CN104174417A - Aluminum phosphate catalyst as well as preparation method and application thereof - Google Patents
Aluminum phosphate catalyst as well as preparation method and application thereof Download PDFInfo
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- CN104174417A CN104174417A CN201410443134.0A CN201410443134A CN104174417A CN 104174417 A CN104174417 A CN 104174417A CN 201410443134 A CN201410443134 A CN 201410443134A CN 104174417 A CN104174417 A CN 104174417A
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Abstract
The invention relates to a mesoporous aluminum phosphate catalyst and a preparation method thereof as well as application of the mesoporous aluminum phosphate catalyst in a process for preparing bulk chemical acetaldehyde by lactic acid decarbonylation. The preparation method comprises the following steps: putting aluminum nitrate and phosphoric acid in an aqueous solution, and then preparing aluminum phosphate by using an ammonia precipitation method; and then, putting aluminum phosphate in a muffle furnace for calcination, tabletting, crushing and selecting 20-40-mesh particles to obtain the mesoporous aluminum phosphate catalyst. Lactic acid obtained by biomass fermentation is taken as a raw material, and the reaction temperature is 250-400 DEG C. Under the reaction condition of atmospheric pressure, carrier gas with the raw material synthesizes acetaldehyde by using a high-temperature gas-solid catalytic method, and the adopted catalyst is the prepared mesoporous aluminum phosphate. The aluminum phosphate has good acetaldehyde selectivity and strong catalytic stability (248 hours). As the aluminum phosphate catalyst has the advantages of environment friendliness, low cost, high catalytic activity, good stability, high acetaldehyde selectivity and high lactic acid conversion rate, and is easy to prepare, so that the aluminum phosphate catalyst has high commercial development value.
Description
Technical field
The present invention relates to catalyst preparation and derived energy chemical technical field, particularly a kind of mesoporous aluminum phosphate Catalysts and its preparation method and prepare the application in acetaldehyde technique at catalysis lactic acid decarbonylation.
Background technology
Take living beings as raw material development chemical industry, is a sustainable development process route.In biomass material, lactic acid is very important.Its reason is to contain in its molecule 2 active functional groups: hydroxyl and carboxyl.Therefore, in academia and industrial quarters, conventionally lactic acid is used as to a biological plateform molecules.For example, lactic acid can be prepared acrylic acid, condensation reaction by dehydration and prepares 2,3-pentanedione, decarbonylation and prepare that acetaldehyde, hydrogenation reaction can be prepared propionic acid, polymerisation is prepared PLA (bio-medical material) etc.Acetaldehyde has very extensive and important purposes as the intermediate of organic synthesis.Acetaldehyde can be used for manufacturing acetic acid, aceticanhydride, accounts for 50%～70% of total amount; Acetaldehyde also can be used for producing n-butanol, the products such as 2-Ethylhexyl Alcohol, pyridine, pentaerythrite, and these products are again the raw materials of other chemical and medicine industries.Thereby the market demand of acetaldehyde is very large.
In lactic acid molecules just because of in there are 2 functional groups simultaneously, this is also for selective chemical utilization has brought very large difficulty.Its difficulty is mainly, in chemical reaction, often Liang Ge functional group all can participate in, and forms numerous accessory substances, makes later separation difficulty, and raw material availability is low.The problem that the catalyst of reporting at present exists can be summed up as 3 aspects: 1) during catalyst selective high, its catalytic activity (feed stock conversion) is low again; 2), when the activity of catalyst is very high, often there is the selectively on the low side again of reaction; 3) activity and selectivity of catalyst is still in acceptable situation, and the life-span of catalyst is partially short again.
Research by early stage is found, lactic acid decarbonylation reaction, and the acidity of required catalyst is moderate the most important, and highly acid position is more few better in addition.Containing the compound of aluminium as aluminium oxide as catalyst or carrier already studied person be familiar with.Aluminium conduct+3 valency cation, has Lewis acidity.And lactic acid de-carbonyl reaction needs acid catalysis, this just becomes possibility for selecting aluminum contained compound to become decarbonylation catalyst.In addition, combine with anion, can effectively regulate the acidity of aluminum phosphate.Phosphoric acid is as middle strong acid, acid than a little less than sulfuric acid many.The aluminum sulfate that aluminium ion and sulfate anion are combined to form, passes through NH
3-TPD analyzes discovery, although there is a large amount of intermediate acid positions, also has the strong acidic site of a great deal of.Lactic acid decarbonylation is tested and has also been proved, the stability of catalyst is not good enough, only 50h.Select to be combined to form aluminum phosphate with phosphoric acid, its catalytic performance may be better than aluminum sulfate as catalyst agent again.
