CN104085907B - The preparation method of large pore volume, high viscosity pseudo-boehmite - Google Patents
The preparation method of large pore volume, high viscosity pseudo-boehmite Download PDFInfo
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Abstract
The present invention discloses a kind of large pore volume, the preparation method of high viscosity pseudo-boehmite, comprise the following steps: dust technology and sodium aluminate solution are made glue in synthesis reactor, and flow in the process of plastic, pH is first kept to stablize, then dust technology and sodium metaaluminate are alternately added, neutralizer is made alternately to be in acid, in the environment of alkali, pH is stabilized in stated limit before terminating by neutralization again, then in washing kettle after aging certain time, it is pumped into plate-and-frame filter press with binder, repeatedly wash, it is dried in drying room after obtained pseudo-boehmite (nitric acid aluminium glue), pulverizer is pulverized. by the way, the present invention is with NaAlO2~HNO3For operational path, make full use of the intrinsic viscosity of nitric acid and the pseudo-boehmite character that viscosity increases under sour environment and in and process utilize pH to wave the way being conducive to enlarged hole to hold, prepare the appearance >=0.80ml/g that portals, molten index >=99% of glue, can and radius >=400, hole? pseudo-boehmite.
Description
Technical field
The present invention relates to fine chemistry industry synthesis field, particularly relate to the preparation method of a kind of large pore volume, high viscosity pseudo-boehmite.
Background technology
Pseudo-boehmite belongs to a kind of series product of chemical aluminum oxide, and it is nontoxic, tasteless, in white colloid (wet product) or powder (dry powder). It has netted space structure, turns into having the thixotropy etc. of viscosity colloidal substances so that the features such as this product has crystalline phase purity height, peptization performance is good, cohesiveness is strong, thixotropy gel under having bigger space, flourishing specific surface area, sour environment.
Pseudo-boehmite is 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. It is widely used in the industries such as petrochemical complex, chemical fertilizer, papermaking, coating, environmental protection, sky point, medicine, daily use chemicals, artificial artificial limb, aerospace, it is the type material that a class has wide development prospect.
The height of the molten index of glue reflects the quality of the cohesiveness of pseudo-boehmite.Cohesiveness is more good, and the binding agent viscosity of making is more high, and catalyzer or support of the catalyst intensity are more high, and product physical and chemical performance is all right. No matter but the molten index of pseudo-boehmite glue that at present prepared by acid method, alkali method, carborization or alcohol aluminium method is the highest about 95%, it is very difficult to improve again, which limits the further development and application of pseudo-boehmite.
In addition, the high pseudo-boehmite hole of general viscosity holds less, and the molten index of pseudo-boehmite glue prepared such as carborization can reach about 95%, and hole holds general at below 0.5ml/g, and the bigger general viscosity of pseudo-boehmite of Kong Rong is just low, such as NaAlO2-Al2(SO4)3��NaAlO2-AlCl3��NaAlO2-Al(NO3)3��NH4OH-AlCl3Deng, Kong Rongke reaches more than 0.8ml/g, the molten index of glue generally below 90%, have even below 30%. Therefore, concerning pseudo-boehmite, enlarged hole appearance and the molten index of glue are the problems of a contradiction simultaneously. The pseudo-boehmite that Kong Rong little, viscosity are high is suitable for making binding agent; And the low pseudo-boehmite of Kong Rong great, viscosity is suitable for doing catalyzer or support of the catalyst. If the preparation molten index height of plastic emitting, and no matter hole holds big pseudo-boehmite 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 the preparation method of high viscosity pseudo-boehmite, the method is with NaAlO2~HNO3For operational path, make full use of the intrinsic viscosity of nitric acid and the pseudo-boehmite character that viscosity increases under sour environment and in and process utilize pH to wave the way being conducive to enlarged hole to hold, prepare the appearance >=0.8ml/g that portals, molten index >=99% of glue, can and the pseudo-boehmite of radius >=400, hole.
For solving the problems of the technologies described above, the present invention provides a kind of large pore volume, and the preparation method of high viscosity pseudo-boehmite, comprises the following steps:
(1) by NaOH and Al (OH)3Mass concentration is counted as 50��300g/L, causticity factor alpha preparing still is made into taking aluminum oxidek(NaAlO2Na in solution2The substance withdrawl syndrome of O and Al2O3The ratio of substance withdrawl syndrome) be 0.8��1.0 NaAlO2Solution.
Under mechanical stirring, (2) by dense HNO3Slowly add in the dilution trap that deionized water is housed, it is made into the HNO of concentration 10-40%3Solution.
