CN109054651A - A kind of preparation method of polishing powder from rare earth - Google Patents

A kind of preparation method of polishing powder from rare earth Download PDF

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Publication number
CN109054651A
CN109054651A CN201811013520.0A CN201811013520A CN109054651A CN 109054651 A CN109054651 A CN 109054651A CN 201811013520 A CN201811013520 A CN 201811013520A CN 109054651 A CN109054651 A CN 109054651A
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polishing
rare earth
powder
polishing powder
fluoride
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CN109054651B (en
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史茜赟
张鑫
史志新
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Ruiang Optoelectronic Technology Guangdong Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The present invention relates to a kind of preparation methods of polishing powder from rare earth, belong to polishing grinding technical field.Rare earth nitrate solution and stearic acid are under the catalytic action of sodium hydroxide in the present invention, generate rare-earth stearate precipitating, the auxiliary additives such as wax powder, fluoride, petroleum sulfonate, alcohols material are wherein added, keeps the polishing powder thermal stability of preparation good, will not cause to scratch in glass surface;A small amount of petroleum sulfonate is added in polishing powder, layer protecting film can be formed being polished surface after polishing, prevent the corrosion for being polished surface by hand perspiration;A small amount of fluoride is added in polishing powder, can make to be polished surface has the effect for sending out blue light micro-;Appropriate alcohols material is added in polishing powder, it can guarantee the uniformity of entire polishing powder, the brightness for being polished surface can be improved simultaneously, auxiliary element of some animal and plant waxes as polishing powder is added in polishing powder, glossy fine and smooth sense, the enhancing that polishing powder can be enhanced are polished the brightness on surface, and polishing effect is good.

Description

A kind of preparation method of polishing powder from rare earth
Technical field
The present invention relates to a kind of preparation methods of polishing powder from rare earth, belong to polishing grinding technical field.
Background technique
Currently, the glass cover-plate of the electronic products such as mobile phone, tablet computer and liquid crystal display is required to throw by chemical machinery The realization of light process is surface flattening, while improving surface smoothness.With the continuous upgrading of electronic product quality, especially The extensive use of ito glass, planarization and smoothness requirements to glass surface also step up, this is just to glass surface polishing Propose higher technical requirements.
Industrial glass polishes single unit system mainly by Workpiece carrier, the platform of storing polishing pad and slurry feeder three Divide and is combined into.When chemically-mechanicapolish polishing to glass material, workpiece is rotated under the drive of carrier, pressure head with On the polishing pad being equally rotating under certain pressure effect, the polishing slurries being made of abrasive material and chemical solution are in workpiece It is flowed between the two with polishing pad.At this point, due to chemical substance and abrasive material and workpiece surface generation hydrolysis or corruption in slurry The chemical reaction such as erosion forms one layer of oxidation film easily removed in workpiece surface.Later with the machine of abrasive material and polishing pad in slurry This tunic is removed in tool effect, and is flowed away with polishing slurries, so that workpiece exposes new surface.Hereafter polishing slurries are undergone again Chemical attack and mechanism, be removed again.Circulation carries out above-mentioned polishing slurries and acts on the chemical machinery of workpiece, just Complete the chemically mechanical polishing to workpiece.Polishing efficiency mainly determined by the polishing activity and precision of abrasive material, cerium-rich rare earth Polishing powder is the polish abrasive being most widely used in current industrial glass polishing process.
High-cerium rare-earth polishing powder depends mainly on the chemical activity and polished of its own to the polishing characteristic of glass material Mechanical abrasive action in journey, the high-cerium rare-earth polishing powder prepared by suitable synthesis condition, contained cerium oxide is to oxidation Silicon has high chemical polishing activity, have if existing simultaneously the mixed rare-earth oxide such as fluorine cerium lanthanum oxide in polishing powder compared with High pellet hardness ensure that under mechanical abrasive action during the polishing process, the stability of polishing powder grain graininess, to improve Polishing powder service life cycle.
