CN102580785B - Hydrated alumina forming matter and preparation method thereof - Google Patents
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Abstract
Provided are hydrated alumina forming matter and a preparation method thereof. The hydrated alumina forming matter comprises hydrated alumina and cellulose ether. The radial crushing strength of the forming matter is larger than or equal to 12N/mm, the water absorption rate is 0.4 to 1.5, and a delta value is smaller than or equal to 10%. Delta = ((Q1-12)/Q1)*100%, wherein the Q1 is the radial crushing strength of the hydrated alumina forming matter, and the Q2 is the radial crushing strength of the hydrated alumina forming matter soaked for 30 minutes in water and dried. The hydrated alumina forming matter is high in radial crushing strength and water absorption rate and low in strength loss rate, and can be directly used as an adsorbent or a carrier without being roasted.
Description
Technical field
The present invention relates to a kind of hydrated alumina forming matter and preparation method thereof.
Background technology
In conventional method, aluminium oxide, particularly gama-alumina, because it has better pore structure, specific surface and heat-resistant stability, the carrier of Chang Zuowei adsorbent or loaded catalyst uses.This aluminium oxide is conventionally by hydrated alumina, as boehmite etc. through moulding, dry after, high-temperature roasting obtains again.
Based on above-mentioned cognition, and the hydrated alumina forming matter of preparing according to conventional method meets water or aqueous solution and is easy to the feature of efflorescence, it is generally acknowledged and hydrated alumina forming matter directly can not be used as adsorbent or carrier.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of hydrated alumina forming matter newly, that can directly be used as adsorbent or carrier use and preparation method thereof.
The present invention relates to following invention:
1, a hydrated alumina forming matter, contains hydrated alumina and cellulose ether, and the radially crushing strength of described article shaped is more than or equal to 12N/mm, and water absorption rate is 0.4-1.5, and δ value is for being less than or equal to 10%; Wherein, δ=((Q1-Q2)/Q1) × 100%, Q1 is radially crushing strength of hydrated alumina forming matter, Q2 is hydrated alumina forming matter through water soaking 30 minutes, radially crushing strength after drying.
2, according to the article shaped described in 1, it is characterized in that, the radially crushing strength of described article shaped is 15-30N/mm, and water absorption rate is 0.6-1, and δ is less than or equal to 5%.
3, according to the article shaped described in 1 or 2, it is characterized in that, taking described article shaped as benchmark, the content of described cellulose ether is 0.5-8 % by weight.
4, according to the article shaped described in 3, it is characterized in that, taking described article shaped as benchmark, the content of described cellulose ether is 1-6 % by weight.
5, according to the article shaped described in 4, it is characterized in that, taking described article shaped as benchmark, the content of described cellulose ether is 2-5 % by weight.
6, according to the article shaped described in 1, it is characterized in that, described cellulose ether is selected from one or more in methylcellulose, HEMC, hydroxypropyl methylcellulose.
7, according to the article shaped described in 6, it is characterized in that, described cellulose ether is methylcellulose, HEMC and their mixture.
8, according to the article shaped described in 1, it is characterized in that, described hydrated alumina is selected from one or more in boehmite, boehmite, aluminium hydroxide, three water-aluminum hydroxides.
9, according to the article shaped described in 8, it is characterized in that, described hydrated alumina is boehmite.
10, according to the article shaped described in 1, it is characterized in that, contain starch, taking described article shaped as benchmark, the content of described starch is no more than 8 % by weight.
11, according to the article shaped described in 1, it is characterized in that, described starch is sesbania powder, and taking described article shaped as benchmark, the content of described starch is no more than 5 % by weight.
12, a kind of preparation method of hydrated alumina forming matter, comprise hydrated alumina, cellulose ether and water mixing, moulding dry, the consumption of described each component and moulding and dry condition make the radially crushing strength of final molding thing be more than or equal to 12N/mm, water absorption rate is 0.4-1.5, and δ value is for being less than or equal to 10%; Wherein, δ=((Q1-Q2)/Q1) × 100%, Q1 is radially crushing strength of hydrated alumina forming matter, Q2 is hydrated alumina forming matter through water soaking 30 minutes, radially crushing strength after drying.
