CN103769230B - A kind of preparation method of silicon-containing alumina dry glue - Google Patents
A kind of preparation method of silicon-containing alumina dry glue Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of silicon-containing alumina dry glue.The method includes: flyash is joined strong alkali solution and processes, it is filtrated to get siliceous and aluminum alkaline solution, then carry out and flow plastic reacting with acid aluminium salt solution by siliceous and aluminum alkaline solution, it is then passed through filter, washing, obtain silicon-containing alumina dry glue the most after drying, fired after obtain silicon-containing alumina.The method makes full use of flyash, the most cheap, and improves the added value of flyash, and the silicon-containing alumina pore volume of gained is big, and aperture is big, is particularly suited for use as weight, the carrier component of slag hydrotreating catalyst.
Description
Technical field
The present invention relates to the preparation method of a kind of silicon-containing alumina dry glue, the preparation method of a kind of silicon-containing alumina dry glue being applicable to heavy oil or catalyst for hydrotreatment of residual oil carrier material.
Background technology
Common heavy oil, the carrier matrix of residual oil hydrocatalyst are aluminium oxide.Due to heavy oil, residual oil character is severe, so heavy oil, the kind of residual oil hydrocatalyst is many, consumption is big and catalyst uses the cycle short, therefore, heavy oil is prepared in requirement, the raw alumina of residual oil hydrocatalyst carrier must be cheap, simultaneously, owing to the relative molecular weight of petroleum is increasing, in order to reduce the diffusional resistance that macromolecular reaction runs into, to accommodate more carbon deposit and metal deposit etc., also require that heavy oil, residual oil hydrocatalyst carrier has bigger aperture and pore volume and suitable acidity, duct, large aperture can be played passage and accommodate the effect of metal deposit, make the more efficiently utilization of catalyst inner surface；Bigger pore volume can accommodate more impurity, to guarantee catalyst service life；Suitable acidity can ensure that catalyst has certain hydrogenation activity, and the activity of such catalyst and stability just can be improved.
First, cheap aluminium oxide to be prepared, it is necessary to assure the low in raw material price of Borolon.At present, aluminium oxide the most typically has three kinds of preparation methoies:
(1) the neutralization reaction of aluminium salt and alkali, such as Alchlor process:
AlCl3+3NH4OH → Al(OH)3+3NH4Cl
(2) aluminium salt and the metathesis reaction of aluminate, such as aluminum sulfate method:
Al2(SO4)3+6NaAlO2+12H2O → 8Al(OH)3+3Na2SO4
(3) the neutralization reaction of aluminate and acid, such as carbonizatin method:
2NaAlO2+CO2+3H2O → 2Al(OH)3+Na2CO3
The raw material generally preparing aluminium oxide all must assure that without any impurity, and therefore, the price of the raw material of Borolon is higher than the like product that grade is low, so the price of aluminium oxide of synthesis is also relatively expensive.
Secondly, the support acidity prepared with aluminium oxide merely is weak, and mainly L acid, and B-acid is the most weak or without B-acid, easily and active metal component generation strong interaction and form inactive species, thus affect the performance of catalyst.Therefore, for regulating the acidity of catalyst carrier, appropriate auxiliary agent can be added according to different requirements, such as Si, Ti and P etc. in aluminium oxide building-up process.The acidity to improve carrier such as typical Si source many employings waterglass, Ludox and molecular sieve.
USP4721696 describes the preparation method of a kind of silicon-containing alumina, with aluminum nitrate and sodium aluminate as raw material, uses pH in 2 ~ 10 swing methods, adds sodium silicate in the aluminium hydroxide vacation colloidal sol obtained, and obtains silicon-containing alumina after scrubbed, dry, roasting.The method preparation process is the most complicated.
CN01118437.X describes the preparation method of a kind of cracking catalyst for petroleum hydrocarbon, and it is by after clay slurry acid treatment, adds boehmite, water glass solution, adds Alumina gel, add molecular sieve pulp, be spray-dried, wash.The method is applicable to the preparation of the molecular sieve catalyst of silicon-aluminum containing substrate.< the small-bore proportion of 5nm is relatively big, is not suitable for as heavy oil or residual oil hydrocatalyst material for the catalyst of preparation.
