CN107502202A - Floride-free polishing powder from rare earth composition and preparation method thereof - Google Patents
Floride-free polishing powder from rare earth composition and preparation method thereof Download PDFInfo
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- CN107502202A CN107502202A CN201710957300.2A CN201710957300A CN107502202A CN 107502202 A CN107502202 A CN 107502202A CN 201710957300 A CN201710957300 A CN 201710957300A CN 107502202 A CN107502202 A CN 107502202A
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- rare earth
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- Organic Chemistry (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
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Abstract
The present invention relates to a kind of floride-free polishing powder from rare earth composition and preparation method thereof, it is calculated in mass percent, the content of cerium oxide is 90% 99.5%, and the content of samarium oxide is 0.5% 10%.The present invention is to be co-precipitated the composition of cerium oxide and samarium oxide by precipitating reagent, and is dehydrated and is post-processed again after being washed, and precipitating reagent used is the one or more in carbonate, oxalates or hydroxide.Floride-free polishing powder from rare earth prepared by the present invention carries out mobile phone glass polishing experiments on RL 13B polishing machines, polishing speed is higher by 15% or so than in the market others polishing powder from rare earth, better than floride-free cerium based relief polishing powder, improve the performance of floride-free cerium-based rare earth polishing powder, the quality of polishing powder from rare earth is improved, the fluctuation of polishing powder from rare earth price caused by reducing rare earth price fluctuation.
Description
Technical field
The invention belongs to rare earth material technical field, is specifically related to a kind of floride-free polishing powder from rare earth composition and its preparation
Method.
Background technology
The polishing powder from rare earth in China can probably be divided into two major classes according to production technology, and one kind is floride-free cerium-based polish
Powder, such polishing powder typically require CeO2/TREO>98%, it is other to turn into lanthanum or praseodymium；One kind is fluorine-containing lanthanum cerium mischmetal polishing
Powder, La-Ce-Pr polishing powder from rare earth.Two class polishing powders respectively have advantage and disadvantage in glass polishing, and first kind relative polishing rate is big, but
It is short life, consumption is big；The major advantage of second class is that raw material is easy to get, service life length, but due to making in production process
With hydrofluoric acid, waste gas caused by calcination needs to carry out special disposal ability qualified discharge.
The raw material production of polishing powder from rare earth is a series of by the selecting of concentrate, alkaline hydrolysis, sour molten, extract and separate, precipitation etc.
Technique, during it is seriously polluted；As national environmental protection dynamics is constantly lifted, produce the second class fluorine-containing polishing powder there is also
The situation that expenses of environmental protection improves constantly.
With the continuous expansion of mobile phone market, the state constantly risen is presented to the demand of mobile phone glass cover-plate polishing powder
Gesture, therefore the friendly polishing powder from rare earth of development environment and its production technology are particularly important and extremely urgent.
Rare earth market are because larger fluctuation often occur in Market Reasons, price, even 10 times of fluctuation sometimes, therefore
In the case of not increasing rare earth supply, low price element, poor efficiency element is made full use of preferably to suppress rare earth element
Excessive price fluctuation, stable Supply and demand market.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, there is provided one kind polishing compound powder, it is dilute to improve floride-free cerium base
The performance of native polishing powder, the quality of polishing powder from rare earth is lifted, the ripple of polishing powder from rare earth price caused by reducing rare earth price fluctuation
It is dynamic, lift the polishing speed and precision to glass；Present invention simultaneously provides its preparation method.
A kind of floride-free polishing powder from rare earth composition of the present invention, is calculated in mass percent, and raw material composition is as follows：Oxidation
The content of cerium is 90%-99.5%, and the content of samarium oxide is 0.5%-10%.
It is calculated in mass percent, the content of cerium oxide is 95%-98%, and the content of samarium oxide is 2%-5%.
