CN105600812B - Method for preparing high-viscosity and superfine pseudo boehmite coating adhesive - Google Patents
Method for preparing high-viscosity and superfine pseudo boehmite coating adhesive Download PDFInfo
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- CN105600812B CN105600812B CN201510980993.8A CN201510980993A CN105600812B CN 105600812 B CN105600812 B CN 105600812B CN 201510980993 A CN201510980993 A CN 201510980993A CN 105600812 B CN105600812 B CN 105600812B
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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
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
- C01F7/142—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent with carbon dioxide
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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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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Abstract
The invention discloses a method for preparing high-viscosity and superfine pseudo boehmite coating adhesive. The method comprises the steps: CO2 gas and a NaAlO2 solution can form adhesive in a bell-jar type rotary filling continuous gas-liquid reactor, the NaAlO2 solution is evenly sprayed down from the upper portion, CO2 gas evenly enters from the lower portion, and is mixed reversely with the NaAlO2 solution and has a chemical reaction with the NaAlO2 solution under the condition of certain temperature and pH; then a reaction product is pressed into a plate-and-frame filter press by a pressing pump after aging certain time in a washing kettle, and is washed for a plurality of times, and the pseudo boehmite coating adhesive (aluminum carbonate adhesive) is obtained; then the adhesive is dried in a drying room and pulverized in a pulverizer. In this manner, the method prepares the high-viscosity and superfine pseudo boehmite coating adhesive with the cheap CO2 gas and NaAlO2 solution as the raw materials, the primary particle size of the product is 10-60 nm, the pore volume is larger than 1.0cm <3>/g, the specific surface area is larger than 600m<2>/g, and the gelation index reaches 99% or more; the method has the advantages of low production cost, good performance and high market competitiveness.
Description
Technical field
The present invention relates to a kind of fabricating technology of boehmite film glue, and in particular to a kind of high viscosity, ultra-fine
The preparation method of boehmite film glue.
Background technology
Boehmite also known as monohydrate alumina, false boehmite, English name：Pseudo Bohemite, point
Minor：Al2O3·n H2O (1 ＜ n ＜ 3), nontoxic, tasteless, odorless, white colloidal shape（Wet product）Or powder（Dry product）, crystalline phase is pure
Degree is high, peptization performance is good, and caking property is strong, with specific surface it is high, pore volume is big the features such as, it contains aquosity for thixotropy gel.
Boehmite is widely used in purifying vehicle exhaust, industrial tail gas net as efficient plastics and binding agent
Change, printing paper film, coating, high-grade ceramic, effective catalyst and catalyst carrier, cosmetics filler and inorganic material film etc..It is main
It is related to the industries such as petrochemical industry, chemical fertilizer, papermaking, coating, environmental protection, space division, medicine, daily use chemicals, artificial artificial limb, Aero-Space, is
One class has the new material of broad based growth future.
It is to utilize CO that carbonizatin method prepares boehmite film glue2In gas and NaA1O2Solution is preparing.The spy of the method
Point is can be with reference to aluminium manufacturer's actual conditions, using intermediate product NaAlO2Solution and CO2Waste gas, as reaction raw materials, is that cost is minimum
Process route.All improved a lot than before using product purity, specific surface area, pore volume, peptization index obtained in the method,
But can not be with other production methods（As acid precipitation method, subtract the precipitation method, alkyl aluminum hydrolysis method）The product of preparation is in technical indicator
Compare., typically in 90 below %, specific surface area is in 150 ~ 450 m for the boehmite peptization index that particularly prepared by the method2/
G or so, the cm of pore volume 0.15 ~ 0.83/ g, it is difficult to improve again, significantly limit the promotion and application of carbonizatin method.And peptization index
Height reflect the quality of boehmite caking property, caking property is better, and plastics viscosity is higher, stickup just firmly, no
Easily scaling.
The content of the invention
The invention mainly solves the technical problem of providing a kind of high viscosity, the preparation side of ultra-fine boehmite film glue
Method, with cheap CO2Gas and NaAlO2Solution is raw material, prepares high viscosity, ultra-fine boehmite, and its product is once
Particle diameter is 10～60 nm, and pore volume is more than 1.0 cm3/ g, specific surface area is more than 600 m2/ g, peptization index reach 99 % with
On, with low production cost, performance is good, the strong advantage of the market competitiveness.
