CN1272253C - Process for preparing lithium nickelate and process for preparing enamel using it as adherence promotor - Google Patents
Process for preparing lithium nickelate and process for preparing enamel using it as adherence promotor Download PDFInfo
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- CN1272253C CN1272253C CN 200410066605 CN200410066605A CN1272253C CN 1272253 C CN1272253 C CN 1272253C CN 200410066605 CN200410066605 CN 200410066605 CN 200410066605 A CN200410066605 A CN 200410066605A CN 1272253 C CN1272253 C CN 1272253C
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- enamel
- lithium nickelate
- adhesive agent
- preparation
- crystal
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Abstract
The present invention discloses a preparation method of a lithium nickelate enamel adhesive agent. Li2CO3 and Ni(NO3)2.6H2O are uniformly mixed according to the proportion of 1:10 to 40, and the temperature and the holding time are controlled to prepare an ultrafine lithium nickelate crystal. The present invention also discloses a preparation method of enamel with lithium nickelate as an adhesive agent. Lithium nickelate is introduced into base enamel by a milling method, and temperature is controlled for melting, ball milling, grinding and burning to obtain enamel. The preparation method overcomes the disadvantage of scalelike crack of enamel products. The adhesion strength of enamel is greatly enhanced, the rate of finished products and the quality of enamel products are enhanced, and the preparation method can generate considerable economic benefits for enterprises. In addition, the preparation method has the advantages of easy operation, production technology simplification and production cost reduction, and opens up a new field of the application of enameled colored glaze.
Description
Technical field
The present invention relates to a kind of preparation method and a kind of enamelled making method of enamel adhesive agent, particularly relate to a kind of synthetic method of ultra-fine lithium nickelate powder crystal and this ultra-fine lithium nickelate powder crystal is incorporated into base enamel as the enamel adhesive agent, increase substantially the enamelware making method of adherence strength.
Background technology
According to foreign literature Journal of Crystal Growth, v 234, and n 1, January, and 2002, p176-183 report, lithium nickelate synthetic and the report of using, but the raw materials used oxyhydroxide that mostly is lithium and nickel, the cost height, crystal grain is big, the adherence effect is little.
Enamelled adhesive agent such as nickel oxide and cobalt oxide in the tradition enamel technology, all be to be incorporated in the base enamel by molten adding, because general adhesive agent granularity is big, active little, less to enamelled adherence promoter action, institute's dosage is also very big, effect is undesirable, and, both the enamel coating structure was produced detrimentally affect, as produced fish-scaling effect because require addition many, influence the enamel outward appearance, also do not calculate very much economically.
Summary of the invention
Technical problem to be solved by this invention provides a kind of synthetic method of ultra-fine lithium nickelate powder crystal and this ultra-fine lithium nickelate powder crystal is added in the base enamel as enamel adhesive agent mill, increase substantially the making method of the enamelware of adherence strength, to solve the deficiency of aforesaid method.
For solving the problems of the technologies described above the technical solution adopted in the present invention be: the making method of ultra-fine lithium nickelate enamel adhesive agent comprises the steps:
A. industrial chemicals Quilonum Retard and nickelous nitrate are pressed Li
2CO
3: Ni (NO
3)
2.6H
2O=1: 10～40 mixed is even.
B. be incubated 0.5～1 hour down at 80～150 ℃, be incubated 2～2.5 hours down at 200～300 ℃, insulation is 2.5～3.5 hours under 500～560 ℃, naturally cools to room temperature then, makes the ultra-fine lithium nickelate crystal of mean particle size less than 1um.
Ultra-fine lithium nickelate crystal comprises the steps: as the enamel making method of adhesive agent
A. base enamel is mixed by composition proportion and put into crucible, 1000～1500 ℃ of fusings down, quenching in water is pulled oven dry out then.
B. ultra-fine lithium nickelate crystal is mixed with the base enamel that step a obtains, ball milling, grinding are 1～2 hour then, and the oven dry of sieving at last makes the base enamel mill addition.
