CN102212693A - Process for preparing silver nitrate and aluminum nitrate nonahydrate from waste silver catalyst of ethylene oxidation method - Google Patents
Process for preparing silver nitrate and aluminum nitrate nonahydrate from waste silver catalyst of ethylene oxidation method Download PDFInfo
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- CN102212693A CN102212693A CN2010105891733A CN201010589173A CN102212693A CN 102212693 A CN102212693 A CN 102212693A CN 2010105891733 A CN2010105891733 A CN 2010105891733A CN 201010589173 A CN201010589173 A CN 201010589173A CN 102212693 A CN102212693 A CN 102212693A
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- silver
- nitrate
- aluminum
- aluminum nitrate
- silver nitrate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention relates to a process for preparing silver nitrate and aluminum nitrate nonahydrate from waste silver catalyst of an ethylene oxidation method, which comprises the following steps: reacting waste silver catalyst and carrier thereof (waste residue) in a corrosion-resistant reactor (the pure mass ratio of pure substance silver to nitric acid solution is 1:(0.58-0.98)) to generate a silver nitrate/aluminum nitrate mixed solution, filtering to obtain a small amount of impurity filter cake, and sending the impurity filter cake for incineration or burial; sending the obtained clear silver nitrate/aluminum nitrate filtrate for further processing; sending the obtained clear solution into a reduced pressure distiller to carry out reduced pressure distillation; discharging when the clear solution is concentrated into a saturated solution, and cooling for crystallization and separation, wherein the silver nitrate and aluminum nitrate polyhydrate crystal are respectively precipitated according to different freezing points, and nonahydrate can be filled if water is not sufficient by amortized computation; and washing, and drying to obtain the products silver nitrate and aluminum nitrate nonahydrate crystal. The waste silver catalyst and carrier thereof (waste residue) are used as raw materials for preparing the silver bromide and aluminum tribromide hexahydrate, thereby changing wastes into valuable substances and creating considerable economic benefit.
Description
Technical field
The invention belongs to the comprehensive utilization technique field of oil organic chemical industry deep processing spent catalyst, the method for useless silver catalyst preparation Silver Nitrate of especially a kind of oxidation of ethylene method and nine water aluminum nitrates.
Background technology
The oxidation of ethylene method be ethene and air or oxygen in the presence of silver catalyst, directly gaseous oxidation generates oxyethane, forms condensed fluid absorbing by the absorption tower water.The ethene of oxidizing reaction does not continue reaction in pump around circuit reactor, and circulation absorbs until whole formation oxyethane liquid.Absorption liquid obtains the oxyethane finished product through desorb rectifying.
Most important link has been come catalyzed reaction with catalyzer silver exactly in this oxidizing reaction, and any material of silver and discord the inside reacts, so the effect of catalyzer silver is irreplaceable.Occuping above-mentioned reason, to use the cost of catalyzer silver be very high, falls as waste discharge again after katalysis is finished, not only uneconomical but also not environmental protection.Therefore research and develop catalyzer silver or other catalyzer, it is very important making it to turn waste into wealth, timely, requisite.
Its quantity discharged of oxidation of ethylene method silver catalyst will be discharged 0.0002 ton for producing product per ton, 0.2 kilogram of production discharging just per ton, and the inside also has alumina carrier to mix the abbreviation alum clay.Wherein the content of catalyzer silver is 15%, and remaining is aluminium sesquioxide all.The present invention utilizes silver catalyst and carrier waste residue thereof to prepare the method for Silver Nitrate and nine water aluminum nitrates.
Summary of the invention
Technical problem to be solved by this invention is, silver catalyst and carrier waste residue thereof are handled, comprehensive utilization, the method for preparing Silver Nitrate and nine water aluminum nitrates, a kind of method with useless silver catalyst preparation Silver Nitrate of oxidation of ethylene method and nine water aluminum nitrates is provided, this method has effectively utilized useless silver catalyst to prepare value products such as Silver Nitrate and nine water aluminum nitrates, has both created economic worth, has eliminated pollution again.
