CN101450812A - Method for preparing nano pseudo boehmite and microchannel reactor - Google Patents
Method for preparing nano pseudo boehmite and microchannel reactor Download PDFInfo
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- CN101450812A CN101450812A CNA200710158754XA CN200710158754A CN101450812A CN 101450812 A CN101450812 A CN 101450812A CN A200710158754X A CNA200710158754X A CN A200710158754XA CN 200710158754 A CN200710158754 A CN 200710158754A CN 101450812 A CN101450812 A CN 101450812A
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Abstract
The invention relates to an inorganic nanometer material and a micro-channel reactor, in particular to a method for preparing nanometer pseudoboemite and a micro-channel reactor. Two paths of liquid-phase reaction liquids are conveyed into the micro-channel reactor through an advection pump and finish a precipitation reaction in the micro-channel reactor, and then a high-purity nanometer material is obtained through a series of post treatments. The method adopts a single-channel micro-reactor and a multi-channel micro-reactor. The method has the advantages of controllable process, good mixing effect of raw materials, quick reaction, high-flux operation, continuous reaction process, large operation elasticity, high time space yield, high product purity, controllable particle size dimension, and narrow particle size distribution.
Description
Technical field
The present invention relates to inorganic nano material and micro passage reaction, specifically a kind ofly be applicable to the method for utilizing the direct precipitin reaction production of liquid-liquid nano material and realize the micro passage reaction that this method adopts; It utilizes micro passage reaction, prepares highly purified nano pseudo boehmite with neutralisation.
Background technology
Micro passage reaction refers generally to the reactor of reaction channel width below 1mm.At the beginning of the nineties, the investigator begins to attempt microreactor is applied to chemical reaction.In the time of short more than ten years, this technology has obtained significant progress all over the world.Various reaction types, as liquid-liquid reactions, gas-liquid reaction, catalyzed reactions etc. can be carried out in micro passage reaction.The beginning of this century, the preparation nano material has caused people's extensive interest in micro passage reaction.A lot of scientific research institutions and colleges and universities have all carried out the work of this respect.The maximum characteristics of micro passage reaction are that size is little, thereby can realize that good microcosmic mixes.For the production of nano material, the microcosmic degree of mixing is very important processing condition, and it directly has influence on the quality of prepared nano material.Utilize microreactor to prepare nano material and have clear superiority.Yet the preparation nano material has several common features in the microchannel at present: reaction density is low, flow velocity is slow, output little (John deMello, Andrew deMello, LabChip, 2004:11N; Jingxi Ju, Cangfeng Zeng, Lixiong Zhang, Nanping Xu, Chem.Eng.J., 2006,116:115).Yes is undivided with the characteristics of micro passage reaction itself for such process characteristic, still and be not suitable for industrial production in enormous quantities.Therefore high flow rate in the microchannel, high density ground production nano material is challenging, and has the research direction of great realistic meaning.
Pseudo-boehmite is γ-Al
2O
3Important presoma, in industry, be widely used.Its preparation process directly has influence on the performance of final product.Utilizing the neutralization reaction of sodium metaaluminate and Tai-Ace S 150 is wherein a kind of important method with the preparation nano pseudo boehmite.
The blending ratio of sodium metaaluminate and Tai-Ace S 150 directly has influence on the pH value of mixing solutions, thereby has influence on the crystal formation of final product.Under acidic conditions, what obtain is gelatinous hydrated alumina, belongs to amorphous material.And the pH value is when too high, and what obtain is aluminum hydroxide crystals.Have only the suitable condition of control, just can obtain the pseudo-boehmite crystal.And during with the reactor of large volume,, causing the local proportion inequality because that the inside reactor microcosmic mixes is inhomogeneous, resulting pseudo-boehmite crystal is impure, wherein is mingled with other crystal formations such as aluminium hydroxide.This is the major defect that traditional law system is equipped with pseudo-boehmite.The preparation pseudo-boehmite does not appear in the newspapers as yet in the microchannel.
Summary of the invention
The object of the present invention is to provide a kind of method that can produce the high-purity nano pseudo-boehmite expeditiously, and the microreactor that will use of this method.