C. to the enamel processing that eliminates rust and degrease with metal base plate, dry for standby.
D. to enamel base plate application of slip enamel, then 80～100 ℃ of oven dry, 840～880 ℃ fire enamel.
Wherein, the weight percent content of described base enamel is as follows:
SiO
2 48.0～50.0 Al
2O
3 4.0～7.0 B
2O
3 15.0～19.0
K
2O 4.0～6.0 Na
2O 14.0～16.0 CaF
2 4.5～7.0
Na
2SiF
6 2.0～4.0
The weight percent content of described base enamel mill addition is as follows:
Base enamel 100 clay 6.0-11.0 quartz sand 0-18
Sodium Nitrite 0.1-0.2 lithium nickelate crystal 0.3-1.0 water 40-60
Lithium nickelate crystal and base enamel mixing and ball milling, grinding preferably are crushed to 80～120 orders.
Described enamel can be that steel, cast iron and other can the enamelled materials with baseboard material.Enamel eliminated rust and degrease with base plate handle to adopt 5～10% HCl or H
2SO
4With 8% industry fertilizer soap powder solution.
Advantage of the present invention is: introduce a small amount of ultra-fine lithium nickelate crystal, can increase substantially the enamelled adherence strength, improved the yield rate and the quality product of enamel product.
Introduce a small amount of ultra-fine lithium nickelate crystal, can reduce the hydrogen that metallic iron and water molecules produce, produced little and uniform bubble structure has increased the elasticity of enamel coating and the storage space of hydrogen, reduced thus or overcome to cause enamelware to produce the defective of fishscale owing to hydrogen pressure is excessive.
Because the introducing amount is few, can not influence original physical and chemical performance of enamel and enamelled production technique.Manufacture craft of the present invention is simple, and is with low cost, safe and reliable, can produce in batches.
Ultra-fine lithium nickelate is synthetic and use the quick-fried defective of squama that has overcome enamel product, has increased substantially the enamelled adherence strength, has improved the yield rate and the quality product of enamel product, for enterprise produces considerable economic.And easy and simple to handle, simplified production technique, also reduced production cost, and opened up and once warded off the frontier that coloured glaze is used.
Principle of the present invention is: utilize nickel oxide to combine with active alkalimetal oxide, by the solid-liquid phase reaction, control crystalline nucleation and crystalline growth technique condition have been developed superfine high reactivity lithium nickelate.Through the application of slip, burn till, the enamel material of making can finely improve adherence, to squama is quick-fried extremely strong restraining effect is arranged again.Adopting nickelous nitrate and Quilonum Retard is raw material, by the solid-liquid phase reaction, and by controlling the temperature and time of crystalline nucleation and crystal growth, synthesizes the ultra-fine lithium nickelate crystal that particle diameter is less than or equal to 1 micron.With ultra-fine lithium nickelate crystal as the enamelled adhesive agent, the mode that adds by mill is incorporated in the base enamel, changed the The Nomenclature Composition and Structure of Complexes at enamel layer and metallic iron interface, promoted of the mutually mutual diffusion of enamel element with the metallic iron element, form transition layer structure at the enamel interface, increased substantially the enamelled adherence strength thus.By introducing ultra-fine lithium nickelate crystal, reduced the hydrogen that metallic iron and water molecules produce, produced little and uniform bubble structure has increased the elasticity of enamel coating and the storage space of hydrogen, reduced thus or overcome to cause enamelware to produce the defective of fishscale owing to hydrogen pressure is excessive.
Embodiment
Embodiment 1
Adopt common industrial chemicals nickelous nitrate (Ni (NO
3)
2.6H
2O) and Quilonum Retard (Li
2CO
3), press Li
2CO
3: Ni (NO
3)
2.6H
2O=4: 96 ratio mixes.
Be incubated 1 hour down at 100 ℃, be incubated 2.5 hours down at 200 ℃, insulation is 3.5 hours under 500 ℃, naturally cools to room temperature then, makes the ultra-fine lithium nickelate crystal of mean particle size less than 1um.
