CN115771909A - Method for coproducing hexanol and pseudo-boehmite - Google Patents
Method for coproducing hexanol and pseudo-boehmite Download PDFInfo
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- CN115771909A CN115771909A CN202211295796.9A CN202211295796A CN115771909A CN 115771909 A CN115771909 A CN 115771909A CN 202211295796 A CN202211295796 A CN 202211295796A CN 115771909 A CN115771909 A CN 115771909A
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- Prior art keywords
- aluminum
- aluminum powder
- hexanol
- filtering
- activating material
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- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 title claims abstract description 62
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 23
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 65
- 239000000463 material Substances 0.000 claims abstract description 30
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 150000004645 aluminates Chemical class 0.000 claims abstract description 13
- 239000007822 coupling agent Substances 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 11
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- -1 tri-n-hexylaluminum alkoxide Chemical class 0.000 claims abstract description 4
- 230000003213 activating effect Effects 0.000 claims description 24
- 239000002994 raw material Substances 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 claims description 4
- 239000008188 pellet Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 3
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000001833 catalytic reforming Methods 0.000 description 1
- 150000004682 monohydrates Chemical class 0.000 description 1
- 238000001935 peptisation Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
Abstract
The invention relates to the technical field of compounds, in particular to a method for coproducing hexanol and pseudoboehmite. The method comprises the following steps: putting aluminum powder into a ball mill, adding an aluminate coupling agent, uniformly mixing, performing ball milling to obtain an aluminum powder activated material, putting the aluminum powder activated material, aluminum trichloride and n-hexyl alcohol into a reaction kettle, uniformly mixing, then performing heating reaction, and filtering to obtain a mixed solution of tri-n-hexylalkoxy aluminum; adding deionized water into a reaction kettle, adding a mixed solution of tri-n-hexylaluminum alkoxide, reacting, and filtering to obtain a liquid of n-hexanol and a solid of aluminum oxyhydroxide; adding deionized water into the aluminum oxyhydroxide, heating to aging, filtering, drying the filter residue, and crushing to obtain the pseudo-boehmite. The aluminate coupling agent of the invention carries out ball milling on the aluminum powder, so that the specific surface area of the aluminum powder is increased, the reaction activity of the aluminum powder and the n-hexanol is increased, the yield of the prepared target product is higher than that of the prior art, and the requirement of actual production is met.
Description
Technical Field
The invention relates to the technical field of compounds, in particular to a method for coproducing hexanol and pseudoboehmite.
Background
Pseudo-boehmite, also known as monohydrate alumina, is an important catalyst raw material and is widely applied in the petrochemical field such as catalytic cracking, hydrogenation, reforming and the like. Besides being an important catalyst carrier, the pseudo-boehmite is also a main adhesive for preparing other various catalysts and has a considerable effect.
The large pore volume of the pseudo-boehmite can be directly used as a catalyst carrier, the small pore volume can be used as an adhesive of the catalyst carrier, and the pseudo-boehmite produced by an alcoaluminum method represented by Germany Sasol company abroad has the characteristics of 99% of peptization index, fast sol-gel process and good thixotropy, so that the market of the pseudo-boehmite used as the adhesive in the field of catalysts is unique. At present, manufacturers in China also adopt an aluminum alkoxide method to prepare pseudo-boehmite products. Firstly, the high-purity aluminum ingot is adopted for reaction, the cost of the prepared pseudoboehmite is high, the preparation cost basically reaches the market price, and the popularization is difficult; secondly, the crystallinity of the produced pseudoboehmite product is low, the thixotropic time is long when the pseudoboehmite product meets acid, the gel forming index is low, and some pseudoboehmite products even contain three aluminum miscellaneous items and have low quality.
Based on the situation, the invention provides a method for coproducing hexanol and pseudo-boehmite.
Disclosure of Invention
The invention aims to provide a method for co-producing hexanol and pseudo-boehmite.
