CN108126694A - Azithromycin production platinum carbon catalyst and preparation method thereof - Google Patents
Azithromycin production platinum carbon catalyst and preparation method thereof Download PDFInfo
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- CN108126694A CN108126694A CN201711428096.1A CN201711428096A CN108126694A CN 108126694 A CN108126694 A CN 108126694A CN 201711428096 A CN201711428096 A CN 201711428096A CN 108126694 A CN108126694 A CN 108126694A
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- platinum
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- azithromycin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1856—Phosphorus; Compounds thereof with iron group metals or platinum group metals with platinum group metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0207—Pretreatment of the support
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
Abstract
A kind of azithromycin production platinum carbon catalyst, is made of platinum and activated carbon, and on the basis of the weight of the activated carbon, the mass fraction of platinum is 3%；Preparation method includes the following steps：Step 1) impregnates activated carbon using phosphorus-containing compound, then dries, under nitrogen atmosphere with 450 550 DEG C of temperature calcination 2h；Step 2) prepares the platinum acid chloride solution of 10 20g/L；Platinum acid chloride solution is introduced into activated carbon by step 3), and 2 4h of excessive dipping, drying, then the gaseous mixture reductase 12 h of logical hydrogen and nitrogen under 250 300 DEG C of temperature condition are carried out under conditions of temperature is 70 90 DEG C, pressure is 3 5MPa.The activity of platinum carbon catalyst can be increased substantially and apply mechanically number, and improve the anti-toxicity energy of platinum carbon catalyst.
Description
Technical field
The invention belongs to noble metal catalyst preparing technical fields, and in particular to a kind of azithromycin production is catalyzed with platinum charcoal
Agent and preparation method thereof.
Background technology
Azithromycin is by one of derivative of macrolides of transformation, is obtained after being modified in erythromycin structure
A kind of macrolides broad-spectrum antibiotic, mainly by being combined with bacterium 50S ribosomal subunits, the displacement of blocking peptide prevents
The synthesis of bacterial peptide and reach antibacterial action.Current azithromycin production is to be obtained by erythromycin oxime through Beckmann rearrangement
To erythromycin 6,9- imines ethers, then, it is that reducing agent is restored or using noble metal to urge through sodium borohydride or potassium borohydride
Agent carries out pressure hydration and restores to obtain.When noble metal pressure hydration is used to restore, platinum charcoal or rhodium Pd/carbon catalyst are mainly used,
And in actual production, it is contemplated that cost factor generally carries out hydrogenating reduction using platinum carbon catalyst.But platinum charcoal is being used to urge
When agent carries out hydrogenating reduction, poisoning easily occurs for catalyst, activity declines, and selective phenomena such as being deteriorated, causes catalyst set
Too low with number, production cost is excessively high.Therefore, the anti-toxicity energy of platinum carbon catalyst how is reduced, improves platinum carbon catalyst
Activity and number is applied mechanically as one of difficulties studied in azithromycin preparation process.
Due to the single active constituent of platinum carbon catalyst generally use, the knot of carrier is had been focused into its linguistic term
Structure and metal platinum are in the distribution situation of carrier, and this really also has a huge impact the performance of catalyst.Due to catalysis
Reaction is carried out on the surface of platinum particles, and therefore, the dispersion degree of platinum is higher, and the activity of catalyst is higher, and service life is longer.
At present, the carrier of platinum carbon catalyst is mainly using powdered activated carbon, platinum particles and carried by active carbon poor to platinum particles adsorptivity
Active force between body is weak, and metal easily occurs during recycling and comes off, service life is short.
The preparation of platinum carbon catalyst mainly has the methods of traditional infusion process, the precipitation method and colloidal solution method, but institute at present
The active component particles range of the catalyst of preparation is wide, grain size is big, be unevenly distributed, dispersion degree is low, it is difficult to prepare highly selective
The platinum carbon catalyst of high activity long-life.Such as infusion process, during platinum carbon catalyst is prepared, platinum nucleus can be in the liquid phase
Or grow up, reunite on carrier surface, the active component particles range of prepared catalyst is wide, grain size is big, platinum dispersion degree is low, difficult
To prepare the platinum carbon catalyst of high activity long-life.Platinum carbon catalyst active component prepared by colloidal solution method counts greatly absolutely exposed
Carrier carbon surface is deposited on, can not solve the problems, such as active component Platinum Nanoparticles and Carbon supports adhesion-tight, the initial stage in catalysis is reacted
Catalyst activity is high, but is catalyzed later stage activity rapid decrease, repeatable to apply mechanically that number is few, service life is short.