13, according to the method described in 12, it is characterized in that, it is 15-30N/mm that the consumption of described each component and moulding and dry condition make the radially crushing strength of final described article shaped, and water absorption rate is 0.6-1, and δ is less than or equal to 5%.
14, according to the method described in 12 or 13, it is characterized in that, taking described article shaped as benchmark, it is 0.5-8 % by weight that the consumption of each component makes the content of the described cellulose ether in final molding thing, described drying condition comprises: temperature 60 C is to being less than 350 DEG C, drying time 1-48 hour.
15, according to the method described in 14, it is characterized in that, taking described article shaped as benchmark, it is 1-6 % by weight that the consumption of each component makes the content of the described cellulose ether in final molding thing, and described drying condition comprises: temperature 80-300 DEG C, drying time 2-24 hour.
16, according to the method described in 15, it is characterized in that, taking described article shaped as benchmark, it is 2-5 % by weight that the consumption of each component makes the content of the described cellulose ether in final molding thing, and described drying condition comprises: temperature 120-250 DEG C, drying time 2-12 hour.
17, according to the method described in 12, it is characterized in that, described cellulose ether is selected from one or more in methylcellulose, HEMC, hydroxypropyl methylcellulose.
18, according to the method described in 17, it is characterized in that, described cellulose ether is methylcellulose, HEMC and their mixture.
19, according to the method described in 12, it is characterized in that, described hydrated alumina is selected from one or more in boehmite, boehmite, aluminium hydroxide, three water-aluminum hydroxides.
20, according to the method described in 19, it is characterized in that, described hydrated alumina is boehmite.
21, according to the method described in 12, it is characterized in that, comprise a step of introducing starch in forming process, taking described article shaped as benchmark, the introduction volume of described starch is no more than 8 % by weight.
22, according to the article shaped described in 21, it is characterized in that, described starch is sesbania powder, and taking described article shaped as benchmark, the introduction volume of described starch is no more than 5 % by weight.
According to hydrated alumina forming matter provided by the invention, the radially crushing strength of preferred described article shaped is 15-30N/mm, and water absorption rate is 0.6-1, and δ is less than or equal to 5%.Wherein, δ=((Q1-Q2)/Q1) × 100%, Q1 is radially crushing strength of hydrated alumina forming matter, Q2 is hydrated alumina forming matter through water soaking 30 minutes, the radially crushing strength through 120 DEG C of heating, dryings after 4 hours.The size of δ value is representing hydrated alumina forming matter variation (or being called loss of strength rate) to crushing strength through water soaking anteroposterior diameter.In the present invention, the described article shaped radially measuring method of crushing strength is carried out according to RIPP 25-90 catalyst compressive resistance determination method, has detailed introduction about the article shaped concrete steps that radially crushing strength is measured at RIPP25-90, does not repeat here.
Described water absorption rate refers to the weight value added after excessive deionized water immersion 30min for dry hydrated alumina forming matter.The present invention adopts following concrete grammar to measure: first 120 DEG C of testing samples are dried 4 hours.Take out sample, be positioned in desiccator and be cooled to room temperature, with 40 mesh standard sieve screenings, take oversize 20g (numbering: w1) testing sample, add 50g deionized water, soak 30min, filter, solid phase drains 5min, weigh solid phase weight (numbering: w2), solid phase is transferred in baking oven, and 120 DEG C of heating, dryings 4 hours, are positioned over and in desiccator, are cooled to room temperature.Water absorption rate=(w1-w2)/w1
Under the prerequisite that is enough to make radially crushing strength, water absorption rate and the loss of strength rate of article shaped to meet the demands, the present invention is not particularly limited the content of cellulose ether, in concrete embodiment, taking hydrated alumina forming matter total amount as benchmark, the content of cellulose ether is preferably 0.5-8 % by weight, more preferably 1-6 % by weight, is more preferably 2-5 % by weight.Described cellulose ether preferably in methylcellulose, HEMC, hydroxypropyl methylcellulose one or more, further preferably methylcellulose, HEMC and their mixture wherein.
