CN105413754A - Method for preparing bone carrier catalyst - Google Patents
Method for preparing bone carrier catalyst Download PDFInfo
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- CN105413754A CN105413754A CN201510920279.XA CN201510920279A CN105413754A CN 105413754 A CN105413754 A CN 105413754A CN 201510920279 A CN201510920279 A CN 201510920279A CN 105413754 A CN105413754 A CN 105413754A
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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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/26—Chromium
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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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
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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
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B37/00—Reactions without formation or introduction of functional groups containing hetero atoms, involving either the formation of a carbon-to-carbon bond between two carbon atoms not directly linked already or the disconnection of two directly linked carbon atoms
- C07B37/02—Addition
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B41/00—Formation or introduction of functional groups containing oxygen
- C07B41/04—Formation or introduction of functional groups containing oxygen of ether, acetal or ketal groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B41/00—Formation or introduction of functional groups containing oxygen
- C07B41/12—Formation or introduction of functional groups containing oxygen of carboxylic acid ester groups
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- Engineering & Computer Science (AREA)
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Abstract
The invention relates to a method for preparing a bone carrier catalyst, and belongs to the field of catalyst preparation. The method includes the steps that abandoned bovine bones are used as raw materials, the bovine bones are put into a pot to be cooked and degreased, the degreased bovine bones are dried and put into a carbonizing stove to be carbonized, the carbonized bovine bones are immersed into a mixed solution of magnesium nitrate and chromic nitrate, the mixture is placed into an ultrasonator to be subjected to an oscillating reaction and put into a muffle furnace to be heated to a set temperature in a temperature programming mode after being dried, and the aggregate carrier catalyst is obtained after high-temperature calcination.
Description
Technical field
The present invention relates to a kind of preparation method of aggregate carried catalyst, belong to field of catalyst preparation.
Background technology
Along with industrialized growing, the equilibrium state of harmonious co-existence between man and nature is destroyed in a lot of fields.As accounted for the increasing of the maximum fossil energy use of energy-output ratio, the exhaustion gradually of fossil energy requires that the mankind must gradually reduce fossil energy share, increase renewable with novel energy share, also human knowledge is made to have arrived the recyclability of the importance of environmental protection and the energy, the feature of environmental protection for the significance of human development to the energy system transition of setting up sustainable development, so living beings obtain and pay attention to more widely because of its low emission, the natural characteristic such as never exhausted.
Natural prodcuts, as the incomplete charing of the materials such as carbohydrate, starch and cellulose, can produce the Carbon Materials of rigidity.These Carbon Materials are made up of many polycyclic aromatic charcoals, after carrying out sulfonation modifying, can prepare and stable have certain acidity and have the catalyst of better catalytic activity this kind of Carbon Materials deriving from common natural prodcuts.
Summary of the invention
The technical problem that the present invention mainly solves, for being applied to petrochemical industry at present, the solid sulfoacid catalyst of the industries such as smelting is raw material mainly with non-renewable charcoal sources such as oil, high and the defect such as non-renewable of cost of material, provide a kind of preparation method of aggregate carried catalyst, the method with discarded ox bone for raw material, first put it into boiling degreasing in pot, drying is afterwards put into retort and is carbonized, immersed in magnesium nitrate and chromic nitrate mixed solution again, be placed on oscillating reactions in ultrasonator, namely a kind of aggregate carried catalyst is obtained after putting into Muffle furnace temperature programming to design temperature high-temperature calcination after drying.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) take the ox bone that 1 ~ 2kg meat-packing plant leaves over, first reject meat slag unnecessary on bone with cutter, put it into iron pan afterwards, in pot, add deionized water, submergence ox bone, be heated to 100 ~ 105 DEG C afterwards, boiling 1 ~ 2h is to ox bone degreasing;
(2) put in an oven by the ox bone after degreasing, set temperature is 105 ~ 110 DEG C, dry 1 ~ 2h, afterwards drying is obtained ox bone and puts into and estimate after material pulverizer pulverizes, cross 30 ~ 40 mesh standard sieves, obtain ox bone fragment, for subsequent use;
(3) above-mentioned obtained ox bone fragment is put into retort, first with the ramp to 250 DEG C of 40 ~ 45 DEG C/min, insulation 30 ~ 60min, again with the ramp to 350 DEG C of 0.8 ~ 0.9 DEG C/min, insulation 90 ~ 100min, ox bone is carried out charing process, after being cooled to room temperature, being placed in drier and preserving;
(4) magnesium nitrate nitrogen radio-frequency is resolved into magnesia, nitrogen radio-frequency frequency is 5 ~ 10MHz, spent acid is added subsequently in reaction bulb, slow stirring, rotating speed is 80 ~ 100r/min, adds the chromium nitrate solution that concentration is 0.2 ~ 0.5mol/L after having stirred again, magnetic agitation 5 hours, rotating speed is 500 ~ 600r/min, obtains maceration extract;
(5) poured in 2L beaker by above-mentioned obtained charing ox bone, and add maceration extract in beaker, until will carbonize ox bone submergence, be placed in sonic oscillation instrument, sonic oscillation reaction 1 ~ 2h, supersonic frequency is 25 ~ 35KHz, and ultrasonic power is 100W;
(6) after sonic oscillation terminates, the charing aggregate of loaded metal ion is put into Muffle furnace, is warming up to 500 ~ 600 DEG C, high-temperature calcination 2 ~ 3h, after being cooled to room temperature, namely obtain a kind of aggregate carried catalyst.