Invention content
The present invention provides a kind of azithromycin production platinum carbon catalyst and preparation method thereof, and the technology mainly solved is asked
Topic is：First, the powdered activated carbon in existing platinum carbon catalyst as carrier is poor to platinum particles adsorptivity, platinum particles with
Active force between absorbent charcoal carrier is weak, and metal easily occurs during recycling and comes off, thereby using short life；Its
Secondary, the active component particles range of the platinum carbon catalyst prepared by existing conventional method is wide, grain size is big, is unevenly distributed, divides
Divergence is low, it is difficult to prepare highly selective, high activity, the platinum carbon catalyst of long-life.
In order to solve the above technical problems, the present invention provides a kind of azithromycin production platinum carbon catalyst, by active gold
Belong to and carrier composition, the active metal be platinum, the carrier be P Modification activated carbon, using the weight of the activated carbon as
Benchmark, the mass fraction of platinum is 2-4%.
It is preferable over：On the basis of the weight of the activated carbon, the mass fraction of the platinum is 3%.
The present invention provides a kind of preparation method of azithromycin production platinum carbon catalyst, includes the following steps：
Step 1) prepares P Modification activated carbon, at normal temperatures, use mass fraction for 5% phosphorus compound to activated carbon into
The excessive dipping 4-8h of row, is then evaporated, dry, and nitrogen roasting 2h is led under 500 DEG C of temperature condition；
Step 2) prepares platinum precursor solution, weighs chloroplatinic acid, deionized water is added to be diluted to 10-20g/L, under stiring,
With sodium hydrate regulator solution pH to 2, chloroplatinic acid precursor solution, as platinum acid chloride solution is made；
The platinic acid solution being configured in step 2) is added in impregnation reactor, then adds in step by the load of step 3) platinum
It is rapid 1) in obtained P Modification activated carbon, be uniformly mixed, reactor be heated to 80 DEG C, is then applied into impregnation reactor
Plus-pressure keeps 2h at this pressure to 3-5Mpa；
Maceration extract in step 3) is evaporated by the reduction of step 4) platinum, then the dry 8h under 105 DEG C of temperature condition,
It is warming up to 250-300 DEG C later and is passed through H2-N2Gaseous mixture reductase 12 h, the H2-N2Hydrogen volume score is 5% in gaseous mixture, i.e.,
Obtain azithromycin production platinum carbon catalyst.
It is preferable over：The phosphorus-containing compound is sodium phosphate, arbitrary in sodium tripolyphosphate, sodium metaphosphate, sodium pyrophosphate
A kind of or arbitrary proportion mixture of any two.
Compared with prior art, the present invention it has the following advantages：
1st, azithromycin production of the invention is compared with the more traditional platinum carbon catalyst of platinum carbon catalyst, since activated carbon is used
Phosphorus compound is modified, and activated carbon has the aperture of bigger, is conducive to the dipping of active constituent, while have phosphorus on carrier
Compound is more advantageous to absorption of the metal platinum active constituent in activated carbon surface；
2nd, the method that the preparation method of azithromycin production platinum carbon catalyst of the invention employs impregnating by pressure solves
Platinum is difficult to be tightly held by activated carbon or adsorb the drawbacks of slow, while enter activity by the suitable platinum of variation of pressure
Inside charcoal, so as to improve conversion of the reactant in hydrogenation process；
3rd, catalyst of the present invention erythromycin 6 suitable for azithromycin production, 9- imines ethers add hydrogen, enable to platinum charcoal
The activity of catalyst is high, service life is long, repeats and applies mechanically, and improve the anti-toxicity energy of platinum carbon catalyst.
Specific embodiment
Below in conjunction with preferred embodiment a kind of azithromycin production platinum carbon catalyst and its preparation side are provided to the present invention
Method is further described.
Embodiment 1, a kind of preparation method of azithromycin production platinum carbon catalyst, step are specific as follows.