CN92112511.9 discloses a kind of heavy-oil hydrogenation denitrification catalyst, and the feature of this catalyst is to add low sodium Ludox during carrier extruded moulding to increase the pore volume of carrier, makes pore size distribution more concentrate simultaneously, and adds the acid amount of carrier.SiO on carrier2Content 14～19wt%, pore volume 0.55 ~ 0.65ml/g, average pore size is less.Although this patent adds low sodium Ludox, improve support acidity, but aperture is the least, be not suitable for heavy oil, residual oil compared with the hydrogenation process of macromolecular reaction thing.
CN02109422.5 discloses a kind of mink cell focus and hydrotransforming catalyst for residual oil and preparation method thereof, catalyst uses a kind of silicon-containing alumina to be support material, the preparation process of silicon-containing alumina uses and adds a small amount of silicon during plastic, adds the silicon of surplus after plastic or in ageing process.This catalyst pore-size distribution is concentrated mainly on 5-10nm.It is silicon source owing to selecting sodium silicate, it is ensured that having relatively low sodium content in product, washing process can produce substantial amounts of waste water, to environment.
Flyash is a kind of industrial residue that coal-fired boiler in thermal power plant is discharged, and is one of industrial solid castoff that at present discharge capacity is maximum the most in the world, and not only serious environment pollution endangers human health, but also takies a large amount of soil.The main component of flyash is aluminium oxide and silicon oxide.Flyash is mainly used in the aspects such as construction material, hydraulic engineering, road engineering, and added value is low.The utilization that becomes more meticulous flyash is concentrated mainly in silicon, the extraction of aluminum and application.Such as: CN200810115355.X discloses a kind of method preparing metallurgical-grade aluminum oxide.Entitled the research of pure zeolite molecular sieve " the flyash step-leached sial prepare " that " silicate circular " volume 26 the 1st phase (2007) delivers, is to utilize the sial in flyash for synthesizing X-type, A type, the pure zeolite product of p-type.
Summary of the invention
For the deficiencies in the prior art, the invention provides the preparation method of a kind of silicon-containing alumina dry glue.The method makes full use of flyash, the most cheap, and improves the added value of flyash, and the silicon-containing alumina pore volume of gained is big, and aperture is big, is particularly suited for use as weight, the carrier component of slag hydrotreating catalyst.
The preparation method of silicon-containing alumina dry glue of the present invention, including:
(1) flyash is joined strong alkali solution to process, be then filtered to remove residue, obtain siliceous and aluminum alkaline solution；
(2) the acid aluminum salt solution of preparation；
(3) use and flow plastic method, acid aluminium salt solution stream that the alkaline solution of siliceous and aluminum step (1) obtained and step (2) obtain carry out plastic reaction, control gelling temperature at least 50 DEG C, preferably 50 ~ 95 DEG C, more preferably 60 ~ 90 DEG C, controlling plastic pH value is 7.0 ~ 10.5, preferably 7.5 ~ 9.5；
(4) serosity of step (4) gained is filtered, washing, obtain silicon-containing alumina dry glue after drying.
The granularity of the flyash described in step (1) is preferably more than 200 mesh.Alumina content 15wt%～50wt% in described flyash, silica content 30wt%～60wt%.
Flyash is joined strong alkali solution and processes by step (1), and treatment temperature is at least 100 DEG C, preferably 100 ~ 180 DEG C, more preferably 120 ~ 150 DEG C, and the process time is 2 ~ 8 hours, preferably 4 ~ 6 hours.
Strong alkali solution described in step (1) is one or both mixed solutions in sodium hydroxide, potassium hydroxide, preferably sodium hydroxide solution.Described flyash is 1 ~ 6mL/g, preferably 2 ~ 4mL/g with the liquid-solid ratio of strong alkali solution.The molal quantity adding highly basic in described strong alkali solution is 2.6 ~ 5.0 times of aluminum molal quantity in flyash, preferably 2.8 ~ 4.0, more preferably 3.0 ~ 3.4.
In the alkaline solution of the siliceous and aluminum described in step (1), the total concentration of silicon and aluminum is calculated as 120 ~ 220g/L with aluminium oxide and silicon oxide gross mass, preferably 160 ~ 200g/L.
One or more of step (2) described acid aluminium salt preferably sulfuric acid aluminum, aluminum nitrate, aluminum chloride etc., are more highly preferred to aluminum sulfate.The concentration of described acid aluminium salt solution is 40 ~ 100gAl2O3/ L, preferably 50 ~ 80gAl2O3/L。
It is 30 ~ 80 minutes that step (3) controls gelation time.
