WO2023246315A1 - Preparation method for pseudo-boehmite with high specific surface area - Google Patents
Preparation method for pseudo-boehmite with high specific surface area Download PDFInfo
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- WO2023246315A1 WO2023246315A1 PCT/CN2023/091717 CN2023091717W WO2023246315A1 WO 2023246315 A1 WO2023246315 A1 WO 2023246315A1 CN 2023091717 W CN2023091717 W CN 2023091717W WO 2023246315 A1 WO2023246315 A1 WO 2023246315A1
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- boehmite
- surface area
- specific surface
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- solution
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- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000011148 porous material Substances 0.000 claims abstract description 22
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 18
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 18
- 239000011734 sodium Substances 0.000 claims abstract description 18
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- JTXUVYOABGUBMX-UHFFFAOYSA-N didodecyl hydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(=O)OCCCCCCCCCCCC JTXUVYOABGUBMX-UHFFFAOYSA-N 0.000 claims abstract description 8
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 36
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical group [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 9
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 9
- 239000001099 ammonium carbonate Substances 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 5
- CXRFDZFCGOPDTD-UHFFFAOYSA-M Cetrimide Chemical compound [Br-].CCCCCCCCCCCCCC[N+](C)(C)C CXRFDZFCGOPDTD-UHFFFAOYSA-M 0.000 claims description 4
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 230000032683 aging Effects 0.000 abstract 1
- 239000012295 chemical reaction liquid Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000004523 catalytic cracking Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- -1 Aluminum alkoxide Chemical class 0.000 description 3
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 3
- 229910001388 sodium aluminate Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- NGPZJQXXJCDBDS-UHFFFAOYSA-N dodecane-1-sulfonic acid;sodium Chemical group [Na].CCCCCCCCCCCCS(O)(=O)=O NGPZJQXXJCDBDS-UHFFFAOYSA-N 0.000 description 2
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- LDMOEFOXLIZJOW-UHFFFAOYSA-N 1-dodecanesulfonic acid Chemical compound CCCCCCCCCCCCS(O)(=O)=O LDMOEFOXLIZJOW-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- 238000005216 hydrothermal crystallization Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 229910006636 γ-AlOOH Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
- C01P2006/16—Pore diameter
Definitions
- the invention belongs to the technical field of catalyst carriers, and specifically relates to a method for preparing high specific surface area pseudo-boehmite.
- Catalysts for catalytic cracking are mainly composed of active components and catalyst carriers. Catalysts for catalytic cracking were mainly studied in the past by modifying molecular sieves to find active components with better activity and high catalytic efficiency. In recent years, with the incorporation of heavy oil, residual oil and other macromolecules into catalytic cracking raw materials, people have The research center has shifted to finding macroporous carrier materials with high specific surface area, large pore volume, and uniform distribution of surface acidic sites.
- Pseudo-boehmite is also called pseudo-boehmite and pseudo-boehmite.
- the finished product is a white, non-toxic, odorless powder with a spatial network structure, so it has a large specific surface area, pore volume and average pore diameter.
- Pseudo-boehmite is mainly used as catalyst, binder and carrier in the petrochemical industry.
- the main methods for preparing pseudo-boehmite are: (1) Aluminum alkoxide method. Aluminum reacts with alcohol to form aluminum alkoxide, which is then reduced to aldehyde and then transformed into a new aluminum alkoxide. It is hydrolyzed to obtain high-purity pseudo-boehmite. Preparation by this method It is complicated and the pore size of the obtained product is small, which cannot meet the needs of catalytic cracking. (2) Acid method, a preparation method using aluminum salt and alkalinity as raw materials. The process of preparing pseudo-boehmite by this method is simple and the raw materials are easily available. However, the reaction conditions of this method are difficult to control and the product quality is likely to be unstable.
- the object of the present invention is to provide a method for preparing high specific surface area pseudo-boehmite.
- a method for preparing high specific surface area pseudo-boehmite following the following steps:
- step (3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry.
- the amount of water added in step (1) is 10-25% of the reactor volume.
- the concentration of the sodium metaaluminate solution is 30-120gAl 2 O 3 /L, and the flow rate added to the reactor is 15-50 mL/min.
- the surfactant is a mixture of di(dodecyl)phosphate and tetradecyltrimethylammonium bromide in a mass ratio of 1:1.
- the surfactant includes an active component and a co-surfactant, the active component is sodium dodecyl sulfonate, the co-surfactant is n-amyl alcohol, and the mass ratio is 1:1.
- the concentration of the surfactant solution is 0.05-0.5g/mL, and the flow rate added to the reactor is 5-10mL/min.
- the pore expanding agent is ammonium bicarbonate and/or urea.
- the concentration of the pore expander solution is 0.1-0.5g/mL, and the flow rate added to the reactor is 2-5mL/min.
