CN106517296A - Method for preparing cerium oxide by using herbaceous plant precipitating agent - Google Patents
Method for preparing cerium oxide by using herbaceous plant precipitating agent Download PDFInfo
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- CN106517296A CN106517296A CN201611052631.3A CN201611052631A CN106517296A CN 106517296 A CN106517296 A CN 106517296A CN 201611052631 A CN201611052631 A CN 201611052631A CN 106517296 A CN106517296 A CN 106517296A
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- cerium oxide
- herbaceous plant
- precipitant
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for preparing cerium oxide by using a herbaceous plant precipitating agent. The method comprises the following steps: adding a rare earth cerium solution of which the concentration is 0.1 to 2 mol/L in a reaction kettle, and heating to 20 to 100 DEG C; adding the herbaceous plant precipitating agent in the reaction kettle, wherein the mass ratio of a solution of the herbaceous plant precipitating agent and a solute in the rare earth cerium solution is (5 to 50) : 1; obtaining white crystalline precipitate when the pH (Potential of Hydrogen) value of a reaction system is up to 6 to 8; enabling the precipitate and a mother solution to commonly standing under room temperature for aging for 0 to 72 hours; firing the white precipitate under 800 to 1200 DEG C for 1 to 5 hours after filtering and washing, thus obtaining a faint yellow cerium oxide product. According to the method disclosed by the invention, ammonium hydrogen carbonate is not consumed, environment protection is realized, and the cerium oxide product of which the precipitate crystal form is good and the purity is high can be prepared.
Description
Technical field
The present invention relates to a kind of inorganic material preparation process technology, specifically, is related to a kind of herbaceous plant precipitant system
The method of preparing cerium oxide.
Background technology
Cerium oxide (CeO2) it is one of staple product in light rare earth.Because which has good physicochemical properties, therefore
The fields such as civilian, military and high-tech obtain preferably application.Such as in rare earth glass, ceramics, catalyst, polishing powder, luminous
The application of the aspects such as material constantly develops, and prospect is preferable.
China produces CeO2Technology and equipment Jing update with it is perfect, have been enter into the global same industry rank of advanced units
In.The Technology commonly used in China's industrialized production at present has following several:1) chemical oxidization method, including air oxidation process and
Potassium permanganate oxidation method；2) roasting oxidation method；3) extraction separation method, including P204And P507The extraction point in sulphuric acid or hydrochloric acid medium
From.
Air oxidation process is mixing rare earth hydrate (RE (OH)3) it is raw material, it is slurried with water, and adjusts concentration and acid
Degree, is heated to 85 DEG C, the Ce (OH) being passed through during air makes serosity3It is oxidized to Ce (OH)4, then chemically treated make CeO2Product.
The method is to produce thick CeO at present2Key industry method, process is brief, and equipment is few, operation easily, the oxygenation efficiency of cerium and recovery
Rate is higher, and yield is big, and labor condition is good, but product quality is low.Roasting oxidation method with mixed rare earth concentrate (w (REO) >=
50%, w (CeO250%) and fluoro-carbon-cerium ore concentrate (w (REO)) >=50%, w (CeO) ≈2) 50%) ≈ as raw material, concentrate is put
The roasting at 700～800 DEG C in the rotary calciner, makes rare earth be changed into REO, Ce therein3+It is oxidized to Ce4+(CeO2), use
Carry out chemical treatment after sulfuric acid leaching again and make CeO2Product.The product purity of this technique is high, and labor condition is good, but CeO2Return
Yield is low, and process is slightly long.
Extraction separation method is with RE2(SO4)3Or RECl3For raw material, P is used204Or P507Extraction Ce3+It is allowed to and other rare earth elements
Separate, then use hydrochloric acid back extraction, then Jing precipitations, calcination to make CeO2Product.The technical process is simple and can be continuous, required to set
Standby less, processing ease, products obtained therefrom CeO2Purity and the response rate are all higher.Therefore it is at present industrial mainly using extract and separate,
Technique productions CeO of ignition of precipitate2。
Oxalic acid and ammonium hydrogen carbonate are all industrially to prepare the conventional precipitant of cerium oxide, and oxalate precipitation process has precipitate
Crystal formation is good, it is easy to the advantages of filtering, and ammonium bicarbonate precipitation method has the advantages that low cost, but the precipitation waste water that the method is produced contains
The NH of high concentration4Cl, if directly discharged, can cause the eutrophication of water body, and urgent need exploitation is new to be precipitated without ammonia and nitrogen pollution
Technique.