Step 1) Activated Carbon Pretreatment (prepares P Modification activated carbon), at normal temperatures, takes 10g activated carbons, by 10g activated carbons
It adds in the sodium radio-phosphate,P-32 solution that mass fraction is 5% and excessively impregnates 4-8h, be then evaporated maceration extract, then in 105 DEG C of temperature strip
It is dry under part, nitrogen roasting 2h is led under 500 DEG C of temperature condition；
Step 2) prepares platinum precursor solution (preparing platinum acid chloride solution), weighs 0.83g chloroplatinic acid crystals, adds deionization
Water is diluted to 50mL, under agitation, with sodium hydrate regulator solution pH to 2, chloroplatinic acid precursor solution is made；
The platinic acid solution being configured in step 2) is added in impregnation reactor, then adds in step by the load of step 3) platinum
It is rapid 1) in obtained P Modification activated carbon, be uniformly mixed, reactor be heated to 70 DEG C, is then applied into impregnation reactor
Plus-pressure keeps 2h at this pressure to 3Mpa；
Maceration extract in step 3) is evaporated by the reduction of step 4) platinum, then the dry 8h under 105 DEG C of temperature condition,
H later2-N2250-300 DEG C of reductase 12 h, the H are heated under gaseous mixture atmosphere2-N2Hydrogen volume score is 5% in gaseous mixture,
Obtain azithromycin production platinum carbon catalyst.
Embodiment 2, a kind of preparation method of azithromycin production platinum carbon catalyst, step are specific as follows.
Step 1) Activated Carbon Pretreatment (prepares P Modification activated carbon), at normal temperatures, takes 10g activated carbons, by 10g activated carbons
It adds in the sodium tripolyphosphate solution that mass fraction is 5% and excessively impregnates 4-8h, be then evaporated maceration extract, then in 105 DEG C of temperature
It is dry under the conditions of degree, nitrogen roasting 2h is led under 500 DEG C of temperature condition；
Step 2) prepares platinum precursor solution (preparing platinum acid chloride solution), weighs 0.83g chloroplatinic acid crystals, adds deionization
Water is diluted to 50mL, under agitation, with sodium hydrate regulator solution pH to 2, chloroplatinic acid precursor solution is made；
The platinic acid solution being configured in step 2) is added in impregnation reactor, then adds in step by the load of step 3) platinum
It is rapid 1) in obtained P Modification activated carbon, be uniformly mixed, reactor be heated to 80 DEG C, is then applied into impregnation reactor
Plus-pressure keeps 2h at this pressure to 3Mpa；
Maceration extract in step 3) is evaporated by the reduction of step 4) platinum, then the dry 8h under 105 DEG C of temperature condition,
H later2-N2250-300 DEG C of reductase 12 h, the H are heated under gaseous mixture atmosphere2-N2Hydrogen volume score is 5% in gaseous mixture,
Obtain azithromycin production platinum carbon catalyst.
Embodiment 3, a kind of preparation method of azithromycin production platinum carbon catalyst, step are specific as follows.
Step 1) Activated Carbon Pretreatment (prepares P Modification activated carbon), at normal temperatures, takes 10g activated carbons, by 10g activated carbons
It adds in the sodium radio-phosphate,P-32 solution that mass fraction is 5% and excessively impregnates 4-8h, be then evaporated maceration extract, then in 105 DEG C of temperature strip
It is dry under part, nitrogen roasting 2h is led under 500 DEG C of temperature condition；
Step 2) prepares platinum precursor solution (preparing platinum acid chloride solution), weighs 0.83g chloroplatinic acid crystals, adds deionization
Water is diluted to 50mL, under agitation, with sodium hydrate regulator solution pH to 2, chloroplatinic acid precursor solution is made；
The platinic acid solution being configured in step 2) is added in impregnation reactor, then adds in step by the load of step 3) platinum
It is rapid 1) in obtained P Modification activated carbon, be uniformly mixed, reactor be heated to 80 DEG C, is then applied into impregnation reactor
Plus-pressure keeps 2h at this pressure to 4Mpa；
Maceration extract in step 3) is evaporated by the reduction of step 4) platinum, then the dry 8h under 105 DEG C of temperature condition,
H later2-N2250-300 DEG C of reductase 12 h, the H are heated under gaseous mixture atmosphere2-N2Hydrogen volume score is 5% in gaseous mixture,
Obtain azithromycin production platinum carbon catalyst.
Embodiment 4, a kind of azithromycin production platinum carbon catalyst preparation method, step are specific as follows.
