CN115872838A - Method for preparing high-purity aluminum isopropoxide by continuous method - Google Patents
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- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 48
- 238000011437 continuous method Methods 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 86
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 18
- 239000002808 molecular sieve Substances 0.000 claims description 16
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000007795 chemical reaction product Substances 0.000 claims description 15
- 239000003999 initiator Substances 0.000 claims description 13
- 238000004821 distillation Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 8
- 238000002386 leaching Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- 229960002523 mercuric chloride Drugs 0.000 claims description 3
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 239000011630 iodine Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 17
- 239000000463 material Substances 0.000 abstract description 14
- 239000000126 substance Substances 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 238000010924 continuous production Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 229910052728 basic metal Inorganic materials 0.000 abstract description 2
- 150000003818 basic metals Chemical class 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 description 25
- 239000000047 product Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 12
- 208000012839 conversion disease Diseases 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000008188 pellet Substances 0.000 description 4
- 230000000977 initiatory effect Effects 0.000 description 3
- 208000005156 Dehydration Diseases 0.000 description 2
- -1 aluminum alkoxide Chemical class 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 238000005844 autocatalytic reaction Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000013462 industrial intermediate Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000013024 troubleshooting Methods 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
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Abstract
The invention belongs to the field of synthesis of basic metal organic chemical materials, and discloses a method for preparing high-purity aluminum isopropoxide by a continuous method. The method disclosed by the invention can be used for preparing high-purity aluminum isopropoxide by a continuous method, effectively solving the problems of low production efficiency, difficulty in purity improvement and high production cost existing in an intermittent reaction production process, improving the production efficiency, ensuring the product purity, the productivity and the like by virtue of the unique advantages of continuous production while carrying out mass production, fully meeting the market demand and having good industrial prospect.
Description
Technical Field
The invention belongs to the field of synthesis of basic metal organic chemical materials, particularly relates to a method for preparing high-purity aluminum isopropoxide, and particularly relates to a method for preparing high-purity aluminum isopropoxide by a continuous method.
Background
The alumina has wide application and requirements in various fields by virtue of the characteristics of stable property, unique porous structure and the like, but with the development of science and technology, higher requirements are also put forward on the purity of the alumina. The internationally accepted preparation process of high-purity alumina is mainly realized by hydrolyzing aluminum alkoxide and then roasting, wherein the hydrolysis method of aluminum isopropoxide is the most applied method. The basic principle of preparing high-purity alumina from aluminum isopropoxide is that aluminum isopropoxide is hydrolyzed to obtain water and alumina, and high-purity alumina powder with different crystal structures can be obtained in a specific roasting environment, so that the method has an important significance for improving the purity of the raw material aluminum isopropoxide for the high-purity alumina. Aluminum isopropoxide is also a classical industrial intermediate material, is commonly used as a dehydrating agent, a waterproofing agent, a reducing agent and a precursor material of a catalyst, and has higher and higher requirements on the purity of aluminum isopropoxide as the application of aluminum materials in the fields of catalysis, photoelectricity and aerospace is increasingly extensive, and the high-efficiency production of aluminum isopropoxide with the purity of 5N or more (the mass purity of aluminum isopropoxide is more than or equal to 99.999%) becomes a direction of key research of chemists.
At present, the initiator commonly used in the production of aluminum isopropoxide is aluminum isopropoxide, aluminum chloride, mercuric chloride, iodine, copper chloride and the like. In patent CN1478767, a method for preparing aluminum isopropoxide is disclosed, wherein metal aluminum and a catalytic assistant are added into a synthesis reaction kettle, wherein the adding process of the metal aluminum is divided into multiple times, the adding amount of the metal aluminum is 20wt% -50wt% of the total, the adding amount of the catalytic assistant accounts for 70wt% -80wt% of the total materials, then isopropanol is added into the synthesis reaction kettle at a constant speed, the isopropanol accounts for 20wt% -30wt% of the total materials, the temperature of the gas discharged from a reflux condenser is between 27 ℃ and 29 ℃, and the temperature of the entering gas is between 72 ℃ and 75 ℃.