Aluminum phosphate is a kind of catalysis material with the two catalytic centers of soda acid, as catalyst or catalyst carrier, is widely used in the multiple reaction that comprises alkylation, oxidative dehydrogenation, catalytic cracking, reformation, isomerization.Yet the preparation condition of catalyst may affect Acidity of Aikalinity, pore structure, specific surface of catalyst etc., thereby have influence on catalytic activity and the stability of catalyst.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of high-performance, and the preparation method of the aluminium phosphate catalyst of high stability is intended to solve the selective problems of catalytic reaction.
The invention provides a kind of mesoporous aluminum phosphate catalyst, this aluminium phosphate catalyst be take the solution that aluminum nitrate that aluminium, phosphorus mol ratio is 1:1 and phosphorylated ligand are made 0.3-0.6mmol/L, and regulate pH in 70-90 ℃ of stirring, to make aluminum phosphate white precipitate after 4-6 by ammoniacal liquor, afterwards described aluminum phosphate white precipitate is dried and is placed on 500-600 ℃ of roasting 5-7h in Muffle furnace, by gained pressed powder, pulverizing, get 20-40 object particle and obtain described mesoporous aluminum phosphate catalyst.
Wherein, described aluminium phosphate catalyst is mesoporous aluminum phosphate; The aperture of described mesoporous aluminum phosphate is 10-20nm; Its total acid bit density is 3.5-4mmol/g, and weak acid position, middle strong acidic site density are 3-3.7mmol/g.
The preparation method of described mesoporous phosphoric acid catalyst comprises the following steps: aluminum nitrate and the phosphorylated ligand that aluminium, phosphorus mol ratio is 1:1 of take made 0.3-0.6mmol/L solution, it is 4-6 that the ammoniacal liquor that is 25% with mass fraction regulates pH value, at 70-90 ℃, rapid stirring is to producing aluminum phosphate white precipitate, gained aluminum phosphate is deposited in to dry 120-140min under 70-90 ℃ of condition, driedly be placed on 500-600 ℃ of roasting 5-7h in Muffle furnace, the aluminum phosphate pressed powder of gained, pulverize, get 20-40 object particle as catalyst.
The present invention also provides a kind of described aluminium phosphate catalyst preparation method gained aluminium phosphate catalyst to prepare the application in acetaldehyde technique at lactic acid decarbonylation.
Aluminium phosphate catalyst is prepared the application in acetaldehyde technique at lactic acid decarbonylation, comprises the following steps: described mesoporous aluminum phosphate catalyst is added to end-blocking in reaction tube, wherein add the volume of aluminium phosphate catalyst to account for the 5-15% of reaction tube volume; With carrier gas, carry lactic acid aqueous solution by the reaction tube of described aluminium phosphate catalyst is housed, 3-8 ℃/min temperature programming is to reaction temperature, and reaction temperature is 250-400 ℃, and lactic acid concn is 15-40wt%, charging rate is 1-8ml/h, and the flow velocity of carrier gas is 0.5-8mL/min.
Wherein, described carrier gas is nitrogen.Described reaction tube is inertia material, is preferably quartzy material.
The method of the invention is prepared aluminium phosphate catalyst, surface has moderate acid position and accounts for the overwhelming majority, strong acidic site is few, thereby aluminum phosphate has the selective and superpower catalytic stability of good acetaldehyde (248 hours), in preparing acetaldehyde technique, catalysis lactic acid decarbonylation there is higher catalytic activity.This mesoporous aluminum phosphate catalyst for example, under 325 ℃ of conditions, the conversion ratio 100% of lactic acid, acetaldehyde be selectively greater than 92%.Catalyst moves 248h continuously, catalyst selectively almost constant, and the conversion ratio of lactic acid only has reduction by a small margin.In addition, this mesoporous aluminum phosphate has very strong adaptability to the variation of reaction environment, can bear the acute variation of reaction condition, and when flow rate of carrier gas, lactic acid concn, charging rate change, slight fluctuation only occurs for the conversion ratio of lactic acid and acetaldehyde selective.Though existing bibliographical information is with aluminum sulfate (industry and engineering chemistry research (Industrial & Engineering Chemistry Research), the U.S., 2014,53,10138-10327), heteropoly acid (Green Chemistry (Green Chemistry), the Britain of silicon load, 2010,12,1910) as catalyst, at lactic acid decarbonylation reaction, prepare acetaldehyde, but the mesoporous aluminum phosphate catalyst that catalyst performance relates to far away from this patent.Aluminium phosphate catalyst preparation of the present invention is simple, environmental protection, and with low cost, catalytic activity is high, good stability, and acetaldehyde conversion ratio selective and lactic acid is high, has very high commercial development to be worth.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the invention will be further described:
Fig. 1 is the infrared spectrum of aluminium phosphate catalyst;
Fig. 2 is the X-ray powder diffraction figure of aluminium phosphate catalyst;
Fig. 3-5th, the scanned photograph of aluminium phosphate catalyst;
What Fig. 6 was aluminium phosphate catalyst at the conversion ratio of different time catalysis lactic acid decarbonylation lactic acid and acetaldehyde is selective.