To solve above-mentioned technical problem, one aspect of the present invention is：There is provided a kind of high viscosity, ultra-fine plan thin
The preparation method of diaspore film glue, it is characterised in that comprise the following steps：
Step one, by NaOH and Al (OH)3It is made in kettle is prepared with aluminum oxide and counts mass concentration as 10～200 g/L,
Causticity factor alphak（NaAlO2Na in solution2The substance withdrawl syndrome and Al of O2O3Substance withdrawl syndrome ratio）For 0.70～1.15
NaAlO2Solution；
Step 2, by CO2Storage pot liquid CO2Decompression is changed into gaseous state and sends into gas buffer tank, keeps gas pressure to exist
0.2～0.5 MPa；
Step 3, unlatching bell-jar rotation filler continuous gas liquid reactions device, by the NaAlO for preparing2Solution is with 4～25 L/
Min flow velocitys rotate filler continuous gas liquid reactions device top feed pipe and are transported in rotation inner core, while from below by bell-jar
It is passed through CO2Gas, and certain gas flow is kept, control reacting liquid pH value 7～11；
Step 4, unlatching bell-jar rotation filler continuous gas liquid reactions device chuck cooling water, by adjusting cooling water flow,
Controlling reaction temperature makes gas be fully contacted generation chemical reaction with solution at 15～75 DEG C；
Step 5, reactant liquor importing washing kettle is carried out it is aging, aging temperature control at 30～100 DEG C, ageing time control
System is in 30～120 min；
Step 6, will be aging after liquid binder be pumped into plate and frame filter press, then with the water that temperature is 30～60 DEG C
Repeatedly washed, until Na2Till O content is qualified；
Step 7, the wet cake after washing is placed in drying room it is dried, temperature control is intended thin at 100～120 DEG C
Diaspore igloss is controlled in 20～35 %；
Step 8, dried filter cake are crushed, and fineness is 800～1000 mesh；
In a preferred embodiments of the invention, the step（1）Middle NaAlO2Solution concentration is controlled in 50～150 g/L,
Causticity coefficient is controlled 0.85～0.95.
In a preferred embodiments of the invention, the step（3）Middle NaAlO2Solution flow rate is controlled in 8～15 L/min,
Reacting liquid pH value is controlled 9～10.
In a preferred embodiments of the invention, the step（4）Middle reaction temperature is controlled at 30～60 DEG C.
In a preferred embodiments of the invention, the step（5）The control of middle aging temperature at 50～80 DEG C, ageing time
For 45～100 min.
In a preferred embodiments of the invention, the step（7）Middle boehmite igloss is controlled in 25～30 %.
The invention has the beneficial effects as follows：A kind of high viscosity of the present invention, the preparation method of ultra-fine boehmite film glue, with
Cheap CO2Gas and NaAlO2Solution is raw material, prepares high viscosity, ultra-fine boehmite.The primary particle grain of its product
Footpath is 10～60 nm, and pore volume is more than 1.0 cm3/ g, specific surface area is more than 600 m2/ g, peptization index reaches 99 more than %, has
Low production cost, performance is good, the strong advantage of the market competitiveness.
Specific embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described enforcement
Example is only a part of embodiment of the present invention, rather than the embodiment of whole.Based on the embodiment in the present invention, this area is common
All other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.