In patent CN 102992959, a method for preparing aluminum isopropoxide by using water-containing isopropanol is disclosed, wherein the water content in the isopropanol as a raw material liquid is required to be higher than 0.3wt%, and the main process comprises the following steps: adding aluminum isopropoxide into isopropanol, heating and stirring to fully dissolve the aluminum isopropoxide, then adding metal aluminum and a catalyst, heating to 82-100 ℃, returning the evaporated isopropanol to the reaction device again through a reflux device, wherein the aluminum sheets are completely consumed in the reaction kettle without being replenished in the midway process, and finishing the reaction. And then carrying out normal pressure distillation, recovering the isopropanol in the reaction kettle, recycling the isopropanol after treatment, and carrying out subsequent drying on the distillation product to obtain the dry aluminum isopropoxide powder.
At present, the production mode of aluminum isopropoxide is mostly an intermittent process carried out in a normal-pressure kettle, the production efficiency is low, and the whole production cycle of products is prolonged. In addition, a catalyst needs to be introduced, the source of product impurities is increased, the dissipation of by-product hydrogen needs to be carefully treated, the amount of produced products is controlled, and the like, so that the subsequent purification of aluminum isopropoxide, potential safety hazard troubleshooting and high-efficiency production are difficult, and the market demand cannot be met. For the defects existing in the batch production process at present, the batch production process needs to be further improved, or a continuous production process is adopted to further improve the production efficiency and the purity of the product.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing high-purity aluminum isopropoxide by a continuous process, which at least partially solves the problems of the prior art.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
a method for preparing high-purity aluminum isopropoxide by a continuous method comprises the steps of filling a single metal into a fixed bed reactor, leaching a bed layer of the fixed bed reactor by using an isopropanol solution containing an initiator, then continuously injecting the isopropanol into the fixed bed reactor, pressurizing and heating for reaction, collecting a reaction product, and drying after reduced pressure distillation to obtain the high-purity aluminum isopropoxide.
Preferably, the method also comprises the step of removing water from the isopropanol until the water content of the isopropanol is less than or equal to 0.5wt% before the isopropanol is injected into the fixed bed reactor.
Preferably, in the method, the isopropanol is dewatered by fully mixing a quantitative molecular sieve and an isopropanol solution and then standing for adsorption treatment.
Preferably, in the method, the molecular sieve type is at least one of 3A, 4A and 5A; the diameter specification of the molecular sieve is 0.5mm-3.0mm; the water removal time of the molecular sieve is 4-24 h.
Preferably, the purity of the metal aluminum in the method is more than or equal to 99.7%, the purity of the isopropanol is more than or equal to 99.0%, and the initiator in the method is at least one of aluminum isopropoxide, copper chloride, aluminum chloride, mercury chloride and iodine; the content of the initiator is 0.05wt% to 0.1wt%.
Preferably, in the method, the pressure heating is carried out for reaction under the reaction pressure of 0.5MPa to 10MPa, the reaction temperature of 80 ℃ to 200 ℃ and the reaction time of 4h to 12h.
Preferably, the flow space velocity of the isopropanol in the method is 5h -1 ～12h -1 。
Preferably, in the method, the reaction temperature of the reduced pressure distillation is 80-150 ℃, and the pressure is 0.01-0.1 Mpa.
Preferably, in the method, the drying temperature is 60-150 ℃, and the drying time is 6-24 h.
According to the technical scheme, the invention provides the method for preparing the high-purity aluminum isopropoxide by the continuous method. The method disclosed by the invention can be used for preparing high-purity aluminum isopropoxide by a continuous method, effectively solving the problems of low production efficiency, difficulty in purity improvement and high production cost existing in an intermittent reaction production process, improving the production efficiency, ensuring the product purity, the productivity and the like by virtue of the unique advantages of continuous production while carrying out mass production, fully meeting the market demand and having good industrial prospect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a reaction scheme for preparing high-purity aluminum isopropoxide by the continuous method.
