CN1062135A - Method for producing aluminum alkoxide - Google Patents
Method for producing aluminum alkoxide Download PDFInfo
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- CN1062135A CN1062135A CN 91111372 CN91111372A CN1062135A CN 1062135 A CN1062135 A CN 1062135A CN 91111372 CN91111372 CN 91111372 CN 91111372 A CN91111372 A CN 91111372A CN 1062135 A CN1062135 A CN 1062135A
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- Prior art keywords
- aluminium
- aluminum
- reaction
- alcohol
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- -1 aluminum alkoxide Chemical class 0.000 title abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000004411 aluminium Substances 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000012190 activator Substances 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- QKEOZZYXWAIQFO-UHFFFAOYSA-M mercury(1+);iodide Chemical compound [Hg]I QKEOZZYXWAIQFO-UHFFFAOYSA-M 0.000 claims description 7
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(II) oxide Inorganic materials [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 claims description 7
- CECABOMBVQNBEC-UHFFFAOYSA-K aluminium iodide Chemical compound I[Al](I)I CECABOMBVQNBEC-UHFFFAOYSA-K 0.000 claims description 6
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 abstract description 5
- 230000035484 reaction time Effects 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 35
- 238000005194 fractionation Methods 0.000 description 25
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 17
- 238000004821 distillation Methods 0.000 description 16
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 14
- 239000000047 product Substances 0.000 description 13
- 238000010025 steaming Methods 0.000 description 10
- 238000010992 reflux Methods 0.000 description 9
- 239000012043 crude product Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- JPUHCPXFQIXLMW-UHFFFAOYSA-N aluminium triethoxide Chemical compound CCO[Al](OCC)OCC JPUHCPXFQIXLMW-UHFFFAOYSA-N 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229960002523 mercuric chloride Drugs 0.000 description 1
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a production method of organic aluminium alkoxide, and is characterized by that it uses metal aluminium and excess alcohol to make reaction in the presence of catalyst, then firstly fractionates out excess alcohol and then distills out aluminium alkoxide product. The method has the advantages of short reaction time, high yield of high-quality products, simple process and the like.
Description
The present invention is reacted in the presence of activator by metallic aluminium and excessive alcohol about a kind of production method of organic aluminium alcoholates.
Aluminium alcoholates claims aluminum alkoxide again, and wherein the aluminium alcoholates that is made of 1-4 carbon atom claims the low-carbon (LC) aluminium alcoholates, and 4 above carbon atoms constitute is called the high-carbon aluminium alcoholates, and molecule becomes Al(OR)
3The purposes of aluminium alcoholates is mainly as dewatering agent, catalyzer, the raw material of water-resisting agent, also can be used for pharmaceutical industry, and with aluminium alcoholates particularly the further hydrolysis of low-carbon (LC) aluminium alcoholates to prepare high-purity ultra-fine alumina be the scheme of thinking comparatively feasible at present, this has also further widened the Application Areas of aluminium alcoholates, about the manufacturing reported in literature of aluminium alcoholates seldom, julid chemical plant, known Shanghai manufacture level isopropanol aluminium system adopts aluminium wire or aluminium foil and excessive anhydrous isopropyl alcohol heating reflux reaction in the presence of the aluminum chloride activator, treat aluminium all dissolve the back first underpressure distillation remove alcohol again vacuum distilling obtain aluminium alcoholates, similar approach once had report in the document at home and abroad, CN85100218 for example, Wilds A, L, org Reactior 21178(1944) and G C Whitaker, Adv Chem Ser 23, all related to the aluminum ethylate of aluminum isopropylate in document 184(1959), the aluminum methylate preparation method, except the aluminum methylate reaction is not that metal-salt is as the activator, alcohol all need adopt activator with the reaction of aluminium, and the activator kind only is confined to these two kinds in mercury chloride or aluminum chloride.
Experiment shows, adopts the above-mentioned activator reaction times longer, and large usage quantity, and activator remains in distillation tube wall and polluted product easily, reduces quality product also need clear up or change the distillation tube wall and influenced the technical process operation when situation is serious.
The objective of the invention is to overcome the deficiency of above-mentioned prior art existence and provide a kind of new activator of pure aluminium production process that is used for to improve the raw material that aluminium alcoholates production efficiency and the highly purified aluminium alcoholates of further preparation are used as the preparation high-purity super fine alumina.