- the drying temperature in step (3) is 100-150°C, and the drying time is 6-10h.
- the pseudo-boehmite prepared by the present invention has a high specific surface area, and the surfactants di(dodecyl) phosphate, tetradecyltrimethylammonium bromide and dodecyl sulfonic acid
- the combined use of sodium and n-pentanol increases the specific surface area and pore size of the product, and the pore size distribution of the produced product is uniform.
- a method for preparing high specific surface area pseudo-boehmite following the following steps:
- step (3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 120°C and the drying time is 8 hours.
- a method for preparing high specific surface area pseudo-boehmite following the following steps:
- the concentration of the sodium aluminate solution is 35gAl 2 O 3 /L, and the flow rate added to the reactor is 18mL/min;
- the surfactant includes an active component and a co-surfactant, and the active component is dodecyl sulfonic acid Sodium, the co-surfactant is n-amyl alcohol, and the mass ratio is 1:1;
- the concentration of the surfactant solution is 0.1g/mL, and the flow rate added to the reactor is 5mL/min;
- the concentration of the urea solution is 0.1 g/mL, the flow rate added to the reactor is 2mL/min;
- step (3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 100°C and the drying time is 10 hours.
- a method for preparing high specific surface area pseudo-boehmite following the following steps:
- step (3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 150°C and the drying time is 6 hours.
- a method for preparing high specific surface area pseudo-boehmite following the following steps:
- step (3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 120°C and the drying time is 8 hours.
- a method for preparing high specific surface area pseudo-boehmite following the following steps:
- step (3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 120°C and the drying time is 8 hours.
- a method for preparing high specific surface area pseudo-boehmite following the following steps:
- step (3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 100°C and the drying time is 10 hours.
- a method for preparing high specific surface area pseudo-boehmite following the following steps:
- the concentration of the sodium aluminate solution is 35gAl 2 O 3 /L, and the flow rate added to the reactor is 18mL/min;
- the surfactant includes an active component and a co-surfactant, and the active component is dodecyl sulfonic acid Sodium, the co-surfactant is n-amyl alcohol, and the mass ratio is 1:1;
- the concentration of the surfactant solution is 0.1g/mL, and the flow rate added to the reactor is 5mL/min;
- the concentration of the urea solution is 0.1 g/mL, the flow rate added to the reactor is 2mL/min;
- step (3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 100°C and the drying time is 10 hours.
- the pseudoboehmite prepared in Examples 1-3 and Comparative Examples 1-4 was selected as the sample to be tested.
- the pore structure of the sample was measured using the Autosorb-6B physical adsorption instrument produced by Quantachrome Company in the United States.
- the pore structure of the test sample was weighed about 0.05g of the sample to be tested and placed in a specific sample tube, and degassed and pretreated at 300°C in a vacuum environment. 8h, remove water and impurities.
- the adsorption-desorption analysis was carried out at 77K liquid nitrogen temperature.
- the specific surface area, pore volume and average pore diameter were calculated using the BET and BJH equations respectively. The results are shown in Table 1.
Abstract
Disclosed in the present invention is a preparation method for a pseudo-boehmite with a high specific surface area. The preparation method comprises: firstly, adding water to a reactor, heating same to 55-75ºC, and then adding a sodium metaaluminate solution, a surfactant solution and a pore-enlarging agent solution for reaction; adjusting the pH of the reaction liquid to 7.5-9.0 with ammonia water, setting the water bath temperature to be 85-95ºC, aging same, and stirring same for 1-3 h; and finally, separating the obtained materials, and filtering and drying the obtained slurry to obtain a pseudo-boehmite. The pseudo-boehmite prepared in the present invention has a high specific surface area. By means of the combined use of di(dodecyl)phosphate and ammonium tetradecyl trimethyl bromide surfactants and of sodium dodecyl sulfonate and n-pentanol surfactants, the specific surface area and the pore diameter of the product are increased, and the prepared product has a uniform pore diameter distribution.
Description
本发明属于催化剂载体技术领域，具体涉及一种高比表面积拟薄水铝石制备方法。The invention belongs to the technical field of catalyst carriers, and specifically relates to a method for preparing high specific surface area pseudo-boehmite.
催化裂化的催化剂主要由活性组分和催化剂载体两方面组成。催化裂化的催化剂在过去主要进行分子筛改性研究，寻找活性较好，催化效率高的活性组分为主，近年来随着将重油、渣油等大分子掺入到催化裂化原料中，使得人们的研究中心转移到寻找具有高比表面积、大孔体积、表面酸性位点分布均匀的大孔载体材料上来。Catalysts for catalytic cracking are mainly composed of active components and catalyst carriers. Catalysts for catalytic cracking were mainly studied in the past by modifying molecular sieves to find active components with better activity and high catalytic efficiency. In recent years, with the incorporation of heavy oil, residual oil and other macromolecules into catalytic cracking raw materials, people have The research center has shifted to finding macroporous carrier materials with high specific surface area, large pore volume, and uniform distribution of surface acidic sites.