For achieving the above object, the technical solution used in the present invention is:
A kind of preparation method of nano pseudo boehmite utilizes the direct precipitin reaction of liquid-liquid to prepare nano material in the microreactor that has at least two imports and an outlet, comprises the following steps:
1) with 0.1～1.0mol/l sodium aluminate solution and two strands of aqueous phase solutions of 0.01～0.5mol/l alum liquor respectively via the constant-flux pump that can accurately control flow velocity (strict control flow velocity, make them be subjected to pump pressure and handle, make logistics in the constant-flux pump with the bottom of the speed overboard pump of control) be delivered to two inlets of micro passage reaction;
Alum liquor is delivered to the flow rates of micro passage reaction at 1～10ml/min;
The volume flow ratio of sodium aluminate solution and alum liquor is 3～10;
2) two strands of aqueous phase solutions in micro passage reaction, contact and mix react after, flow out from the exit of reactor and to enter sedimentation tank;
3) product in the sedimentation tank carries out ageing processing and the dry purpose product that gets.
Described sodium aluminate solution concentration is preferably 0.3～0.7mol/l, alum liquor concentration is preferably 0.05～0.2mol/l, the flow velocity that alum liquor is delivered to micro passage reaction is preferably 8～10ml/min, the flow-ratio control of sodium metaaluminate and Tai-Ace S 150 is in certain limit, to control suitable pH value, volume flow ratio is preferably 6～8.
Can in reaction product, add Na before the ageing
2CO
3Solution, pH value to 8.5～9.5 of improving solution; The ageing temperature need be controlled, and can be controlled with water-bath or oil bath pan or alternate manner, and temperature range is at 20 ℃～90 ℃; Digestion time is 0.5h～72h; The ageing temperature is preferably 25 ℃～60 ℃, and digestion time is preferably 2h～48h; Sample after ageing is finished washs with whizzer, and puts into baking oven and dry.
Be used to realize the micro passage reaction of aforesaid method, comprise at least two substrates;
Be arranged in wherein at least three microchannels of arbitrary substrate, i.e. at least two intake vents are with at least one reaction channel that links to each other with intake vent respectively;
And at least two imports that are connected with intake vent respectively, with an outlet that is connected with reaction channel.
The import microchannel can be consistent with the microchannel characteristic dimension, also can be different when intake vent than the internal diameter of reaction channel hour, can improve the intensity of reactant bump, improve the microcosmic mixed effect, the hydraulic radius scope of microchannel should be below 1mm, preferably at 0.2mm-1.0mm.The microchannel length range is at 0.2cm～50cm, preferred 1cm～4cm.
Every intake vent can be provided with one or more than one branches;
When intake vent is provided with the branch of one or more, link to each other with the semicircular arc microchannel between higher level microchannel and the subordinate microchannel, and the equivalent diameter size of microchannel to successively decrease step by step, the amplitude of successively decreasing is at 20-80%.
Angle between at least two intake vents that link to each other with reaction channel can be arbitrarily angled, is preferably 60～180 °.
Connect sealing or adopt vacuum diffusion welding to connect with stainless steel bolt between the described substrate.
Between the two import microchannels certain angle is arranged, preferred 60～180 °.Intake vent can be that single passage also can be a hyperchannel.When intake vent is hyperchannel, link to each other with the semicircular arc microchannel between higher level microchannel and the subordinate microchannel, the microchannel size is successively decreased step by step, and the amplitude of successively decreasing is at 20%-80%;
The present invention has following advantage:
Owing to adopt micro passage reaction, make that reaction process is controlled, raw material good mixing effect, speed of response are fast, can carry out the high-throughput operation; Reaction process is continuous, turndown ratio is big; Space-time yield height, product purity height, controlled, the narrow diameter distribution of particle diameter yardstick.
Description of drawings
Fig. 1 is a reaction process device block diagram;
Fig. 2 is a multi-channel reaction device pictorial diagram;
Fig. 3 is the XRD figure of sample; Wherein: 1, industrial goods pseudo-boehmite XRD figure, 2, example 1 sample XRD figure, 3, example 3 sample XRD figure;
Fig. 4 is the TEM figure of sample.