According to hydrated alumina forming matter provided by the invention, wherein can contain the adjuvant component that does not affect or be of value to radially crushing strength, water absorption rate and the δ value of improving described article shaped.For example, contain starch and add component, described starch can be the powder being obtained through pulverizing by vegetable seeds arbitrarily, as sesbania powder.
Described hydrated alumina is selected from any hydrated alumina that can be used as adsorbent and catalyst carrier precursor, for example, can be boehmite, boehmite, aluminium hydroxide, three water-aluminum hydroxides, preferably boehmite.
According to the preparation method of hydrated alumina forming matter provided by the invention, described forming method can be prior art arbitrarily, and to this, the present invention is not particularly limited.For example, described forming method can be the forming method of extrusion, spraying, round as a ball, compressing tablet and their combination.For ensureing carrying out smoothly of moulding, in the time of moulding, can in material (being the mixture of hydrated alumina and cellulose ether), introduce auxiliary agent and water etc. herein, for example, in the time adopting the moulding of extrusion method, comprise by described hydrated alumina and cellulose ether and water, containing or do not mix containing extrusion aid, then extrusion molding, obtain wet bar, then drying obtains article shaped of the present invention.Described auxiliary agent is selected from starch, and described starch can be the powder being obtained through pulverizing by vegetable seeds arbitrarily, as sesbania powder.The method that preferred forming method is extruded moulding.
Hydrated alumina forming matter provided by the invention has lower loss of strength rate after higher radially crushing strength, water absorption rate and water suction, can directly use as adsorbent or carrier without roasting.
Detailed description of the invention
To further illustrate the present invention by embodiment below.
Agents useful for same in example, except special instruction, is chemically pure reagent.
Embodiment 1
Get the boehmite powder 100g that catalyst Chang Ling branch company produces, add 4.0g methylcellulose, 3.0g sesbania powder and 95mL deionized water, be fully uniformly mixed, by banded extruder kneading evenly after, extruded moulding obtains the wet article shaped of aluminium hydroxide.By wet hydrogen aluminium oxide article shaped be positioned in baking oven 150 DEG C dry 12 hours.Radially crushing strength, water absorption rate and the δ value (loss of strength rate) of measuring dry aftershaping carrier, the results are shown in table 1.
Embodiment 2
Get the boehmite powder 50g that catalyst Chang Ling branch company produces, self-control unformed aluminium hydroxide powder 50g, add 2.0g methylcellulose, 3.0g HEMC and 95mL deionized water, fully be uniformly mixed, after even by banded extruder kneading, extruded moulding obtains the wet article shaped of aluminium hydroxide.By wet hydrogen aluminium oxide article shaped be positioned in baking oven 220 DEG C dry 6 hours.Radially crushing strength, water absorption rate and the δ value of measuring dry aftershaping carrier, the results are shown in table 1.
Embodiment 3
Get the boehmite powder 60g that catalyst Chang Ling branch company produces, three water-aluminum hydroxide 40g, add 1.0g methylcellulose, 2.0g hydroxypropyl methylcellulose, 3.0g sesbania powder and 95mL deionized water, fully be uniformly mixed, by banded extruder kneading evenly after, extruded moulding obtains the wet article shaped of aluminium hydroxide.By wet hydrogen aluminium oxide article shaped be positioned in baking oven 80 DEG C dry 12 hours.Radially crushing strength, water absorption rate and the δ value of measuring dry aftershaping carrier, the results are shown in table 1.
Embodiment 4
Get the boehmite SB powder 100g that Sasol company produces, add 3.0g HEMC and 90mL deionized water, be fully uniformly mixed, by banded extruder kneading evenly after, extruded moulding obtains moulding bar.Aluminium hydroxide moulding bar be positioned in baking oven 150 DEG C dry 12 hours.Radially crushing strength, water absorption rate and the δ value of measuring dry aftershaping carrier, the results are shown in table 1.