In order to achieve the above object, the present invention provides a method for co-producing hexanol and pseudoboehmite, comprising the steps of:
(1) Putting aluminum powder into a ball mill, adding an aluminate coupling agent, mixing uniformly, adding steel balls, and performing ball milling at room temperature in a nitrogen atmosphere to obtain an aluminum powder activating material;
(2) Putting an aluminum powder activating material, aluminum trichloride and n-hexyl alcohol into a reaction kettle, uniformly mixing, then heating to 100-110 ℃, reacting for 30-40 min, and filtering to obtain a mixed solution of tri-n-hexylalkoxy aluminum;
(3) Adding deionized water into a reaction kettle, heating to 70-80 ℃, adding 1/3-1/4 of mixed solution of tri-n-hexylalkoxy aluminum every 5-6 min, continuously reacting for 20-30 min after finishing dripping, standing for 15-20 min, and filtering to obtain n-hexanol as liquid and aluminum oxyhydroxide as solid;
(4) Taking hydroxy alumina, adding deionized water, heating to 90-100 ℃, aging for 10-12 h, filtering, drying filter residue at 110-120 ℃, and crushing to obtain the pseudo-boehmite.
Preferably, in the step (1), the ratio of aluminum powder to aluminum powder is 1: 0.02-0.03 adding aluminate coupling agent and mixing evenly.
Preferably, the aluminate coupling agent is an aluminate coupling agent with an acetyl group.
Preferably, the aluminate coupling agent with acetyl groups is aluminum triacetylacetonate.
Preferably, in the step (1), the mass ratio of the material balls is 1: 5-8, adding steel balls with the diameter of 4.0-5.0 mm, and ball-milling for 5-10 min at 800-900 rpm.
Preferably, the mass ratio of the aluminum powder activating material to the n-hexanol in the step (2) is 1;
preferably, the mass ratio of the aluminum powder activating material to the aluminum trichloride in the step (2) is 1;
preferably, in the step (3), the feed-liquid ratio of the added water to the aluminum powder activating material is 1g: 5-6 ml;
preferably, in the step (4), the feed-liquid ratio of the added water to the aluminum powder activating material is 1g:20 to 30ml;
preferably, the n-hexanol is recovered and then continuously used as a raw material to react with an aluminum powder activating material, wherein the mass ratio of the aluminum powder activating material to the recovered n-hexanol is 1;
compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the aluminum powder is subjected to ball milling by using the aluminate coupling agent, so that the specific surface area of the aluminum powder is increased, the reaction activity of the aluminum powder in the reaction with n-hexanol is increased, the yield of the prepared target product is higher than that of the prior art, and the requirement of actual production is met.
2. The n-hexanol prepared by the method has high purity, can be continuously recycled, and improves the utilization rate of raw materials.
3. The raw materials of the invention are sufficient in China and proper in price, so that the large-scale production of the invention is not limited by too high cost; meanwhile, the preparation method is simple, the total production cost is low, and the industrial large-scale production is facilitated.
Detailed Description
Example 1
The specific raw materials were weighed as in table 1, and the preparation steps were as follows:
(1) Putting aluminum powder into a ball mill, adding triacetylacetone aluminum, and uniformly mixing, wherein the mass ratio of the aluminum powder to the material balls is 1:5 adding a steel ball with the diameter of 4.0mm, and performing ball milling for 10min at the room temperature and at the speed of 800rpm in the nitrogen atmosphere to obtain an aluminum powder activating material;
(2) Putting an aluminum powder activating material, aluminum trichloride and n-hexyl alcohol into a reaction kettle, uniformly mixing, heating to 100 ℃, reacting for 40min, and filtering to obtain a mixed solution of tri-n-hexylalkoxy aluminum;
(3) Adding deionized water into a reaction kettle, heating to 70 ℃, adding 1/3 of mixed solution of tri-n-hexylalkoxy aluminum every 5min, continuously reacting for 30min after finishing dripping, standing for 20min, and filtering, wherein the liquid is n-hexanol, and the solid is hydroxy aluminum oxide;
(4) Adding deionized water into hydroxy alumina, heating to 90 ℃, aging for 12h, filtering, drying filter residue at 110 ℃, and crushing to obtain the pseudo-boehmite.