Embodiment
As shown in Figure 1, be used to realize that the device of present method comprises:
1) two liquid constant-flux pumps;
2) micro passage reaction; Comprise two substrates;
Be arranged in wherein three microchannels of arbitrary substrate, i.e. two intake vents are with a reaction channel that links to each other with intake vent respectively;
And two imports that are connected with intake vent respectively, with an outlet that is connected with reaction channel.Every intake vent can be provided with one or more than one branches;
Intake vent is established three grades of shuntings, link to each other with the semicircular arc microchannel between higher level microchannel and the subordinate microchannel, and the equivalent diameter size of microchannel successively decreases step by step, and the amplitude of successively decreasing is 20%, and the last grade shunting has 8 branches.
3) be used for the utility appliance such as beaker of splendid attire raw material and reactant;
4) reduce the check valve that fluid fluctuates;
5) connect the plastics tubing of each equipment.
1) 9.84 gram sodium aluminates is dissolved in the 200ml tap water, be mixed with the solution of 0.6mol/l, 6.84g Tai-Ace S 150 is dissolved in the 200ml tap water, be mixed with the solution of 0.1mol/l.
2) import sodium aluminate and alum liquor with two constant-flux pumps respectively to two imports of single pass reactor, two strands of solution mix at the interface bump, and proceed reaction along reaction channel.Keeping the Tai-Ace S 150 flow velocity is 9ml/min, regulates the sodium aluminate solution flow velocity, and recording product pH value in the exit is 7.5.
3) aluminum salt solution in collection exit adds small amount of N a
2CO
3Solution is regulated pH value to 9.Put into 45 ℃ of water-bath ageing 24h.Then with whizzer washing 3 times.Put into 110 ℃ of heating of baking oven 10h, oven dry, feed stock conversion 100%; Product after the oven dry is milled into powder, makes XRD analysis, obtain nano level purpose product-pure pseudo-boehmite.TEM figure shows that the gained material is the silky nano pseudo-boehmite.
1) the 4.92g sodium aluminate is dissolved in the 200ml tap water, be mixed with the solution of 0.3mol/l, 3.42g Tai-Ace S 150 is dissolved in the 200ml tap water, be mixed with the solution of 0.05mol/l.
2) import sodium aluminate and alum liquor with two constant-flux pumps respectively to two imports of single pass reactor, two strands of solution mix at the interface bump, and react along reaction channel.Constant Tai-Ace S 150 flow velocity is 8ml/min, regulates the flow velocity of sodium aluminate solution, and recording product pH value in the exit is 8.
3) aluminum salt solution in collection exit adds small amount of N a
2CO
3Solution makes the pH value rise to 9.5.Put into 60 ℃ of water-bath ageing 4h.Then with whizzer washing 3 times.Put into 110 ℃ of heating of baking oven 10h, oven dry, feed stock conversion 100%; Product after the oven dry is milled into powder, obtains nano level purpose product-pure pseudo-boehmite.
Constant Tai-Ace S 150 flow velocity is 9ml/min, regulates the flow velocity of sodium aluminate solution, and recording product pH value in the exit is 6.Collect the aluminum salt solution in exit, add small amount of N a
2CO
3Solution makes the pH value rise to 8.5.Ageing 48h under 25 ℃ of room temperatures.All the other conditions are with embodiment 1.Obtain nano level purpose product-pure pseudo-boehmite at last, feed stock conversion 100%.
Embodiment 4
11.48g sodium aluminate dissolves in the 200ml tap water, is mixed with the solution of 0.7mol/l, and 13.68g Tai-Ace S 150 is dissolved in the 200ml tap water, is mixed with the solution of 0.2mol/l.Constant Tai-Ace S 150 flow velocity is 10ml/min.Put into 60 ℃ of water-bath ageing 2h.Then with whizzer washing 3 times.Put into 110 ℃ of heating of baking oven 10h, oven dry.All the other conditions are with embodiment 1.Obtain nano level purpose product-pure pseudo-boehmite at last, feed stock conversion 100%.