Currently, how polishing powder in the market on application performance improves polishing speed, widespread practice if primarily focusing on It is the grain graininess for improving polishing powder, by increasing the mechanism in polishing process to improve polishing speed, traditional mode of production is dilute It is easy to reunite present in the method for native cerium based relief polishing powder, average grain diameter is big, particle diameter distribution is wide, sphericity is poor and production cost is high etc. Disadvantage.Therefore, it deposits to be easy to cause to scratch in glass surface during the polishing process and is easy sedimentation etc. with polishing powder in polishing process Applied defect.
Summary of the invention
The technical problems to be solved by the invention: it is easy to cause in glass surface during the polishing process for existing polishing powder The problem with polishing effect difference is scratched, a kind of preparation method of polishing powder from rare earth is provided.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
According to parts by weight, 20~26 parts of rare earth nitrate solutions, 30~40 parts of stearic acid, 5~15 parts of wax powders, 1~6 are weighed respectively Part fluoride, 1~3 part of mass fraction are 0.1% petroleum sulfonate, 1~3 part of alcohols material, 0.1~0.6 part of concentration are Stearic acid, wax powder, fluoride, mass fraction are 0.1% petroleum sulfonate, alcohols object by the sodium hydrate aqueous solution of 1.0mol/L Matter, rare earth nitrate solution are stirred, and obtain multiple emulsion, and at the uniform velocity dropwise addition concentration is water-soluble for the sodium hydroxide of 1.0mol/L Liquid, 20~30min of constant temperature at being 50~60 DEG C in temperature, obtains suspension, filters while hot, obtain filter residue, by filter residue deionized water Washing 3~5 times, filter residue after must washing will be that 1~2h is dried at 80~90 DEG C after filter residue vacuum filtration after washing and in temperature, Filter residue must be dried, by dry filter residue calcination processing, cooled to room temperature is to get polishing powder from rare earth.
The rare earth nitrate solution is lanthanum nitrate cerium solution, and wherein the mass ratio of lanthanum cerium is 1: 4.
The wax powder is any in paraffin powder, crystallite wax powder, carnauba wax powder, insect wax powder and Japanese haze tallow powder Combination.
The fluoride is one of ammonium fluoride, sodium fluoride or potassium fluoride.
The alcohols material is one of methanol, ethyl alcohol, benzyl alcohol and ethylene glycol.
The stir process be 65~75 DEG C in temperature at stearic acid is melted, obtain lotion, wax powder, fluorination be added Object, mass fraction are 0.1% petroleum sulfonate, alcohols material, stir 20~30min in the case where revolving speed is 100~160r/min, obtain Rare earth nitrate solution is added in mixed emulsion, is 65~75 DEG C in temperature, revolving speed is that 20~30min is stirred under 80~100r/min.
The calcination processing be placed in resistance furnace be 600~900 DEG C in temperature at calcine 1~3h.
The present invention is compared with other methods, and advantageous effects are:
(1) rare earth nitrate solution and stearic acid generate rare-earth stearate precipitating under the catalytic action of sodium hydroxide in the present invention, The auxiliary additives such as wax powder, fluoride, petroleum sulfonate, alcohols material are wherein added, keep the polishing powder thermal stability of preparation good, Will not cause to scratch in glass surface, and polishing effect is good, have good chemical stability, at the working temperature abrasive material not with Surface is thrown to chemically react;Stearic acid has good lubricity and good brightener, has under room temperature good A small amount of petroleum sulfonate is added in chemical stability in polishing powder, can form one layer of protection being polished surface after polishing Film prevents the corrosion for being polished surface by hand perspiration;A small amount of fluoride is added in polishing powder, fluoride exists during the polishing process It is polished surface to chemically react, can make to be polished surface has the effect for sending out blue light micro-;Appropriate alcohols is added in polishing powder Substance, it is ensured that the uniformity of entire polishing powder, while the brightness for being polished surface can be improved, it is added in polishing powder Auxiliary element of some animal and plant waxes as polishing powder, glossy fine and smooth sense, the enhancing that polishing powder can be enhanced are polished surface Brightness;
(2) addition of fluoride forms spherical little particle so that particle is refined, and reduces reunion in the present invention, by In fluorine element in conjunction with the lanthanum atom being solid-solubilized in ceria lattice, so that lanthanum is precipitated in ceria structure cell, in crystal boundary Or sub boundary forms little particle, hinders the reunion of cerium oxide particle.
