CN104085907A - Method for preparing large-pore-volume high-viscosity pseudo bohemite - Google Patents
Method for preparing large-pore-volume high-viscosity pseudo bohemite Download PDFInfo
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- CN104085907A CN104085907A CN201410347664.5A CN201410347664A CN104085907A CN 104085907 A CN104085907 A CN 104085907A CN 201410347664 A CN201410347664 A CN 201410347664A CN 104085907 A CN104085907 A CN 104085907A
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Abstract
The invention discloses a method for preparing large-pore-volume high-viscosity pseudo bohemite. The method comprises the following steps: reacting dilute nitric acid with a sodium metaaluminate solution in a synthesis reactor to prepare gelatin, keeping the pH value stable in the gelatin forming process, alternatively adding dilute nitric acid and sodium metaaluminate, so that the neutralization solution is alternatively positioned in acid and base environments, stabilizing the pH value in a specified range before neutralization is ended, aging in a washing kettle for a certain time, pressing the mixture into a plate-and-frame filter press through a pressing pump, washing for several times, and preparing pseudo bohemite (aluminum nitrate gelatin), drying the pseudo bohemite in a drying room, and crushing the pseudo bohemite in a crusher. According to the mode, NaAlO2-HNO3 serves as a process route, and the pseudo bohemite of which the pore volume is more than or equal to 0.80ml/g, the peptization index is more than or equal to 99 percent and the most accessible radius is more than or equal to 400 angstroms is prepared by fully utilizing the viscosity of nitric acid, the property that the viscosity of the pseudo bohemite is increased in an acid environment and a method for increasing the pore volume due to pH fluctuation in the neutralization process.
Description
Technical field
The present invention relates to the synthetic field of fine chemistry industry, particularly relate to the preparation method of a kind of large pore volume, the rich diaspore of high viscosity plan.
Background technology
Intend a kind of series product that rich diaspore belongs to chemical aluminum oxide, it is nontoxic, tasteless, the colloid that is white in color (wet product) or powder (dry powder).It has netted space structure, has and under larger space, flourishing specific surface area, sour environment, becomes the thixotropy etc. with viscosity colloidal substances, makes this product have the features such as crystalline phase purity is high, peptization performance good, cohesiveness is strong, thixotropy gel.
Intend rich diaspore and be widely used as coating highly effective binder, high-grade ceramic, effective catalyst and support of the catalyst, sorbent material, siccative, submicron/nanometer level abrasive substance and polishing material, makeup filler and inorganic material film etc.Being widely used in the industries such as petrochemical complex, chemical fertilizer, papermaking, coating, environmental protection, empty point, medicine, daily use chemicals, artificial artificial limb, aerospace, is the type material that a class has wide development prospect.
The height of peptization index has reflected the close-burning quality of intending rich diaspore.Cohesiveness is better, and the binding agent viscosity of making is higher, and catalyzer or support of the catalyst intensity are higher, and product physical and chemical performance is all right.No matter but at present the standby rich diaspore peptization index of plan of acid system, alkaline process, carborization or aluminium alcoholates legal system is the highest in 95% left and right, is difficult to improve again, this has just limited the further development and application of intending rich diaspore.
In addition, the rich diaspore pore volume of plan that general viscosity is high is less, and the rich diaspore peptization index of plan of preparing as carborization can reach 95% left and right, and pore volume is generally below 0.5ml/g, and the larger rich general viscosity of diaspore of plan of pore volume is just low, as NaAlO
2-Al
2(SO
4)
3, NaAlO
2-AlCl
3, NaAlO
2-Al (NO
3)
3, NH
4oH-AlCl
3deng, more than pore volume can reach 0.8 ml/g, peptization index generally below 90%, have even below 30%.Therefore,, concerning intending rich diaspore, increase pore volume and peptization index is the problem of a contradiction simultaneously.The rich suitable binding agent that does of diaspore of plan that pore volume is little, viscosity is high; And rich suitable catalyzer or the support of the catalyst done of diaspore of the plan that pore volume is large, viscosity is low.If it is high to prepare peptization index, and the large plan of pore volume is won diaspore no matter as binding agent, or as catalyzer, its physical and chemical performance all has a distinct increment, and application prospect is more wide.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of large pore volume, and high viscosity is intended the preparation method of rich diaspore, and the method is with NaAlO
2~ HNO
3for operational path, make full use of self viscosity of nitric acid and intend the rich diaspore character that viscosity increases under sour environment and N-process utilizes pH to wave to be conducive to increase the way of pore volume, prepare pore volume>=0.8ml/g, peptization index>=99%, can and the rich diaspore of plan of pore radius>=400.