Characteristics of the present invention are to adopt iodide as activator, metallic aluminium and excessive alcohol heating for dissolving in the presence of the activator iodide that are generally trace are reacted, fractionate out superfluous alcohol back redistillation then earlier and get the aluminium alcoholates product, the aluminium alcoholates foreign matter content that obtains is very low, the quality products yield that reaction obtains is very high, finishing the reaction times adopted aluminum chloride or mercuric chloride catalyst agent required time to shorten 1-3 doubly more originally, consumption is also than reducing 2-5 doubly, and white solid (mainly being the activator influence) collophore phenomenon appears in fractionation process hardly, goods of the present invention all meet table 1,2 listed technical requirements, the correlation technique parameter that the correlation data system that table 3 provides adopts identical reaction mass to obtain in the presence of different activators.
In the present invention, adopt the iodide activator as preferred version in the reaction of low-carbon alcohol and metallic aluminium, described iodide are red mercury iodide or aluminum iodide etc. preferably, add-on is the 0.02%(weight ratio of pure add-on) more than, be advisable with 0.06% upper limit, be higher than this upper limit also can, only be some the waste with unnecessary.In the present invention if employing purity is metallic aluminium and the low-carbon alcohol reaction more than 99.6%, once or second distillation will obtain purity and reach 99.99% low-carbon (LC) aluminium alcoholates, and the high purity product yield is higher, utilizes residue behind the single flash to drop into the reaction redistillation once more and claims the single flash flow process just of fractionation once more) will make the elaboration yield greater than more than 90 percent.The present invention does not need by distillation for several times if will obtain senior pure low-carbon (LC) aluminium alcoholates, and only need single flash and once more fractionation get final product, and foreign matter content is very little, adopt extraction colorimetry to detect the iodine foreign matter content that activator may bring, illustrate that all this foreign matter content can ignore and do not influence the final product quality.Table 4 has provided various embodiments of the present invention goods technical parameter index.Annotate: for the first time, fractionation includes in single flash once more, only has once more its absolute alcohol system that adds reaction of fractionated embodiment to dissolve the last time residue of reaction distillation remainder, so it doesn't matter fractionation for the first time.
Example 1. is that 99.8% industrial rafifinal is contained in 1 liter of round-bottomed flask of reflux condensing tube with 27 gram purity, adding 350～500 milliliters dehydrated alcohol And adds 0.1 gram red mercury iodide and heats 80～95 ℃ carry out back flow reaction in oil bath, after finishing building-up reactions in 3 hours, carry out first fractionation, promptly reclaimed at the dehydrated alcohol that steams surplus more than 80 ℃ earlier, oil bath is risen to 200～220 ℃ then and carry out underpressure distillation, get aluminum ethylate 122 grams, the ethanol rate of recovery 80.5% in the first fractionation, aluminum ethylate productive rate 75.3%; Clear liquid after the resistates that has not steamed in the flask after first fractionation leaches with 350～500 milliliters of dehydrated alcohols refluxes in the same device with the 27 industrial rafifinals that restrain purity 99.8% again.Building-up reactions and fractionation (fractionation once more), the fractionation ethanol rate of recovery 97% once more, aluminum ethylate productive rate 93.4%.
Example 2. is that 99.8% industrial rafifinal is contained in 1 liter of round-bottomed flask of reflux condensing tube with 27 gram purity, the anhydrous isopropyl alcohol And that adds 300 milliliters adds 0.1 gram aluminum iodide, in oil bath, heat 83～95 ℃ and carry out back flow reaction, carry out primary fractionation after finishing building-up reactions in 4 hours, promptly steaming superfluous anhydrous isopropyl alcohol more than 85 ℃ earlier, reclaim Virahol 47.9 grams, then oil bath is risen to 180～190 ℃ of vacuum fractionations and go out aluminum isopropylate 157.2 grams, isopropanol recovering rate 79.4% in the first fractionation, aluminum isopropylate productive rate 77.1%; Clear liquid after the resistates that has not steamed in the flask after first fractionation leaches with 300 milliliters of anhydrous isopropyl alcohols is again with 27 to restrain purity be that 99.8% industrial rafifinal carries out building-up reactions and fractionation (fractionation once more) in the same device, the rate of fractionation isopropanol recovering once more 95.7%, aluminum isopropylate productive rate 95.6%, obtain aluminum isopropylate product purity 99.98～99.99%, again through single flash (purify distillation or title second distillation), aluminum isopropylate product condition 〉=94.99%, wherein Al
2O
3Content 25.44%.