拟薄水铝石也称假一水软铝石、假勃姆石，成品为白色无毒、无味的粉末，具有空间网状结构，因而具有较大的比表面积、孔体积和平均孔径。在石油化工行业中拟薄水铝石主要用作催化剂、粘结剂和载体。Pseudo-boehmite is also called pseudo-boehmite and pseudo-boehmite. The finished product is a white, non-toxic, odorless powder with a spatial network structure, so it has a large specific surface area, pore volume and average pore diameter. Pseudo-boehmite is mainly used as catalyst, binder and carrier in the petrochemical industry.
拟薄水铝石制备方法主要有：(1)醇铝法，铝和醇反应形成醇铝，然后还原成醛再转变为新的醇铝，水解得到高纯度拟薄水铝石，该方法制备复杂，得到的产物孔径小，不能满足催化裂化的需求。(2)酸法，以铝盐和碱性为原料的制备方法，此法制备拟薄水铝石过程简单，原料易得，但是该方法反应条件较难控制，容易造成产品质量不稳定。(3)碱法，以铝酸盐和酸性物质为原料，通过AlO2-和H+反应生成γ-AlOOH·nH2O，该方法制备得到的产物硬团聚明显，并且在碱性环境中偏铝酸钠容易生成三水铝石。水热合成法：是目前国内
外关注度较高的一种晶体制备方法，该方法通过控制反应条件调控产物的颗粒大小和形貌，有水热醇铝法、水热铝盐法、和水热晶化法等。这些方法制备得到的拟薄水铝石具有较高的结晶度，样品松散，孔径相对集中，但是该方法反应时间长，制备过程需要有机模板剂，成本高，反应条件控制难度大。The main methods for preparing pseudo-boehmite are: (1) Aluminum alkoxide method. Aluminum reacts with alcohol to form aluminum alkoxide, which is then reduced to aldehyde and then transformed into a new aluminum alkoxide. It is hydrolyzed to obtain high-purity pseudo-boehmite. Preparation by this method It is complicated and the pore size of the obtained product is small, which cannot meet the needs of catalytic cracking. (2) Acid method, a preparation method using aluminum salt and alkalinity as raw materials. The process of preparing pseudo-boehmite by this method is simple and the raw materials are easily available. However, the reaction conditions of this method are difficult to control and the product quality is likely to be unstable. (3) Alkali method, using aluminate and acidic substances as raw materials, generates γ-AlOOH·nH 2 O through the reaction of AlO 2- and H + . The product prepared by this method has obvious hard agglomeration, and tends to be unstable in an alkaline environment. Sodium aluminate easily forms gibbsite. Hydrothermal synthesis method: currently the most popular method in China A crystal preparation method that attracts a lot of external attention, this method regulates the particle size and morphology of the product by controlling the reaction conditions, including the hydrothermal aluminum alcoholate method, the hydrothermal aluminum salt method, and the hydrothermal crystallization method. The pseudoboehmite prepared by these methods has high crystallinity, loose samples, and relatively concentrated pore sizes. However, this method has a long reaction time, requires organic templates during the preparation process, is high in cost, and is difficult to control the reaction conditions.
发明内容Contents of the invention
本发明的目的在于提供一种高比表面积拟薄水铝石制备方法。The object of the present invention is to provide a method for preparing high specific surface area pseudo-boehmite.
一种高比表面积拟薄水铝石制备方法，按照如下步骤进行：A method for preparing high specific surface area pseudo-boehmite, following the following steps:
(1)在反应器中加入水，加热至55-75℃，然后加入偏铝酸钠溶液、表面活性剂溶液和扩孔剂溶液进行反应；(1) Add water to the reactor, heat to 55-75°C, then add sodium metaaluminate solution, surfactant solution and pore expander solution to react;
(2)氨水调节反应液pH至7.5-9.0，水浴温度为85-95℃，老化，搅拌1-3h；(2) Adjust the pH of the reaction solution to 7.5-9.0 with ammonia water, set the water bath temperature to 85-95°C, age, and stir for 1-3 hours;
(3)将步骤(2)所得物料进行分离，得到的浆液经过滤、干燥后得到拟薄水铝石。(3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry.
步骤(1)中所述水的加入量为反应器体积的10-25％。The amount of water added in step (1) is 10-25% of the reactor volume.