The specific embodiment
Below in conjunction with the embodiment in the present invention and accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment mono-
Adopt ammonia precipitation process legal system for mesoporous aluminum phosphate, take 2.3g phosphoric acid (85wt%), 7.5g aluminum nitrate (Al (NO
3)
39H
2o) be dissolved in 50ml water, it is 5 that ammoniacal liquor with 25% regulates pH value, at 80 ℃, rapid stirring is to producing white precipitate, gained is deposited in to dry 130min under 80 ℃ of conditions, driedly be placed on 550 ℃ of roasting 6h in Muffle furnace, the aluminum phosphate pressed powder of gained, pulverizes, and gets 20-40 object particle and is labeled as MAP3 as aluminium phosphate catalyst.Select a long 400mm, the quartz ampoule that internal diameter is 4mm, fills in the above-mentioned preparing catalyst of 0.1300g in quartz ampoule, and catalyst length in pipe is 30mm, the two ends of catalyst silica wool end-blocking, and the length of this silica wool is 30mm.With nitrogen, carry lactic acid aqueous solution by the above-mentioned quartz ampoule that installs catalyst, 5 ℃/min temperature programming to 380 ℃, lactic acid concn is 20wt%, and the flow velocity of nitrogen is 1mL/min, and entering lactic acid aqueous solution speed is 1 ml/hour.
Control Example 1
Take the aluminum nitrate (Al (NO of 7.5g
3)
39H
2o) and 7.6g sodium phosphate (Na (PO
4)
312H
2o), be dissolved in respectively in 50mL distilled water, then the two solution mixed, reaction forms aluminum phosphate precipitation, uses distilled water cyclic washing, until the PH of distilled water is to neutral.In drying box, dry 4h at 120 ℃, is then placed under 550 ℃ of conditions of Muffle furnace and calcines 6h, obtains aluminium phosphate catalyst and is labeled as MAP1.By the aluminum phosphate pressed powder of above-mentioned gained, pulverize, get 20～40 object particles standby as catalyst, select a long 400mm, internal diameter is the quartz ampoule of 3mm, and the above-mentioned preparing catalyst of 0.1306g is filled in quartz ampoule, and catalyst length in pipe is 30mm, the two ends of catalyst silica wool end-blocking, the length of this silica wool is 30mm.With nitrogen, carry lactic acid aqueous solution by the above-mentioned quartz ampoule that installs catalyst, 5 ℃/min temperature programming to 380 ℃, lactic acid concn is 20wt%, and the flow velocity of nitrogen is 1mL/min, and entering lactic acid aqueous solution speed is 1 ml/hour.
Control Example 2
Synthesising mesoporous aluminum phosphate under effect with citric acid auxiliary agent, by 4.2g citric acid, 2.3g phosphoric acid (85wt%), 7.5g aluminum nitrate (Al (NO
3)
39H
2o) be dissolved in 50ml water, it is 5 that 25% the ammoniacal liquor of take regulates pH value, under 80 ℃ of conditions, that citric acid, aluminum nitrate, phosphoric acid are evenly formed is solid-state for rapid stirring, gained solid is placed in to baking oven to be dried after 30min under 150 ℃ of conditions, taking-up is placed in tube furnace under air atmosphere, 800 ℃ of roasting 6h, are labeled as MAP2 by the aluminium phosphate catalyst of gained.By the aluminum phosphate pressed powder of above-mentioned gained, pulverize, get 20～40 object particles standby as catalyst, select a long 400mm, internal diameter is the quartz ampoule of 3mm, and the above-mentioned preparing catalyst of 0.2986g is filled in quartz ampoule, and catalyst length in pipe is 30mm, the two ends of catalyst silica wool end-blocking, the length of this silica wool is 30mm.With nitrogen, carry lactic acid aqueous solution by the above-mentioned quartz ampoule that installs catalyst, 5 ℃/min temperature programming to 380 ℃, lactic acid concn is 20wt%, and the flow velocity of nitrogen is 1mL/min, and entering lactic acid aqueous solution speed is 1 ml/hour.