Embodiment 1：
The preparation method of a kind of high viscosity, ultra-fine boehmite film glue, specifically includes following steps：
Step one, by NaOH and Al (OH)3It is made in kettle is prepared with aluminum oxide and counts mass concentration as 60 g/L, causticity system
Number αk（NaAlO2Na in solution2The substance withdrawl syndrome and Al of O2O3Substance withdrawl syndrome ratio）For 0.88 NaAlO2It is molten
Liquid；
Step 2, by CO2Storage pot liquid CO2Decompression is changed into gaseous state and sends into gas buffer tank, keeps gas pressure to exist
0.3 MPa;
Step 3, unlatching bell-jar rotation filler continuous gas liquid reactions device, by the NaAlO for preparing2Solution is with 10 L/min
Flow velocity rotates filler continuous gas liquid reactions device top feed pipe and is transported in rotation inner core, while being passed through from below by bell-jar
CO2Gas, and certain gas flow is kept, control reacting liquid pH value 9.0;
Step 4, unlatching bell-jar rotation filler continuous gas liquid reactions device chuck cooling water, by adjusting cooling water flow,
Controlling reaction temperature makes gas be fully contacted generation chemical reaction with solution at 45 DEG C;
Step 5, reactant liquor importing washing kettle is carried out aging, at 45 DEG C, ageing time control exists for aging temperature control
50 min;
Step 6, will be aging after liquid binder be pumped into plate and frame filter press, then carried out with the water of 40 DEG C of temperature many
Secondary washing, until Na2Till O content is qualified;
Step 7, the wet cake after washing is placed in drying room it is dried, temperature control is intended thin at 100～120 DEG C
Diaspore igloss is controlled in 26 %;
Step 8, dried filter cake are crushed, it is desirable to which fineness is in 800 mesh.
The comparative example of embodiment 1
The step of according to embodiment 1, except that filler continuous gas liquid reactions device is rotated without bell-jar, but with general
Logical carbonization reactor, measures sample data and is shown in Table 1.
Embodiment 2：
The present embodiment provides a kind of high viscosity, the preparation method of ultra-fine boehmite film glue, specifically includes following step
Suddenly：
Step one, by NaOH and Al (OH)3It is made in kettle is prepared with aluminum oxide and counts mass concentration as 100 g/L, causticity
Factor alphak（NaAlO2Na in solution2The substance withdrawl syndrome and Al of O2O3Substance withdrawl syndrome ratio）For 0.9 NaAlO2It is molten
Liquid;
Step 2, by CO2Storage pot liquid CO2Decompression is changed into gaseous state and sends into gas buffer tank, keeps gas pressure to exist
0.3 MPa;
Step 3, unlatching bell-jar rotation filler continuous gas liquid reactions device, by the NaAlO for preparing2Solution is with 15 L/min
Flow velocity rotates filler continuous gas liquid reactions device top feed pipe and is transported in rotation inner core, while being passed through from below by bell-jar
CO2Gas, and certain gas flow is kept, control reacting liquid pH value 9.5;
Step 4, unlatching bell-jar rotation filler continuous gas liquid reactions device chuck cooling water, by adjusting cooling water flow,
Controlling reaction temperature makes gas be fully contacted generation chemical reaction with solution at 50 DEG C;
Step 5, reactant liquor importing washing kettle is carried out aging, at 55 DEG C, ageing time control exists for aging temperature control
75 min;
Step 6, will be aging after liquid binder be pumped into plate and frame filter press, then carried out with the water of 40 DEG C of temperature many
Secondary washing, until Na2Till O content is qualified;
Step 7, the wet cake after washing is placed in drying room it is dried, temperature control is intended thin at 100～120 DEG C
Diaspore igloss is controlled in 28 %;
Step 8, dried filter cake are crushed, it is desirable to which fineness is in 800 mesh.
The comparative example of embodiment 2
The step of according to embodiment 2, except that step（3）In, it is not to be continuously added to NaAlO2Solution, but one
Secondary property puts into a certain amount of NaAlO2Solution, or else it is open close enter CO2 gases, make pH value constantly decrease up to pH value reach 9.5 react
Terminate, measure sample data and be shown in Table 1.