所述偏铝酸钠溶液浓度为30-120gAl2O3/L，加入反应器的流速为15-50mL/min。The concentration of the sodium metaaluminate solution is 30-120gAl 2 O 3 /L, and the flow rate added to the reactor is 15-50 mL/min.
所述表面活性剂为二(十二烷基)磷酸酯和十四烷基三甲基溴化铵按照质量比1：1混合的混合物。The surfactant is a mixture of di(dodecyl)phosphate and tetradecyltrimethylammonium bromide in a mass ratio of 1:1.
所述表面活性剂包括活性组分和助表面活性剂，所述活性组分为十二烷基磺酸钠，助表面活性剂为正戊醇，质量比为1：1。The surfactant includes an active component and a co-surfactant, the active component is sodium dodecyl sulfonate, the co-surfactant is n-amyl alcohol, and the mass ratio is 1:1.
所述表面活性剂溶液的浓度为0.05-0.5g/mL，加入反应器的流速
为5-10mL/min。The concentration of the surfactant solution is 0.05-0.5g/mL, and the flow rate added to the reactor is 5-10mL/min.
所述扩孔剂为碳酸氢铵和/或尿素。The pore expanding agent is ammonium bicarbonate and/or urea.
所述扩孔剂溶液的浓度为0.1-0.5g/mL，加入反应器的流速为2-5mL/min。The concentration of the pore expander solution is 0.1-0.5g/mL, and the flow rate added to the reactor is 2-5mL/min.
步骤(3)所述干燥温度为100-150℃，干燥时间为6-10h。The drying temperature in step (3) is 100-150°C, and the drying time is 6-10h.
本发明的有益效果：本发明制备的拟薄水铝石，比表面积高，表面活性剂二(十二烷基)磷酸酯和十四烷基三甲基溴化铵以及十二烷基磺酸钠和正戊醇的组合使用，增大产物的比表面积和孔径，并且制得的产物孔径分布均匀。Beneficial effects of the present invention: the pseudo-boehmite prepared by the present invention has a high specific surface area, and the surfactants di(dodecyl) phosphate, tetradecyltrimethylammonium bromide and dodecyl sulfonic acid The combined use of sodium and n-pentanol increases the specific surface area and pore size of the product, and the pore size distribution of the produced product is uniform.
为了便于理解本发明，下面将对本发明进行更全面的描述。但是，本发明可以以许多不同的形式来实现，并不限于本文所描述的实施例。相反地，提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。In order to facilitate an understanding of the invention, the invention will be described more fully below. However, the invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that a thorough understanding of the present disclosure will be provided.
实施例1Example 1
一种高比表面积拟薄水铝石制备方法，按照如下步骤进行：A method for preparing high specific surface area pseudo-boehmite, following the following steps:
(1)在反应器中加入水，加热至65℃，然后加入偏铝酸钠溶液、表面活性剂溶液和碳酸氢铵溶液进行反应；所述水的加入量为反应器体积的15％；所述偏铝酸钠溶液浓度为80gAl2O3/L，加入反应器的流速为30mL/min；所述表面活性剂为二(十二烷基)磷酸酯和十四烷基三甲基溴化铵按照质量比1：1混合的混合物；所述表面活性剂溶液的浓度为0.2g/mL，加入反应器的流速为7mL/min；所述碳酸氢铵溶液
的浓度为0.2g/mL，加入反应器的流速为3mL/min；(1) Add water to the reactor, heat it to 65°C, and then add sodium metaaluminate solution, surfactant solution and ammonium bicarbonate solution to react; the amount of water added is 15% of the reactor volume; The concentration of the sodium metaaluminate solution is 80gAl 2 O 3 /L, and the flow rate added to the reactor is 30mL/min; the surfactant is di(dodecyl) phosphate and tetradecyl trimethyl bromide. A mixture of ammonium mixed according to a mass ratio of 1:1; the concentration of the surfactant solution is 0.2g/mL, and the flow rate added to the reactor is 7mL/min; the ammonium bicarbonate solution The concentration is 0.2g/mL, and the flow rate added to the reactor is 3mL/min;
(2)氨水调节反应液pH至8.5，水浴温度为90℃，老化，搅拌2h；(2) Adjust the pH of the reaction solution to 8.5 with ammonia water, set the water bath temperature to 90°C, age, and stir for 2 hours;
(3)将步骤(2)所得物料进行分离，得到的浆液经过滤、干燥后得到拟薄水铝石；所述干燥温度为120℃，干燥时间为8h。(3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 120°C and the drying time is 8 hours.