Embodiment 5
Get the boehmite SB powder 100g that Sasol company produces, add 3.0g HEMC, 2g hydroxypropyl methylcellulose, 3.0g sesbania powder and 90mL deionized water, fully be uniformly mixed, by banded extruder kneading evenly after, extruded moulding obtains moulding bar.Aluminium hydroxide moulding bar be positioned in baking oven 250 DEG C dry 4 hours.Radially crushing strength, water absorption rate and the δ value of measuring dry aftershaping carrier, the results are shown in table 1.
Embodiment 6
Get the boehmite powder 100g that Yantai, Shandong Heng Hui Chemical Co., Ltd. produces, add 5.0g hydroxypropyl methylcellulose, 3.0g sesbania powder and 90mL deionized water, be fully uniformly mixed, by banded extruder kneading evenly after, extruded moulding obtains moulding bar.Moulding bar be positioned in baking oven 120 DEG C dry 4 hours.Radially crushing strength, water absorption rate and the δ value of measuring dry aftershaping carrier, the results are shown in table 1.
Comparative example 1
Get the boehmite powder 100g that catalyst Chang Ling branch company produces, add red fuming nitric acid (RFNA) 2.5mL, 3.0g sesbania powder and 95mL deionized water, be fully uniformly mixed, by banded extruder kneading evenly after, extruded moulding obtains moulding bar.Moulding bar be positioned in baking oven 80 DEG C dry 4 hours.Measure the intensity of dried strip.Take 10g gained dried strip and add 50mL deionized water, be soaked in water 30 minutes, measure radially crushing strength, water absorption rate and the δ value of dry aftershaping carrier, the results are shown in table 1.
Comparative example 2
Get the boehmite SB powder 100g that Condea company produces, add 20ml aluminium colloidal sol, 3.0g sesbania powder and 90mL deionized water, be fully uniformly mixed, by banded extruder kneading evenly after, extruded moulding obtains moulding bar.Moulding bar be positioned in baking oven 150 DEG C dry 4 hours.Moulding bar be positioned in baking oven 150 DEG C dry 4 hours.Measure the intensity of dried strip.Take 10g gained dried strip and add 50mL deionized water, be soaked in water 30 minutes, measure radially crushing strength, water absorption rate and the δ value of dry aftershaping carrier, the results are shown in table 1.
Comparative example 3
Get the boehmite powder 100g that Yantai, Shandong Heng Hui Chemical Co., Ltd. produces, add 5.0mL acetic acid, 3.0g sesbania powder and 90mL deionized water, be fully uniformly mixed, by banded extruder kneading evenly after, extruded moulding obtains moulding bar.Moulding bar be positioned in baking oven 180 DEG C dry 4 hours.Measure the intensity of dried strip.Take 10g gained dried strip and add 50mL deionized water, be soaked in water 30 minutes, measure radially crushing strength, water absorption rate and the δ value of dry aftershaping carrier, the results are shown in table 1.
Comparative example 4
Get the boehmite powder 100g that catalyst Chang Ling branch company produces, add red fuming nitric acid (RFNA) 2.5mL, 3.0g sesbania powder and 95mL deionized water, be fully uniformly mixed, by banded extruder kneading evenly after, extruded moulding obtains moulding bar.Moulding bar be positioned in baking oven 80 DEG C dry 4 hours.600 DEG C of roastings of dried strip 4 hours.Radially crushing strength, water absorption rate and the δ value of measuring roasting aftershaping carrier, the results are shown in table 1.
Table 1
Soaking effect when this embodiment 7-12 and comparative example 5-10 are used for hydrated alumina forming matter provided by the invention is described as drier.
Embodiment 7
The boehmite article shaped dried strip of getting in embodiment 1 was put into 600 DEG C of roastings of Muffle furnace after 4 hours, and recording butt is 71.2%.