Embody rule method of the present invention is: when esterification, addition or aldolisation carry out, add the catalyst that 1 ~ 5g the present invention obtains, under the effect of catalyst, product yield reaches more than 90%, and reaction rate improves 40 ~ 50%.
The invention has the beneficial effects as follows: the present invention obtains catalyst and instead of non-renewable resources as raw material using biological material ox bone, production process environmental protection, the catalyst efficiency produced is high, with low cost, reuses number of times apparently higher than typical catalyst.
Detailed description of the invention
Take the ox bone that 1 ~ 2kg meat-packing plant leaves over, first reject meat slag unnecessary on bone with cutter, put it into iron pan afterwards, in pot, add deionized water, submergence ox bone, be heated to 100 ~ 105 DEG C afterwards, boiling 1 ~ 2h is to ox bone degreasing; Put in an oven by the ox bone after degreasing, set temperature is 105 ~ 110 DEG C, dry 1 ~ 2h, afterwards drying is obtained ox bone and puts into and estimate after material pulverizer pulverizes, cross 30 ~ 40 mesh standard sieves, obtain ox bone fragment, for subsequent use; Above-mentioned obtained ox bone fragment is put into retort, first with the ramp to 250 DEG C of 40 ~ 45 DEG C/min, insulation 30 ~ 60min, again with the ramp to 350 DEG C of 0.8 ~ 0.9 DEG C/min, insulation 90 ~ 100min, ox bone is carried out charing process, after being cooled to room temperature, being placed in drier and preserving; Magnesium nitrate nitrogen radio-frequency is resolved into magnesia, nitrogen radio-frequency frequency is 5 ~ 10MHz, spent acid is added subsequently in reaction bulb, slow stirring, rotating speed is 80 ~ 100r/min, adds the chromium nitrate solution that concentration is 0.2 ~ 0.5mol/L after having stirred again, magnetic agitation 5 hours, rotating speed is 500 ~ 600r/min, obtains maceration extract; Poured in 2L beaker by above-mentioned obtained charing ox bone, and add maceration extract in beaker, until will carbonize ox bone submergence, be placed in sonic oscillation instrument, sonic oscillation reaction 1 ~ 2h, supersonic frequency is 25 ~ 35KHz, and ultrasonic power is 100W; After sonic oscillation terminates, the charing aggregate of loaded metal ion is put into Muffle furnace, is warming up to 500 ~ 600 DEG C, high-temperature calcination 2 ~ 3h, after being cooled to room temperature, namely obtain a kind of aggregate carried catalyst.
Example 1
Take the ox bone that 1kg meat-packing plant leaves over, first reject meat slag unnecessary on bone with cutter, put it into iron pan afterwards, in pot, add deionized water, submergence ox bone, be heated to 100 DEG C afterwards, boiling 1h is to ox bone degreasing; Put in an oven by the ox bone after degreasing, set temperature is 105 DEG C, dry 1h, drying is obtained after ox bone puts into and estimate material pulverizer pulverizes afterwards, crosses 30 mesh standard sieves, obtain ox bone fragment, for subsequent use; Above-mentioned obtained ox bone fragment is put into retort, first with the ramp to 250 DEG C of 40 DEG C/min, insulation 30min, again with the ramp to 350 DEG C of 0.8 DEG C/min, insulation 90min, carries out charing process by ox bone, after being cooled to room temperature, being placed in drier and preserving; Magnesium nitrate nitrogen radio-frequency is resolved into magnesia, nitrogen radio-frequency frequency is 5MHz, spent acid is added subsequently in reaction bulb, slow stirring, rotating speed is 80r/min, adds the chromium nitrate solution that concentration is 0.2mol/L after having stirred again, magnetic agitation 5 hours, rotating speed is 500r/min, obtains maceration extract; Poured in 2L beaker by above-mentioned obtained charing ox bone, and add maceration extract in beaker, until will carbonize ox bone submergence, be placed in sonic oscillation instrument, sonic oscillation reaction 1h, supersonic frequency is 25KHz, and ultrasonic power is 100W; After sonic oscillation terminates, the charing aggregate of loaded metal ion is put into Muffle furnace, is warming up to 500 DEG C, high-temperature calcination 2h, after being cooled to room temperature, namely obtain a kind of aggregate carried catalyst.