Specific embodiment
According to parts by weight, weigh respectively 20~26 parts of rare earth nitrate solutions, 30~40 parts of stearic acid, 5~15 parts of wax powders, 1~6 part of fluoride, 1~3 part of mass fraction are 0.1% petroleum sulfonate, 1~3 part of alcohols material, 0.1~0.6 part of concentration are Stearic acid is melted at being 65~75 DEG C in temperature, obtains lotion, wax powder, fluorination is added by the sodium hydrate aqueous solution of 1.0mol/L Object, mass fraction are 0.1% petroleum sulfonate, alcohols material, stir 20~30min in the case where revolving speed is 100~160r/min, obtain Rare earth nitrate solution is added in mixed emulsion, is 65~75 DEG C in temperature, and revolving speed is that 20~30min is stirred under 80~100r/min, Multiple emulsion, at the uniform velocity dropwise addition concentration be 1.0mol/L sodium hydrate aqueous solution, temperature be 50~60 DEG C at constant temperature 20~ 30min obtains suspension, filters while hot, obtains filter residue, and filter residue is washed with deionized 3~5 times, and filter residue after must washing will wash It is dry 1~2h at 80~90 DEG C after filter residue is filtered by vacuum afterwards and in temperature, obtains dry filter residue, dry filter residue is placed in resistance furnace In temperature be 600~900 DEG C at calcine 1~3h, cooled to room temperature is to get polishing powder from rare earth.
Example 1
According to parts by weight, 20 parts of rare earth nitrate solutions, 30 parts of stearic acid, 5 parts of wax powders, 1 part of fluoride, 1 part of matter are weighed respectively Amount score is 0.1% petroleum sulfonate, the sodium hydrate aqueous solution that 1 part of alcohols material, 0.1 part of concentration are 1.0mol/L, in temperature It is to melt stearic acid at 65 DEG C, obtains lotion, it is 0.1% petroleum sulfonate, alcohols object that wax powder, fluoride, mass fraction, which is added, Matter stirs 20min in the case where revolving speed is 100r/min, obtains mixed emulsion, rare earth nitrate solution is added, and is 65 DEG C in temperature, revolving speed To stir 20min under 80r/min, multiple emulsion is obtained, the sodium hydrate aqueous solution that concentration is 1.0mol/L is at the uniform velocity added dropwise, in temperature It is constant temperature 20min at 50 DEG C, obtains suspension, filter while hot, obtain filter residue, filter residue is washed with deionized 3 times, is filtered after must washing Slag will be dry 1h at 80 DEG C after filter residue vacuum filtration after washing and in temperature, obtain dry filter residue, dry filter residue is placed in resistance 1h is calcined at being 600 DEG C in temperature in furnace, cooled to room temperature is to get polishing powder from rare earth.
Example 2
According to parts by weight, 23 parts of rare earth nitrate solutions, 35 parts of stearic acid, 10 parts of wax powders, 3 parts of fluorides, 2 parts of matter are weighed respectively Amount score is 0.1% petroleum sulfonate, the sodium hydrate aqueous solution that 2 parts of alcohols materials, 0.3 part of concentration are 1.0mol/L, in temperature It is to melt stearic acid at 70 DEG C, obtains lotion, it is 0.1% petroleum sulfonate, alcohols object that wax powder, fluoride, mass fraction, which is added, Matter stirs 25min in the case where revolving speed is 130r/min, obtains mixed emulsion, rare earth nitrate solution is added, and is 70 DEG C in temperature, revolving speed To stir 25min under 90r/min, multiple emulsion is obtained, the sodium hydrate aqueous solution that concentration is 1.0mol/L is at the uniform velocity added dropwise, in temperature It is constant temperature 25min at 55 DEG C, obtains suspension, filter while hot, obtain filter residue, filter residue is washed with deionized 4 times, is filtered after must washing Slag will be dry 1.5h at 85 DEG C after filter residue vacuum filtration after washing and in temperature, obtain dry filter residue, dry filter residue is placed in electricity 2h is calcined at being 750 DEG C in temperature in resistance furnace, cooled to room temperature is to get polishing powder from rare earth.