Step 1) Activated Carbon Pretreatment (prepares P Modification activated carbon), at normal temperatures, takes 10g activated carbons, by 10g activated carbons
It adds in the sodium radio-phosphate,P-32 solution that mass fraction is 5% and excessively impregnates 4-8h, be then evaporated maceration extract, then in 105 DEG C of temperature strip
It is dry under part, nitrogen roasting 2h is led under 500 DEG C of temperature condition；
Step 2) prepares platinum precursor solution (preparing platinum acid chloride solution), weighs 0.83g chloroplatinic acid crystals, adds deionization
Water is diluted to 50mL, under agitation, with sodium hydrate regulator solution pH to 2, chloroplatinic acid precursor solution is made；
The platinic acid solution being configured in step 2) is added in impregnation reactor, then adds in step by the load of step 3) platinum
It is rapid 1) in obtained P Modification activated carbon, be uniformly mixed, reactor be heated to 80 DEG C, is then applied into impregnation reactor
Plus-pressure keeps 2h at this pressure to 5Mpa；
Maceration extract in step 3) is evaporated by the reduction of step 4) platinum, then the dry 8h under 105 DEG C of temperature condition,
H later2-N2250-300 DEG C of reductase 12 h, the H are heated under gaseous mixture atmosphere2-N2Hydrogen volume score is 5% in gaseous mixture,
Obtain azithromycin production platinum carbon catalyst.
Embodiment 5, a kind of azithromycin production platinum carbon catalyst preparation method, step are specific as follows.
Step 1) Activated Carbon Pretreatment (prepares P Modification activated carbon), at normal temperatures, takes 10g activated carbons, by 10g activated carbons
It adds in the sodium phosphate and sodium metaphosphate solution that mass fraction is 5% and excessively impregnates 4-8h, be then evaporated maceration extract, then 105
DEG C temperature condition under it is dry, nitrogen roasting 2h is led under 500 DEG C of temperature condition；
Step 2) prepares platinum precursor solution (preparing platinum acid chloride solution), weighs 0.83g chloroplatinic acid crystals, adds deionization
Water is diluted to 50mL, under agitation, with sodium hydrate regulator solution pH to 2, chloroplatinic acid precursor solution is made；
The platinic acid solution being configured in step 2) is added in impregnation reactor, then adds in step by the load of step 3) platinum
It is rapid 1) in obtained P Modification activated carbon, be uniformly mixed, reactor be heated to 80 DEG C, is then applied into impregnation reactor
Plus-pressure keeps 2h at this pressure to 4Mpa；
Maceration extract in step 3) is evaporated by the reduction of step 4) platinum, then the dry 8h under 105 DEG C of temperature condition,
H later2-N2250-300 DEG C of reductase 12 h, the H are heated under gaseous mixture atmosphere2-N2Hydrogen volume score is 5% in gaseous mixture,
Obtain azithromycin production platinum carbon catalyst.
By the catalyst of conventional platinum charcoal and embodiment 1-5 for its activity of azithromycin production evaluation, specific method：Take one
Determine the 6 of quality, 9 imines ethers are dissolved in methanol and being placed in autoclave, add in 3% platinum carbon catalyst of certain mass, nitrogen displacement
After three times, hydrogen is passed through, is reacted to when hydrogen presses unchanged and stops reaction, is separated by filtration catalyst, filtrate is adjusted centainly with alkali
After pH, filtering and drying product obtain dihydro homoerythromycin, while detect its purity with liquid phase.
Result of 1 catalyst of table in 6,9 imines ethers add hydrogen
From the point of view of 1 result of table, the activity of the platinum carbon catalyst prepared by the present invention is compared with traditional conventional platinum charcoal, conversion
The raising that rate and selectivity are all shown sometimes, while conventional platinum charcoal carries out applying mechanically experiment, conventional platinum charcoal with 3 two kinds of catalyst of embodiment
5% is reduced applying mechanically 10 times or so its yields, and embodiment 3 just reduces 3% after 50 times, this result further illustrates
Catalyst can be repeated as many times and apply mechanically.
The above is only presently preferred embodiments of the present invention, and any restrictions are not done to the present invention, every according to invention skill
Any simple modification, change and the equivalent structure that art essence makees above example change, and still fall within the technology of the present invention
In the protection domain of scheme.