Embody rule method of the present invention is: when esterification, addition or aldolisation carry out, add the catalyst that 1g the present invention obtains, under the effect of catalyst, product yield reaches more than 90%, and reaction rate improves 40%.
Example 2
Take the ox bone that 1kg meat-packing plant leaves over, first reject meat slag unnecessary on bone with cutter, put it into iron pan afterwards, in pot, add deionized water, submergence ox bone, be heated to 103 DEG C afterwards, boiling 1h is to ox bone degreasing; Put in an oven by the ox bone after degreasing, set temperature is 108 DEG C, dry 1h, drying is obtained after ox bone puts into and estimate material pulverizer pulverizes afterwards, crosses 35 mesh standard sieves, obtain ox bone fragment, for subsequent use; Above-mentioned obtained ox bone fragment is put into retort, first with the ramp to 250 DEG C of 43 DEG C/min, insulation 45min, again with the ramp to 350 DEG C of 0.8 DEG C/min, insulation 95min, carries out charing process by ox bone, after being cooled to room temperature, being placed in drier and preserving; Magnesium nitrate nitrogen radio-frequency is resolved into magnesia, nitrogen radio-frequency frequency is 8MHz, spent acid is added subsequently in reaction bulb, slow stirring, rotating speed is 90r/min, adds the chromium nitrate solution that concentration is 0.4mol/L after having stirred again, magnetic agitation 5 hours, rotating speed is 550r/min, obtains maceration extract; Poured in 2L beaker by above-mentioned obtained charing ox bone, and add maceration extract in beaker, until will carbonize ox bone submergence, be placed in sonic oscillation instrument, sonic oscillation reaction 1h, supersonic frequency is 30KHz, and ultrasonic power is 100W; After sonic oscillation terminates, the charing aggregate of loaded metal ion is put into Muffle furnace, is warming up to 550 DEG C, high-temperature calcination 2h, after being cooled to room temperature, namely obtain a kind of aggregate carried catalyst.
Embody rule method of the present invention is: when esterification, addition or aldolisation carry out, add the catalyst that 3g the present invention obtains, under the effect of catalyst, product yield reaches more than 90%, and reaction rate improves 45%.
Example 3
Take the ox bone that 2kg meat-packing plant leaves over, first reject meat slag unnecessary on bone with cutter, put it into iron pan afterwards, in pot, add deionized water, submergence ox bone, be heated to 105 DEG C afterwards, boiling 2h is to ox bone degreasing; Put in an oven by the ox bone after degreasing, set temperature is 110 DEG C, dry 2h, drying is obtained after ox bone puts into and estimate material pulverizer pulverizes afterwards, crosses 40 mesh standard sieves, obtain ox bone fragment, for subsequent use; Above-mentioned obtained ox bone fragment is put into retort, first with the ramp to 250 DEG C of 45 DEG C/min, insulation 30 ~ 60min, again with the ramp to 350 DEG C of 0.9 DEG C/min, insulation 100min, carries out charing process by ox bone, after being cooled to room temperature, being placed in drier and preserving; Magnesium nitrate nitrogen radio-frequency is resolved into magnesia, nitrogen radio-frequency frequency is 10MHz, spent acid is added subsequently in reaction bulb, slow stirring, rotating speed is 100r/min, adds the chromium nitrate solution that concentration is 0.5mol/L after having stirred again, magnetic agitation 5 hours, rotating speed is 600r/min, obtains maceration extract; Poured in 2L beaker by above-mentioned obtained charing ox bone, and add maceration extract in beaker, until will carbonize ox bone submergence, be placed in sonic oscillation instrument, sonic oscillation reaction 2h, supersonic frequency is 35KHz, and ultrasonic power is 100W; After sonic oscillation terminates, the charing aggregate of loaded metal ion is put into Muffle furnace, is warming up to 600 DEG C, high-temperature calcination 3h, after being cooled to room temperature, namely obtain a kind of aggregate carried catalyst.