Example 3
According to parts by weight, 26 parts of rare earth nitrate solutions, 40 parts of stearic acid, 15 parts of wax powders, 6 parts of fluorides, 3 parts of matter are weighed respectively Amount score is 0.1% petroleum sulfonate, the sodium hydrate aqueous solution that 3 parts of alcohols materials, 0.6 part of concentration are 1.0mol/L, in temperature It is to melt stearic acid at 75 DEG C, obtains lotion, it is 0.1% petroleum sulfonate, alcohols object that wax powder, fluoride, mass fraction, which is added, Matter stirs 30min in the case where revolving speed is 160r/min, obtains mixed emulsion, rare earth nitrate solution is added, and is 75 DEG C in temperature, revolving speed To stir 30min under 100r/min, multiple emulsion is obtained, the sodium hydrate aqueous solution that concentration is 1.0mol/L is at the uniform velocity added dropwise, in temperature Degree is constant temperature 30min at 60 DEG C, obtains suspension, filters while hot, obtain filter residue, filter residue is washed with deionized 5 times, after obtaining washing Filter residue will be dry 2h at 90 DEG C after filter residue vacuum filtration after washing and in temperature, obtain dry filter residue, dry filter residue is placed in electricity 3h is calcined at being 900 DEG C in temperature in resistance furnace, cooled to room temperature is to get polishing powder from rare earth.
Polishing powder from rare earth prepared by the present invention and commercially available polishing powder are detected, specific testing result such as following table table 1:
Detection method:
All polishing powders carry out 3 kilograms of polishing powders of performance comparison by same condition and are added in 30L water, stir 10min, mistake After 200 meshes, polishing experiments are carried out in domestic certain factory's mobile phone glass polishing producing line.Polishing machine platform model 16B, polished glass 5 Very little healthy and free from worry GG4, revolving speed 200rpm, polishing time 30min.Each sample take polishing 100 sheet glass after the 101st to 600 into Row detection, comparison thickness of cutting, scuffing situation, degree of cleaning, service life, specific testing result are shown in Table 1.
Thickness of cutting is the mean value of polishing front and back glass thickness variations.
Yield is surface quality, has being included into for scuffing bad.That is the yields of every group of 500 sheet glass of detection comparison.
Cleaning is the percentage that the fraction defective detected after being often cleaned by ultrasonic accounts for every group of 500 sheet glass.
The case where service life is polishing experiments front and back, and polishing powder sample granularity declines.
1 polishing powder from rare earth performance characterization of table
Polishing powder from rare earth prepared by the present invention as shown in Table 1, thickness of cutting is big, yields is higher, promotes polishing efficiency.With wide Wealthy market value and application prospect.