Detailed Description
The invention discloses a method for preparing high-purity aluminum isopropoxide by a continuous method.
According to the method, isopropanol and simple substance metal aluminum with common purity are used as raw materials, isopropanol solutions compounded by different initiators are used for leaching a reactant bed layer to serve as a reaction initiation catalyst, then the isopropanol solutions are injected into a fixed bed reactor under the constant feeding flow, autocatalysis continuous synthesis can be carried out after the reaction initiation of aluminum alkoxide, and high-purity aluminum isopropoxide powder can be obtained after subsequent distillation and drying processes are carried out on reaction products.
In the method, the pressure of the fixed bed reactor is 0.5-10.0 Mpa, and the reactor material is acid-base resistant.
The isopropanol dehydration is to fully mix a quantitative molecular sieve and an isopropanol solution and perform standing adsorption treatment.
In the method, the purity of the used reaction raw material isopropanol is more than or equal to 99.0 percent, the diameter of the used moisture removing molecular sieve is 0.5mm-3.0mm, a 4A grade molecular sieve is preferred, and the diameter specification is preferably 0.5mm-1.0mm; the time of molecular sieve dehydration treatment is preferably 4h-48h, preferably 6h-24h, and the detected water content of the isopropanol is less than or equal to 0.5wt%, preferably less than or equal to 0.15wt%; the purity of the simple substance metallic aluminum is more than or equal to 99.7 percent, preferably more than or equal to 99.9 percent, the metallic aluminum can be processed into ingots, wires, strips, blocks and the like without limitation, and the filling requirement and the material supplementing requirement of the fixed bed reactor can be met.
In the method, the reaction initiator is prepared by mixing one or more of aluminum isopropoxide, aluminum chloride, mercuric chloride, iodine, copper chloride and the like with isopropanol, the concentration of the compound solution is 0.05-0.1 wt%, preferably the aluminum isopropoxide, and 0.08wt%, and the bed layer metallic aluminum raw material is fully leached. The initiator solution can be recycled.
In the method, the processed simple substance metallic aluminum (without limitation, ingots, wires, strips, blocks and the like) is filled into a fixed bed reactor, a material supplementing port is arranged, and the flow air speed ratio of a feeding pump is 5.0-12.0h -1 The reaction temperature is 80-200 ℃, the reaction pressure is 0.5-10.0 Mpa, the reaction time is 4-12 h, and the optimal air speed ratio is 8.0-10.0h -1 The reaction temperature is 120-150 ℃, the reaction pressure is 1.5-3.0 Mpa, and the reaction time is 8-10 h.
In the method, the aluminum isopropoxide product obtained by continuous bed reaction is collected into a distillation tower, the distillation temperature is 85-180 ℃, the operation pressure is reduced, and the pressure range is as follows: 0.01MPa to 0.1MPa, preferably the distillation temperature is 135 ℃ to 155 ℃, and the pressure range is as follows: 0.05Mpa to 0.08Mpa, the drying temperature is 60 ℃ to 150 ℃, and the drying time is 6h to 24h, preferably 120 ℃/12h.
For a further understanding of the present invention, reference will now be made in detail to the following examples. It should be noted that, in the case of no conflict, the features in the following embodiments and examples may be combined with each other; moreover, all other embodiments that can be derived by one of ordinary skill in the art from the embodiments disclosed herein without making any creative effort fall within the scope of the present disclosure.
Examples 1,
Mixing 10g of a 4A molecular sieve with 200ml of isopropanol solution, standing for dewatering, detecting the water content after 12 hours, and filtering for later use. 30g of 99.9% purity aluminum strip was processed into aluminum pellets having a diameter of about 0.5cm, and charged into a fixed bed reactor.