Embodiment 3：
The present embodiment provides a kind of high viscosity, the preparation method of ultra-fine boehmite film glue, specifically includes following step
Suddenly：
Step one, by NaOH and Al (OH)3It is made in kettle is prepared with aluminum oxide and counts mass concentration as 120 g/L, causticity
Factor alpha αk（NaAlO2Na in solution2The substance withdrawl syndrome and Al of O2O3Substance withdrawl syndrome ratio）For 0.92 NaAlO2
Solution;
Step 2, by CO2Storage pot liquid CO2Decompression is changed into gaseous state and sends into gas buffer tank, keeps gas pressure to exist
0.3MPa;
Step 3, unlatching bell-jar rotation filler continuous gas liquid reactions device, by the NaAlO for preparing2Solution is with 12 L/min
Flow velocity rotates filler continuous gas liquid reactions device top feed pipe and is transported in rotation inner core, while being passed through from below by bell-jar
CO2Gas, and certain gas flow is kept, control reacting liquid pH value 9.8;
Step 4, unlatching bell-jar rotation filler continuous gas liquid reactions device chuck cooling water, by adjusting cooling water flow,
Controlling reaction temperature makes gas be fully contacted generation chemical reaction with solution at 55 DEG C;
Step 5, reactant liquor importing washing kettle is carried out aging, at 60 DEG C, ageing time control exists for aging temperature control
85 min;
Step 6, will be aging after liquid binder be pumped into plate and frame filter press, then carried out with the water of 40 DEG C of temperature many
Secondary washing, until Na2Till O content is qualified;
Step 7, the wet cake after washing is placed in drying room it is dried, temperature control is intended thin at 100～120 DEG C
Diaspore igloss is controlled in 29 %;
Step 8, dried filter cake are crushed, it is desirable to which fineness is in 800 mesh.
The comparative example of embodiment 3
The step of according to embodiment 3, except that step（1）NaAlO2Concentration of polymer solution be 200 g/L, causticity system
Number is 1.15；Step（3）Middle NaAlO2Solution flow rate be 25 L/min, reacting liquid pH value 11；Step（4）Middle reaction temperature 75
℃；Step（5）100 DEG C of middle aging temperature, the min of ageing time 120；Step（7）Middle boehmite igloss is controlled in 30 %.
Measure sample data and be shown in Table 1.
Embodiment 4：
The present embodiment provides a kind of high viscosity, the preparation method of ultra-fine boehmite film glue, specifically includes following step
Suddenly：
Step one, by NaOH and Al (OH)3It is made in kettle is prepared with aluminum oxide and counts mass concentration as 50 g/L, causticity
Factor alphak（NaAlO2Na in solution2The substance withdrawl syndrome and Al of O2O3Substance withdrawl syndrome ratio）For 0.85 NaAlO2It is molten
Liquid;
Step 2, by CO2Storage pot liquid CO2Decompression is changed into gaseous state and sends into gas buffer tank, keeps gas pressure to exist
0.3 MPa;
Step 3, unlatching bell-jar rotation filler continuous gas liquid reactions device, by the NaAlO for preparing2Solution is flowed with 8 L/min
Speed rotates filler continuous gas liquid reactions device top feed pipe and is transported in rotation inner core, while being passed through from below by bell-jar
CO2Gas, and certain gas flow is kept, control reacting liquid pH value 9.0;
Step 4, unlatching bell-jar rotation filler continuous gas liquid reactions device chuck cooling water, by adjusting cooling water flow,
Controlling reaction temperature makes gas be fully contacted generation chemical reaction with solution at 35 DEG C;
Step 5, reactant liquor importing washing kettle is carried out aging, at 50 DEG C, ageing time control exists for aging temperature control
45 min;
Step 6, will be aging after liquid binder be pumped into plate and frame filter press, then carried out with the water of 40 DEG C of temperature many
Secondary washing, until Na2Till O content is qualified;
Step 7, the wet cake after washing is placed in drying room it is dried, temperature control is intended thin at 100～120 DEG C
Diaspore igloss is controlled in 25 %;
Step 8, dried filter cake are crushed, it is desirable to which fineness is in 800 mesh.
The comparative example of embodiment 4
The step of according to embodiment 4, except that step（1）NaAlO2Concentration of polymer solution be 10 g/L, causticity system
Number is 0.70；Step（3）Middle NaAlO2Solution flow rate be 4 L/min, reacting liquid pH value 7；Step（4）15 DEG C of middle reaction temperature；
Step（5）30 DEG C of middle aging temperature, the min of ageing time 30；Step（7）Middle boehmite igloss is controlled in 20 %.Measure
Sample data is shown in Table 1.