Claims (7)

1. a kind of preparation method of polishing powder from rare earth, it is characterised in that specific steps are as follows:
According to parts by weight, 20~26 parts of rare earth nitrate solutions, 30~40 parts of stearic acid, 5~15 parts of wax powders, 1~6 are weighed respectively Part fluoride, 1~3 part of mass fraction are 0.1% petroleum sulfonate, 1~3 part of alcohols material, 0.1~0.6 part of concentration are Stearic acid, wax powder, fluoride, mass fraction are 0.1% petroleum sulfonate, alcohols object by the sodium hydrate aqueous solution of 1.0mol/L Matter, rare earth nitrate solution are stirred, and obtain multiple emulsion, and at the uniform velocity dropwise addition concentration is water-soluble for the sodium hydroxide of 1.0mol/L Liquid, 20~30min of constant temperature at being 50~60 DEG C in temperature, obtains suspension, filters while hot, obtain filter residue, by filter residue deionized water Washing 3~5 times, filter residue after must washing will be that 1~2h is dried at 80~90 DEG C after filter residue vacuum filtration after washing and in temperature, Filter residue must be dried, by dry filter residue calcination processing, cooled to room temperature is to get polishing powder from rare earth.
2. a kind of preparation method of polishing powder from rare earth according to claim 1, it is characterised in that the nitric acid rare earth is molten Liquid is lanthanum nitrate cerium solution, and wherein the mass ratio of lanthanum cerium is 1: 4.
3. a kind of preparation method of polishing powder from rare earth according to claim 1, it is characterised in that the wax powder is paraffin Any combination in powder, crystallite wax powder, carnauba wax powder, insect wax powder and Japanese haze tallow powder.
4. a kind of preparation method of polishing powder from rare earth according to claim 1, it is characterised in that the fluoride is fluorine Change one of ammonium, sodium fluoride or potassium fluoride.
5. a kind of preparation method of polishing powder from rare earth according to claim 1, it is characterised in that the alcohols material is One of methanol, ethyl alcohol, benzyl alcohol and ethylene glycol.
6. a kind of preparation method of polishing powder from rare earth according to claim 1, it is characterised in that the stir process is Stearic acid is melted at being 65~75 DEG C in temperature, obtains lotion, it is 0.1% mahogany acid that wax powder, fluoride, mass fraction, which is added, Salt, alcohols material stir 20~30min in the case where revolving speed is 100~160r/min, obtain mixed emulsion, rare earth nitrate solution is added, It is 65~75 DEG C in temperature, revolving speed is that 20~30min is stirred under 80~100r/min.
7. a kind of preparation method of polishing powder from rare earth according to claim 1, it is characterised in that the calcination processing is Be placed in resistance furnace temperature be 600~900 DEG C at calcine 1~3h.
CN201811013520.0A 2018-08-31 2018-08-31 Preparation method of rare earth polishing powder Active CN109054651B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110591418A (en) * 2019-10-21 2019-12-20 中昊黑元化工研究设计院有限公司 Equipment and method for preparing carbon black by plasma countercurrent cracking of gaseous hydrocarbon
CN112645636A (en) * 2020-12-10 2021-04-13 郑州艾克思建材有限公司 Composite efficient brightener and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU920060A1 (en) * 1980-06-13 1982-04-15 Предприятие П/Я Р-6670 Method of producing polishing powder
CN101475777A (en) * 2008-11-07 2009-07-08 上海华明高纳稀土新材料有限公司 High precision rare earth polishing powder and preparation thereof
CN105505226A (en) * 2015-12-02 2016-04-20 包头市新源抛光粉有限公司 Rare earth polishing powder and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU920060A1 (en) * 1980-06-13 1982-04-15 Предприятие П/Я Р-6670 Method of producing polishing powder
CN101475777A (en) * 2008-11-07 2009-07-08 上海华明高纳稀土新材料有限公司 High precision rare earth polishing powder and preparation thereof
CN105505226A (en) * 2015-12-02 2016-04-20 包头市新源抛光粉有限公司 Rare earth polishing powder and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110591418A (en) * 2019-10-21 2019-12-20 中昊黑元化工研究设计院有限公司 Equipment and method for preparing carbon black by plasma countercurrent cracking of gaseous hydrocarbon
CN112645636A (en) * 2020-12-10 2021-04-13 郑州艾克思建材有限公司 Composite efficient brightener and preparation method thereof
CN112645636B (en) * 2020-12-10 2022-06-21 郑州艾克思建材有限公司 Composite efficient brightener and preparation method thereof

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