Patented technology CN105603222A discloses a kind of preparation method of herbaceous plant rare-earth precipitation agent, present invention application
The herbaceous plant precipitant prepares cerium oxide, and the method does not consume ammonium hydrogen carbonate, environmental protection, and precipitate crystal formation can be obtained
It is good, the high cerium oxide product of purity.
The content of the invention
Technical problem solved by the invention is to provide a kind of method for preparing cerium oxide with herbaceous plant precipitant, does not disappear
Consumption ammonium hydrogen carbonate, environmental protection, and can be obtained that precipitate crystal formation is good, the high cerium oxide product of purity.
Technical scheme is as follows：
A kind of method for preparing cerium oxide with herbaceous plant precipitant, including：
The cerium solution of 0.1～2mol/L of concentration is added in reactor and 20～100 DEG C are heated to, and is added thereto to
Herbaceous plant precipitant, herbaceous plant precipitant liquid quality are 5～50 with Solute mass ratio in cerium solution：1, reactant
When being that pH value reaches 6～8, white crystalline precipitation is obtained；
Will precipitation and mother solution in the common still aging 0～72h of room temperature, white precipitate is Jing filtering, after washing, 800～
1200 DEG C of 1～5h of calcination, obtain faint yellow cerium oxide product.
Further：Cerium solution adopts solution of cerium chloride by oxidation or cerous nitrate solution.
Further：Cerium solution is using cerium chloride and the mixed solution of cerous nitrate.
Further：The solution of cerium chloride by oxidation of 100L concentration 0.5mol/L is added in reactor and 40 DEG C are heated to, thereto
130L herbaceous plant precipitant, pH value of reaction system is added to reach 7, obtain white crystalline precipitation；To precipitate with mother solution in room temperature
Common still aging 12h, after white precipitate filtration, washing, in 800 DEG C of calcination 4h, obtains faint yellow cerium oxide product.
Further：The cerous nitrate solution of 10L concentration 0.92mol/L is added in reactor and 60 DEG C are heated to, thereto
20L herbaceous plant precipitant, pH value of reaction system is added to reach 6.5, obtain white crystalline precipitation；To precipitate with mother solution in room temperature
Common still aging 4h, after white precipitate filtration, washing, in 1000 DEG C of calcination 3h, obtains faint yellow cerium oxide product.
Further：The cerous nitrate solution of 1m3 concentration 0.75mol/L is added in reactor and 93 DEG C are heated to, thereto
2m3 herbaceous plant precipitant, pH value of reaction system is added to reach 7, obtain white crystalline precipitation；Will be precipitation common in room temperature with mother solution
With still aging 24h, after white precipitate filtration, washing, in 1100 DEG C of calcination 2h, faint yellow cerium oxide product is obtained.
Further：The solution of cerium chloride by oxidation of 10M3 concentration 1.5mol/L is added in reactor and 93 DEG C are heated to, thereto
4M3 herbaceous plant precipitant, pH value of reaction system is added to reach 6.7, obtain white crystalline precipitation；To precipitate with mother solution in room temperature
Common still aging 12h, after white precipitate filtration, washing, in 1200 DEG C of calcination 2h, obtains faint yellow cerium oxide product.
Compared with prior art, the technology of the present invention effect includes：The present invention prepares oxidation using the herbaceous plant precipitant
Cerium, the method do not consume ammonium hydrogen carbonate, environmental protection, and can be obtained that precipitate crystal formation is good, the high cerium oxide product of purity.
1st, the present invention prepares cerium oxide using herbaceous plant precipitant, and product yield is more than 98%；
2nd, the present invention prepares cerium oxide with herbaceous plant precipitant, and the precipitation for obtaining easily is filtered, washed, and is suitable to industrial metaplasia
Produce；
3rd, the present invention prepares cerium oxide using herbaceous plant precipitant and may replace ammonium hydrogencarbonate, the oxalic acid that current technology is used
Deng industrial chemicals, do not produce containing ammonia nitrogen or acid-bearing wastewater, can also effectively solving production enterprise while enterprise's production capacity is reduced
The discharge of wastewater problem of industry.
Description of the drawings
Fig. 1 is the process chart of the method for preparing cerium oxide in the present invention with herbaceous plant precipitant.
