by the method of example 1, except that the amount of the magnet powder used in step (2) was 20g, and the iron content of the iron-impurity-removed aluminum isopropoxide alcohol solution obtained was as shown in Table 1.
Example 7
Iron impurities in the isopropoxy aluminum alcohol solution were removed by the method of example 1, except that the magnetic substance content of the magnet powder used in step (2) was 98.0 mass%, and the iron content in the obtained isopropoxy aluminum alcohol solution with iron impurities removed was as shown in table 1.
Example 8
The iron impurities in the isopropoxy aluminum alcohol solution were removed in the same manner as in example 1, except that the magnet powder added in step (2) had a particle size of 425 to 850 μm, and the iron content in the obtained isopropoxy aluminum alcohol solution from which iron impurities were removed was as shown in table 1.
Example 9
The iron impurity in the isopropoxy aluminum alcohol solution was removed by the method of example 1, except that (2) hydroxylamine hydrochloride and magnet powder were added to the alkoxy aluminum alcohol solution and the mixture was stirred for 2 hours, and the iron content in the isopropoxy aluminum alcohol solution with iron impurity removed was as shown in table 1.
Example 10
The iron impurity in the isopropoxy aluminum alcohol solution was removed by the method of example 1, except that (2) after adding hydroxylamine hydrochloride and magnet powder to the alkoxy aluminum alcohol solution, stirring reaction and filtration were carried out at 55 ℃ to obtain an isopropoxy aluminum alcohol solution from which the iron impurity was removed, the iron content of which is shown in table 1.
Example 11
The iron impurity in the isopropoxy aluminum alcohol solution was removed by the method of example 1, except that the reducing agent used in step (2) was 10g of aluminum beans having a purity of 99.999% by mass, which were treated with 40ml of hydrochloric acid having a concentration of 5% by mass before use, and then washed with 200ml of deionized water, and the iron content in the isopropoxy aluminum alcohol solution from which the iron impurity was removed was obtained as shown in table 1.
Comparative example 1
The iron impurity in the aluminum isopropoxide alcohol solution was removed as in example 1 except that the reducing agent hydroxylamine hydrochloride was not added in step (2), and the iron content in the aluminum isopropoxide alcohol solution obtained after filtration was as shown in Table 1.
Comparative example 2
The iron impurities in the solution of aluminum isopropoxide alcohol were removed as in example 1, except that aluminum powder was used in place of the magnet powder in the step (2), and the iron content in the solution of aluminum isopropoxide alcohol obtained after filtration was as shown in Table 1.
TABLE 1
As can be seen from Table 1, the method of the present invention has a better effect of removing iron impurities from the alkoxyaluminumhanol solution than the comparative example in which the reducing agent is not added and the aluminum powder is used instead of the magnet powder as the filter aid.
Claims (9)
1. A method for removing iron impurities in alkoxy aluminum comprises the steps of adding a reducing agent and magnet powder into an alcoholic solution of alkoxy aluminum to fully react, wherein the mass ratio of the added reducing agent to the alcoholic solution of alkoxy aluminum is 0.01-0.5, the mass ratio of the added magnet powder to the alcoholic solution of alkoxy aluminum is 0.02-0.8, filtering a reaction product to remove solids, and thus obtaining the alcoholic solution of alkoxy aluminum with iron impurities removed, wherein the reducing agent is selected from one or more of simple substance aluminum, hydroxylamine hydrochloride and ascorbic acid, and the alkoxy carbon number of the alkoxy aluminum is 2-12.
2. The method according to claim 1, wherein the alcohol solution of aluminum alkoxide has an aluminum alkoxide content of 60 to 99.9 mass%.
3. The method of claim 1, wherein the alcoholic solution of aluminum alkoxide is a fresh solution prepared by reacting aluminum with an excess of alcohol, or a solution prepared by adding alcohol to aluminum alkoxide.
4. The method according to claim 1, wherein the magnet powder has a particle size of 50 to 1000 μm.
5. The method according to claim 1, wherein the magnetic powder contains 90 to 100 mass% of the magnetic material.
6. The method according to claim 1, wherein the reaction time after adding the reducing agent and the magnet powder is 0.5 to 6 hours.
7. The method as set forth in claim 1, wherein the reaction temperature after adding the reducing agent and the magnet powder is 5 to 100 ℃ higher than the solidifying point of the alkoxyaluminumhydrin alcohol solution.
8. The method as set forth in claim 1, wherein the reaction temperature after adding the reducing agent and the magnet powder is 50 to 230 ℃.
9. The process as claimed in claim 1, wherein the temperature at which the reaction product is filtered is from 5 to 100 ℃ above the condensation point of the alcoholic solution of the aluminum alkoxide.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1513762A (en) * | 2003-08-12 | 2004-07-21 | 大连理工大学 | Purification technology of removing trace iron in alfol salt using complexation-crystallization method |
| CN102050700A (en) * | 2009-10-28 | 2011-05-11 | 中国石油化工股份有限公司 | Method for preparing alkoxy aluminum |
| WO2012100556A1 (en) * | 2011-01-26 | 2012-08-02 | Lianyungang Lianlian Chemicals Co., Ltd. | Process for the preparation and solidification of lower aluminum alkoxide |
| CN106673960A (en) * | 2015-11-11 | 2017-05-17 | 中国石油化工股份有限公司 | Preparation method of high-purity aluminum alkoxide |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB825972A (en) * | 1957-05-16 | 1959-12-23 | Ici Ltd | Improvements in and relating to the production of alumina |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1513762A (en) * | 2003-08-12 | 2004-07-21 | 大连理工大学 | Purification technology of removing trace iron in alfol salt using complexation-crystallization method |
| CN102050700A (en) * | 2009-10-28 | 2011-05-11 | 中国石油化工股份有限公司 | Method for preparing alkoxy aluminum |
| WO2012100556A1 (en) * | 2011-01-26 | 2012-08-02 | Lianyungang Lianlian Chemicals Co., Ltd. | Process for the preparation and solidification of lower aluminum alkoxide |
| CN106673960A (en) * | 2015-11-11 | 2017-05-17 | 中国石油化工股份有限公司 | Preparation method of high-purity aluminum alkoxide |
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