Preparing 20ml of 0.1wt% aluminum isopropoxide/isopropanol solution, fully leaching the bed layer aluminum particles, closing the reactor, heating and pressurizing to perform reaction, wherein the reaction temperature is 150 ℃, the reaction pressure is 1.5Mpa, and the flow air speed ratio of a feed pump is 8.0h -1 And the reaction time is 8h, and reaction products are collected at a discharge hole after the reaction is finished.
Distilling and purifying the reaction product at 150 ℃ under the reduced pressure of 0.1Mpa, and then placing the reaction product in a drying oven at 120 ℃ for drying for 24h to obtain dry aluminum isopropoxide powder, wherein the reaction conversion rate and the product purity are shown in Table 1.
Examples 2,
Mixing 10g of a 4A molecular sieve with 300ml of isopropanol solution, standing for dewatering, detecting the water content after 12 hours, and filtering for later use. 50g of 99.9% purity aluminum strip was processed into aluminum pellets having a diameter of about 1.0cm, and charged into a fixed bed reactor.
Preparing 30ml,0.05wt% aluminium isopropoxide/isopropanol solution, fully leaching the aluminum particles in the bed layer, closing the reactor, heating and pressurizing to perform reaction at 180 ℃, the reaction pressure of 3.0Mpa and the flow air speed ratio of the feeding pump of 5.0h -1 And the reaction time is 8h, and a reaction product is collected at a discharge hole after the reaction is finished.
Distilling and purifying the reaction product at 150 ℃ under the reduced pressure of 0.08Mpa, and then putting the reaction product in a drying oven at 120 ℃ for drying for 24h to obtain dry aluminum isopropoxide powder, wherein the reaction conversion rate and the product purity are shown in Table 1.
Examples 3,
Mixing 10g of a 4A molecular sieve with 200ml of isopropanol solution, standing for dewatering, detecting the water content after 12 hours, and filtering for later use. 30g of 99.9% purity aluminum strip was processed into aluminum pellets having a diameter of about 0.5cm, and charged into a fixed bed reactor.
Preparing 20ml of 0.1wt% aluminum isopropoxide/isopropanol solution, fully leaching the bed layer aluminum particles, closing the reactor, heating and pressurizing to perform reaction, wherein the reaction temperature is 120 ℃, the reaction pressure is 2.0Mpa, and the flow air speed ratio of a feed pump is 8.0h -1 And the reaction time is 8h, and a reaction product is collected at a discharge hole after the reaction is finished.
Distilling and purifying the reaction product at 140 ℃ under the reduced pressure of 0.1Mpa, and then placing the reaction product in a drying oven at 120 ℃ for drying for 24 hours to obtain dry aluminum isopropoxide powder, wherein the reaction conversion rate and the product purity are shown in Table 1.
Examples 4,
Mixing 10g of a 4A molecular sieve with 200ml of isopropanol solution, standing for dewatering, detecting the water content after 12 hours, and filtering for later use. 30g of 99.9% purity aluminum strip was processed into aluminum pellets having a diameter of about 0.8cm, and charged into a fixed bed reactor.
Preparing 20ml and 0.05wt% of aluminum isopropoxide/isopropanol solution, fully leaching bed aluminum particles, closing a reactor, heating and pressurizing to perform reaction, wherein the reaction temperature is 120 ℃, the reaction pressure is 1.0Mpa, and the flow air-speed ratio of a feed pump is 12.0h -1 And the reaction time is 8h, and reaction products are collected at a discharge hole after the reaction is finished.
Distilling and purifying the reaction product at 155 ℃ under the reduced pressure of 0.08Mpa, and then placing the reaction product in a drying oven at 120 ℃ for drying for 24 hours to obtain dry aluminum isopropoxide powder, wherein the reaction conversion rate and the product purity are shown in Table 1.
Comparative examples 1,
A high-purity isopropanolammonium aluminum material was prepared as in example 1, except that the water content of the isopropanolammonium solution was 2.0wt%, the reaction conversion and the product purity were the same as those shown in Table 1.