Specific embodiment
Technical solution of the present invention is elaborated below with reference to example embodiment.However, example embodiment can
Implement in a variety of forms, and be not understood as limited to embodiment set forth herein；Conversely, thesing embodiments are provided so that
The design of example embodiment more comprehensively and completely, and is comprehensively conveyed to those skilled in the art by the present invention.
The method that cerium oxide is prepared with herbaceous plant precipitant is a kind of low cost, in mother liquor of precipitation of ammonium waste water without ammonia nitrogen
The preparation technology of cerium oxide, specifically includes following steps：
Step 1：Add in reactor 0.1～2mol/L of concentration (in terms of REO) cerium solution and be heated to 20～
100 DEG C, it is added thereto to herbaceous plant precipitant, herbaceous plant precipitant liquid quality and Solute mass in cerium solution
(being counted with REO) ratio is as 5～50:1, when pH value of reaction system reaches 6～8, obtain the white crystalline precipitation of easy filtration；
Cerium solution adopts solution of cerium chloride by oxidation or cerous nitrate solution, or molten with the mixing of cerous nitrate using cerium chloride
Liquid.
Step 2：Will precipitation and mother solution in the common still aging 0～72h of room temperature, white precipitate is Jing filtering, after washing,
800～1200 DEG C of 1～5h of calcination, obtain faint yellow cerium oxide product.
After testing, product yield is more than 98%, NH in mother solution4 +Concentration is less than 2mg/L.
Embodiment 1
The solution of cerium chloride by oxidation of 100L concentration 0.5mol/L is added in reactor and 40 DEG C are heated to, and is added thereto to 130L
Herbaceous plant precipitant, pH value of reaction system reach 7, obtain the white crystalline precipitation of easy filtration, will precipitate with mother solution in room temperature
Common still aging 12h, after white precipitate filtration, washing, in 800 DEG C of calcination 4h, obtains faint yellow cerium oxide product, product
Yield is more than 99.2%, NH in mother liquor of precipitation of ammonium4 +Concentration is 1.5mg/L.
Embodiment 2
The cerous nitrate solution of 10L concentration 0.92mol/L is added in reactor and 60 DEG C are heated to, and is added thereto to 20L
Herbaceous plant precipitant, pH value of reaction system reach 6.5, obtain the white crystalline precipitation of easy filtration, will precipitate with mother solution in room
Warm common still aging 4h, after white precipitate filtration, washing, in 1000 DEG C of calcination 3h, obtains faint yellow cerium oxide product, produces
Product yield is more than 99.3%, NH in mother liquor of precipitation of ammonium4 +Concentration is 0.8mg/L.
Embodiment 3
1M is added in reactor3The cerous nitrate solution of concentration 0.75mol/L is simultaneously heated to 93 DEG C, is added thereto to 2M3Grass
This plant precipitant, pH value of reaction system reach 7, obtain the white crystalline precipitation of easily filtration, will be precipitation common in room temperature with mother solution
With still aging 24h, after white precipitate filtration, washing, in 1100 DEG C of calcination 2h, faint yellow cerium oxide product, product is obtained
Yield is more than 98.8%, NH in mother liquor of precipitation of ammonium4 +Concentration is 1.0mg/L.
Embodiment 4
10M is added in reactor3The solution of cerium chloride by oxidation of concentration 1.5mol/L is simultaneously heated to 93 DEG C, is added thereto to 4M3Grass
This plant precipitant, pH value of reaction system reach 6.7, obtain the white crystalline precipitation of easy filtration, will precipitate with mother solution in room temperature
Common still aging 12h, after white precipitate filtration, washing, in 1200 DEG C of calcination 2h, obtains faint yellow cerium oxide product, produces
Product yield is more than 99.5%, NH in mother solution4 +Concentration is 1.2mg/L.
Term used herein is explanation and exemplary, and nonrestrictive term.As the present invention can be with various
Form be embodied as without deviating from invention it is spiritual or substantive, it should therefore be appreciated that above-described embodiment be not limited to it is any aforesaid
Details, and should widely explaining in the spirit and scope limited by appended claims, thus fall into claim or its etc.
Whole changes and remodeling in the range of effect all should be appended claims and be covered.
Claims (7)
1. a kind of method for preparing cerium oxide with herbaceous plant precipitant, including：
The cerium solution of 0.1～2mol/L of concentration is added in reactor and 20～100 DEG C are heated to, and is added thereto to draft
Plant precipitant, herbaceous plant precipitant liquid quality are 5～50 with Solute mass ratio in cerium solution：1, reaction system pH
When value reaches 6～8, white crystalline precipitation is obtained；
Will precipitation and mother solution in the common still aging 0～72h of room temperature, white precipitate is Jing filtering, after washing, at 800～1200 DEG C
1～5h of calcination, obtains faint yellow cerium oxide product.