(3) in synthesis reactor, first add a certain amount of deionized water, it is heated to 60-100 DEG C under mechanical stirring, then by rare HNO3Solution and NaAlO2Solution continuously and flows plastic with 5��20L/min flow velocity, keeps temperature of reaction, and stablizes neutralizer pH6��9.
(4) start first time variation after spending 20 minutes, first add NaAlO2PH is controlled 10��10.5 by solution, then stops to add NaAlO2Solution-stabilized 10��20min, then add HNO3PH is controlled 3��4 by solution, then stops to add HNO3Solution-stabilized 10��20min, so alternately variation is once a circulation.
(5) circulating 2��6 times in repeating step 4, neutralization terminates, and reaction end pH is stabilized in 6��9, then carries out aging, and digestion time controls at 20��60min.
(6) the liquid binder after aging is pumped into plate-and-frame filter press, then repeatedly washs with the water of temperature 30��60 DEG C, until Na2Till O content is qualified.
(7) wet cake after washing being placed in drying room and is dried, temperature controls at 100��120 DEG C, and pseudo-boehmite igloss controls 20��40%.
(8) dried filter cake is pulverized, it is desired to fineness is at 320��600 orders.
In the present invention's preferred embodiments, NaAlO in described step (1)2Strength of solution is 100��250g/L.
In the present invention's preferred embodiments, rare HNO in described step (2)3Strength of solution optimum control is 15��30%.
In the present invention's preferred embodiments, in described step (3), neutralizer temperature optimum control is at 70��80 DEG C, and neutralizer pH optimum control is 7��8.
In the present invention's preferred embodiments, in described step (5), pH number of oscillations optimum control is at 3-5 time, and digestion time the best is 30��45min.
In the present invention's preferred embodiments, in described step (6), washings optimum temps controls at 40��50 DEG C.
In the present invention's preferred embodiments, described step (7) is intended rich diaspore igloss optimum control 28��32%.
In the present invention's preferred embodiments, described large pore volume, the technical parameter of high viscosity pseudo-boehmite is: molten index >=99% of glue, Kong Rong >=0.80ml/g, specific surface area >=200m2/ g, can and radius >=400, hole.
The invention has the beneficial effects as follows:
1, with NaAlO2~HNO3For operational path, make full use of the intrinsic viscosity of nitric acid and thixotropic character that pseudo-boehmite turns into having viscosity colloidal substances under sour environment prepares high viscosity pseudo-boehmite;
2, utilize in and the pH character that alternately variation is conducive to pseudo-boehmite primary particle to increase in process, increase pseudo-boehmite mesopore, prepares pseudo-thin diasphore with great pore volume;
3, prepared Kong Rong >=0.80ml/g, molten index >=99% of glue, can and the rich diaspore of plan of radius >=400, hole, solve the contradiction that the molten index of glue can not increase simultaneously with hole appearance. Compared with tradition pseudo-boehmite, there is more excellent physical and chemical performance, also there is bigger application prospect.
Embodiment
It is clearly and completely described to the technical scheme in the embodiment of the present invention below, it is clear that described embodiment is only a part of embodiment of the present invention, instead of whole embodiments. Based on the embodiment in the present invention, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1:
The present embodiment provides the preparation method of a kind of large pore volume, high viscosity pseudo-boehmite, specifically comprises the following steps:
(1) by NaOH and Al (OH)3Mass concentration is counted as 120g/L, causticity factor alpha preparing still is made into taking aluminum oxidek(NaAlO2Na in solution2The substance withdrawl syndrome of O and Al2O3The ratio of substance withdrawl syndrome) be 0.9 NaAlO2Solution.
Under mechanical stirring, (2) by dense HNO3Slowly add in the dilution trap that deionized water is housed, it is made into the HNO of concentration 20%3Solution.
(3) in synthesis reactor, first add a certain amount of deionized water, it is heated to 75 DEG C under mechanical stirring, then by rare HNO3Solution and NaAlO2Solution continuously and flows plastic with 5��20L/min flow velocity, keeps temperature of reaction, and stablizes neutralizer pH7.5.
Start first time variation after (4) 20 minutes, first add NaAlO2PH is controlled 10��10.5 by solution, then stops to add NaAlO2Solution-stabilized 10��20min, then add HNO3PH is controlled 3��4 by solution, then stops to add HNO3Solution-stabilized 10��20min, so alternately a circulation is once calculated in variation.
(5) repeating above-mentioned circulation 3 times, neutralization terminates, and reaction end pH is stabilized in 7.5, then carries out aging, and digestion time controls at 30min.
(6) the liquid binder after aging is pumped into plate-and-frame filter press, then repeatedly washs with the water of temperature 45 DEG C, until Na2Till O content is qualified.