The specific activity of aluminium phosphate catalyst prepared by distinct methods
The structure and properties of the aluminum phosphate of first being prepared by distinct methods characterizes, and result is as table 1-2, shown in Fig. 3-5.From analytical test result, preparation method has certain impact to the physical property of catalyst and structure.Catalyst catalytic performance prepared by three kinds of methods is as shown in table 3, and the data in table 3 are the mean value of three parallel tests.When not adding catalyst, lactic acid only has 25% conversion has occurred; And having added catalyst (any one in three kinds of catalyst), lactic acid has all been realized and having been transformed completely, shows really to have risen catalytic action.In addition, observe the selective of acetaldehyde, three kinds of catalyst have provided inconsistent result, and the acetaldehyde in embodiment mono-is selectively better than in control Example.The preparation method of this explanation catalyst has obvious influence to the performance of catalyst.
The physical property of the aluminum phosphate that the different preparation methods of table 1 obtain
| Aluminium phosphate catalyst | Specific area (m 2/g) | Pore volume (cm 3/g) | Average pore size (nm) |
| Embodiment mono- | 171.1 | 0.9 | 15.5 |
| Control Example 1 | 74.8 | 1.1 | 63.8 |
| Control Example 2 | 40.8 | 0.1 | 8.9 |
The ammonia adsorption desorption data (NH of table 2 aluminium phosphate catalyst
3-TPD)
The catalytic performance of table 3 aluminium phosphate catalyst
Following examples are that mesoporous aluminum phosphate is prepared the application in acetaldehyde at lactic acid decarbonylation.
Embodiment tri-
0.1358g particle diameter is at 20～40 object mesoporous aluminum phosphates, be placed in the quartz ampoule that internal diameter is 4mm, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst is placed in to heating furnace, open nitrogen and pass into 0.5ml/min, open heater, mode with 3 ℃/min temperature programming makes temperature reach 250 ℃, steady temperature, 1ml/h passes into 20% lactic acid aqueous solution, collects product, for colourless transparent liquid, analyze product, the conversion ratio of lactic acid is 40%, acetaldehyde be selectively 98%.
Embodiment tetra-
0.1358g particle diameter is at 20～40 object mesoporous aluminum phosphates, be placed in the quartz ampoule that internal diameter is 4mm, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst is placed in to heating furnace, open nitrogen and pass into 1ml/min, open heater, mode with 8 ℃/min temperature programming makes temperature reach 275 ℃, steady temperature, 8ml/h passes into 20% lactic acid aqueous solution, collects product, for colourless transparent liquid, analyze product, the conversion ratio of lactic acid is 85%, acetaldehyde be selectively 97%.
Embodiment five
0.1378g particle diameter is at 20～40 object mesoporous aluminum phosphates, be placed in the quartz ampoule that internal diameter is 4mm, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst is placed in to heating furnace, open nitrogen and pass into 2ml/min, open heater, mode with 5 ℃/min temperature programming makes temperature reach 300 ℃, steady temperature, 6ml/h passes into 20% lactic acid aqueous solution, collects product, for colourless transparent liquid, analyze product, the conversion ratio of lactic acid is 99%, acetaldehyde be selectively 96%.
Embodiment six
0.1378g particle diameter is at 20～40 object mesoporous aluminum phosphates, be placed in the quartz ampoule that internal diameter is 4mm, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst is placed in to heating furnace, open nitrogen and pass into 3ml/min, open heater, mode with 4 ℃/min temperature programming makes temperature reach 325 ℃, steady temperature, 4ml/h passes into 20% lactic acid aqueous solution, collects product, for colourless transparent liquid, analyze product, the conversion ratio of lactic acid is 100%, acetaldehyde be selectively 96%.
