CN107720791A - A kind of method for preparing high purity pseudoboehmite adhesive - Google Patents
A kind of method for preparing high purity pseudoboehmite adhesive Download PDFInfo
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- CN107720791A CN107720791A CN201710982824.7A CN201710982824A CN107720791A CN 107720791 A CN107720791 A CN 107720791A CN 201710982824 A CN201710982824 A CN 201710982824A CN 107720791 A CN107720791 A CN 107720791A
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- aluminium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
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- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a kind of method for preparing high purity pseudoboehmite adhesive, belong to inorganic functional material technical field.Product purity prepared by this method is high, and peptization index and thixotropy are easily controlled, and can meet both at home and abroad the fields such as catalyst are to adhesive boehmite the needs of.Whole preparation process belongs to Environmentally-sound technology without waste discharge；Preparation flow is simple simultaneously, and operating procedure is simple, cost is low.The present invention manufacturing cost and it is environment-friendly etc. all show significant competitive advantage and profit margin, it is particularly significant in terms of catalyst boehmite adhesive production domesticization is realized.In addition, the raw material that uses of the present invention is the aluminium-alcohol salt of low-carbon alcohols, and long-chain aluminium-alcohol salt technics comparing, have the advantages that toxicity is low, easy purification.
Description
Technical field
The invention belongs to inorganic functional material technical field, is related specifically to a kind of preparation side of boehmite adhesive
Method.
Background technology
Boehmite also known as monohydrate alumina, it is a kind of important activator raw material, in petrochemical field as being catalyzed
Cracking, hydrogenation, reformation etc. are widely used.Boehmite is in addition to itself being a kind of important catalyst carrier, also simultaneously
It is the main adhesive for making other a variety of acid catalysts, there is considerable effect.
Technical parameter index when boehmite is used as adhesive with it as catalyst carrier when index it is notable not
Together, as adhesive, purity, peptization index, gel thixotropy etc. are focused more on.Adhesive is with boehmite production method master
To include alkoxide hydrolysis and the inorganic aluminate precipitation method etc..Although inorganic aluminate precipitation method technique is simple, cost is relatively low, through into
Boehmite impurity content height (such as Na obtained after the process such as glue, aging, separation and washing and drying2O content is higher than
0.1%), slurry amount is big (often producing 1 ton of boehmite needs with more than 20 tons slurries), particularly as gluing
Peptization index is relatively low (typically not greater than 70%) during agent, and sol-gel process is slow, thixotropy will generally be up to 1 week very
Sol-gel transition can not be realized to some adhesives, it is difficult to obtain the product for meeting adhesive requirement.Foreign countries are with Germany
Sasol companies are used as adhesive by the high purity pseudoboehmite that the aluminium-alcohol salt Hydrolyze method of representative produces in catalyst field
Market is dominance, and peptization index is up to 99%, and sol-gel process is fast, thixotropy is good (typically smaller than 90 minutes).But
More than the C6 higher alcohols that the method uses have certain toxicity, and production cost is higher.Before this, the patent that we apply《It is prepared by one kind
The method of high purity pseudoboehmite》The boehmite of the preparation is also only capable of reaching 70% in terms of peptization index, and colloidal sol-
Gel thixotropy is more than 24 hours, still can not meet the requirement of adhesive products.
Under contrast, the present invention is on the aluminium-alcohol salt hydrolysis for producing high-purity boehmite basis with the lower alcohol containing below C4
On, a kind of preparation method of boehmite adhesive is proposed, its key technical indexes is：Product crystalline phase is AlOOHxH2O,
Al2O3Content is not less than 70%wt (weight/mass percentage composition, similarly hereinafter), Na2O content is not higher than 0.015%wt, specific surface area is more than
200m2/ g, bulk density are more than 750kg/m3, peptization index reach 99% and more than, sol-gel thixotropy be less than 90 minutes.
The content of the invention
The present invention proposes a kind of preparation method of boehmite adhesive, and its product purity is high, peptization index and thixotroping
Property is easily controlled, and operating procedure is simple, cost is low, without waste discharge, can meet both at home and abroad in fields such as catalyst to adhesive
With the demand of boehmite.