Example 3. with 27 gram purity be respectively 99～99.6% commercial-purity aluminium or 〉=99.97% rafifinal is contained in 1 liter of reflux condensing tube last time in the surplus thing round-bottomed flask that responds in distillation back, the anhydrous isopropyl alcohol And that adds 300 milliliters adds 0.2 gram red mercury iodide, in oil bath, be heated to 83～95 ℃ and carry out back flow reaction, finished building-up reactions in 3 hours, carry out fractionation once more, promptly earlier be respectively 48.7 grams steaming superfluous anhydrous isopropyl alcohol more than 85 ℃, 52.6 gram, after with oil bath rise to 180～190 ℃ of following vacuum fractionations go out aluminum isopropylate be respectively 192 the gram, 201 grams, the rate of fractionation isopropanol recovering once more is respectively 92.8%, 97.8%, the aluminum isopropylate productive rate is respectively 94.1%, 98.4%, aluminum isopropylate purity is respectively 99.97～99.98%, 〉=99.99%.
Example 4. is that 99.8% industrial rafifinal is contained in 10 liters of reaction vessels of reflux condensing tube with 540 gram purity, add 6 liters of And of anhydrous isopropyl alcohol and add 2 gram aluminum iodides, being heated to 89～95 ℃ in oil bath carries out back flow reaction and finished that to carry out fractionation once more after the building-up reactions be single flash in 4 hours, earlier steaming superfluous Virahol more than 85 ℃, temperature is risen to 180～190 ℃ then, steam aluminum isopropylate, wherein reclaim Virahol 825 grams, aluminum isopropylate crude product 338 grams (technical grade product), elaboration 3660 gram (its purity 99～99.98%, can make the SILVER REAGENT product), this elaboration is steamed purification through secondary again, can get purity 〉=99.99%, fractionation aluminum isopropylate total yield is 96% once more, wherein the elaboration yield is 88.5%, through second distillation purification aluminum isopropylate total yield is 92.2%, and wherein the elaboration yield is 85%, and the isopropanol recovering rate is 86.4%.
It is 99-99.98 that single flash obtains aluminum isopropylate crude product purity, can be used as down the raw material of second distillation or as the SILVER REAGENT product.
Example 5. is that 99.8% industrial rafifinal is contained in 10 liters of reaction vessels of reflux condensing tube with 540 gram purity, add anhydrous different pure 6 liters of And and add 2 gram red mercury iodides, in oil bath, be heated to 83～95 ℃ and carry out back flow reaction, carry out fractionation once more (distillation for the first time) after finishing building-up reactions in 4 hours, steaming superfluous Virahol more than 85 ℃, steam aluminum isopropylate under 180～190 ℃ and get aluminum isopropylate crude product 331.6 grams, elaboration 3665.9 grams, product purity≤99.99%, purity is purity＞99.99% after 〉=99.99%, three distillations are purified after second distillation is purified, the aluminum isopropylate total yield: a steaming yield is 95.8%; Two steaming yield are 91.8%, three steaming yield are 88.0%, elaboration total yield wherein: one to steam yield be 88.1%, it is that 80.9%, one steaming crude product can be used as technical grade product that two steamings are further divided into 84.4%, three steaming yield, two steam crude product purity near 99.99%, can be used as the raw material of next second distillation or make the SILVER REAGENT product, three steam crude product purity 〉=99.99%, can make three distillatory raw materials next time.
Example 6. adopts examples 1～example 5 to reclaim superfluous dehydrated alcohol and anhydrous isopropyl alcohol, and by the method steps of example 1, example 2, example 3 reflux building-up reactions and fractionation, 3 results are similar to example 1, example 2, example for the result of gained respectively.