Comparative examples 2,
A high-purity aluminum isopropoxide material was prepared as in example 2, except that the concentration of the reaction initiator aluminum isopropoxide/isopropanol solution was 0.02wt%, and the reaction efficiency and the product purity were as shown in table 1, except that the conditions were the same.
Comparative examples 3,
A high purity aluminum isopropoxide material was prepared as in example 3, except that the purity of the reaction raw material, elemental metal, aluminum, was 95%, the reaction conversion and product purity were as shown in Table 1, except that the conditions were the same.
Comparative examples 4,
A high purity aluminum isopropoxide material was prepared as in example 4, except that the ratio of feed pump flow to air speed was 3.0h -1 The reaction conversion and the product purity are shown in Table 1, except for the same conditions.
TABLE 1 conversion and product purity of aluminum isopropoxide Table
| Sample numbering | Conversion rate | Purity of the product |
| Example 1 | 100％ | 99.993％ |
| Example 2 | 100％ | 99.995％ |
| Example 3 | 100％ | 99.990％ |
| Example 4 | 100％ | 99.992％ |
| Comparative example 1 | 0％ | / |
| Comparative example 2 | 98％ | 99.992％ |
| Comparative example 3 | 100％ | 99.93％ |
| Comparative example 4 | 90％ | 99.991％ |
As can be seen from the results in Table 1, the reaction conversion rates in examples 1 to 4 were all 100%, and the product purities were all 99.990% or more. The raw material of comparative example 1 has too high water content, and the reaction is not initiated; comparative example 2 the initiator concentration is too low, the reaction initiation time is prolonged, and the product purity is not influenced; comparative example 3 the low purity aluminum starting material can yield an aluminum isopropoxide product with a purity of 3N or greater; comparative example 4 has a low air velocity ratio, reduces the conversion rate, and does not affect the product purity.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for preparing high-purity aluminum isopropoxide by a continuous method is characterized in that a single metal is filled into a fixed bed reactor, an isopropanol solution containing an initiator is used for leaching a bed layer of the fixed bed reactor, then isopropanol is continuously injected into the fixed bed reactor to be pressurized and heated for reaction, a reaction product is collected, and the high-purity aluminum isopropoxide is obtained after reduced pressure distillation and drying.
2. The method of claim 1 further comprising the step of removing water from the isopropanol to a water content of 0.5 wt.% or less prior to injecting the isopropanol into the fixed bed reactor.
3. The method according to claim 2, wherein the isopropanol is dewatered by fully mixing a quantitative molecular sieve with an isopropanol solution and carrying out standing adsorption treatment.
4. The method of claim 3, wherein the molecular sieve type is at least one of 3A, 4A, 5A; the diameter specification of the molecular sieve is 0.5mm-3.0mm; the water removal time of the molecular sieve is 4-24 h.
5. The method of claim 1, wherein the metallic aluminum purity is greater than or equal to 99.7%, and the isopropanol purity is greater than or equal to 99.0%.
6. The method of claim 1, wherein the initiator is at least one of aluminum isopropoxide, copper chloride, aluminum chloride, mercuric chloride, iodine; the content of the initiator in the isopropanol solution containing the initiator is 0.05wt% -0.1wt%.
7. The method of claim 1, wherein the pressure heating is performed at a reaction pressure of 0.5Mpa to 10Mpa, a reaction temperature of 80 ℃ to 200 ℃, and a reaction time of 4h to 12h.
8. The method according to claim 1, wherein the flow space velocity of the isopropanol is 5h -1 ～12h -1 。
9. The method according to claim 1, wherein the reduced pressure distillation is carried out at a reaction temperature of 80 ℃ to 150 ℃ and a pressure of 0.01 to 0.1MPa.
10. The method according to claim 1, wherein the drying temperature is 60-150 ℃ and the drying time is 6-24 h.
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| CN102898275A (en) * | 2012-11-05 | 2013-01-30 | 苏州晶瑞化学有限公司 | Preparation method for high-purity isopropyl alcohol |
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