Technical scheme：
A kind of method for preparing high purity pseudoboehmite adhesive, using the aluminium-alcohol salt of the alcohol containing below C4 and deionized water as
Raw material, it is dilute above with hexamethylene, petroleum ether, containing one or both of below C4 alcohol, toluene or tetrahydrofuran organic solvent
Release agent, hydrolysis generation Pseudo-boehmite occurs after organic solvent diluting forms solution with water for aluminium-alcohol salt, then by its
It is aged under the conditions of certain temperature and auxiliary agent, most obtains high purity pseudoboehmite adhesive through drying afterwards.
Comprise the following steps that：
Under agitation, hydrolyzate is added in the organic solution of aluminium-alcohol salt for step 1., in 50~80 DEG C of temperature strips
2~8h of hydrolysis under part；
Described hydrolyzate is mixed by deionized water and the alcohol containing below C4, the mol ratio of deionized water and alcohol for 10~
40:1；
In the organic solution of described aluminium-alcohol salt organic solvent used be hexamethylene, petroleum ether of the boiling point less than 150 DEG C,
It is mixed above containing one or both of below C4 alcohol, toluene, tetrahydrofuran；
The weight/mass percentage composition of aluminium-alcohol salt is 20%wt~95%wt in the organic solution of described aluminium-alcohol salt, preferential to choose
50%wt~90%wt；
Described deionized water and the mol ratio of aluminium-alcohol salt are 2~30:1；
Described aluminium-alcohol salt is reacted by aluminium and alcohol, and is obtained through distillation or solvent extraction purifying, Na in aluminium-alcohol salt2O amounts are
Below 0.006%wt；
Gained hydrolysate in step 1 is aged 2-24 hours by step 2. under 40~100 DEG C and auxiliary agent existence condition, then
Through 60~260 DEG C of dryings, high purity pseudoboehmite adhesive is obtained；
Described auxiliary agent be sulfuric acid, nitric acid, containing below C4 carboxylic acids, citric acid, oleic acid, urea, ammonia, pyridine, triethanolamine,
Laruyl alcohol, the fatty alcohol containing C4-C8, EO-PO type polyethers Pluronic F127 (F127), PULLRONIC F68-polyoxy
One kind in ethylene block copolymer (P123), cetomacrogol 1000, polyethylene glycol 2000, Macrogol 4000, beta-schardinger dextrin
Or two or more mixing；
Described auxiliary agent and the mass ratio of aluminium-alcohol salt are 0.01~1:10.
Described organic solvent and auxiliary agent recycles in preparation system.
Beneficial effects of the present invention：Whole preparation process belongs to Environmentally-sound technology without waste discharge；Preparation flow letter simultaneously
It is single, it is easily controlled.The present invention manufacturing cost and it is environment-friendly etc. all show significant competitive advantage and profit margin,
It is particularly significant in terms of catalyst boehmite adhesive production domesticization is realized.In addition, what the present invention used
Raw material is the aluminium-alcohol salt of low-carbon alcohols, and long-chain aluminium-alcohol salt technics comparing, has the advantages that toxicity is low, easy purification.
Embodiment
The embodiment of the present invention is further illustrated below in conjunction with technical scheme.
Embodiment 1
Take 1020g aluminium isopropoxides (Na2O content is not higher than 0.004%wt) it is put into 200g isopropanols in 3L reactors,
Stirring and dissolving at 50~75 DEG C, after then adding 5~8h of hydrolyzate hydrolysis, bar is present into 90 DEG C and auxiliary agent in hydrolysate
It is aged 24 hours under part, then solid product after ageing is moved into drier, 12h is dried under the conditions of 60 DEG C, is obtained high-purity
Spend boehmite adhesive.The Al of boehmite2O3Content is 65~75%, Na2O content is not higher than 0.015%wt, than
Surface area is 230~250m2/ g, bulk density are 760~790kg/m3, pore volume is 0.45~0.5mL/g, and peptization index reaches
More than 99%, sol-gel thixotropy is less than 90 minutes.