The technical solution adopted for the present invention to solve the technical problems is: the method for useless silver catalyst preparation Silver Nitrate of oxidation of ethylene method and nine water aluminum nitrates comprises the steps:
To give up silver catalyst and carrier waste residue thereof reacts in the corrosion-resistant reactor with pure mass ratio 1:0.58-0.98 with pure substance silver and salpeter solution, start agitator, carry out chemical reaction, reaction generates the mixing solutions of Silver Nitrate and aluminum nitrate, filters to obtain a spot of impurity filter cake and send to and burn or bury; Obtain clarifying Silver Nitrate and aluminum nitrate filtrate is sent to further processing;
Above-mentioned clarifying Silver Nitrate and the aluminum nitrate mixing solutions of obtaining sent to and carried out underpressure distillation in the underpressure distillation device, when being condensed into saturated solution, ejecting crystallisation by cooling separates, what at first separate out according to the difference of their zero pour is Silver Nitrate, evaporate nine crystallization water yields that reach aluminum nitrate according to conversion afterwards and just separate out nine water aluminum nitrate crystal, if can be filled to the amount of nine crystal water through the conversion water shortage, obtain Silver Nitrate and nine water aluminum nitrate crystal products through washing, drying again.
Its chemical equation is: 3Ag+4HNO
3(rare)=====3AgNO
3+ 2H
2O+NO
Al
2O
3?+6?HNO
3=====2Al(NO
3)
3·?9H
2O+3H
2O
The invention has the beneficial effects as follows: one, the invention provides a kind of method with useless silver catalyst preparation Silver Nitrate of oxidation of ethylene method and nine water aluminum nitrates, this method has effectively utilized the material of silver catalyst and carrier waste residue thereof to form, silver catalyst and carrier waste residue thereof are handled, Silver Nitrate and nine water aluminum nitrates are prepared in comprehensive utilization.Its two, Silver Nitrate and nine water aluminum nitrate purposes are wide, are two kinds of products that economic worth is bigger, have improved the economic benefit of Processing Ag catalyzer and carrier waste residue thereof, have created the repayment of very big income.Its three, less investment to the Processing Ag catalyzer and the carrier waste residue prepares Silver Nitrate and nine water aluminum nitrates are particularly suitable, be we can say and opened up a new road.Its four, the purity height of preparation, quality is guaranteed.Its five, this method has effectively been avoided the secondary pollution of oil organic chemical industry deep processing industries, turns waste into wealth in primary emission, becomes valuable Silver Nitrate and nine water aluminum nitrate products at last, creates considerable economic.
Embodiment
Embodiment 1, and the method for useless silver catalyst preparation Silver Nitrate of oxidation of ethylene method and nine water aluminum nitrates comprises the steps:
Get the catalyzer silver content and be 15%, aluminium sesquioxide content is 85% useless silver catalyst and carrier waste residue 500 kilograms of preparations Silver monobromide and six water aluminum bromides, to give up silver catalyst and carrier waste residue thereof reacts in the corrosion-resistant reactor with pure mass ratio 1:0.58 with pure substance silver and salpeter solution, start agitator, carry out chemical reaction, reaction generates the mixing solutions of the Silver Nitrate of aluminum nitrate and 88 kilograms, filters to obtain a spot of impurity filter cake and send to and burn or bury; Obtain clarifying Silver Nitrate and aluminum nitrate filtrate is sent to further processing;
Above-mentioned clarifying Silver Nitrate and the aluminum nitrate mixing solutions of obtaining sent to and carried out underpressure distillation in the underpressure distillation device, when being condensed into saturated solution, ejecting crystallisation by cooling separates, what at first separate out according to the difference of their zero pour is Silver Nitrate, evaporate nine crystallization water yields that reach aluminum nitrate according to conversion afterwards and just separate out nine water aluminum nitrate crystal, if can be filled to the amount of nine crystal water through the conversion water shortage, obtain Silver Nitrate and nine water aluminum nitrate crystal products through washing, drying again.
