CN113773671A - Preparation method of high-dispersity nano flaky zinc borate powder - Google Patents
Preparation method of high-dispersity nano flaky zinc borate powder Download PDFInfo
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- CN113773671A CN113773671A CN202111191904.3A CN202111191904A CN113773671A CN 113773671 A CN113773671 A CN 113773671A CN 202111191904 A CN202111191904 A CN 202111191904A CN 113773671 A CN113773671 A CN 113773671A
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/04—Compounds of zinc
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
Abstract
The invention discloses a preparation method of high-dispersity nano flaky zinc borate powder, which comprises the steps of adding zinc nitrate hexahydrate into ammonia water (NH 3. H2O), stirring for 1-4 hours to fully dissolve solids, then adding distilled water, heating to 50-80 ℃, and stirring for 2-6 hours for later use; adding boric acid into distilled water, heating to 60-80 ℃, stirring for 1-3 hours to obtain a boric acid solution, then adding cyclohexanol, ethanol, sodium dodecyl sulfate and dopamine, continuously stirring for 0.5-2 hours, then transferring to a polytetrafluoroethylene high-pressure reaction kettle, and reacting for 20-30 hours at 120-150 ℃; and cooling the reaction kettle after the reaction is finished, filtering, washing for 3-5 times by using distilled water, and drying in vacuum to obtain the zinc borate nano powder.
Description
Technical Field
The invention belongs to the technical field of preparation of nano-scale borate, and particularly relates to a preparation method of high-dispersity nano flaky zinc borate powder.
Background
In recent years, the development of the science of the nano material powerfully promotes the development of a novel lubricating oil additive, and the application of the nano material to a lubricating system is a brand new research field. Because the nano material has the characteristics of large specific surface area, high diffusion, easy sintering, reduced melting point and the like, the novel lubricating material prepared on the basis of the nano material is applied to a friction system and has the functions of friction reduction and wear resistance in a mode different from the traditional load additive. The novel lubricating material can form a layer of easily-sheared film on the friction surface, reduce the friction coefficient, and can fill and repair the friction surface to a certain extent to play a role in resisting wear. The borate lubricating oil additive has good extreme pressure wear-resistant and friction-reducing performance, thermal oxidation stability, corrosion resistance and sealing adaptability, is nontoxic and tasteless, and particularly has better extreme pressure wear-resistant performance under low kinematic viscosity, thereby being beneficial to energy conservation, consumption reduction and environmental protection. But its use is limited because the problem of oil solubility has not been solved. This problem is solved when the particle size of such inorganic particles is reduced to the nanometer level. The magnesium borate powder with the particle size of about 10 nanometers is reported to be capable of effectively improving the abrasion resistance and the extreme pressure property of the base oil, reducing the friction coefficient of the lubricating oil and forming a layer of ferrous boride film on the surface of a steel part.
Disclosure of Invention
The invention aims to provide a preparation method of high-dispersity nano flaky zinc borate powder, which comprises the following steps:
s1: zinc nitrate hexahydrate is added to ammonia (NH)3·H2And O) stirring for 1-4 h to fully dissolve the solid, then adding distilled water, raising the temperature to 50-80 ℃, and stirring for 2-6 h for later use.
S2: adding boric acid into distilled water, heating to 60-80 ℃, stirring for 1-3 hours to obtain a boric acid solution, then adding cyclohexanol, ethanol, sodium dodecyl sulfate and dopamine, continuously stirring for 0.5-2 hours, then transferring to a polytetrafluoroethylene high-pressure reaction kettle, and reacting for 20-30 hours at 120-150 ℃.
And S3, cooling the reaction kettle after the reaction is finished, filtering, washing for 3-5 times by using distilled water, and drying in vacuum to obtain the zinc borate nano powder.
Further, the ammonia water (NH)3·H2O) concentration is 10-13.5 mol/L.
Further, the zinc nitrate hexahydrate and ammonia water (NH)3·H2The mass-volume ratio of O) to distilled water is (10-40) g, (20-90) mL, (50-400) mL.
Further, the concentration of the boric acid solution is 2.5% -4.2%.
Further, the mass ratio of cyclohexanol, ethanol, sodium dodecyl sulfate and dopamine in step S3 is (10-20): (20-50): (6-12): (12-20).