实施例2Example 2
一种高比表面积拟薄水铝石制备方法，按照如下步骤进行：A method for preparing high specific surface area pseudo-boehmite, following the following steps:
(1)在反应器中加入水，加热至55℃，然后加入偏铝酸钠溶液、表面活性剂溶液和尿素溶液进行反应；所述水的加入量为反应器体积的12％；所述偏铝酸钠溶液浓度为35gAl2O3/L，加入反应器的流速为18mL/min；所述表面活性剂包括活性组分和助表面活性剂，所述活性组分为十二烷基磺酸钠，助表面活性剂为正戊醇，质量比为1：1；所述表面活性剂溶液的浓度为0.1g/mL，加入反应器的流速为5mL/min；所述尿素溶液的浓度为0.1g/mL，加入反应器的流速为2mL/min；(1) Add water to the reactor, heat it to 55°C, and then add sodium metaaluminate solution, surfactant solution and urea solution to react; the amount of water added is 12% of the reactor volume; The concentration of the sodium aluminate solution is 35gAl 2 O 3 /L, and the flow rate added to the reactor is 18mL/min; the surfactant includes an active component and a co-surfactant, and the active component is dodecyl sulfonic acid Sodium, the co-surfactant is n-amyl alcohol, and the mass ratio is 1:1; the concentration of the surfactant solution is 0.1g/mL, and the flow rate added to the reactor is 5mL/min; the concentration of the urea solution is 0.1 g/mL, the flow rate added to the reactor is 2mL/min;
(2)氨水调节反应液pH至7.8，水浴温度为85℃，老化，搅拌3h；(2) Adjust the pH of the reaction solution to 7.8 with ammonia water, set the water bath temperature to 85°C, age, and stir for 3 hours;
(3)将步骤(2)所得物料进行分离，得到的浆液经过滤、干燥后得到拟薄水铝石；所述干燥温度为100℃，干燥时间为10h。(3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 100°C and the drying time is 10 hours.
实施例3
Example 3
一种高比表面积拟薄水铝石制备方法，按照如下步骤进行：A method for preparing high specific surface area pseudo-boehmite, following the following steps:
(1)在反应器中加入水，加热至75℃，然后加入偏铝酸钠溶液、表面活性剂溶液和扩孔剂溶液进行反应；所述水的加入量为反应器体积的25％；所述偏铝酸钠溶液浓度为110gAl2O3/L，加入反应器的流速为40mL/min；所述表面活性剂为二(十二烷基)磷酸酯和十四烷基三甲基溴化铵按照质量比1：1混合的混合物；所述表面活性剂溶液的浓度为0.5g/mL，加入反应器的流速为10mL/min；所述扩孔剂为碳酸氢铵和尿素，质量比1：1；所述扩孔剂溶液的浓度为0.4g/mL，加入反应器的流速为4mL/min；(1) Add water to the reactor, heat it to 75°C, and then add sodium metaaluminate solution, surfactant solution and pore expander solution to react; the amount of water added is 25% of the reactor volume; The concentration of the sodium metaaluminate solution is 110gAl 2 O 3 /L, and the flow rate added to the reactor is 40 mL/min; the surfactants are di(dodecyl) phosphate and tetradecyl trimethyl bromide. A mixture of ammonium mixed according to a mass ratio of 1:1; the concentration of the surfactant solution is 0.5g/mL, and the flow rate added to the reactor is 10mL/min; the pore expander is ammonium bicarbonate and urea, with a mass ratio of 1 : 1; The concentration of the pore expander solution is 0.4g/mL, and the flow rate added to the reactor is 4mL/min;
(2)氨水调节反应液pH至9.0，水浴温度为95℃，老化，搅拌1h；(2) Adjust the pH of the reaction solution to 9.0 with ammonia water, set the water bath temperature to 95°C, age, and stir for 1 hour;
(3)将步骤(2)所得物料进行分离，得到的浆液经过滤、干燥后得到拟薄水铝石；所述干燥温度为150℃，干燥时间为6h。(3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 150°C and the drying time is 6 hours.
对比例1Comparative example 1
一种高比表面积拟薄水铝石制备方法，按照如下步骤进行：A method for preparing high specific surface area pseudo-boehmite, following the following steps:
(1)在反应器中加入水，加热至65℃，然后加入偏铝酸钠溶液、二(十二烷基)磷酸酯溶液和碳酸氢铵溶液进行反应；所述水的加入量为反应器体积的15％；所述偏铝酸钠溶液浓度为80gAl2O3/L，加入反应器的流速为30mL/min；所述二(十二烷基)磷酸酯溶液的浓度为0.2g/mL，加入反应器的流速为7mL/min；所述碳酸氢铵溶液的浓度为0.2g/mL，加入反应器的流速为3mL/min；
(1) Add water to the reactor, heat to 65°C, and then add sodium metaaluminate solution, di(dodecyl)phosphate solution and ammonium bicarbonate solution to react; the amount of water added is 15% of the volume; the concentration of the sodium metaaluminate solution is 80gAl 2 O 3 /L, and the flow rate added to the reactor is 30mL/min; the concentration of the di(dodecyl) phosphate solution is 0.2g/mL , the flow rate added to the reactor is 7mL/min; the concentration of the ammonium bicarbonate solution is 0.2g/mL, and the flow rate added to the reactor is 3mL/min;
(2)氨水调节反应液pH至8.5，水浴温度为90℃，老化，搅拌2h；(2) Adjust the pH of the reaction solution to 8.5 with ammonia water, set the water bath temperature to 90°C, age, and stir for 2 hours;
(3)将步骤(2)所得物料进行分离，得到的浆液经过滤、干燥后得到拟薄水铝石；所述干燥温度为120℃，干燥时间为8h。(3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 120°C and the drying time is 8 hours.