Example 2
The specific raw materials were weighed as in table 1, and the preparation steps were as follows:
(1) Putting aluminum powder into a ball mill, adding aluminum triacetylacetonate, and uniformly mixing, wherein the mass ratio of the material balls is 1:8, adding a steel ball with the diameter of 5.0mm, and ball-milling for 5min at room temperature and 900rpm in a nitrogen atmosphere to obtain an aluminum powder activating material;
(2) Putting an aluminum powder activating material, aluminum trichloride and n-hexyl alcohol into a reaction kettle, uniformly mixing, then heating to 110 ℃, reacting for 30min, and filtering to obtain a mixed solution of tri-n-hexylalkoxy aluminum;
(3) Adding deionized water into a reaction kettle, heating to 80 ℃, adding 1/4 of tri-n-hexylalkoxy aluminum mixed solution every 6min, continuously reacting for 20min after finishing dripping, standing for 15min, and filtering to obtain liquid n-hexyl alcohol and solid hydroxy aluminum oxide;
(4) Adding deionized water into hydroxy alumina, heating to 100 ℃, aging for 10h, filtering, drying filter residue at 120 ℃, and crushing to obtain the pseudo-boehmite.
Example 3
The specific raw materials were weighed as in table 1, and the preparation steps were as follows:
(1) Putting aluminum powder into a ball mill, adding aluminum triacetylacetonate, and uniformly mixing, wherein the mass ratio of the material balls is 1:8, adding a steel ball with the diameter of 5.0mm, and performing ball milling for 10min at the room temperature and 900rpm in the nitrogen atmosphere to obtain an aluminum powder activating material;
(2) Putting an aluminum powder activating material, aluminum trichloride and n-hexyl alcohol into a reaction kettle, uniformly mixing, heating to 110 ℃, reacting for 40min, and filtering to obtain a mixed solution of tri-n-hexylalkoxy aluminum;
(3) Adding deionized water into a reaction kettle, heating to 80 ℃, adding 1/4 of tri-n-hexylalkoxy aluminum mixed solution every 6min, continuously reacting for 30min after finishing dripping, standing for 20min, and filtering to obtain liquid n-hexyl alcohol and solid hydroxy aluminum oxide;
(4) Adding deionized water into hydroxy alumina, heating to 100 ℃, aging for 12h, filtering, drying filter residue at 120 ℃, and crushing to obtain the pseudo-boehmite.
Comparative example 1
The specific raw materials were weighed in Table 1, and the procedure was the same as in example 3 except that no silane coupling agent was used.
The specific raw materials were weighed as in table 1, and the preparation steps were as follows:
(1) Taking aluminum powder, putting the aluminum powder into a ball mill, and mixing the aluminum powder and the ball mill according to a ball mass ratio of 1:8, adding a steel ball with the diameter of 5.0mm, and ball-milling for 10min at room temperature and 900rpm in a nitrogen atmosphere to obtain an aluminum powder activating material;
(2) Putting an aluminum powder activating material, aluminum trichloride and n-hexyl alcohol into a reaction kettle, uniformly mixing, heating to 110 ℃, reacting for 40min, and filtering to obtain a mixed solution of tri-n-hexylalkoxy aluminum;
(3) Adding deionized water into a reaction kettle, heating to 80 ℃, adding 1/4 of tri-n-hexylalkoxy aluminum mixed solution every 6min, continuously reacting for 30min after finishing dripping, standing for 20min, and filtering to obtain liquid n-hexyl alcohol and solid hydroxy aluminum oxide;
(4) Adding deionized water into hydroxy aluminum oxide, heating to 100 ℃, aging for 12h, filtering, drying the filter residue at 120 ℃, and crushing to obtain the pseudo-boehmite.
TABLE 1
Determination of pseudoboehmite yield and purity
The pseudo-boehmite prepared in examples 1 to 3 and comparative example 1 was taken, and the yield and purity were calculated based on the mass of the aluminum powder charged. The results are shown in Table 4.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A method for co-producing hexanol and pseudoboehmite, characterized in that the method comprises the following steps:
(1) Putting aluminum powder into a ball mill, adding an aluminate coupling agent, mixing uniformly, adding steel balls, and performing ball milling at room temperature in a nitrogen atmosphere to obtain an aluminum powder activating material;
(2) Putting an aluminum powder activating material, aluminum trichloride and n-hexyl alcohol into a reaction kettle, uniformly mixing, heating to 100-110 ℃, reacting for 30-40 min, and filtering to obtain a mixed solution of tri-n-hexylalkoxy aluminum;
(3) Adding deionized water into a reaction kettle, heating to 70-80 ℃, adding 1/3-1/4 of mixed solution of tri-n-hexylalkoxy aluminum every 5-6 min, continuously reacting for 20-30 min after finishing dripping, standing for 15-20 min, and filtering to obtain liquid of n-hexanol and solid of hydroxy aluminum oxide;
(4) Taking hydroxyl alumina, adding deionized water, heating to 90-100 ℃, aging for 10-12 h, filtering, drying filter residue at 110-120 ℃, and crushing to obtain the pseudo-boehmite.