Embodiment 5
Import sodium aluminate and alum liquor with two constant-flux pumps respectively to two imports of multi-channel reaction device, two strands of solution mix at the interface bump, and at the reaction chamber internal reaction.Constant Tai-Ace S 150 flow velocity is 50ml/min.All the other conditions are with embodiment 1.Obtain nano level purpose product-pure pseudo-boehmite at last, feed stock conversion 100%.
Comparative example
The industrial goods pseudo-boehmite is made XRD analysis, and what obtain is the pseudo-boehmite product that is mingled with aluminium hydroxide impurity, and product is impure.
Claims (9)
1. the preparation method of a nano pseudo boehmite utilizes the direct precipitin reaction of liquid-liquid to prepare nano material in the microreactor that has at least two imports and an outlet, comprises the following steps:
1) 0.1～1.0mol/l sodium aluminate solution and two strands of aqueous phase solutions of 0.01～0.5mol/l alum liquor are delivered to two inlets of micro passage reaction respectively via the constant-flux pump that can accurately control flow velocity;
Alum liquor is delivered to the flow rates of micro passage reaction at 1～10ml/min;
The volume flow ratio of sodium aluminate solution and alum liquor is 3～10;
2) two strands of aqueous phase solutions in micro passage reaction, contact and mix react after, flow out from the exit of reactor and to enter sedimentation tank;
3) product in the sedimentation tank carries out ageing processing and the dry purpose product that gets.
2. the method for claim 1, it is characterized in that: described sodium aluminate solution concentration is 0.3～0.7mol/l, alum liquor concentration is 0.05～0.2mol/l, the flow velocity that alum liquor is delivered to micro passage reaction is 8～10ml/min, and the throughput ratio of sodium metaaluminate and Tai-Ace S 150 is 6～8.
3. the method for claim 1 is characterized in that: can add Na before the ageing in reaction product
2CO
3Solution, pH value to 8.5～9.5 of improving solution; 20 ℃～90 ℃ of ageing temperature; Digestion time is 0.5h～72h.
4. method as claimed in claim 3 is characterized in that: the ageing temperature is 25 ℃～60 ℃, and digestion time is 2h～48h.
5. a micro passage reaction that is used to realize claim 1 preparation method is characterized in that: comprise two substrates at least;
Be arranged in wherein at least three microchannels of arbitrary substrate, i.e. at least two intake vents are with at least one reaction channel that links to each other with intake vent respectively;
And at least two imports that are connected with intake vent respectively, with an outlet that is connected with reaction channel.
6. micro passage reaction as claimed in claim 5 is characterized in that: the hydraulic radius scope of microchannel is at 0.2mm-1.0mm.
7. micro passage reaction as claimed in claim 5 is characterized in that:
Every intake vent can be provided with one or more than one branches;
When intake vent is provided with the branch of one or more, link to each other with the semicircular arc microchannel between higher level microchannel and the subordinate microchannel, and the equivalent diameter size of microchannel to successively decrease step by step, the amplitude of successively decreasing is at 20-80%.
8. micro passage reaction as claimed in claim 5 is characterized in that: the angle between at least two intake vents that link to each other with reaction channel is 60～180 °.
9. micro passage reaction as claimed in claim 5 is characterized in that: connect sealing or adopt vacuum diffusion welding to connect with stainless steel bolt between the described substrate.