After the reaction of step (3) plastic terminates, it may be preferred to through overaging.Described aging condition is as follows: aging temperature at least 50 DEG C, preferably 50 ~ 95 DEG C, more preferably 65 ~ 90 DEG C, and ageing time is less than 90 minutes, preferably 10 ~ 90 minutes, is more highly preferred to 10 ~ 60 minutes.
Drying condition described in step (4): 100 ~ 150 DEG C are dried 2 ~ 6 hours, preferably 110 ~ 130 DEG C, are dried 4 ~ 6 hours.
The preparation method of silicon-containing alumina of the present invention, including: the silicon-containing alumina dry glue of step (4) gained, through roasting, obtains silicon-containing alumina, wherein roasting condition: 500 ~ 950 DEG C of roastings 2 ~ 6 hours, preferably 600 ~ 900 DEG C roastings 3 ~ 5 hours.
In the inventive method, basic aluminate can be added as required in the alkaline solution of the siliceous and aluminum of step (1).Described basic aluminate is one or more in sodium metaaluminate, potassium metaaluminate, preferably sodium metaaluminate.After adding basic aluminate, in the alkaline solution of the siliceous and aluminum of gained, the total concentration of silicon and aluminum is calculated as 120 ~ 220g/L with aluminium oxide and silicon oxide gross mass, preferably 160 ~ 200g/L.
In silicon-containing alumina of the present invention, the content of silicon dioxide is 1wt% ~ 50wt%, preferably 2wt% ~ 40wt%.Silicon-containing alumina character of the present invention is as follows: pore volume is 0.75-1.10mL/g, and specific surface area is 280-350m2/ g, pore size distribution is as follows: the pore volume in the hole of bore dia ＜ 6nm accounts for less than the 20% of total pore volume, and the pore volume in the hole of bore dia ＞ 15nm accounts for more than the 30% of total pore volume.
In the present invention, porous and specific surface area are to use low temperature liquid nitrogen absorption method analysis, and silica content is to use metric measurement.
The inventive method is with flyash for silicon source and part aluminum source, aluminum source and the silicon source of synthesis silicon-containing alumina are widened, the silicon-containing alumina price making synthesis is greatly lowered, and improves the added value of flyash, also solves the Heavy environmental pollution problem that flyash brings.
The main component of the flyash used by the inventive method is Al2O3And SiO2, wherein possibly together with Fe3+、Ca2+、Mg2+、Ti4+Deng material, flyash is first made to react with strong alkali solution, generation soluble aluminum hydrochlorate and silicate, and Fe3+、Ca2+、Mg2+、Ti4+Then generate precipitation with alkali reaction stay in residue Deng material, make siliceous and aluminum alkaline solution, then with acid aluminium salt solution flowing, prepare big pore volume, wide-aperture silicon-containing alumina.Pore structure and the surface acidity of this silicon-containing alumina are suitable, it is adaptable to as weight, the carrier component of catalyst for hydrotreatment of residual oil, especially hydrodesulfurization and the carrier component of de-carbon residue catalyst.
It is an advantage of the current invention that, in prepared silicon-containing alumina dry glue, the content regulation of silicon oxide is simple, prepare the silicon-containing alumina that silicone content is higher, also a large amount of waste water will not be produced, owing to aluminum source and the silicon source of alkalescence exist in the form of an ion, precipitate under acid solution effect simultaneously, allow silicon to be better dispersed in aluminium oxide, and combine with the alumina backbone generated, so, the silicon oxide that siliceous aluminium hydroxide prepared by the present invention adds can function well as the purpose of modification, modified aluminas, increases the acidity of catalyst.
Detailed description of the invention
It is addressed further under the technical characteristic of the present invention below by embodiment, but is not limited to embodiment.Wt% is mass fraction.
Embodiment 1
Weigh and consist of SiO244.28wt%、Al2O348.80wt%、Fe2O33.29wt%, CaO2.56wt% and granularity 200 mesh full by flyash 500g, join in the 2500mL solution containing sodium hydroxide 287g, stirring, process 4 hours under the conditions of 130 DEG C, reaction filters residue after terminating, and obtains siliceous and aluminum alkaline solution.Above-mentioned mixed solution is adjusted so that Al in solution with sodium aluminate solution2O3、SiO2Concentration summation is 160g/L, stand-by.
Preparation is containing Al2O3For the aluminum sulfate solution 5000mL of 50g/L, stand-by.