Adopt composition proportion base enamel as shown in table 1, at first base enamel is mixed by composition proportion and put into crucible, 1100 ℃ of fusings down, quenching in water is pulled oven dry out then
The prescription of table 1 base enamel
| Chemical constitution | SiO 2 | Al 2O 3 | B 2O 3 | K 2O | Na 2O | CaF 2 | Na 2SiF 6 |
| Hundred parts of ratios of weight | 48.0 | 6.5 | 16.0 | 5.0 | 15.5 | 6.6 | 2.4 |
As the enamelled adhesive agent, the mode that adds by mill is introduced in this base enamel and is mixed with base enamel with ultra-fine lithium nickelate crystal, and the blended ratio is as shown in table 2, and ball milling ground 2 hours then, crosses 120 mesh sieves at last, pours dry for standby in the enamelled vessel into.
The prescription of table 2 base enamel mill addition
| Chemical constitution | Base enamel | Clay | Sodium Nitrite | The lithium nickelate crystal | Water |
| Hundred parts of ratios of weight | 100 | 6.5 | 0.15 | 0.5 | 50 |
Get thick 100 * 100 * 0.6 the steel plate that is of a size of, with the processing that eliminates rust and degrease of the industry fertilizer soap powder solution of 10% HCl and 8%, pull dry for standby out respectively.
Employing is soaked the mode of warding off 100 * 100 * 0.6 steel plate is carried out application of slip enamel, dries at 80 ℃ then, burns till at 840 ℃, makes enamel.
With ball falling impact method (national standard), the enamelled adherence strength to be tested, test result is thread, proves that adherence is good.
Embodiment 2
Adopt common industrial chemicals nickelous nitrate (Ni (NO
3)
2.6H
2O) and Quilonum Retard (Li
2CO
3), press Li0
2CO
3: Ni (NO
3)
2.6H
2O=8: 92 ratio mixes.
Be incubated 0.5 hour down at 150 ℃, be incubated 2 hours down at 300 ℃, insulation is 2.5 hours under 560 ℃, naturally cools to room temperature then, makes the ultra-fine lithium nickelate crystal of mean particle size less than 1um.
Adopt composition proportion base enamel as shown in table 1, at first base enamel is mixed by composition proportion and put into crucible, 1500 ℃ of fusings down, quenching in water is pulled oven dry out then
The prescription of table 1 base enamel
| Chemical constitution | SiO 2 | Al 2O 3 | B 2O 3 | K 2O | Na 2O | CaF 2 | Na 2SiF 6 |
| Hundred parts of ratios of weight | 50.0 | 4.5 | 18.0 | 5.0 | 14.0 | 5.1 | 3.4 |
As the enamelled adhesive agent, the mode that adds by mill is introduced in this base enamel and is mixed with base enamel with ultra-fine lithium nickelate crystal, and the blended ratio is as shown in table 2, and ball milling ground 1 hour then, crosses 80 mesh sieves at last, pours dry for standby in the enamelled vessel into.
The prescription of table 2 base enamel mill addition
| Chemical constitution | Base enamel | Clay | Quartz sand | Sodium Nitrite | The lithium nickelate crystal | Water |
| Hundred parts of ratios of weight | 100 | 10.0 | 18.0 | 0.15 | 0.5 | 50 |
Get thick 100 * 100 * 8 the cast iron that is of a size of, carry out the rust cleaning of Cast Iron Surface and the processing that degreases with oil firing and sandblast respectively.
Employing sprays mode 100 * 100 * 8 cast iron is carried out application of slip enamel, dries at 100 ℃ then, burns till at 880 ℃, makes enamel.
With ball falling impact method (national standard), the enamelled adherence strength to be tested, test result is no any porcelain that takes off, and proves that adherence is good.