For solving the problems of the technologies described above, the invention provides a kind of large pore volume, high viscosity is intended the preparation method of rich diaspore, comprises the following steps:
(1) by NaOH and Al (OH)
3be made into taking aluminum oxide mass concentration as 50～300g/L causticity factor alpha preparing in still
k(NaAlO
2na in solution
2amount of substance concentration and the Al of O
2o
3the ratio of amount of substance concentration) be 0.8～1.0 NaAlO
2solution.
(2) under mechanical stirring, by dense HNO
3slowly add in the dilution trap that deionized water is housed, be made into the HNO of concentration 10-40%
3solution.
(3) in synthesis reactor, first add a certain amount of deionized water, under mechanical stirring, be heated to 60-100 DEG C, then by rare HNO
3solution and NaAlO
2solution with 5～20L/min flow velocity continuously and flow plastic, keeps temperature of reaction, and stable neutralizer pH 6～9.
(4) excessively after 20 minutes, start variation for the first time, first add NaAlO
2solution is controlled at 10～10.5 by pH, then stops to add NaAlO
2solution-stabilized 10～20min, then add HNO
3solution is controlled at 3～4 by pH, then stops to add HNO
3solution-stabilized 10～20min, so alternately variation is once a circulation.
(5) in repeating step 4, circulate 2～6 times, neutralization finishes, and reaction end pH is stabilized in 6～9, then carries out agingly, and digestion time is controlled at 20～60min.
(6) liquid after aging is pumped into plate-and-frame filter press with binder, then repeatedly washs with the water of 30～60 DEG C of temperature, until Na
2till till O content is qualified.
(7) wet cake after washing is placed in drying room and is dried, temperature is controlled at 100～120 DEG C, intends rich diaspore igloss and is controlled at 20～40%.
(8) dried filter cake is pulverized, and requires fineness at 320～600 orders.
In preferred embodiments of the present invention, NaAlO in described step (1)
2strength of solution is 100～250g/L.
In preferred embodiments of the present invention, rare HNO in described step (2)
3strength of solution optimum control is 15～30%.
In preferred embodiments of the present invention, in described step (3), neutralizer temperature optimum control is at 70～80 DEG C, and neutralizer pH optimum control is 7～8.
In preferred embodiments of the present invention, in described step (5), pH number of oscillations optimum control is at 3-5 time, and digestion time the best is 30～45min.
In preferred embodiments of the present invention, in described step (6), washings optimum temps is controlled at 40～50 DEG C.
In preferred embodiments of the present invention, in described step (7), intend rich diaspore igloss optimum control 28～32%.
In preferred embodiments of the present invention, described large pore volume, the technical parameter that high viscosity is intended rich diaspore is: peptization index>=99%, pore volume>=0.80ml/g, specific surface area>=200m
2/ g, can and pore radius>=400.
The invention has the beneficial effects as follows:
1, with NaAlO
2~ HNO
3for operational path, make full use of self viscosity of nitric acid and intend rich diaspore and under sour environment, become thixotropic character with viscosity colloidal substances and prepare high viscosity and intend rich diaspore.
2, utilize pH in N-process alternately to change the character that is conducive to intend rich diaspore primary particle increase, increase and intend winning diaspore mesopore, prepare large pore volume and intend winning diaspore.
3, prepared pore volume >=0.80ml/g, peptization index >=99%, can and the rich diaspore of plan of pore radius >=400, solved the contradiction that peptization index and pore volume can not increase simultaneously.Intend rich diaspore with tradition and compare, there is more excellent physical and chemical performance, also there is larger application prospect.
Embodiment
To the technical scheme in the embodiment of the present invention be clearly and completely described below, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making all other embodiment that obtain under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1:
The present embodiment provides a kind of large pore volume, high viscosity to intend the preparation method of rich diaspore, specifically comprises the following steps:
(1) by NaOH and Al (OH)
3be made into taking aluminum oxide mass concentration as 120g/L causticity factor alpha preparing in still
k(NaAlO
2na in solution
2amount of substance concentration and the Al of O
2o
3the ratio of amount of substance concentration) be 0.9 NaAlO
2solution.
(2) under mechanical stirring, by dense HNO
3slowly add in the dilution trap that deionized water is housed, be made into the HNO of concentration 20%
3solution.