2. the method for preparing cerium oxide with herbaceous plant precipitant as claimed in claim 1, it is characterised in that：Cerium solution is adopted
With solution of cerium chloride by oxidation or cerous nitrate solution.
3. the method for preparing cerium oxide with herbaceous plant precipitant as claimed in claim 1, it is characterised in that：Cerium solution is adopted
With cerium chloride and the mixed solution of cerous nitrate.
4. the method for preparing cerium oxide with herbaceous plant precipitant as described in claims 1 or 2, it is characterised in that：To reaction
The solution of cerium chloride by oxidation of 100L concentration 0.5mol/L is added in kettle and 40 DEG C are heated to, and is added thereto to 130L herbaceous plant precipitation
Agent, pH value of reaction system reach 7, obtain white crystalline precipitation；To precipitate with mother solution in the common still aging 12h of room temperature, will be white
After color precipitation filtration, washing, in 800 DEG C of calcination 4h, faint yellow cerium oxide product is obtained.
5. the method for preparing cerium oxide with herbaceous plant precipitant as described in claims 1 or 2, it is characterised in that：To reaction
The cerous nitrate solution of 10L concentration 0.92mol/L is added in kettle and 60 DEG C are heated to, and is added thereto to 20L herbaceous plant precipitant,
PH value of reaction system reaches 6.5, obtains white crystalline precipitation；To precipitate with mother solution in the common still aging 4h of room temperature, by white
After precipitation filtration, washing, in 1000 DEG C of calcination 3h, faint yellow cerium oxide product is obtained.
6. the method for preparing cerium oxide with herbaceous plant precipitant as described in claims 1 or 2, it is characterised in that：To reaction
1m is added in kettle3The cerous nitrate solution of concentration 0.75mol/L is simultaneously heated to 93 DEG C, is added thereto to 2m3Herbaceous plant precipitant,
PH value of reaction system reaches 7, obtains white crystalline precipitation；To precipitate with mother solution in the common still aging 24h of room temperature, will be white heavy
After shallow lake filtration, washing, in 1100 DEG C of calcination 2h, faint yellow cerium oxide product is obtained.
7. the method for preparing cerium oxide with herbaceous plant precipitant as described in claims 1 or 2, it is characterised in that：To reaction
10M is added in kettle3The solution of cerium chloride by oxidation of concentration 1.5mol/L is simultaneously heated to 93 DEG C, is added thereto to 4M3Herbaceous plant precipitant,
PH value of reaction system reaches 6.7, obtains white crystalline precipitation；To precipitate with mother solution in the common still aging 12h of room temperature, by white
After precipitation filtration, washing, in 1200 DEG C of calcination 2h, faint yellow cerium oxide product is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201611052631.3A CN106517296A (en) | 2016-11-21 | 2016-11-21 | Method for preparing cerium oxide by using herbaceous plant precipitating agent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611052631.3A CN106517296A (en) | 2016-11-21 | 2016-11-21 | Method for preparing cerium oxide by using herbaceous plant precipitating agent |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683248A (en) * | 2004-04-14 | 2005-10-19 | 北京方正稀土科技研究所有限公司 | Process for preparing nano cerium dioxide |
| CN102078879A (en) * | 2010-10-21 | 2011-06-01 | 高旌 | Method for accelerating removal of heavy metals in polluted soil |
| CN102502758A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Method for preparing large-particle cerium oxide |
| CN105603222A (en) * | 2016-02-18 | 2016-05-25 | 广西晧昭环保科技有限公司 | Herbaceous plant rare-earth precipitating agent and preparation method thereof |
-
2016
- 2016-11-21 CN CN201611052631.3A patent/CN106517296A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683248A (en) * | 2004-04-14 | 2005-10-19 | 北京方正稀土科技研究所有限公司 | Process for preparing nano cerium dioxide |
| CN102078879A (en) * | 2010-10-21 | 2011-06-01 | 高旌 | Method for accelerating removal of heavy metals in polluted soil |
| CN102502758A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Method for preparing large-particle cerium oxide |
| CN105603222A (en) * | 2016-02-18 | 2016-05-25 | 广西晧昭环保科技有限公司 | Herbaceous plant rare-earth precipitating agent and preparation method thereof |
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Application publication date: 20170322 |
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