The preparation method of floride-free polishing powder from rare earth composition of the present invention comprises the following steps：
(1) composition of cerium oxide and samarium oxide is co-precipitated by precipitating reagent, and is dehydrated and is washed；
(2) co-precipitate is dried and calcination, obtains the semi-finished product of polishing powder；
(3) above-mentioned semi-finished product are crushed and are classified；
(4) polishing powder after being classified adds auxiliary agent and obtains finished product polishing powder or polishing fluid.
Precipitating reagent is the one or more in carbonate, oxalates or hydroxide.
Carbonate is one kind or more in carbonic acid ammonia, ammonium hydrogen carbonate, sodium acid carbonate, sodium carbonate, saleratus or potassium carbonate
Kind.
Oxalates is the one or more in oxalic acid ammonia, oxalic acid, sodium oxalate or potassium oxalate.
Hydroxide is the one or more in ammoniacal liquor, sodium hydroxide or potassium hydroxide.
Auxiliary agent is LP-1, and LP-1 manufacturer is Shandong Taihe Water Treatment Co., Ltd..
Described drying and calcination are that co-precipitate is dried into 1-6 hours at 80-300 DEG C；Enter at 800-1000 DEG C
Row calcination, and it is incubated 2-6 hours.
Described crushing and classification is that the samarium cerium polishing powder semi-finished product air-flow of acquisition is smashed and is classified, Control granularity D50：
0.5-4 μm, D100：3.5-20μm.
As a preferable technical scheme, the preparation method of floride-free polishing powder from rare earth composition of the present invention, bag
Include following steps：
(1) co-precipitation prepares the composition of samarium and cerium, and is dehydrated and is washed.It is calculated in mass percent, cerium oxide
Content is 90%-99.5%, and the content of samarium oxide is 0.5%-10%, and the content of relatively applicable cerium oxide is 95%-98%, oxygen
The content for changing samarium is 2%-5%.
(2) 1-6 hours are dried at 80-300 DEG C for co-precipitate, then carry out calcination in 800-1000 degree, and protect
Warm 2-6 hours, obtain the semi-finished product of polishing powder；
(3) above-mentioned semi-finished product are crushed and are classified, Control granularity D50：0.5-4 μm, D100：3.5-20μm.
(4) polishing powder after classification adds auxiliary agent and obtains finished product polishing powder or polishing fluid.
From the point of view of content of the rare earth element in Rare Earth Mine and the extensive degree of application, the more element of content is cerium, should
With less, the more element of relative amount is samarium, therefore both oxide prices are ratios compared to other rare earth oxides
Relatively stable.Samarium ion (Sm3+) radius and cerium ion (Ce4+) radius approaches, therefore samarium easily forms solid solution with cerium, it is slightly larger
Samarium ion radius can make partial oxidation cerium lattice deformability, be advantageous to the lifting of polishing performance；The atomic weight of samarium is being thrown greatly compared with cerium
Light time is also beneficial to the lifting of polishing performance.
The present invention by the ratio of selection optimization samarium oxide and cerium oxide has obtained that excellent polishing powder from rare earth can be prepared
The composition of samarium oxide and cerium oxide, and the synthesis of polishing powder from rare earth has been carried out to this composition using suitable method.
The invention has the advantages that：
(1) floride-free polishing powder from rare earth prepared by the present invention carries out mobile phone glass polishing experiments on RL-13B polishing machines, throws
Optical speed is higher by 15% or so than in the market others polishing powder from rare earth, the yield of polishing, the easy cleaning degree of glass and control sample
Condition is worked as, and service life is suitable with fluorine-containing polishing powder from rare earth, better than floride-free cerium based relief polishing powder.
(2) this method has reached the purpose of developing samarium oxide application, make use of simultaneously by preparing floride-free polishing powder from rare earth
The ionic radius of samarium and the characteristics of cerium ion is close, atomic weight is larger, improve the performance of floride-free cerium-based rare earth polishing powder, lifting
The quality of polishing powder from rare earth, the fluctuation of polishing powder from rare earth price caused by reducing rare earth price fluctuation.
Embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
100L cerium chlorides feed liquid and 5L samarium trichloride feed liquids are added in 500L reactor, after stirring, adds carbonic acid
Hydrogen ammonium is co-precipitated.Precipitation washing, obtains 22.34 kilograms of (TREO of samaric carbonate cerium by centrifugation：49.56%, wherein Sm2O3/
TREO：5.02%, CeO2/TREO：94.98%)；Above-mentioned product 300 DEG C of drying 1h, 950 DEG C of calcination 5h in roller kilns；Then
Enter promoting the circulation of qi powder and classification, it is D to obtain granularity50：0.82 μm, D100：10.51 kilograms of 4.02 μm of polishing powder；After being mixed into auxiliary agent LP-1
Polishing powder sample is obtained, labeled as SC-1；Contrast experiment is polished on RL-13B polishing machines, the results are shown in Table 1.
Embodiment 2
100L cerium chlorides feed liquid and 2L samarium trichloride feed liquids are added in 500L reactor, after stirring, adds oxalic acid
It is co-precipitated.Precipitation washing, obtains 21.65 kilograms of (TREO of samaric oxalate cerium by filtering：40.56%, wherein Sm2O3/
TREO：2.11%, CeO2/TREO：97.89%)；Above-mentioned product 250 DEG C of drying 2h, 980 DEG C of calcination 4h in roller kilns；Then
Enter promoting the circulation of qi powder and classification, it is D to obtain granularity50：1.16 μm, D100：8.23 kilograms of 4.02 μm of polishing powder；After being mixed into auxiliary agent LP-1
Polishing powder sample is obtained, labeled as SC-2；Contrast experiment is polished on RL-13B polishing machines, the results are shown in Table 1.
Embodiment 3
100L cerium chlorides feed liquid and 10L samarium trichloride feed liquids are added in 500L reactor, after stirring, adds ammoniacal liquor
It is co-precipitated.Precipitation washing, obtains 40.56 kilograms of (TREO of samaric hydroxide cerium by filtering：27.53%, wherein Sm2O3/
TREO：9.91%, CeO2/TREO：90.09%)；Above-mentioned product dries 3h in 200 DEG C in roller kilns, 920 DEG C of calcination 6h dry
Dry, calcination；Then promoting the circulation of qi powder and classification are entered, it is D to obtain granularity50：0.75 μm, D100：9.87 kilograms of 4.89 μm of polishing powder；It is mixed
Polishing powder sample is obtained after entering auxiliary agent LP-1, labeled as SC-3；Contrast experiment is polished on RL-13B polishing machines, is as a result seen
Table 1.
Comparative example 1
The white fluorine-containing cerium lanthanum oxide polishing powder from rare earth of certain domestic major company's production, granularity D50 are purchased from the market：
0.95 μm, D100：4.11 μm, labeled as BJ-1.
Comparative example 2
The red floride-free cerium praseodymium polishing powder from rare earth of buying from the market, granularity D50：0.96 μm, D100：4.69 μm, it is labeled as
BJ-2。
Comparative example 3
Take floride-free cerium-based rare earth polishing powder C-A1 (Zibo Baosteel Lingzhi Rare Earth Hi-tech Co., Ltd.'s production), granularity
For D50：1.12 μm, D100：3.98 μm, labeled as BJ-3.
Comparative example 4
Taking fluorine-containing red oxidization La-Ce-Pr polishing powder from rare earth LCPF-A01S, (Zibo Baogang ganoderma lucidum Xitu Hi-Tech skill share has
Limit company produces), granularity D50：1.16 μm, D100：4.71 μm, labeled as BJ-4.
The performance detection experiment condition of polishing powder：All polishing powders are added in 15L water by 2 kilograms, after stirring,
Experiment is polished, tests the large-scale polishing machine of type RL-13B types, glass is 5 cun of healthy and free from worry GG4, and pressure is 100 kilograms, rotating speed
28rpm.The polishing speed of different polishing powders, glass surface quality, easy cleaning degree, the use of polishing powder are contrasted after the completion of polishing
Life-span.