Embodiment 2
Take 1020g aluminium isopropoxides (Na2O content is not higher than 0.004%wt) it is put into 1000g isopropanols in 3L reactors,
Mechanical agitation is uniform at 55~65 DEG C, then adds hydrolyzate, hydrolysis 2h, hydrolysate is existed in 60 DEG C and auxiliary agent
Under the conditions of be aged 2 hours, then ageing product is moved into drier, 1h is dried under the conditions of 180~240 DEG C, is obtained high-purity
Spend boehmite adhesive.The Al of boehmite2O3Content is 75~78%, Na2O content is not higher than 0.015%wt, than
Surface area is 250~340m2/ g, bulk density are 790~810/L, and pore volume is 0.8~1.2mL/g, and peptization index reaches 99%
More than, sol-gel thixotropy is less than 90 minutes.
Claims (10)
- A kind of 1. method for preparing high purity pseudoboehmite adhesive, it is characterised in that step is as follows：Under agitation, hydrolyzate is added in the organic solution of aluminium-alcohol salt for step 1., under 50~80 DEG C of temperature conditionss 2~8h of hydrolysis；Described hydrolyzate is mixed by deionized water and the alcohol containing below C4, and the mol ratio of deionized water and alcohol is 10~40: 1；The weight/mass percentage composition of aluminium-alcohol salt is 20%wt~95%wt in the organic solution of described aluminium-alcohol salt；Described deionized water and the mol ratio of aluminium-alcohol salt are 2~30:1；Gained hydrolysate in step 1 is aged 2-24 hours by step 2. under 40~100 DEG C and auxiliary agent existence condition, then through 60 ~260 DEG C of dryings, obtain high purity pseudoboehmite adhesive；Described auxiliary agent and the mass ratio of aluminium-alcohol salt are 0.01~1:10.
- 2. according to the method for claim 1, it is characterised in that described aluminium-alcohol salt is reacted by aluminium and alcohol, and through distillation or Solvent extraction purifying obtains, Na in aluminium-alcohol salt2O amounts are below 0.006%wt.
- 3. method according to claim 1 or 2, it is characterised in that used in the organic solution of described aluminium-alcohol salt to have Solvent be hexamethylene, boiling point less than 150 DEG C petroleum ether, containing one or both of below C4 alcohol, toluene, tetrahydrofuran with Upper mixing.
- 4. method according to claim 1 or 2, it is characterised in that described auxiliary agent is sulfuric acid, nitric acid, containing below C4 carboxylics Acid, citric acid, oleic acid, urea, ammonia, pyridine, triethanolamine, laruyl alcohol, the fatty alcohol containing C4-C8, EO-PO type polyethers Pluronic F127, polyoxyethylene-poly-oxypropylene polyoxyethylene block copolymer, cetomacrogol 1000, polyethylene glycol 2000, One or both of Macrogol 4000, beta-schardinger dextrin are mixed above.
- 5. according to the method for claim 3, it is characterised in that described auxiliary agent be sulfuric acid, nitric acid, containing below C4 carboxylic acids, Citric acid, oleic acid, urea, ammonia, pyridine, triethanolamine, laruyl alcohol, the fatty alcohol containing C4-C8, EO-PO type polyethers Pluronic F127, polyoxyethylene-poly-oxypropylene polyoxyethylene block copolymer, cetomacrogol 1000, polyethylene glycol 2000, polyethylene glycol 4000th, one or both of beta-schardinger dextrin is mixed above.
- 6. according to the method described in claim 1,2 or 5, it is characterised in that aluminium-alcohol salt in the organic solution of described aluminium-alcohol salt Weight/mass percentage composition be 50%wt~90%wt.
- 7. according to the method for claim 3, it is characterised in that the quality of aluminium-alcohol salt in the organic solution of described aluminium-alcohol salt Percentage composition is 50%wt~90%wt.
- 8. according to the method for claim 4, it is characterised in that the quality of aluminium-alcohol salt in the organic solution of described aluminium-alcohol salt Percentage composition is 50%wt~90%wt.