对比例2Comparative example 2
一种高比表面积拟薄水铝石制备方法，按照如下步骤进行：A method for preparing high specific surface area pseudo-boehmite, following the following steps:
(1)在反应器中加入水，加热至65℃，然后加入偏铝酸钠溶液、十四烷基三甲基溴化铵溶液和碳酸氢铵溶液进行反应；所述水的加入量为反应器体积的15％；所述偏铝酸钠溶液浓度为80gAl2O3/L，加入反应器的流速为30mL/min；所述表面活性剂溶液的浓度为0.2g/mL，加入反应器的流速为7mL/min；所述碳酸氢铵溶液的浓度为0.2g/mL，加入反应器的流速为3mL/min；(1) Add water to the reactor, heat to 65°C, then add sodium metaaluminate solution, tetradecyltrimethylammonium bromide solution and ammonium bicarbonate solution to react; the amount of water added is 15% of the volume of the reactor; the concentration of the sodium metaaluminate solution is 80gAl 2 O 3 /L, and the flow rate added to the reactor is 30mL/min; the concentration of the surfactant solution is 0.2g/mL, and the flow rate added to the reactor The flow rate is 7mL/min; the concentration of the ammonium bicarbonate solution is 0.2g/mL, and the flow rate added to the reactor is 3mL/min;
(2)氨水调节反应液pH至8.5，水浴温度为90℃，老化，搅拌2h；(2) Adjust the pH of the reaction solution to 8.5 with ammonia water, set the water bath temperature to 90°C, age, and stir for 2 hours;
(3)将步骤(2)所得物料进行分离，得到的浆液经过滤、干燥后得到拟薄水铝石；所述干燥温度为120℃，干燥时间为8h。(3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 120°C and the drying time is 8 hours.
对比例3Comparative example 3
一种高比表面积拟薄水铝石制备方法，按照如下步骤进行：A method for preparing high specific surface area pseudo-boehmite, following the following steps:
(1)在反应器中加入水，加热至55℃，然后加入偏铝酸钠溶液、表面活性剂溶液和尿素溶液进行反应；所述水的加入量为反应器体积
的12％；所述偏铝酸钠溶液浓度为35gAl2O3/L，加入反应器的流速为18mL/min；所述表面活性剂包括活性组分和助表面活性剂，所述活性组分为十二烷基磺酸钠，助表面活性剂为正戊醇，质量比为1：1；所述表面活性剂溶液的浓度为0.1g/mL，加入反应器的流速为5mL/min；所述尿素溶液的浓度为0.1g/mL，加入反应器的流速为2mL/min；(1) Add water to the reactor, heat it to 55°C, then add sodium metaaluminate solution, surfactant solution and urea solution to react; the amount of water added is the volume of the reactor 12%; the concentration of the sodium metaaluminate solution is 35gAl 2 O 3 /L, and the flow rate added to the reactor is 18mL/min; the surfactant includes an active component and a co-surfactant, and the active component is sodium dodecyl sulfonate, the co-surfactant is n-amyl alcohol, and the mass ratio is 1:1; the concentration of the surfactant solution is 0.1g/mL, and the flow rate added to the reactor is 5mL/min; so The concentration of the urea solution is 0.1g/mL, and the flow rate added to the reactor is 2mL/min;
(2)氨水调节反应液pH至7.8，水浴温度为85℃，老化，搅拌3h；(2) Adjust the pH of the reaction solution to 7.8 with ammonia water, set the water bath temperature to 85°C, age, and stir for 3 hours;
(3)将步骤(2)所得物料进行分离，得到的浆液经过滤、干燥后得到拟薄水铝石；所述干燥温度为100℃，干燥时间为10h。(3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 100°C and the drying time is 10 hours.