(7) wet cake after washing being placed in drying room and is dried, temperature controls at 100��120 DEG C, and pseudo-boehmite igloss controls 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, the difference is that the alternately variation of the pH without 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 the preparation method of a kind of large pore volume, high viscosity pseudo-boehmite, specifically comprises the following steps:
(1) by NaOH and Al (OH)3Mass concentration is counted as 150g/L, causticity factor alpha preparing still is made into taking aluminum oxidek(NaAlO2Na in solution2The substance withdrawl syndrome of O and Al2O3The ratio of substance withdrawl syndrome) be 0.92 NaAlO2Solution.
Under mechanical stirring, (2) by dense HNO3Slowly add in the dilution trap that deionized water is housed, it is made into the HNO of concentration 25%3Solution.
(3) in synthesis reactor, first add a certain amount of deionized water, it is heated to 70 DEG C under mechanical stirring, then by rare HNO3Solution and NaAlO2Solution continuously and flows plastic with 5��20L/min flow velocity, keeps temperature of reaction, and stablizes neutralizer pH7.8.
Start first time variation after (4) 20 minutes, first add NaAlO2PH is controlled 10��10.5 by solution, then stops to add NaAlO2Solution-stabilized 10��20min, then add HNO3PH is controlled 3��4 by solution, then stops to add HNO3Solution-stabilized 10��20min, so alternately a circulation is once calculated in variation.
(5) repeating above-mentioned circulation 4 times, neutralization terminates, and reaction end pH is stabilized in 7.8, then carries out aging, and digestion time controls at 35min.
(6) the liquid binder after aging is pumped into plate-and-frame filter press, then repeatedly washs with the water of temperature 50 DEG C, until Na2Till O content is qualified.
(7) wet cake after washing being placed in drying room and is dried, temperature controls at 100��120 DEG C, and pseudo-boehmite igloss controls 29%.
(8) dried filter cake is pulverized, and smashing fineness is at 450 orders.
Embodiment 2 comparative example
According to the step of embodiment 2, the difference is that pH alternately variation 8 times of step (5), record sample data in table 1.
Embodiment 3:
The present embodiment provides the preparation method of a kind of large pore volume, high viscosity pseudo-boehmite, specifically comprises the following steps:
(1) by NaOH and Al (OH)3Mass concentration is counted as 200g/L, causticity factor alpha preparing still is made into taking aluminum oxidek(NaAlO2Na in solution2The substance withdrawl syndrome of O and Al2O3The ratio of substance withdrawl syndrome) be 1.0 NaAlO2Solution.
Under mechanical stirring, (2) by dense HNO3Slowly add in the dilution trap that deionized water is housed, it is made into the HNO of concentration 28%3Solution.
(3) in synthesis reactor, first add a certain amount of deionized water, it is heated to 80 DEG C under mechanical stirring, then by rare HNO3Solution and NaAlO2Solution continuously and flows plastic with 5��20L/min flow velocity, keeps temperature of reaction, and stablizes neutralizer pH8.0.
Start first time variation after (4) 20 minutes, first add NaAlO2PH is controlled 10��10.5 by solution, then stops to add NaAlO2Solution-stabilized 10��20min, then add HNO3PH is controlled 3��4 by solution, then stops to add HNO3Solution-stabilized 10��20min, so alternately a circulation is once calculated in variation.
(5) repeating above-mentioned circulation 3 times, neutralization terminates, and reaction end pH is stabilized in 8.0, then carries out aging, and digestion time controls at 40min.
(6) the liquid binder after aging is pumped into plate-and-frame filter press, then repeatedly washs with the water of temperature 40 DEG C, until Na2Till O content is qualified.
(7) wet cake after washing being placed in drying room and is dried, temperature controls at 100��120 DEG C, and pseudo-boehmite igloss controls 31%.
(8) dried filter cake is pulverized, and smashing fineness is at 420 orders.
Embodiment 3 comparative example
According to the step of embodiment 3, the difference is that rare HNO of step (2), (3), (4)3Replace with rare HCl, record sample data in table 1.
Embodiment 4:
The present embodiment provides the preparation method of a kind of large pore volume, high viscosity pseudo-boehmite, specifically comprises the following steps:
(1) by NaOH and Al (OH)3Mass concentration is counted as 250g/L, causticity factor alpha preparing still is made into taking aluminum oxidek(NaAlO2Na in solution2The substance withdrawl syndrome of O and Al2O3The ratio of substance withdrawl syndrome) be 1.0 NaAlO2Solution.
Under mechanical stirring, (2) by dense HNO3Slowly add in the dilution trap that deionized water is housed, it is made into the HNO of concentration 30%3Solution.
(3) in synthesis reactor, first add a certain amount of deionized water, it is heated to 76 DEG C under mechanical stirring, then by rare HNO3Solution and NaAlO2Solution continuously and flows plastic with 5��20L/min flow velocity, keeps temperature of reaction, and stablizes neutralizer pH7.6.