Measure hygroscopic capacity: the desiccator container of getting boehmite dried strip that N1 (g) embodiment 1 obtains and put into bottom and be equipped with deionized water, under room temperature, place 10 days, N2 (g) weighs, hygroscopic capacity=((N2-N1)/(butt × N1)) × 100% (lower same), the results are shown in table 2.
Comparative example 5
Get boehmite article shaped dried strip in embodiment 1 through 600 DEG C of roastings the article shaped after 4 hours, measure its hygroscopic capacity, the results are shown in table 2.
Embodiment 8
The boehmite article shaped dried strip of getting in embodiment 2 was put into 600 DEG C of roastings of Muffle furnace after 4 hours, and recording butt is 70.3%.
The hygroscopic capacity of the boehmite dried strip obtaining according to embodiment 7 same methods mensuration embodiment 2, the results are shown in table 2.
Comparative example 6
Get boehmite article shaped dried strip in embodiment 2 through 600 DEG C of roastings the article shaped after 4 hours.Measure its hygroscopic capacity, the results are shown in table 2.
Embodiment 9
The boehmite article shaped dried strip of getting in embodiment 3 was put into 600 DEG C of roastings of Muffle furnace after 4 hours, and recording butt is 68.9%.
The hygroscopic capacity of the boehmite dried strip obtaining according to embodiment 7 same methods mensuration embodiment 3, the results are shown in table 2.
Comparative example 7
Get boehmite article shaped dried strip in embodiment 3 through 600 DEG C of roastings the article shaped after 4 hours.Measure its hygroscopic capacity, the results are shown in table 2.
Embodiment 10
The boehmite article shaped dried strip of getting in embodiment 4 was put into 600 DEG C of roastings of Muffle furnace after 4 hours, and recording butt is 68.9%.
The hygroscopic capacity of the boehmite dried strip obtaining according to embodiment 7 same methods mensuration embodiment 4, the results are shown in table 2.
Comparative example 8
Get boehmite article shaped dried strip in embodiment 4 through 600 DEG C of roastings the article shaped after 4 hours.Measure its hygroscopic capacity, the results are shown in table 2.
Embodiment 11
The boehmite article shaped dried strip of getting in embodiment 5 was put into 600 DEG C of roastings of Muffle furnace after 4 hours, and recording butt is 68.9%.
The hygroscopic capacity of the boehmite dried strip obtaining according to embodiment 7 same methods mensuration embodiment 5, the results are shown in table 2.
Contrast 9
Get boehmite article shaped dried strip in embodiment 5 through 600 DEG C of roastings the article shaped after 4 hours.Measure its hygroscopic capacity, the results are shown in table 2.
Embodiment 12
The boehmite article shaped dried strip of getting in embodiment 6 was put into 600 DEG C of roastings of Muffle furnace after 4 hours, and recording butt is 68.9%.
The hygroscopic capacity of the boehmite dried strip obtaining according to embodiment 7 same methods mensuration embodiment 6, the results are shown in table 2.
Comparative example 10
Get boehmite article shaped dried strip in embodiment 6 through 600 DEG C of roastings the article shaped after 4 hours.Measure its hygroscopic capacity, the results are shown in table 2.
Table 2
| Embodiment | Weight | Butt, % | Hygroscopic capacity/% |
| 7 | 20.0 | 71.2 | 67.8 |
| Comparative example 5 | 20.0 | 100.0 | 63.8 |
| 8 | 20.0 | 70.3 | 56.8 |
| Comparative example 6 | 20.0 | 100.0 | 54.6 |
| 9 | 20.0 | 68.9 | 75.3 |
| Comparative example 7 | 20.0 | 100.0 | 73.1 |
| 10 | 20.0 | 67.8 | 55.9 |
| Comparative example 8 | 20.0 | 100.0 | 54.8 |
| 11 | 20.0 | 78.2 | 56.7 |
| Comparative example 9 | 20.0 | 100.0 | 54.7 |
| 12 | 20.0 | 71.3 | 65.9 |
| Comparative example 10 | 20.0 | 100.0 | 64.8 |
Claims (18)
1. a bar shaped hydrated alumina forming matter, formed by hydrated alumina, cellulose ether and starch, taking described article shaped as benchmark, the content of described cellulose ether is 0.5-8 % by weight, the content of described starch is 0-8 % by weight, the radially crushing strength of described article shaped is more than or equal to 12N/mm, and water absorption rate is 0.4-1.5, and δ value is for being less than or equal to 10%; Wherein, δ=((Q1-Q2)/Q1) × 100%, Q1 is radially crushing strength of hydrated alumina forming matter, Q2 is hydrated alumina forming matter through water soaking 30 minutes, radially crushing strength after drying.