对比例4Comparative example 4
一种高比表面积拟薄水铝石制备方法，按照如下步骤进行：A method for preparing high specific surface area pseudo-boehmite, following the following steps:
(1)在反应器中加入水，加热至55℃，然后加入偏铝酸钠溶液、表面活性剂溶液和尿素溶液进行反应；所述水的加入量为反应器体积的12％；所述偏铝酸钠溶液浓度为35gAl2O3/L，加入反应器的流速为18mL/min；所述表面活性剂包括活性组分和助表面活性剂，所述活性组分为十二烷基磺酸钠，助表面活性剂为正戊醇，质量比为1：1；所述表面活性剂溶液的浓度为0.1g/mL，加入反应器的流速为5mL/min；所述尿素溶液的浓度为0.1g/mL，加入反应器的流速为2mL/min；(1) Add water to the reactor, heat it to 55°C, and then add sodium metaaluminate solution, surfactant solution and urea solution to react; the amount of water added is 12% of the reactor volume; The concentration of the sodium aluminate solution is 35gAl 2 O 3 /L, and the flow rate added to the reactor is 18mL/min; the surfactant includes an active component and a co-surfactant, and the active component is dodecyl sulfonic acid Sodium, the co-surfactant is n-amyl alcohol, and the mass ratio is 1:1; the concentration of the surfactant solution is 0.1g/mL, and the flow rate added to the reactor is 5mL/min; the concentration of the urea solution is 0.1 g/mL, the flow rate added to the reactor is 2mL/min;
(2)氨水调节反应液pH至7.8，水浴温度为85℃，老化，搅
拌3h；(2) Adjust the pH of the reaction solution to 7.8 with ammonia water, set the water bath temperature to 85°C, age, and stir Mix for 3 hours;
(3)将步骤(2)所得物料进行分离，得到的浆液经过滤、干燥后得到拟薄水铝石；所述干燥温度为100℃，干燥时间为10h。(3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry; the drying temperature is 100°C and the drying time is 10 hours.
实验例：Experimental example:
选取实施例1-3及对比例1-4制备的拟薄水铝石作为被检测样品。样品孔道结构测定采用美国Quantachrome公司生产的Autosorb-6B型物理吸附仪测，试样品的孔结构称取待测样品0.05g左右于特定的样品管中，抽真空环境下300℃脱气预处理8h，除去水和杂质。吸附-脱附分析在77K液氮温度条件下进行，比表面积、孔体积和平均孔径分别采用BET和BJH方程计算，其结果如表1所示。The pseudoboehmite prepared in Examples 1-3 and Comparative Examples 1-4 was selected as the sample to be tested. The pore structure of the sample was measured using the Autosorb-6B physical adsorption instrument produced by Quantachrome Company in the United States. The pore structure of the test sample was weighed about 0.05g of the sample to be tested and placed in a specific sample tube, and degassed and pretreated at 300°C in a vacuum environment. 8h, remove water and impurities. The adsorption-desorption analysis was carried out at 77K liquid nitrogen temperature. The specific surface area, pore volume and average pore diameter were calculated using the BET and BJH equations respectively. The results are shown in Table 1.
表1
注：*代表与实施例1相比，p<0.05；#代表与实施例2相比，p<0.05。 Table 1
Note: * represents p<0.05 compared with Example 1; # represents p<0.05 compared with Example 2.
注：*代表与实施例1相比，p<0.05；#代表与实施例2相比，p<0.05。 Table 1
Note: * represents p<0.05 compared with Example 1; # represents p<0.05 compared with Example 2.
Claims (9)
- 一种高比表面积拟薄水铝石制备方法，其特征在于，按照如下步骤进行：A method for preparing high specific surface area pseudo-boehmite, which is characterized by following the following steps:(1)在反应器中加入水，加热至55-75℃，然后加入偏铝酸钠溶液、表面活性剂溶液和扩孔剂溶液进行反应；(1) Add water to the reactor, heat to 55-75°C, then add sodium metaaluminate solution, surfactant solution and pore expander solution to react;(2)氨水调节反应液pH至7.5-9.0，水浴温度为85-95℃，老化，搅拌1-3h；(2) Adjust the pH of the reaction solution to 7.5-9.0 with ammonia water, set the water bath temperature to 85-95°C, age, and stir for 1-3 hours;(3)将步骤(2)所得物料进行分离，得到的浆液经过滤、干燥后得到拟薄水铝石。(3) Separate the material obtained in step (2), and obtain pseudo-boehmite after filtering and drying the obtained slurry.
- 根据权利要求1所述高比表面积拟薄水铝石制备方法，其特征在于，步骤(1)中所述水的加入量为反应器体积的10-25％。The method for preparing high specific surface area pseudo-boehmite according to claim 1, characterized in that the amount of water added in step (1) is 10-25% of the reactor volume.