The example analyze data of table 1.
Claims (6)
1. a kind of high viscosity, the preparation method of ultra-fine boehmite film glue, it is characterised in that comprise the following steps：
Step one, by NaOH and Al (OH)3It is made in kettle is prepared with aluminum oxide and counts mass concentration as 10～200 g/L, causticity system
Number αkThat is NaAlO2Na in solution2The substance withdrawl syndrome and Al of O2O3The ratio of substance withdrawl syndrome be 0.70～1.15
NaAlO2Solution；
Step 2, by CO2Storage pot liquid CO2Decompression is changed into gaseous state and sends into gas buffer tank, keep gas pressure 0.2～
0.5 MPa；
Step 3, unlatching bell-jar rotation filler continuous gas liquid reactions device, by the NaAlO for preparing2Solution is flowed with 4～25 L/min
Speed rotates filler continuous gas liquid reactions device top feed pipe and is transported in rotation inner core, while being passed through from below by bell-jar
CO2Gas, and certain gas flow is kept, control reacting liquid pH value 7～11；
Step 4, unlatching bell-jar rotation filler continuous gas liquid reactions device chuck cooling water, by adjusting cooling water flow, control
Reaction temperature makes gas be fully contacted generation chemical reaction with solution at 15～75 DEG C；
Step 5, reactant liquor importing washing kettle is carried out aging, at 30～100 DEG C, ageing time control exists for aging temperature control
30～120 min；
Step 6, will be aging after liquid binder be pumped into plate and frame filter press, then carried out with the water that temperature is 30～60 DEG C
Repeatedly washing, until Na2Till O content is qualified；
Step 7, the wet cake after washing is placed in drying room it is dried, temperature control intends thin water aluminium at 100～120 DEG C
Stone igloss is controlled in 20～35 %；
Step 8, dried filter cake are crushed, and fineness is 800～1000 mesh.
2. high viscosity according to claim 1, the preparation method of ultra-fine boehmite film glue, it is characterised in that institute
State NaAlO in step one2Solution concentration control is controlled 0.85～0.95 in 50～150 g/L, causticity coefficient.
3. high viscosity according to claim 1, the preparation method of ultra-fine boehmite film glue, it is characterised in that institute
State NaAlO in step 32Solution flow rate control is controlled 9～10 in 8～15 L/min, reacting liquid pH value.
4. high viscosity according to claim 1, the preparation method of ultra-fine boehmite film glue, it is characterised in that institute
State reaction temperature in step 4 to control at 30～60 DEG C.
5. high viscosity according to claim 1, the preparation method of ultra-fine boehmite film glue, it is characterised in that institute
, at 50～80 DEG C, ageing time is 45～100 min to state aging temperature control in step 5.
6. high viscosity according to claim 1, the preparation method of ultra-fine boehmite film glue, it is characterised in that institute
State boehmite igloss in step 7 to control in 25～30 %.
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| CN110655096B (en) * | 2019-10-21 | 2022-01-14 | 湖南慧璟新材料有限公司 | Preparation method of pseudo-boehmite |
| CN113893795B (en) * | 2021-10-14 | 2023-04-25 | 中北大学 | Continuous aging device and method in pseudo-boehmite preparation process |
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| JP2004300018A (en) * | 2003-03-14 | 2004-10-28 | Nissan Chem Ind Ltd | Method of manufacturing acidic aqueous alumina sol |
| CN1752005A (en) * | 2005-10-25 | 2006-03-29 | 湘潭大学 | Preparation method of ultrafine active aluminium oxide |
| CN100548884C (en) * | 2007-11-09 | 2009-10-14 | 中国铝业股份有限公司 | The preparation method of pseudo-boehmite |
| CN103145161B (en) * | 2013-01-08 | 2015-04-01 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | Method for preparing pseudo-boehmite co-preparation white carbon black by coal gangue |
| CN103449484B (en) * | 2013-08-23 | 2015-07-08 | 中国铝业股份有限公司 | Method for continuously producing pseudoboehmite |
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