In plastic retort, add 1.0L deionized water, be heated with stirring to 70 DEG C.Measuring above-mentioned alkaline solution 1250mL and acid solution 2500mL respectively, and flow to add in retort above two solution, keeping retort pH value is 7.5, keeps retort temperature at 70 DEG C in course of reaction, and gelation time is 50 minutes.Then carry out aging, aging temperature 70 DEG C, ageing time 30min.Serosity after aging is washed till neutrality with the deionized water of 70 DEG C, and 120 DEG C are dried 3 hours, obtain silicon-containing alumina dry glue, through 600 DEG C of roastings 3 hours, obtain silicon-containing alumina A.
Embodiment 2
Other condition, with embodiment 1, simply makes Al in solution2O3、SiO2Concentration summation is 130g/L, prepares silicon-containing alumina B.
Embodiment 3
Weigh and consist of SiO244.28wt%、Al2O348.80wt%、Fe2O33.29wt%, CaO2.56wt% and granularity 200 mesh full by flyash 500g, join in the 2000mL solution containing sodium hydroxide 500g, stirring, process 3 hours under the conditions of 150 DEG C, reaction filters residue after terminating, and obtains siliceous and aluminum alkaline solution.Above-mentioned mixed solution is adjusted so that Al in solution with sodium aluminate solution2O3、SiO2Concentration summation is 160g/L, stand-by.
Preparation is containing Al2O3For the aluminum sulfate solution 5000mL of 60g/L, stand-by.
In plastic retort, add 1.0L deionized water, be heated with stirring to 80 DEG C.Measuring above-mentioned alkaline solution 1250mL and acid solution 2500mL respectively, and flow to add in retort above two solution, keeping retort pH value is 8.5, keeps retort temperature at 80 DEG C in course of reaction, and gelation time is 60 minutes.Then through aging, 80 DEG C of ageing times 40min of aging temperature.Serosity after aging is washed till neutrality with the deionized water of 70 DEG C, and 110 DEG C are dried 5 hours, obtain silicon-containing alumina dry glue, through 700 DEG C of roastings 4 hours, obtain silicon-containing alumina C.
Embodiment 4
Weigh and consist of SiO248.0wt%、Al2O338.0wt%、Fe2O35.0wt%, CaO3.5wt% and granularity 200 mesh full by flyash 500g, join in the 2500mL solution containing sodium hydroxide 287g, stirring, process 4 hours under the conditions of 130 DEG C, reaction filters residue after terminating, and obtains siliceous and aluminum alkaline solution.Above-mentioned mixed solution is adjusted so that Al in solution with sodium aluminate solution2O3、SiO2Concentration summation is 200g/L, stand-by.
Preparation is containing Al2O3For the aluminum sulfate solution 5000mL of 50g/L, stand-by.
In plastic retort, add 1.2L deionized water, be heated with stirring to 85 DEG C.Measuring above-mentioned alkaline solution 1250mL and acid solution 2500mL respectively, and flow to add in retort above two solution, keeping retort pH value is 9.5, keeps retort temperature at 85 DEG C in course of reaction, and gelation time is 35 minutes.Then through aging, aging temperature 85 DEG C, ageing time 20min.Serosity after aging is washed till neutrality with the deionized water of 70 DEG C, and 120 DEG C are dried 4 hours, obtain silicon-containing alumina dry glue, through 750 DEG C of roastings 3 hours, obtain silicon-containing alumina D.
Embodiment 5
Weigh and consist of SiO248.0wt%、Al2O338.0wt%、Fe2O35.0wt%, CaO3.5wt% and granularity 200 mesh full by flyash 500g, join in the 2500mL solution containing sodium hydroxide 500g, stirring, process 6 hours under the conditions of 150 DEG C, reaction filters residue after terminating, and obtains siliceous and aluminum alkaline solution, Al in solution2O3、SiO2Concentration summation is 130g/L, stand-by.
Preparation is containing Al2O3For the aluminum sulfate solution 5000mL of 50g/L, stand-by.
In plastic retort, add 1.2L deionized water, be heated with stirring to 85 DEG C.Measuring above-mentioned alkaline solution 1250mL and acid solution 2500mL respectively, and flow to add in retort above two solution, keeping retort pH value is 9.5, keeps retort temperature at 85 DEG C in course of reaction, and gelation time is 70 minutes.Then through aging, aging temperature 85 DEG C, ageing time 20min.Serosity after aging is washed till neutrality with the deionized water of 70 DEG C, and 120 DEG C are dried 4 hours, obtain silicon-containing alumina dry glue, through 600 DEG C of roastings 3 hours, obtain silicon-containing alumina E.