When surface quality number polishes for detection sample in above-mentioned detection method, the streak number of the scuffing of glass surface is polished
Amount；Cleaning situation number is the polishing powder vestige quantity on polished glass surface after setting-up cleaning；Service life is polishing experiments knot
Shu Hou, the situation that polishing powder sample granularity declines.
The polishing powder polishing performance of table 1 contrasts
Claims (10)
- A kind of 1. floride-free polishing powder from rare earth composition, it is characterised in that：It is calculated in mass percent, raw material composition is as follows：Cerium oxide Content be 90%-99.5%, the content of samarium oxide is 0.5%-10%.
- 2. floride-free polishing powder from rare earth composition according to claim 1, it is characterised in that：It is calculated in mass percent, aoxidizes The content of cerium is 95%-98%, and the content of samarium oxide is 2%-5%.
- A kind of 3. preparation method of the floride-free polishing powder from rare earth composition described in claim 1, it is characterised in that：Specific steps are such as Under：(1) composition of cerium oxide and samarium oxide is co-precipitated by precipitating reagent, and is dehydrated and is washed；(2) co-precipitate is dried and calcination, obtains the semi-finished product of polishing powder；(3) above-mentioned semi-finished product are crushed and are classified；(4) polishing powder after being classified adds auxiliary agent and obtains finished product polishing powder or polishing fluid.
- 4. the preparation method of floride-free polishing powder from rare earth composition according to claim 3, it is characterised in that：Precipitating reagent is carbon One or more in hydrochlorate, oxalates or hydroxide.
- 5. the preparation method of floride-free polishing powder from rare earth composition according to claim 4, it is characterised in that：Carbonate is carbon One or more in sour ammonia, ammonium hydrogen carbonate, sodium acid carbonate, sodium carbonate, saleratus or potassium carbonate.
- 6. the preparation method of floride-free polishing powder from rare earth composition according to claim 4, it is characterised in that：Oxalates is grass One or more in sour ammonia, oxalic acid, sodium oxalate or potassium oxalate.
- 7. the preparation method of floride-free polishing powder from rare earth composition according to claim 4, it is characterised in that：Hydroxide is One or more in ammoniacal liquor, sodium hydroxide or potassium hydroxide.
- 8. the preparation method of floride-free polishing powder from rare earth composition according to claim 3, it is characterised in that：Auxiliary agent is LP- 1。
- 9. the preparation method of floride-free polishing powder from rare earth composition according to claim 3, it is characterised in that：By co-precipitate 1-6 hours are dried at 80-300 DEG C；Calcination is carried out at 800-1000 DEG C, and is incubated 2-6 hours.
- 10. the preparation method of floride-free polishing powder from rare earth composition according to claim 3, it is characterised in that：Described powder Broken and classification is that the samarium cerium polishing powder semi-finished product air-flow of acquisition is smashed and is classified, Control granularity D50：0.5-4 μm, D100：3.5- 20μm。
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| CN112778972A (en) * | 2021-03-10 | 2021-05-11 | 安徽禾臣新材料有限公司 | Polishing powder for fine polishing of electronic display screen and production method thereof |
| CN113969108A (en) * | 2021-11-18 | 2022-01-25 | 东北大学 | Method for preparing polishing solution for optical glass by using cerium enrichment as raw material |
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| CN113969108A (en) * | 2021-11-18 | 2022-01-25 | 东北大学 | Method for preparing polishing solution for optical glass by using cerium enrichment as raw material |
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Denomination of invention: Fluorine free rare earth polishing powder composition and its preparation method Effective date of registration: 20211122 Granted publication date: 20200214 Pledgee: Zibo Linzi sub branch of Bank of Qingdao Co.,Ltd. Pledgor: Zibo Baogang Lingzhi Rare Earth High-Tech Co.,Ltd. Registration number: Y2021980012895 |
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