Embodiment 2, and the method for useless silver catalyst preparation Silver Nitrate of oxidation of ethylene method and nine water aluminum nitrates comprises the steps:
Get the catalyzer silver content and be 15%, aluminium sesquioxide content is 85% useless silver catalyst and carrier waste residue 500 kilograms of preparations Silver monobromide and six water aluminum bromides, to give up silver catalyst and carrier waste residue thereof reacts in the corrosion-resistant reactor with pure mass ratio 1:0.78 with pure substance silver and salpeter solution, start agitator, carry out chemical reaction, reaction generates the mixing solutions of the Silver Nitrate of aluminum nitrate and 118 kilograms, filters to obtain a spot of impurity filter cake and send to and burn or bury; Obtain clarifying Silver Nitrate and aluminum nitrate filtrate is sent to further processing;
Above-mentioned clarifying Silver Nitrate and the aluminum nitrate mixing solutions of obtaining sent to and carried out underpressure distillation in the underpressure distillation device, when being condensed into saturated solution, ejecting crystallisation by cooling separates, what at first separate out according to the difference of their zero pour is Silver Nitrate, evaporate nine crystallization water yields that reach aluminum nitrate according to conversion afterwards and just separate out nine water aluminum nitrate crystal, if can be filled to the amount of nine crystal water through the conversion water shortage, obtain Silver Nitrate and nine water aluminum nitrate crystal products through washing, drying again.
Embodiment 3, and the method for useless silver catalyst preparation Silver Nitrate of oxidation of ethylene method and nine water aluminum nitrates comprises the steps:
Get the catalyzer silver content and be 15%, aluminium sesquioxide content is 85% useless silver catalyst and carrier waste residue 500 kilograms of preparations Silver monobromide and six water aluminum bromides, to give up silver catalyst and carrier waste residue thereof reacts in the corrosion-resistant reactor with pure mass ratio 1:0.98 with pure substance silver and salpeter solution, start agitator, carry out chemical reaction, reaction generates the mixing solutions of the Silver Nitrate of aluminum nitrate and 148.9 kilograms, filters to obtain a spot of impurity filter cake and send to and burn or bury; Obtain clarifying Silver Nitrate and aluminum nitrate filtrate is sent to further processing;
Claims (1)
1. the method for useless silver catalyst preparation Silver Nitrate of oxidation of ethylene method and nine water aluminum nitrates is characterized in that comprising the steps:
To give up silver catalyst and carrier waste residue thereof reacts in the corrosion-resistant reactor with pure mass ratio 1:0.58-0.98 with pure substance silver and salpeter solution, start agitator, carry out chemical reaction, reaction generates the mixing solutions of Silver Nitrate and aluminum nitrate, filters to obtain a spot of impurity filter cake and send to and burn or bury; Obtain clarifying Silver Nitrate and aluminum nitrate filtrate is sent to further processing;
Above-mentioned clarifying Silver Nitrate and the aluminum nitrate mixing solutions of obtaining sent to and carried out underpressure distillation in the underpressure distillation device, when being condensed into saturated solution, ejecting crystallisation by cooling separates, difference according to their zero pour, what at first separate out is Silver Nitrate, nine crystallization water yields that reach aluminum nitrate according to conversion evaporation are just separated out nine water aluminum nitrate crystal afterwards, if can be filled to the amount of nine crystal water through the conversion water shortage, have obtained Silver Nitrate and nine water aluminum nitrate crystal products through washing, drying again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105891733A CN102212693A (en) | 2010-12-15 | 2010-12-15 | Process for preparing silver nitrate and aluminum nitrate nonahydrate from waste silver catalyst of ethylene oxidation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105891733A CN102212693A (en) | 2010-12-15 | 2010-12-15 | Process for preparing silver nitrate and aluminum nitrate nonahydrate from waste silver catalyst of ethylene oxidation method |
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| Publication Number | Publication Date |
|---|---|
| CN102212693A true CN102212693A (en) | 2011-10-12 |
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| CN2010105891733A Pending CN102212693A (en) | 2010-12-15 | 2010-12-15 | Process for preparing silver nitrate and aluminum nitrate nonahydrate from waste silver catalyst of ethylene oxidation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110964906A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Photovoltaic module recycling method |
| CN110964909A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Recovery method of waste photovoltaic module |
| CN110964907A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Recycling method of waste photovoltaic module |
| CN110964908A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Recycling method of photovoltaic module |
-
2010
- 2010-12-15 CN CN2010105891733A patent/CN102212693A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110964906A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Photovoltaic module recycling method |
| CN110964909A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Recovery method of waste photovoltaic module |
| CN110964907A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Recycling method of waste photovoltaic module |
| CN110964908A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Recycling method of photovoltaic module |
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Application publication date: 20111012 |