Table 3 catalyst is to the influence of reaction deadline
| Sequence number | Condition | Catalyst title and consumption | Finish the reaction times (hour) |
| 1 | Be contained in 1 liter of flask of reflux condensing tube with 27 gram aluminium flakes and 300 milliliters of anhydrous isopropyl alcohols, add different catalyst and carrying out back flow reaction at 83～95 ℃ | 0.5 gram mercury chloride | 8 |
| 2 | 0.5 gram mercury chloride | 8 | |
| 3 | 0.5 gram mercury chloride iodine | 8 | |
| 4 | 0.5 gram aluminum chloride | 11 | |
| 5 | 0.5 gram aluminum chloride | 14 | |
| 6 | 0.3 gram aluminum chloride+12 gram aluminum isopropylates | 11 | |
| 7 | 0.3 gram aluminum chloride+12 gram aluminum isopropylates | 10 | |
| 8 | 0.2 gram red mercury iodide | 2.5 | |
| 9 | 0.2 gram aluminum iodide | 3.5 | |
| 10 | 0.1 gram aluminum iodide | 4 | |
| 11 | 0.1 gram red mercury iodide | 3.5 |
Claims (5)
1, a kind of preparation method of aluminium alcoholates is reacted by metallic aluminium and excessive alcohol heating for dissolving in the presence of the activator of trace, fractionates out superfluous alcohol back redistillation then earlier and goes out the aluminium alcoholates product, it is characterized in that the activator that adopts is iodide.
2, the manufacture method of aluminium alcoholates according to claim 1, the alcohol that it is characterized in that participating in reaction is low-carbon alcohol.
3, the manufacture method of aluminium alcoholates according to claim 1 and 2 is characterized in that iodide are red mercury iodide or aluminum iodide, and add-on is the 0.02%(weight ratio of pure add-on) more than.
4, the manufacture method of aluminium alcoholates according to claim 1 and 2, it is characterized in that adopting purity is metallic aluminium and low-carbon alcohol reaction more than 99.6%.
5, the manufacture method of aluminium alcoholates according to claim 3, it is characterized in that adopting purity is metallic aluminium and low-carbon alcohol reaction more than 99.6%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91111372 CN1062135A (en) | 1991-12-11 | 1991-12-11 | Method for producing aluminum alkoxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91111372 CN1062135A (en) | 1991-12-11 | 1991-12-11 | Method for producing aluminum alkoxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1062135A true CN1062135A (en) | 1992-06-24 |
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ID=4910608
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91111372 Pending CN1062135A (en) | 1991-12-11 | 1991-12-11 | Method for producing aluminum alkoxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1062135A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1318363C (en) * | 2003-09-27 | 2007-05-30 | 章浩龙 | Method for fabricating aluminum alkoxide |
| CN102153447A (en) * | 2011-01-26 | 2011-08-17 | 连云港连连化学有限公司 | Method for preparing and curing low-level alkanol aluminum |
| CN102898279A (en) * | 2012-10-19 | 2013-01-30 | 北京理工大学 | Preparation method for solid metal alkoxide |
| CN104230662A (en) * | 2014-09-23 | 2014-12-24 | 成都冠禹科技有限公司 | Preparation method of high-purity 5N aluminum isopropoxide |
| CN114773224A (en) * | 2022-04-29 | 2022-07-22 | 河南新邦化工技术有限公司 | Method for synthesizing nitrile compound by amide dehydration |
-
1991
- 1991-12-11 CN CN 91111372 patent/CN1062135A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1318363C (en) * | 2003-09-27 | 2007-05-30 | 章浩龙 | Method for fabricating aluminum alkoxide |
| CN102153447A (en) * | 2011-01-26 | 2011-08-17 | 连云港连连化学有限公司 | Method for preparing and curing low-level alkanol aluminum |
| WO2012100556A1 (en) * | 2011-01-26 | 2012-08-02 | Lianyungang Lianlian Chemicals Co., Ltd. | Process for the preparation and solidification of lower aluminum alkoxide |
| CN102153447B (en) * | 2011-01-26 | 2013-08-28 | 连云港连连化学有限公司 | Method for preparing and curing low-level alkanol aluminum |
| CN102898279A (en) * | 2012-10-19 | 2013-01-30 | 北京理工大学 | Preparation method for solid metal alkoxide |
| CN102898279B (en) * | 2012-10-19 | 2014-10-15 | 北京理工大学 | Preparation method for solid metal alkoxide |
| CN104230662A (en) * | 2014-09-23 | 2014-12-24 | 成都冠禹科技有限公司 | Preparation method of high-purity 5N aluminum isopropoxide |
| CN104230662B (en) * | 2014-09-23 | 2015-12-02 | 成都冠禹科技有限公司 | A kind of preparation method of high-purity 5N aluminum isopropylate |
| CN114773224A (en) * | 2022-04-29 | 2022-07-22 | 河南新邦化工技术有限公司 | Method for synthesizing nitrile compound by amide dehydration |
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