2. article shaped according to claim 1, is characterized in that, the radially crushing strength of described article shaped is 15-30N/mm, and water absorption rate is 0.6-1, and δ is less than or equal to 5%.
3. article shaped according to claim 1, is characterized in that, taking described article shaped as benchmark, the content of described cellulose ether is 1-6 % by weight.
4. article shaped according to claim 3, is characterized in that, taking described article shaped as benchmark, the content of described cellulose ether is 2-5 % by weight.
5. article shaped according to claim 1, is characterized in that, described cellulose ether is selected from one or more in methylcellulose, HEMC, hydroxypropyl methylcellulose.
6. article shaped according to claim 5, is characterized in that, described cellulose ether is methylcellulose, HEMC and their mixture.
7. article shaped according to claim 1, is characterized in that, described hydrated alumina is selected from one or more in boehmite, boehmite, aluminium hydroxide, three water-aluminum hydroxides.
8. article shaped according to claim 7, is characterized in that, described hydrated alumina is boehmite.
9. article shaped according to claim 1, is characterized in that, described starch is sesbania powder, and taking described article shaped as benchmark, the content of described starch is no more than 5 % by weight.
10. the preparation method of bar shaped hydrated alumina forming matter according to claim 1, comprise hydrated alumina, cellulose ether, starch and water mixing, extruded moulding dry, taking described article shaped as benchmark, the content of described cellulose ether is 0.5-8 % by weight, the content of described starch is 0-8 % by weight, described drying condition comprises: temperature 60 C is to being less than 350 DEG C, drying time 1-48 hour
,the consumption of described each component and extruded moulding and dry condition make the radially crushing strength of final molding thing be more than or equal to 12N/mm, and water absorption rate is 0.4-1.5, and δ value is for being less than or equal to 10%; Wherein, δ=((Q1-Q2)/Q1) × 100%, Q1 is radially crushing strength of hydrated alumina forming matter, Q2 is hydrated alumina forming matter through water soaking 30 minutes, radially crushing strength after drying.
11. methods according to claim 10, is characterized in that, it is 15-30N/mm that the consumption of described each component and moulding and dry condition make the radially crushing strength of final described article shaped, and water absorption rate is 0.6-1, and δ is less than or equal to 5%.
12. methods according to claim 10, is characterized in that, taking described article shaped as benchmark, the content of described cellulose ether is 1-6 % by weight, and described drying condition comprises: temperature 80-300 DEG C, drying time 2-24 hour.
13. methods according to claim 12, it is characterized in that, taking described article shaped as benchmark, it is 2-5 % by weight that the consumption of each component makes the content of the described cellulose ether in final molding thing, described drying condition comprises: temperature 120-250 DEG C, drying time 2-12 hour.
14. methods according to claim 10, is characterized in that, described cellulose ether is selected from one or more in methylcellulose, HEMC, hydroxypropyl methylcellulose.
15. methods according to claim 14, is characterized in that, described cellulose ether is methylcellulose, HEMC and their mixture.
16. methods according to claim 10, is characterized in that, described hydrated alumina is selected from one or more in boehmite, boehmite, aluminium hydroxide, three water-aluminum hydroxides.
17. methods according to claim 16, is characterized in that, described hydrated alumina is boehmite.
18. methods according to claim 10, is characterized in that, described starch is sesbania powder, and taking described article shaped as benchmark, the introduction volume of described starch is no more than 5 % by weight.
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