Claims (6)
1. the preparation method of a lithium nickelate is characterized in that comprising the steps:
A. industrial chemicals Quilonum Retard and nickelous nitrate are pressed Li
2CO
3: Ni (NO
3)
2.6H
2O=1: 10～40 mixed is even;
B. be incubated 0.5～1 hour down at 80～150 ℃, be incubated 2～2.5 hours down at 200～300 ℃, insulation is 2.5～3.5 hours under 500～560 ℃, naturally cools to room temperature then, makes the ultra-fine lithium nickelate crystal of mean particle size less than 1 μ m.
2. the described lithium nickelate of claim 1 is characterized in that comprising the steps: as the enamel making method of adhesive agent
A. base enamel is mixed by composition proportion and put into crucible, 1000～1500 ℃ of fusings down, quenching in water is pulled oven dry out then;
B. ultra-fine lithium nickelate crystal is mixed with the base enamel that step a obtains, ball milling, grinding are 1～2 hour then, and the oven dry of sieving at last makes the base enamel mill addition;
C. to the enamel processing that eliminates rust and degrease with metal base plate, dry for standby;
D. to enamel with metal base plate application of slip enamel, then 80～100 ℃ of oven dry, 840～880 ℃ fire enamel.
3. lithium nickelate according to claim 2 is characterized in that as the enamel making method of adhesive agent: the weight percent content of described base enamel is as follows:
SiO
2 48.0～50.0 Al
2O
3 4.0～7.0 B
2O
3 15.0～19.0
K
2O 4.0～6.0 Na
2O 14.0～16.0 CaF
2 4.5～7.0
Na
2SiF
6 2.0～4.0。
4. lithium nickelate according to claim 2 is characterized in that as the enamel making method of adhesive agent: lithium nickelate crystal and base enamel mixing and ball milling are crushed to 80～120 orders.
5. lithium nickelate according to claim 2 is characterized in that as the enamel making method of adhesive agent: described enamel is steel or cast iron with the material of metal base plate.
6. lithium nickelate according to claim 2 is characterized in that as the enamel making method of adhesive agent: described enamel is eliminated rust and degrease with metal base plate to handle adopt 5～10% HCl or H
2SO
4With 8% industry fertilizer soap powder solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410066605 CN1272253C (en) | 2004-09-23 | 2004-09-23 | Process for preparing lithium nickelate and process for preparing enamel using it as adherence promotor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410066605 CN1272253C (en) | 2004-09-23 | 2004-09-23 | Process for preparing lithium nickelate and process for preparing enamel using it as adherence promotor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1587070A CN1587070A (en) | 2005-03-02 |
| CN1272253C true CN1272253C (en) | 2006-08-30 |
Family
ID=34604060
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410066605 Expired - Fee Related CN1272253C (en) | 2004-09-23 | 2004-09-23 | Process for preparing lithium nickelate and process for preparing enamel using it as adherence promotor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1272253C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408196B (en) * | 2010-09-21 | 2015-01-21 | 湖南立发釉彩科技有限公司 | Fish-scaling-resistant enamel glaze for hot-rolled steel plates |
| CN107507977A (en) * | 2017-07-21 | 2017-12-22 | 苏州宇量电池有限公司 | High magnification lithium nickelate method for preparing anode material |
| CN108863075A (en) * | 2018-07-20 | 2018-11-23 | 吴伟华 | A kind of enamel coating and application method |
-
2004
- 2004-09-23 CN CN 200410066605 patent/CN1272253C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1587070A (en) | 2005-03-02 |
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Ningbo Senmei Metal Products Co., Ltd. Assignor: Donghua University Contract fulfillment period: 2006.11.20 to 2024.9.22 contract change Contract record no.: 2008330001261 Denomination of invention: Process for preparing lithium nickelate and process for preparing enamel using it as adherence promotor Granted publication date: 20060830 License type: Exclusive license Record date: 20081022 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2006.11.20 TO 2024.9.22; CHANGE OF CONTRACT Name of requester: NINGBO SENMEI METAL PRODUCTS CO., LTD. Effective date: 20081022 |
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Granted publication date: 20060830 Termination date: 20091023 |