2. The method according to claim 1, wherein the ratio of the aluminum powder to the aluminum powder in the step (1) is 1: 0.02-0.03 adding aluminate coupling agent and mixing evenly.
3. The method according to claim 2, wherein the aluminate coupling agent is an aluminate coupling agent with an acetyl group.
4. The method according to claim 3, wherein the aluminate coupling agent with acetyl groups is aluminum triacetylacetone.
5. The method according to claim 1, wherein in the step (1), the ratio of the mass of the pellets is 1:5 to 8, adding steel balls with the diameter of 4.0 to 5.0mm, and ball-milling for 5 to 10min at the rpm of 800 to 900.
6. The method according to claim 1, wherein the mass ratio of the aluminum powder activating material to the n-hexanol in the step (2) is 1.
7. The method according to claim 1, wherein the mass ratio of the aluminum powder activating material to the aluminum trichloride in the step (2) is 1.
8. The method according to claim 1, wherein in the step (3), the feed-to-liquid ratio of the added water to the aluminum powder activating material is 1g:5 to 6ml.
9. The method according to claim 1, wherein in the step (4), the feed-to-liquid ratio of the added water to the aluminum powder activating material is 1g:20 to 30ml.
10. The method as claimed in claim 1, wherein the n-hexanol in the step (3) is recovered and then continuously used as a raw material to react with the aluminum powder activating material, and the mass ratio of the aluminum powder activating material to the recovered n-hexanol is 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211295796.9A CN115771909B (en) | 2022-10-21 | 2022-10-21 | Method for co-production of n-hexanol and pseudo-boehmite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211295796.9A CN115771909B (en) | 2022-10-21 | 2022-10-21 | Method for co-production of n-hexanol and pseudo-boehmite |
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| CN115771909A true CN115771909A (en) | 2023-03-10 |
| CN115771909B CN115771909B (en) | 2024-03-29 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3769234A (en) * | 1970-02-09 | 1973-10-30 | Dart Ind Inc | Process for producing activated titanium trichloride-aluminum trichloride |
| JPH10287418A (en) * | 1997-04-15 | 1998-10-27 | Mitsubishi Chem Corp | Production of synthetic quartz powder containing aluminum |
| CN106938851A (en) * | 2016-10-13 | 2017-07-11 | 北京工商大学 | A kind of preparation method of high-purity boehmite |
| CN113800543A (en) * | 2021-09-23 | 2021-12-17 | 大连理工大学 | Method for accelerating hydrothermal conversion rate of aluminum hydroxide into boehmite |
| EP4049972A1 (en) * | 2021-02-26 | 2022-08-31 | Nabaltec AG | Method for the preparation of pseudoboehmite |
-
2022
- 2022-10-21 CN CN202211295796.9A patent/CN115771909B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3769234A (en) * | 1970-02-09 | 1973-10-30 | Dart Ind Inc | Process for producing activated titanium trichloride-aluminum trichloride |
| JPH10287418A (en) * | 1997-04-15 | 1998-10-27 | Mitsubishi Chem Corp | Production of synthetic quartz powder containing aluminum |
| CN106938851A (en) * | 2016-10-13 | 2017-07-11 | 北京工商大学 | A kind of preparation method of high-purity boehmite |
| EP4049972A1 (en) * | 2021-02-26 | 2022-08-31 | Nabaltec AG | Method for the preparation of pseudoboehmite |
| CN113800543A (en) * | 2021-09-23 | 2021-12-17 | 大连理工大学 | Method for accelerating hydrothermal conversion rate of aluminum hydroxide into boehmite |
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| CN115771909B (en) | 2024-03-29 |
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