(3) in synthesis reactor, first add a certain amount of deionized water, under mechanical stirring, be heated to 75 DEG C, then by rare HNO
3solution and NaAlO
2solution with 5～20L/min flow velocity continuously and flow plastic, keeps temperature of reaction, and stable neutralizer pH 7.5.
After (4) 20 minutes, start variation for the first time, first add NaAlO
2solution is controlled at 10～10.5 by pH, then stops to add NaAlO
2solution-stabilized 10～20min, then add HNO
3solution is controlled at 3～4 by pH, then stops to add HNO
3solution-stabilized 10～20min, so alternately a circulation is once calculated in variation.
(5) repeat above-mentioned circulation 3 times, neutralization finishes, and reaction end pH is stabilized in 7.5, then carries out agingly, and digestion time is controlled at 30min.
(6) liquid after aging is pumped into plate-and-frame filter press with binder, then repeatedly washs with the water of temperature 45 C, until Na
2till till O content is qualified.
(7) wet cake after washing is placed in drying room and is dried, temperature is controlled at 100～120 DEG C, intends rich diaspore igloss and is controlled at 30%.
(8) dried filter cake is pulverized, and smashing fineness is at 400 orders.
Embodiment 1 comparative example
According to the step of embodiment 1, difference is without alternately variation of the pH of step (4), (5), but directly equilibrium temperature and pH carry out and flow neutralization, record sample data in table 1.
Embodiment 2:
The present embodiment provides a kind of large pore volume, high viscosity to intend the preparation method of rich diaspore, specifically comprises the following steps:
(1) by NaOH and Al (OH)
3be made into taking aluminum oxide mass concentration as 150g/L causticity factor alpha preparing in still
k(NaAlO
2na in solution
2amount of substance concentration and the Al of O
2o
3the ratio of amount of substance concentration) be 0.92 NaAlO
2solution.
(2) under mechanical stirring, by dense HNO
3slowly add in the dilution trap that deionized water is housed, be made into the HNO of concentration 25%
3solution.
(3) in synthesis reactor, first add a certain amount of deionized water, under mechanical stirring, be heated to 70 DEG C, then by rare HNO
3solution and NaAlO
2solution with 5～20L/min flow velocity continuously and flow plastic, keeps temperature of reaction, and stable neutralizer pH 7.8.
After (4) 20 minutes, start variation for the first time, first add NaAlO
2solution is controlled at 10～10.5 by pH, then stops to add NaAlO
2solution-stabilized 10～20min, then add HNO
3solution is controlled at 3～4 by pH, then stops to add HNO
3solution-stabilized 10～20min, so alternately a circulation is once calculated in variation.
(5) repeat above-mentioned circulation 4 times, neutralization finishes, and reaction end pH is stabilized in 7.8, then carries out agingly, and digestion time is controlled at 35min.
(6) liquid after aging is pumped into plate-and-frame filter press with binder, then repeatedly washs with the water of temperature 50 C, until Na
2till till O content is qualified.
(7) wet cake after washing is placed in drying room and is dried, temperature is controlled at 100～120 DEG C, intends rich diaspore igloss and is controlled at 29%.
(8) dried filter cake is pulverized, and smashing fineness is at 450 orders.
Embodiment 2 comparative examples
According to the step of embodiment 2, difference is that the pH of step (5) alternately changes 8 times, records sample data in table 1.
Embodiment 3:
The present embodiment provides a kind of large pore volume, high viscosity to intend the preparation method of rich diaspore, specifically comprises the following steps:
(1) by NaOH and Al (OH)
3be made into taking aluminum oxide mass concentration as 200g/L causticity factor alpha preparing in still
k(NaAlO
2na in solution
2amount of substance concentration and the Al of O
2o
3the ratio of amount of substance concentration) be 1.0 NaAlO
2solution.
(2) under mechanical stirring, by dense HNO
3slowly add in the dilution trap that deionized water is housed, be made into the HNO of concentration 28%
3solution.
(3) in synthesis reactor, first add a certain amount of deionized water, under mechanical stirring, be heated to 80 DEG C, then by rare HNO
3solution and NaAlO
2solution with 5～20L/min flow velocity continuously and flow plastic, keeps temperature of reaction, and stable neutralizer pH 8.0.
After (4) 20 minutes, start variation for the first time, first add NaAlO
2solution is controlled at 10～10.5 by pH, then stops to add NaAlO
2solution-stabilized 10～20min, then add HNO
3solution is controlled at 3～4 by pH, then stops to add HNO
3solution-stabilized 10～20min, so alternately a circulation is once calculated in variation.