Claims (7)
1. a kind of azithromycin production platinum carbon catalyst, is made of active metal and carrier, it is characterised in that：The work
Property metal be platinum, the carrier is the activated carbon of P Modification, and on the basis of the weight of the activated carbon, the mass fraction of platinum is 2-
4%.
2. a kind of azithromycin production platinum carbon catalyst according to claim 1, it is characterised in that：With the activated carbon
Weight on the basis of, the mass fraction of the platinum is 3%.
A kind of 3. preparation method of the azithromycin production platinum carbon catalyst described in claims 1 or 2, which is characterized in that packet
Include following steps：
Step 1) prepares P Modification activated carbon, and activated carbon using phosphorus-containing compound is impregnated, is then dried, at 450-550 DEG C
Lead to nitrogen roasting 1.8-2.2h under temperature condition；
Step 2) prepares platinum acid chloride solution, takes chloroplatinic acid, deionized water is added to be diluted to 10-20g/L；
The platinum acid chloride solution that step 2) is prepared is introduced into the activated carbon obtained by step 1) by step 3), is 70- in temperature
90 DEG C, pressure keep 2-4h to carry out excessive dipping under conditions of 3-5MPa, then dry, then in 250-300 DEG C of temperature
Under the conditions of lead to the gaseous mixture of hydrogen and nitrogen, hydrogen volume score is 5% in the gaseous mixture, reduction 1.8-2.2h to get to
Azithromycin production platinum carbon catalyst.
4. the preparation method of azithromycin production platinum carbon catalyst according to claim 3, it is characterised in that：Above-mentioned step
It is rapid 1) in, by the activated carbon use mass fraction for 5% phosphorus-containing compound excessively dipping 4-8h, then dry, at 500 DEG C
Temperature condition under lead to nitrogen roasting 2h.
5. the preparation method of azithromycin production platinum carbon catalyst according to claim 4, it is characterised in that：Described
Phosphorus-containing compound is sodium phosphate, any one or any two the arbitrary ratio in sodium tripolyphosphate, sodium metaphosphate, sodium pyrophosphate
Example mixture.
6. the preparation method of azithromycin production platinum carbon catalyst according to claim 5, it is characterised in that：Above-mentioned step
It is rapid 2) in, after chloroplatinic acid is dissolved, with sodium hydrate regulator solution pH to 2.
7. the preparation method of azithromycin production platinum carbon catalyst according to claim 6, it is characterised in that：Above-mentioned step
It is rapid 3) in, after impregnating 2-4h, maceration extract is evaporated, then the dry 8h under 105 DEG C of temperature condition.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112156772A (en) * | 2020-09-30 | 2021-01-01 | 广州大学 | Ion poisoning noble metal catalyst and preparation method and application thereof |
| CN114308023A (en) * | 2021-12-31 | 2022-04-12 | 江苏擎动新能源科技有限公司 | Platinum-carbon catalyst and preparation method thereof |
| CN114433095A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Nickel catalyst and preparation method and application thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4131721A (en) * | 1977-06-17 | 1978-12-26 | Electric Power Research Institute, Inc. | Electrolytic cell having a novel electrode including platinum on a carbon support activated with a phosphorus-oxygen-containing compound |
| CA1148562A (en) * | 1979-02-22 | 1983-06-21 | Alfred J. Bird | Catalyst for the hydrogenation of halogen substituted aromatic nitro compounds |
| CN104084194A (en) * | 2014-07-08 | 2014-10-08 | 郴州高鑫材料有限公司 | Method for preparing high-selectivity platinum-carbon catalyst through vacuum impregnation |
| CN106693961B (en) * | 2017-01-10 | 2018-06-22 | 江西省汉氏贵金属有限公司 | Palladium carbon catalyst and preparation method and application |
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2017
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112156772A (en) * | 2020-09-30 | 2021-01-01 | 广州大学 | Ion poisoning noble metal catalyst and preparation method and application thereof |
| CN114433095A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Nickel catalyst and preparation method and application thereof |
| CN114433095B (en) * | 2020-10-20 | 2024-05-03 | 中国石油化工股份有限公司 | Nickel catalyst and preparation method and application thereof |
| CN114308023A (en) * | 2021-12-31 | 2022-04-12 | 江苏擎动新能源科技有限公司 | Platinum-carbon catalyst and preparation method thereof |
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