- 9. according to the method described in claim 1,2,5,7 or 8, it is characterised in that prepared by described organic solvent and auxiliary agent Recycled in system.
- 10. according to the method for claim 6, it is characterised in that described organic solvent and auxiliary agent follows in preparation system Ring uses.
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| CN201710982824.7A CN107720791A (en) | 2017-10-20 | 2017-10-20 | A kind of method for preparing high purity pseudoboehmite adhesive |
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| CN201710982824.7A CN107720791A (en) | 2017-10-20 | 2017-10-20 | A kind of method for preparing high purity pseudoboehmite adhesive |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110255593A (en) * | 2019-06-20 | 2019-09-20 | 广西玉林市思达粉体技术有限公司 | A kind of method that low cost prepares high-crystallinity, high gumminess boehmite |
| CN110386614A (en) * | 2019-06-20 | 2019-10-29 | 广西玉林市思达粉体技术有限公司 | Preparation method that is a kind of while obtaining large, medium and small aperture boehmite |
| CN110395756A (en) * | 2019-06-20 | 2019-11-01 | 广西玉林市思达粉体技术有限公司 | A method of preparing macropore appearance, multi-pore channel, wide distribution boehmite |
| CN110526266A (en) * | 2019-08-20 | 2019-12-03 | 广州市威格林环保科技有限公司 | A kind of Aluminum sol of binder and preparation method thereof as cleaning catalyst for tail gases of automobiles |
| CN112939039A (en) * | 2021-03-19 | 2021-06-11 | 大连理工大学 | Preparation method of low-sodium pseudo-boehmite |
| CN113149045A (en) * | 2021-04-23 | 2021-07-23 | 上海毅民实业有限公司 | Preparation method of rapid water-soluble hydroxyl-aluminum material |
| CN114702053A (en) * | 2022-03-14 | 2022-07-05 | 大连理工大学 | Steam-assisted method for hydroxylation enrichment of pseudo-boehmite surface |
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| CN104192880A (en) * | 2014-07-18 | 2014-12-10 | 大连理工大学 | Method for preparing high-purity pseudo-boehmite |
| CN104353400A (en) * | 2014-11-12 | 2015-02-18 | 山东恒通晶体材料有限公司 | Preparation method of high-purity high-solid content transparent aluminum sol |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110255593A (en) * | 2019-06-20 | 2019-09-20 | 广西玉林市思达粉体技术有限公司 | A kind of method that low cost prepares high-crystallinity, high gumminess boehmite |
| CN110386614A (en) * | 2019-06-20 | 2019-10-29 | 广西玉林市思达粉体技术有限公司 | Preparation method that is a kind of while obtaining large, medium and small aperture boehmite |
| CN110395756A (en) * | 2019-06-20 | 2019-11-01 | 广西玉林市思达粉体技术有限公司 | A method of preparing macropore appearance, multi-pore channel, wide distribution boehmite |
| CN110395756B (en) * | 2019-06-20 | 2022-02-08 | 广西玉林市思达粉体技术有限公司 | Method for preparing pseudoboehmite with large pore volume, multiple pore channels and wide distribution |
| CN110526266A (en) * | 2019-08-20 | 2019-12-03 | 广州市威格林环保科技有限公司 | A kind of Aluminum sol of binder and preparation method thereof as cleaning catalyst for tail gases of automobiles |
| CN110526266B (en) * | 2019-08-20 | 2022-04-05 | 广州市威格林环保科技有限公司 | Aluminum sol used as binder of automobile exhaust purification catalyst and preparation method thereof |
| CN112939039A (en) * | 2021-03-19 | 2021-06-11 | 大连理工大学 | Preparation method of low-sodium pseudo-boehmite |
| CN113149045A (en) * | 2021-04-23 | 2021-07-23 | 上海毅民实业有限公司 | Preparation method of rapid water-soluble hydroxyl-aluminum material |
| CN114702053A (en) * | 2022-03-14 | 2022-07-05 | 大连理工大学 | Steam-assisted method for hydroxylation enrichment of pseudo-boehmite surface |
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Application publication date: 20180223 |