Comparative example 1
Preparation is containing Al2O3For the aluminum sulfate solution 5000mL of 50g/L, preparation is containing Al2O3For the sodium aluminate solution 3000mL of 160g/L, stand-by.
In plastic retort, add 1.0L deionized water, be heated with stirring to 70 DEG C.Measuring above-mentioned alkaline solution 1250mL and acid solution 2500mL respectively, and flow to add in retort above two solution, keeping retort pH value is 7.5, keeps retort temperature at 70 DEG C in course of reaction, and gelation time is 50 minutes.Acid-base solution reacts after all adding and terminates, and adds waterglass 31.25g(containing SiO226wt%) enter ageing step, aging temperature 70 DEG C, ageing time 30min.Serosity after aging is washed till neutrality with the deionized water of 70 DEG C, and 120 DEG C are dried 3 hours, obtain silicon-containing alumina dry glue, through 600 DEG C of roastings 3 hours, obtain silicon-containing alumina F.
Comparative example 2
Preparation is containing Al2O3For the aluminum sulfate solution 5000mL of 50g/L, preparation 3000mL sodium metaaluminate and waterglass mixed solution so that Al in mixed solution2O3、SiO2Concentration summation is 160g/L, stand-by.
In plastic retort, add 1.0L deionized water, be heated with stirring to 70 DEG C.Measuring above-mentioned alkaline solution 1250mL and acid solution 2500mL respectively, and flow to add in retort above two solution, keeping retort pH value is 7.5, keeps retort temperature at 70 DEG C in course of reaction, and gelation time is 50 minutes.Acid-base solution reacts after all adding and terminates, and enters ageing step, aging temperature 70 DEG C, ageing time 30min.Serosity after aging is washed till neutrality with the deionized water of 70 DEG C, and 120 DEG C are dried 3 hours, obtain silicon-containing alumina dry glue, through 600 DEG C of roastings 3 hours, obtain silicon-containing alumina G.
The physicochemical property of silicon-containing alumina obtained above is listed in table 1.
Table 1 silicon-containing alumina physicochemical property
| Compile Number | A | B | C | D | E | Comparative Example F | Comparative example G |
| Pore volume, mL/g | 0.981 | 1.06 | 0.923 | 0.836 | 0.802 | 0.825 | 0.971 |
| Specific surface area, m2/g | 317 | 344 | 294 | 288 | 286 | 282 | 336 |
| Pore-size distribution, % | |||||||
| <6nm | 7.5 | 9.3 | 12.4 | 16.7 | 19.1 | 25.3 | 29.6 |
| 6~15nm | 47.3 | 50.9 | 50.5 | 46.8 | 49.7 | 43.0 | 32.6 |
| >15nm | 45.2 | 39.8 | 37.1 | 36.5 | 31.2 | 31.7 | 37.8 |
| SiO2, wt% | 2.5 | 6.1 | 21.8 | 35.2 | 40.7 | 2.41 | 2.43 |
| Total acid, mmol/g | 0.482 | 0.473 | 0.453 | 0.436 | 0.428 | 0.397 | 0.402 |
From table 1 it follows that when containing close silicon dioxide in aluminium oxide, use the silicon source that flyash prepares compared with adding sodium silicate, pore size distribution is more concentrated, and too increases the acidity of silicon-containing alumina simultaneously.Therefore it is suitable for being used as the carrier component of the catalyst such as residuum hydrogenating and metal-eliminating, hydrodesulfurization and hydro-conversion.
Claims (19)
1. a preparation method for silicon-containing alumina dry glue, including:
(1) flyash is joined strong alkali solution to process, be then filtered to remove residue, obtain siliceous and aluminum alkaline solution；
(2) the acid aluminum salt solution of preparation；
(3) using and flow plastic method, the acid aluminium salt solution that the alkaline solution of siliceous and aluminum step (1) obtained and step (2) obtain carries out and flows plastic reaction, and controlling gelling temperature is 50 DEG C ~ 95 DEG C, and plastic pH value is 7.0 ~ 10.5；
(4) serosity of step (3) gained is filtered, washing, obtain silicon-containing alumina dry glue after drying.