(5) repeat above-mentioned circulation 3 times, neutralization finishes, and reaction end pH is stabilized in 8.0, then carries out agingly, and digestion time is controlled at 40min.
(6) liquid after aging is pumped into plate-and-frame filter press with binder, then repeatedly washs with the water of 40 DEG C of temperature, until Na
2till till O content is qualified.
(7) wet cake after washing is placed in drying room and is dried, temperature is controlled at 100～120 DEG C, intends rich diaspore igloss and is controlled at 31%.
(8) dried filter cake is pulverized, and smashing fineness is at 420 orders.
Embodiment 3 comparative examples
According to the step of embodiment 3, difference is rare HNO of step (2), (3), (4)
3with rare HCl replacement, record sample data in table 1.
Embodiment 4:
The present embodiment provides a kind of large pore volume, high viscosity to intend the preparation method of rich diaspore, specifically comprises the following steps:
(1) by NaOH and Al (OH)
3be made into taking aluminum oxide mass concentration as 250g/L causticity factor alpha preparing in still
k(NaAlO
2na in solution
2amount of substance concentration and the Al of O
2o
3the ratio of amount of substance concentration) be 1.0 NaAlO
2solution.
(2) under mechanical stirring, by dense HNO
3slowly add in the dilution trap that deionized water is housed, be made into the HNO of concentration 30%
3solution.
(3) in synthesis reactor, first add a certain amount of deionized water, under mechanical stirring, be heated to 76 DEG C, then by rare HNO
3solution and NaAlO
2solution with 5～20L/min flow velocity continuously and flow plastic, keeps temperature of reaction, and stable neutralizer pH 7.6.
After (4) 20 minutes, start variation for the first time, first add NaAlO
2solution is controlled at 10～10.5 by pH, then stops to add NaAlO
2solution-stabilized 10～20min, then add HNO
3solution is controlled at 3～4 by pH, then stops to add HNO
3solution-stabilized 10～20min, so alternately a circulation is once calculated in variation.
(5) repeat above-mentioned circulation 3 times, neutralization finishes, and reaction end pH is stabilized in 7.6, then carries out agingly, and digestion time is controlled at 38min.
(6) liquid after aging is pumped into plate-and-frame filter press with binder, then repeatedly washs with the water of 48 DEG C of temperature, until Na
2till till O content is qualified.
(7) wet cake after washing is placed in drying room and is dried, temperature is controlled at 100～120 DEG C, intends rich diaspore igloss and is controlled at 31%.
(8) dried filter cake is pulverized, and smashing fineness is at 400 orders.
Embodiment 4 comparative examples
According to the step of embodiment 4, difference is the NaAlO in step (1)
2strength of solution is adjusted into 400g/L; (2) the rare HNO in
3strength of solution is adjusted into 40%, records sample data in table 1.
Table 1 example analytical data
Claims (8)
1. a large pore volume, high viscosity is intended the preparation method of rich diaspore, it is characterized in that, comprises the following steps:
(1) by NaOH and Al (OH)
3be made into taking aluminum oxide mass concentration as 50～300g/L causticity factor alpha preparing in still
k(NaAlO
2na in solution
2amount of substance concentration and the Al of O
2o
3the ratio of amount of substance concentration) be 0.8～1.0 NaAlO
2solution;
(2) under mechanical stirring, by dense HNO
3slowly add in the dilution trap that deionized water is housed, be made into the HNO of concentration 10-40%
3solution;
(3) in synthesis reactor, first add a certain amount of deionized water, under mechanical stirring, be heated to 60-100 DEG C, then by rare HNO
3solution and NaAlO
2solution with 5～20L/min flow velocity continuously and flow plastic, keeps temperature of reaction, and stable neutralizer pH 6～9;
(4) excessively after 20 minutes, start variation for the first time, first add NaAlO
2solution is controlled at 10～10.5 by pH, then stops to add NaAlO
2solution-stabilized 10～20min, then add HNO
3solution is controlled at 3～4 by pH, then stops to add HNO
3solution-stabilized 10～20min, so alternately variation is once a circulation;
(5) in repeating step 4, circulate 2～6 times, neutralization finishes, and reaction end pH is stabilized in 6～9, then carries out agingly, and digestion time is controlled at 20～60min;
(6) liquid after aging is pumped into plate-and-frame filter press with binder, then repeatedly washs with the water of 30～60 DEG C of temperature, until Na
2till till O content is qualified;
(7) wet cake after washing is placed in drying room and is dried, temperature is controlled at 100～120 DEG C, intends rich diaspore igloss and is controlled at 20～40%;
(8) dried filter cake is pulverized, and requires fineness at 320～600 orders.