- 根据权利要求1所述高比表面积拟薄水铝石制备方法，其特征在于，所述偏铝酸钠溶液浓度为30-120gAl2O3/L，加入反应器的流速为15-50mL/min。The method for preparing high specific surface area pseudo-boehmite according to claim 1, characterized in that the concentration of the sodium metaaluminate solution is 30-120gAl 2 O 3 /L, and the flow rate added to the reactor is 15-50 mL/min. .
- 根据权利要求1所述高比表面积拟薄水铝石制备方法，其特征在于，所述表面活性剂为二(十二烷基)磷酸酯和十四烷基三甲基溴化铵按照质量比1：1混合的混合物。The method for preparing high specific surface area pseudo-boehmite according to claim 1, wherein the surfactant is di(dodecyl)phosphate and tetradecyltrimethylammonium bromide according to the mass ratio. 1:1 mixture.
- 根据权利要求1所述高比表面积拟薄水铝石制备方法，其特征在于，所述表面活性剂包括活性组分和助表面活性剂，所述活性组分为十二烷基磺酸钠，助表面活性剂为正戊醇，质量比为1：1。The high specific surface area pseudo-boehmite preparation method according to claim 1, wherein the surfactant includes an active component and a co-surfactant, and the active component is sodium dodecyl sulfonate, The co-surfactant is n-pentanol, and the mass ratio is 1:1.
- 根据权利要求1所述高比表面积拟薄水铝石制备方法，其特征在于，所述表面活性剂溶液的浓度为0.05-0.5g/mL，加入反应器的流速为5-10mL/min。 The method for preparing high specific surface area pseudo-boehmite according to claim 1, characterized in that the concentration of the surfactant solution is 0.05-0.5g/mL, and the flow rate added to the reactor is 5-10mL/min.
- 根据权利要求1所述高比表面积拟薄水铝石制备方法，其特征在于，所述扩孔剂为碳酸氢铵和/或尿素。The method for preparing high specific surface area pseudo-boehmite according to claim 1, characterized in that the pore expander is ammonium bicarbonate and/or urea.
- 根据权利要求1所述高比表面积拟薄水铝石制备方法，其特征在于，所述扩孔剂溶液的浓度为0.1-0.5g/mL，加入反应器的流速为2-5mL/min。The method for preparing high specific surface area pseudo-boehmite according to claim 1, characterized in that the concentration of the pore expander solution is 0.1-0.5g/mL, and the flow rate added to the reactor is 2-5mL/min.
- 根据权利要求1所述高比表面积拟薄水铝石制备方法，其特征在于，步骤(3)所述干燥温度为100-150℃，干燥时间为6-10h。 The method for preparing high specific surface area pseudo-boehmite according to claim 1, characterized in that the drying temperature in step (3) is 100-150°C and the drying time is 6-10 h.
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| CN105271328A (en) * | 2015-10-12 | 2016-01-27 | 中国海洋石油总公司 | Aluminium-salt-assisted hydro-thermal synthesis method for pseudo-boehmite |
| CN105347372A (en) * | 2015-11-20 | 2016-02-24 | 中石化催化剂（北京）有限公司 | Production method of large pore volume pseudo boehmite |
| CN111377467A (en) * | 2018-12-28 | 2020-07-07 | 中国石油化工股份有限公司 | Alumina and preparation method thereof |
| US20220055911A1 (en) * | 2018-12-28 | 2022-02-24 | China Petroleum & Chemical Corporation | Pseudo-boehmite, manufacturing process and application thereof |
| CN115231595A (en) * | 2022-06-25 | 2022-10-25 | 扬州中天利新材料股份有限公司 | Preparation method of pseudo-boehmite with high specific surface area |
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| JPH08268715A (en) * | 1995-03-30 | 1996-10-15 | Japan Energy Corp | Production of high purity pseudo-boehmite powder |
| CN103332716B (en) * | 2013-07-16 | 2015-02-25 | 兰州大学 | Preparation method of pseudoboehmite |
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2022
- 2022-06-25 CN CN202210727152.6A patent/CN115231595A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271328A (en) * | 2015-10-12 | 2016-01-27 | 中国海洋石油总公司 | Aluminium-salt-assisted hydro-thermal synthesis method for pseudo-boehmite |
| CN105347372A (en) * | 2015-11-20 | 2016-02-24 | 中石化催化剂（北京）有限公司 | Production method of large pore volume pseudo boehmite |
| CN111377467A (en) * | 2018-12-28 | 2020-07-07 | 中国石油化工股份有限公司 | Alumina and preparation method thereof |
| US20220055911A1 (en) * | 2018-12-28 | 2022-02-24 | China Petroleum & Chemical Corporation | Pseudo-boehmite, manufacturing process and application thereof |
| CN115231595A (en) * | 2022-06-25 | 2022-10-25 | 扬州中天利新材料股份有限公司 | Preparation method of pseudo-boehmite with high specific surface area |
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