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|---|---|---|---|---|
| CN102179218A (en) * | 2011-03-16 | 2011-09-14 | 清华大学 | Reaction-precipitation method for preparing nanoparticles or precursor thereof |
| CN101993052B (en) * | 2009-08-27 | 2013-01-16 | 中国科学院大连化学物理研究所 | Microreaction system for ammonium salt production and application |
| CN102910654A (en) * | 2012-11-08 | 2013-02-06 | 北京化工大学 | Preparation method of fibrous boehmite with large specific surface area and large pore area |
| CN103172097A (en) * | 2013-04-11 | 2013-06-26 | 北京化工大学 | Pseudo-boehmite with large specific surface area and preparation method and application thereof |
| CN103787387A (en) * | 2012-10-29 | 2014-05-14 | 中国石油化工股份有限公司 | Stabilization method of sodium metaaluminate solution and preparation method of pseudo-boehmite |
| CN103880073A (en) * | 2014-03-21 | 2014-06-25 | 南京工业大学 | Method for preparing nano titanium dioxide by applying precipitation process and adopting microreactor |
| CN104671265A (en) * | 2013-11-26 | 2015-06-03 | 中国石油化工股份有限公司 | A method of preparing pseudoboehmite |
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| CN109721088A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | A kind of aluminium hydroxide and preparation method thereof |
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| CN109721087A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | A kind of boehmite and preparation method thereof |
| CN111115669A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | Method for generating solid product by gas-liquid reaction and method for continuously preparing pseudo-boehmite |
| CN112520768A (en) * | 2020-12-13 | 2021-03-19 | 中海油天津化工研究设计院有限公司 | Preparation method of rod-shaped high-purity pseudo-boehmite |
| CN113353929A (en) * | 2021-07-08 | 2021-09-07 | 吕梁学院 | Biomass carbon material and preparation method thereof |
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| CN101993052B (en) * | 2009-08-27 | 2013-01-16 | 中国科学院大连化学物理研究所 | Microreaction system for ammonium salt production and application |
| CN102179218A (en) * | 2011-03-16 | 2011-09-14 | 清华大学 | Reaction-precipitation method for preparing nanoparticles or precursor thereof |
| CN103787387A (en) * | 2012-10-29 | 2014-05-14 | 中国石油化工股份有限公司 | Stabilization method of sodium metaaluminate solution and preparation method of pseudo-boehmite |
| CN103787387B (en) * | 2012-10-29 | 2015-03-25 | 中国石油化工股份有限公司 | Preparation method of pseudo-boehmite |
| CN102910654A (en) * | 2012-11-08 | 2013-02-06 | 北京化工大学 | Preparation method of fibrous boehmite with large specific surface area and large pore area |
| CN102910654B (en) * | 2012-11-08 | 2014-07-30 | 北京化工大学 | Preparation method of fibrous boehmite with large specific surface area and large pore area |
| CN103172097A (en) * | 2013-04-11 | 2013-06-26 | 北京化工大学 | Pseudo-boehmite with large specific surface area and preparation method and application thereof |
| CN104671265B (en) * | 2013-11-26 | 2017-02-15 | 中国石油化工股份有限公司 | A method of preparing pseudoboehmite |
| CN104671265A (en) * | 2013-11-26 | 2015-06-03 | 中国石油化工股份有限公司 | A method of preparing pseudoboehmite |
| CN103880073A (en) * | 2014-03-21 | 2014-06-25 | 南京工业大学 | Method for preparing nano titanium dioxide by applying precipitation process and adopting microreactor |
| CN103880073B (en) * | 2014-03-21 | 2015-04-22 | 南京工业大学 | Method for preparing nano titanium dioxide by applying precipitation process and adopting microreactor |
| CN104692429A (en) * | 2015-02-16 | 2015-06-10 | 北京化工大学 | Controllable preparation method of large-specific-area large-pore-volume boehmite |
| CN109721088A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | A kind of aluminium hydroxide and preparation method thereof |
| CN109721085A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | Aluminium hydroxide and preparation method thereof |
| CN109721087A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | A kind of boehmite and preparation method thereof |
| CN109721088B (en) * | 2017-10-27 | 2021-02-05 | 中国石油化工股份有限公司 | Aluminum hydroxide and preparation method thereof |
| CN109721087B (en) * | 2017-10-27 | 2021-02-05 | 中国石油化工股份有限公司 | Pseudo-boehmite and preparation method thereof |
| CN109721085B (en) * | 2017-10-27 | 2021-03-02 | 中国石油化工股份有限公司 | Aluminum hydroxide and preparation method thereof |
| CN111115669A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | Method for generating solid product by gas-liquid reaction and method for continuously preparing pseudo-boehmite |
| CN112520768A (en) * | 2020-12-13 | 2021-03-19 | 中海油天津化工研究设计院有限公司 | Preparation method of rod-shaped high-purity pseudo-boehmite |
| CN113353929A (en) * | 2021-07-08 | 2021-09-07 | 吕梁学院 | Biomass carbon material and preparation method thereof |
| CN113353929B (en) * | 2021-07-08 | 2022-09-16 | 吕梁学院 | Biomass carbon material and preparation method thereof |
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