Start first time variation after (4) 20 minutes, first add NaAlO2PH is controlled 10��10.5 by solution, then stops to add NaAlO2Solution-stabilized 10��20min, then add HNO3PH is controlled 3��4 by solution, then stops to add HNO3Solution-stabilized 10��20min, so alternately a circulation is once calculated in variation.
(5) repeating above-mentioned circulation 3 times, neutralization terminates, and reaction end pH is stabilized in 7.6, then carries out aging, and digestion time controls at 38min.
(6) the liquid binder after aging is pumped into plate-and-frame filter press, then repeatedly washs with the water of temperature 48 DEG C, until Na2Till O content is qualified.
(7) wet cake after washing being placed in drying room and is dried, temperature controls at 100��120 DEG C, and pseudo-boehmite igloss controls 31%.
(8) dried filter cake is pulverized, and smashing fineness is at 400 orders.
Embodiment 4 comparative example
According to the step of embodiment 4, the difference is that the NaAlO in step (1)2Strength of solution is adjusted to 400g/L; (2) the rare HNO in3Strength of solution is adjusted to 40%, records sample data in table 1.
Table 1 example analytical data.
Claims (8)
1. a large pore volume, the preparation method of high viscosity pseudo-boehmite, it is characterised in that, comprise the following steps:
(1) by NaOH and Al (OH)3Mass concentration is counted as 50��300g/L, causticity factor alpha preparing still is made into taking aluminum oxidek, i.e. NaAlO2Na in solution2The substance withdrawl syndrome of O and Al2O3The ratio of substance withdrawl syndrome, be the NaAlO of 0.8��1.02Solution;
Under mechanical stirring, (2) by dense HNO3Slowly add in the dilution trap that deionized water is housed, it is made into the HNO of concentration 10-40%3Solution;
(3) in synthesis reactor, first add a certain amount of deionized water, it is heated to 60-100 DEG C under mechanical stirring, then by rare HNO3Solution and NaAlO2Solution continuously and flows plastic with 5��20L/min flow velocity, keeps temperature of reaction, and stablizes neutralizer pH6��9;
(4) start first time variation after spending 20 minutes, first add NaAlO2PH is controlled 10��10.5 by solution, then stops to add NaAlO2Solution-stabilized 10��20min, then add HNO3PH is controlled 3��4 by solution, then stops to add HNO3Solution-stabilized 10��20min, so alternately variation is once a circulation;
(5) circulating 2��6 times in repeating step 4, neutralization terminates, and reaction end pH is stabilized in 6��9, then carries out aging, and digestion time controls at 20��60min;
(6) the liquid binder after aging is pumped into plate-and-frame filter press, then repeatedly washs with the water of temperature 30��60 DEG C, until Na2Till O content is qualified;
(7) wet cake after washing being placed in drying room and is dried, temperature controls at 100��120 DEG C, and pseudo-boehmite igloss controls 20��40%;
(8) dried filter cake is pulverized, it is desired to fineness is at 320��600 orders.
2. large pore volume according to claim 1, the preparation method of high viscosity pseudo-boehmite, it is characterised in that, NaAlO in described step (1)2Strength of solution is 100��250g/L.
3. large pore volume according to claim 1, the preparation method of high viscosity pseudo-boehmite, it is characterised in that, rare HNO in described step (2)3Strength of solution controls 15��30%.
4. large pore volume according to claim 1, the preparation method of high viscosity pseudo-boehmite, it is characterised in that, in described step (3), neutralizer temperature controls at 70��80 DEG C, and neutralizer pH controls 7��8.
5. large pore volume according to claim 1, the preparation method of high viscosity pseudo-boehmite, it is characterised in that, in described step (5), pH number of oscillations controls at 3-5 time, and digestion time is 30��45min.
6. large pore volume according to claim 1, the preparation method of high viscosity pseudo-boehmite, it is characterised in that, in described step (6), washings temperature controls at 40��50 DEG C.
7. large pore volume according to claim 1, the preparation method of high viscosity pseudo-boehmite, it is characterised in that, described step (7) is intended rich diaspore igloss and controls 28��32%.
8. large pore volume according to claim 1, the preparation method of high viscosity pseudo-boehmite, it is characterised in that, described large pore volume, the technical parameter of high viscosity pseudo-boehmite is: molten index >=99% of glue, Kong Rong >=0.80mL/g, specific surface area >=200m2/ g, can and radius >=400, hole.
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| CN108910925B (en) * | 2018-09-11 | 2021-02-09 | 淄博齐茂催化剂有限公司 | Preparation method of pseudo-boehmite |
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| 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 |
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