Embody rule method of the present invention is: when esterification, addition or aldolisation carry out, add the catalyst that 5g the present invention obtains, under the effect of catalyst, product yield reaches more than 90%, and reaction rate improves 50%.
Claims (1)
1. a preparation method for aggregate carried catalyst, is characterized in that concrete preparation process is:
(1) take the ox bone that 1 ~ 2kg meat-packing plant leaves over, first reject meat slag unnecessary on bone with cutter, put it into iron pan afterwards, in pot, add deionized water, submergence ox bone, be heated to 100 ~ 105 DEG C afterwards, boiling 1 ~ 2h is to ox bone degreasing;
(2) put in an oven by the ox bone after degreasing, set temperature is 105 ~ 110 DEG C, dry 1 ~ 2h, afterwards drying is obtained ox bone and puts into and estimate after material pulverizer pulverizes, cross 30 ~ 40 mesh standard sieves, obtain ox bone fragment, for subsequent use;
(3) above-mentioned obtained ox bone fragment is put into retort, first with the ramp to 250 DEG C of 40 ~ 45 DEG C/min, insulation 30 ~ 60min, again with the ramp to 350 DEG C of 0.8 ~ 0.9 DEG C/min, insulation 90 ~ 100min, ox bone is carried out charing process, after being cooled to room temperature, being placed in drier and preserving;
(4) magnesium nitrate nitrogen radio-frequency is resolved into magnesia, nitrogen radio-frequency frequency is 5 ~ 10MHz, spent acid is added subsequently in reaction bulb, slow stirring, rotating speed is 80 ~ 100r/min, adds the chromium nitrate solution that concentration is 0.2 ~ 0.5mol/L after having stirred again, magnetic agitation 5 hours, rotating speed is 500 ~ 600r/min, obtains maceration extract;
(5) poured in 2L beaker by above-mentioned obtained charing ox bone, and add maceration extract in beaker, until will carbonize ox bone submergence, be placed in sonic oscillation instrument, sonic oscillation reaction 1 ~ 2h, supersonic frequency is 25 ~ 35KHz, and ultrasonic power is 100W;
(6) after sonic oscillation terminates, the charing aggregate of loaded metal ion is put into Muffle furnace, is warming up to 500 ~ 600 DEG C, high-temperature calcination 2 ~ 3h, after being cooled to room temperature, namely obtain a kind of aggregate carried catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510920279.XA CN105413754A (en) | 2015-12-12 | 2015-12-12 | Method for preparing bone carrier catalyst |
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| CN201510920279.XA CN105413754A (en) | 2015-12-12 | 2015-12-12 | Method for preparing bone carrier catalyst |
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| CN105413754A true CN105413754A (en) | 2016-03-23 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113941324A (en) * | 2021-09-23 | 2022-01-18 | 中国科学技术大学 | Bone-supported catalyst for producing succinic acid and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100880513B1 (en) * | 2007-10-24 | 2009-01-28 | 주식회사 포스코 | Manufacturing method of desulfurization catalyst use of blast furnace slag |
| CN101993068A (en) * | 2010-10-27 | 2011-03-30 | 北京化工大学 | Preparation method of porous structured active carbon |
| CN103121681A (en) * | 2013-01-28 | 2013-05-29 | 江苏国正新材料科技有限公司 | Preparation method of high-performance bone black |
| CN105107527A (en) * | 2015-09-27 | 2015-12-02 | 常州市奥普泰科光电有限公司 | Method for preparing millet carrier catalysts |
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- 2015-12-12 CN CN201510920279.XA patent/CN105413754A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100880513B1 (en) * | 2007-10-24 | 2009-01-28 | 주식회사 포스코 | Manufacturing method of desulfurization catalyst use of blast furnace slag |
| CN101993068A (en) * | 2010-10-27 | 2011-03-30 | 北京化工大学 | Preparation method of porous structured active carbon |
| CN103121681A (en) * | 2013-01-28 | 2013-05-29 | 江苏国正新材料科技有限公司 | Preparation method of high-performance bone black |
| CN105107527A (en) * | 2015-09-27 | 2015-12-02 | 常州市奥普泰科光电有限公司 | Method for preparing millet carrier catalysts |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113941324A (en) * | 2021-09-23 | 2022-01-18 | 中国科学技术大学 | Bone-supported catalyst for producing succinic acid and preparation method thereof |
| CN113941324B (en) * | 2021-09-23 | 2022-09-30 | 中国科学技术大学 | Bone-supported catalyst for producing succinic acid and preparation method thereof |
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Application publication date: 20160323 |