Embodiment seven
0.1300g particle diameter is at 20～40 object mesoporous aluminum phosphates, being placed in interior is the quartz ampoule of 4mm through footpath, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst is placed in to heating furnace, open nitrogen and pass into 4ml/min, open heater, mode with 7 ℃/min temperature programming makes temperature reach 380 ℃, steady temperature, 2ml/h passes into 20% lactic acid aqueous solution, collects product, for light yellow transparency liquid, analyze product, the conversion ratio of lactic acid is 100%, acetaldehyde be selectively 94%.
Embodiment eight
0.1385g particle diameter is at 20～40 object mesoporous aluminum phosphates, be placed in the quartz ampoule that internal diameter is 4mm, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst be placed in to heating furnace, open nitrogen and pass into 5ml/min, open heater, in the mode of 6 ℃/min temperature programming, make temperature reach 325 ℃, steady temperature, 6ml/h continues to pass into 20% lactic acid aqueous solution, product is collected at interval, and 248 hours duration, experimental result as shown in Figure 6.Sample becomes after by the water white transparency starting light yellow, analyzes all collection products, and the conversion ratio of lactic acid is by approximately 80% after initial 100% to 248 hour, selectively substantially the remaining on more than 92% of acetaldehyde.
Embodiment nine
0.1335g particle diameter is at 20～40 object mesoporous aluminum phosphates, be placed in the quartz ampoule that internal diameter is 4mm, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst is placed in to heating furnace, open nitrogen and pass into 6ml/min, open heater, mode with 4 ℃/min temperature programming makes temperature reach 325 ℃, steady temperature, 2ml/h passes into 15% lactic acid aqueous solution, collects product, for colourless transparent liquid, analyze product, the conversion ratio of lactic acid is 100%, acetaldehyde be selectively 97%.
Embodiment ten
0.1335g particle diameter is at 20～40 object mesoporous aluminum phosphates, be placed in the quartz ampoule that internal diameter is 4mm, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst is placed in to heating furnace, open nitrogen and pass into 7ml/min, open heater, mode with 7 ℃/min temperature programming makes temperature reach 325 ℃, steady temperature, 4ml/h passes into 30% lactic acid aqueous solution, collects product, for light yellow transparency liquid, analyze product, the conversion ratio of lactic acid is 100%, acetaldehyde be selectively 91%.
Embodiment 11
0.1335g particle diameter is at 20～40 object mesoporous aluminum phosphates, be placed in the quartz ampoule that internal diameter is 4mm, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst is placed in to heating furnace, open nitrogen and pass into 8ml/min, open heater, mode with 5 ℃/min temperature programming makes temperature reach 325 ℃, steady temperature, 3ml/h passes into 40% lactic acid aqueous solution, collects product, for light yellow transparency liquid, analyze product, the conversion ratio of lactic acid is 97%, acetaldehyde be selectively 92%.
Embodiment 12
0.1323g particle diameter is at 20～40 object mesoporous aluminum phosphates, be placed in the quartz ampoule that internal diameter is 4mm, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst is placed in to heating furnace, open nitrogen and pass into 5ml/min, open heater, mode with 6 ℃/min temperature programming makes temperature reach 325 ℃, steady temperature, 8ml/h passes into 20% lactic acid aqueous solution, collects product, for light yellow transparency liquid, analyze product, the conversion ratio of lactic acid is 99%, acetaldehyde be selectively 95%.
Embodiment 13
0.1368g particle diameter is at 20～40 object mesoporous aluminum phosphates, be placed in the quartz ampoule that internal diameter is 4mm, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst is placed in to heating furnace, open nitrogen and pass into 3ml/min, open heater, mode with 4 ℃/min temperature programming makes temperature reach 325 ℃, steady temperature, passes into 20% lactic acid aqueous solution with 3.0ml/h, collect product, for light yellow transparency liquid, analyze product, the conversion ratio of lactic acid is 99%, acetaldehyde be selectively 95%.
Control Example is to take MAP2 at lactic acid decarbonylation, to prepare the application in acetaldehyde as catalyst below:
0.3000g particle diameter is at 20～40 object mesoporous aluminum phosphate MAP2, be placed in the quartz ampoule that internal diameter is 4mm, with silica wool fixed catalyst aluminum phosphate, then the quartz ampoule that is filled with catalyst be placed in to heating furnace, open nitrogen and pass into 1ml/min, open heater, in the mode of 4 ℃/min temperature programming, make temperature reach 325 ℃, steady temperature, with 1.0ml/h, pass into 20% lactic acid aqueous solution, catalyst moves after 110h continuously, and conversion ratio is reduced to 65%, and acetaldehyde selectively reaches 90% left and right.