2. large pore volume according to claim 1, high viscosity is intended the preparation method of rich diaspore, it is characterized in that NaAlO in described step (1)
2strength of solution is 100～250g/L.
3. large pore volume according to claim 1, high viscosity is intended the preparation method of rich diaspore, it is characterized in that rare HNO in described step (2)
3strength of solution optimum control is 15～30%.
4. large pore volume according to claim 1, high viscosity is intended the preparation method of rich diaspore, it is characterized in that, and in described step (3), neutralizer temperature optimum control is at 70～80 DEG C, and neutralizer pH optimum control is 7～8.
5. large pore volume according to claim 1, high viscosity is intended the preparation method of rich diaspore, it is characterized in that, and in described step (5), pH number of oscillations optimum control is at 3-5 time, and digestion time the best is 30～45min.
6. large pore volume according to claim 1, high viscosity is intended the preparation method of rich diaspore, it is characterized in that, and in described step (6), washings optimum temps is controlled at 40～50 DEG C.
7. large pore volume according to claim 1, high viscosity is intended the preparation method of rich diaspore, it is characterized in that, intends rich diaspore igloss optimum control 28～32% in described step (7).
8. large pore volume according to claim 1, high viscosity is intended the preparation method of rich diaspore, it is characterized in that, described large pore volume, the technical parameter that high viscosity is intended rich diaspore is: peptization index>=99%, pore volume>=0.80ml/g, specific surface area>=200m
2/ g, can and pore radius>=400.
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Cited By (7)
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| CN105709789A (en) * | 2014-12-02 | 2016-06-29 | 中国石油化工股份有限公司 | Heavy oil hydrocracking catalyst, and preparation method and applications thereof |
| CN108623218A (en) * | 2018-05-09 | 2018-10-09 | 甘肃农业大学 | A kind of preparation method of boehmite doping vario-property diatom ooze coating |
| CN108910925A (en) * | 2018-09-11 | 2018-11-30 | 淄博齐茂催化剂有限公司 | A kind of preparation method of boehmite |
| CN109607583A (en) * | 2019-01-28 | 2019-04-12 | 云南文山铝业有限公司 | The Ageing solution recovery system and recovery method of modified aluminas production technology |
| CN110127736A (en) * | 2019-05-28 | 2019-08-16 | 中国铝业股份有限公司 | A kind of preparation method of high glutinous macropore boehmite |
| CN113582212A (en) * | 2021-07-16 | 2021-11-02 | 上海簇睿低碳能源技术有限公司 | Preparation method of pseudo-boehmite for adhesive |
| CN114988444A (en) * | 2022-04-29 | 2022-09-02 | 江苏晶晶新材料有限公司 | Preparation method of nano alumina microspheres special for antibiotic decolorization |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105709789A (en) * | 2014-12-02 | 2016-06-29 | 中国石油化工股份有限公司 | Heavy oil hydrocracking catalyst, and preparation method and applications thereof |
| CN105709789B (en) * | 2014-12-02 | 2018-07-03 | 中国石油化工股份有限公司 | A kind of hydrocracking heavy oil catalyst and its preparation method and application |
| CN108623218A (en) * | 2018-05-09 | 2018-10-09 | 甘肃农业大学 | A kind of preparation method of boehmite doping vario-property diatom ooze coating |
| CN108910925A (en) * | 2018-09-11 | 2018-11-30 | 淄博齐茂催化剂有限公司 | A kind of preparation method of boehmite |
| CN109607583A (en) * | 2019-01-28 | 2019-04-12 | 云南文山铝业有限公司 | The Ageing solution recovery system and recovery method of modified aluminas production technology |
| CN110127736A (en) * | 2019-05-28 | 2019-08-16 | 中国铝业股份有限公司 | A kind of preparation method of high glutinous macropore boehmite |
| CN110127736B (en) * | 2019-05-28 | 2022-02-22 | 中国铝业股份有限公司 | Preparation method of high-viscosity macroporous pseudo-boehmite |
| CN113582212A (en) * | 2021-07-16 | 2021-11-02 | 上海簇睿低碳能源技术有限公司 | Preparation method of pseudo-boehmite for adhesive |
| CN114988444A (en) * | 2022-04-29 | 2022-09-02 | 江苏晶晶新材料有限公司 | Preparation method of nano alumina microspheres special for antibiotic decolorization |
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