The most in accordance with the method for claim 1, it is characterised in that the granularity of the flyash described in step (1) is more than 200 mesh.
The most in accordance with the method for claim 1, it is characterised in that in the flyash described in step (1), alumina content 15wt%～50wt%, silica content 30wt%～60wt%.
The most in accordance with the method for claim 1, it is characterised in that flyash is joined strong alkali solution and processes by step (1), treatment temperature is 100 ~ 180 DEG C, and the process time is 2 ~ 8 hours.
The most in accordance with the method for claim 1, it is characterised in that flyash is joined strong alkali solution and processes by step (1), treatment temperature is 120 ~ 150 DEG C, and the process time is 4 ~ 6 hours.
The most in accordance with the method for claim 1, it is characterised in that the strong alkali solution described in step (1) is one or both mixed solutions in sodium hydroxide, potassium hydroxide.
The most in accordance with the method for claim 1, it is characterised in that described flyash is 1 ~ 6mL/g with the liquid-solid ratio of strong alkali solution, and the molal quantity adding highly basic in described strong alkali solution is 2.6 ~ 5.0 times of aluminum molal quantity in flyash.
The most in accordance with the method for claim 1, it is characterised in that the molal quantity adding highly basic in described strong alkali solution is 2.8 ~ 4.0 times of aluminum molal quantity in flyash.
The most in accordance with the method for claim 1, it is characterised in that in the alkaline solution of the siliceous and aluminum described in step (1), the total concentration of silicon and aluminum is calculated as 120 ~ 220g/L with aluminium oxide and silicon oxide gross mass.
The most in accordance with the method for claim 1, it is characterised in that step (2) described acid aluminium salt is one or more in aluminum sulfate, aluminum nitrate, aluminum chloride, the concentration of described acid aluminium salt solution is 40 ~ 100gAl2O3/L。
11. in accordance with the method for claim 1, it is characterised in that step (2) described acid aluminium salt is aluminum sulfate, and the concentration of described acid aluminium salt solution is 50 ~ 80gAl2O3/L。
12. in accordance with the method for claim 1, it is characterised in that step (3) controls gelling temperature 60 ~ 90 DEG C, and plastic pH value is 7.5 ~ 9.5.
13. in accordance with the method for claim 1, it is characterised in that it is 30 ~ 80 minutes that step (3) controls gelation time.
14. in accordance with the method for claim 1, it is characterised in that after the reaction of step (3) plastic terminates, through overaging, described aging condition is as follows: aging temperature is 50 DEG C ~ 95 DEG C, and ageing time is 10 ~ 90 minutes.
15. in accordance with the method for claim 1, it is characterised in that the drying condition described in step (4): 100 ~ 150 DEG C are dried 2 ~ 6 hours.
16. in accordance with the method for claim 1, it is characterised in that: in the alkaline solution of the siliceous and aluminum of step (1), add basic aluminate；Described basic aluminate is one or more in sodium metaaluminate, potassium metaaluminate, and after adding basic aluminate, in the alkaline solution of the siliceous and aluminum of gained, the total concentration of silicon and aluminum is calculated as 120 ~ 220g/L with aluminium oxide and silicon oxide gross mass.
The preparation method of 17. 1 kinds of silicon-containing aluminas, including: silicon-containing alumina dry glue prepared by claim 1 ~ 16 either method, through roasting, obtains silicon-containing alumina.
18. in accordance with the method for claim 17, it is characterised in that described roasting condition: 500 ~ 950 DEG C of roastings 2 ~ 6 hours.
19. in accordance with the method for claim 17, it is characterised in that in gained silicon-containing alumina, the content of silicon dioxide is 1wt% ~ 50wt%.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0283815A1 (en) * | 1987-03-11 | 1988-09-28 | Phillips Petroleum Company | Silica-modified alumina |
| CN102029192A (en) * | 2009-09-28 | 2011-04-27 | 中国石油化工股份有限公司 | Silicon-containing alumina and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0283815A1 (en) * | 1987-03-11 | 1988-09-28 | Phillips Petroleum Company | Silica-modified alumina |
| CN102029192A (en) * | 2009-09-28 | 2011-04-27 | 中国石油化工股份有限公司 | Silicon-containing alumina and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| "低温碱溶粉煤灰中硅和铝的溶出规律研究";邬国栋等;《环境科学研究》;20061231;第19卷(第1期);第53页正文第2段、第54页第1.2.2节、第56页第3节第1段 * |
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