To sum up explanation, mesoporous aluminum phosphate prepared by the present invention has very strong adaptability to the variation of reaction environment, can bear the acute variation of reaction condition, when flow rate of carrier gas, lactic acid concn, charging rate change, only there is slight fluctuation in the conversion ratio of lactic acid and acetaldehyde selective.
Above-mentioned embodiment is intended to illustrate the present invention and can be professional and technical personnel in the field's realization or use; it will be apparent for those skilled in the art that above-mentioned embodiment is modified; therefore the present invention includes but be not limited to above-mentioned embodiment; any these claims or description of meeting described; meet and principle disclosed herein and novelty, the method for inventive features, technique, product, within all falling into protection scope of the present invention.
Claims (7)
1. a mesoporous aluminum phosphate catalyst, it is characterized in that being made by following methods: take the solution that aluminum nitrate that aluminium, phosphorus mol ratio is 1:1 and phosphorylated ligand make 0.3-0.6mmol/L, and regulate pH in 70-90 ℃ of stirring, to make aluminum phosphate white precipitate after 4-6 by ammoniacal liquor, afterwards described aluminum phosphate white precipitate is dried and is placed on 500-600 ℃ of roasting 5-7h in Muffle furnace, by gained pressed powder, pulverizing, get 20-40 object particle and obtain described mesoporous aluminum phosphate catalyst.
2. mesoporous aluminum phosphate catalyst according to claim 1, is characterized in that: the aperture of described mesoporous aluminum phosphate catalyst is 10-20nm, and total acid bit density is 3.5-4mmol/g, and weak acid position, middle strong acidic site density are 3-3.7mmol/g.
3. a method of preparing mesoporous aluminum phosphate catalyst described in claim 1 or 2, is characterized in that comprising the following steps:
Take the solution that aluminum nitrate that aluminium, phosphorus mol ratio is 1:1 and phosphorylated ligand make 0.3-0.6mmol/L;
It is 4-6 that the ammoniacal liquor that is 25% with mass fraction regulates pH value;
At 70-90 ℃, rapid stirring is to producing aluminum phosphate white precipitate;
Gained aluminum phosphate is deposited in to dry 120-140min under 70-90 ℃ of condition;
After dried, described aluminum phosphate is placed in to Muffle furnace 500-600 ℃ of roasting 5-7h;
The aluminum phosphate pressed powder of gained, pulverizes, and gets 20～40 object particles and obtains described mesoporous aluminum phosphate catalyst.
4. mesoporous aluminum phosphate catalyst according to claim 1 and 2 is prepared the application in acetaldehyde technique at lactic acid decarbonylation.
5. aluminium phosphate catalyst is prepared the application in acetaldehyde technique at lactic acid decarbonylation according to claim 4, it is characterized in that: described mesoporous aluminum phosphate catalyst is added to end-blocking in reaction tube, wherein add the volume of aluminium phosphate catalyst to account for the 5-15% of reaction tube volume; With carrier gas, carry lactic acid aqueous solution by the reaction tube of described aluminium phosphate catalyst is housed, 3～8 ℃/min temperature programming is to reaction temperature, and reaction temperature is 250～400 ℃, and lactic acid concn is 15～40wt%, charging rate is 1～8ml/h, and the flow velocity of carrier gas is 0.5～8mL/min.
6. mesoporous aluminum phosphate catalyst according to claim 5 is prepared the application in acetaldehyde technique at lactic acid decarbonylation, it is characterized in that: described carrier gas is nitrogen.
7. mesoporous aluminum phosphate catalyst according to claim 5 is prepared the application in acetaldehyde technique at lactic acid decarbonylation, it is characterized in that: described reaction tube is inertia material.
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| CN106268886B (en) * | 2016-07-19 | 2019-01-11 | 东莞理工学院 | A kind of carbon-doped mesoporous aluminum phosphate and its preparation method and application |
| CN108043454A (en) * | 2017-12-14 | 2018-05-18 | 吉林师范大学 | A kind of mesoporous basic catalyst and preparation method and application |
| CN108043454B (en) * | 2017-12-14 | 2020-08-07 | 吉林师范大学 | Mesoporous basic catalyst and preparation method and application thereof |
| CN113735086A (en) * | 2021-09-07 | 2021-12-03 | 宁夏沪惠药化科技有限公司 | Aluminum phosphate, preparation method and application thereof, and preparation method of o-hydroxyanisole |
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