Compared with the prior art, the invention has the following beneficial effects:
in the present invention, zinc nitrate hexahydrate is added to ammonia (NH)3·H2Stirring for 1-4 h in O) to fully dissolve the solid, then adding distilled water, raising the temperature to 50-80 ℃, and stirring for 2-6 h for later use; adding boric acid into distilled water, heating to 60-80 ℃, stirring for 1-3 hours to obtain a boric acid solution, then adding cyclohexanol, ethanol, sodium dodecyl sulfate and dopamine, continuously stirring for 0.5-2 hours, then transferring to a polytetrafluoroethylene high-pressure reaction kettle, and reacting for 20-30 hours at 120-150 ℃; and cooling the reaction kettle after the reaction is finished, filtering, washing for 3-5 times by using distilled water, and drying in vacuum to obtain the zinc borate nano powder with high dispersibility.
Drawings
FIG. 1 is a TEM spectrum of nano flaky zinc borate powder prepared in example 1 of the present invention.
Detailed Description
The following embodiments of the present invention are described in detail, and the embodiments are implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Example 1
A preparation method of high-dispersity nano flaky zinc borate powder specifically comprises the following steps:
s1: zinc nitrate hexahydrate is added into ammonia water (NH) with the concentration of 10mol/L3·H2O) stirring for 1 hour to fully dissolve the solid, then adding distilled water, raising the temperature to 50 ℃, and stirring for 2 hours for later use; wherein, zinc nitrate hexahydrate and ammonia (NH)3·H2O) and distilled water in a mass-to-volume ratio of 10g to 20mL to 50 mL.
S2: adding boric acid into distilled water, heating to 60 ℃, stirring for 1h to obtain a boric acid solution with the concentration of 2.5%, then adding cyclohexanol, ethanol, sodium dodecyl sulfate and dopamine, continuously stirring for 0.5h, then transferring to a polytetrafluoroethylene high-pressure reaction kettle, and reacting for 20-30 h at 120 ℃; wherein the mass ratio of cyclohexanol to ethanol to sodium dodecyl sulfate to dopamine is 10: 20: 6: 12.
and S3, cooling the reaction kettle after the reaction is finished, filtering, washing for 3 times by using distilled water, and drying in vacuum to obtain the zinc borate nano powder.
Example 2
A preparation method of high-dispersity nano flaky zinc borate powder specifically comprises the following steps:
s1: adding zinc nitrate hexahydrate into ammonia water (NH 3. H2O) with the concentration of 13.5mol/L, stirring for 4 hours to fully dissolve solids, then adding distilled water, raising the temperature to 80 ℃, and stirring for 6 hours for later use; wherein the mass-volume ratio of the zinc nitrate hexahydrate, the ammonia water (NH 3. H2O) and the distilled water is 40g:90mL:400 mL.
S2: adding boric acid into distilled water, heating to 60-80 ℃, stirring for 1-3 hours to obtain a boric acid solution with the concentration of 2.5% -4.2%, then adding cyclohexanol, ethanol, sodium dodecyl sulfate and dopamine, continuously stirring for 0.5-2 hours, transferring to a polytetrafluoroethylene high-pressure reaction kettle, and reacting for 20-30 hours at 120-150 ℃; wherein the mass ratio of cyclohexanol to ethanol to sodium dodecyl sulfate to dopamine is 20: 50: 12: 20.
and S3, cooling the reaction kettle after the reaction is finished, filtering, washing for 5 times by using distilled water, and drying in vacuum to obtain the zinc borate nano powder.
Example 3
A preparation method of high-dispersity nano flaky zinc borate powder specifically comprises the following steps:
s1: adding zinc nitrate hexahydrate into ammonia water (NH 3. H2O) with the concentration of 11mol/L, stirring for 2 hours to fully dissolve solids, then adding distilled water, raising the temperature to 60 ℃, and stirring for 4 hours for later use; wherein the mass-volume ratio of the zinc nitrate hexahydrate, the ammonia water (NH 3. H2O) and the distilled water is 20g:50mL:100 mL.
S2: adding boric acid into distilled water, heating to 60-80 ℃, stirring for 1-3 h to obtain a boric acid solution with the concentration of 3.2%, then adding cyclohexanol, ethanol, sodium dodecyl sulfate and dopamine, continuously stirring for 0.5-2 h, then transferring to a polytetrafluoroethylene high-pressure reaction kettle, and reacting for 25 h at 140 ℃; wherein the mass ratio of cyclohexanol to ethanol to sodium dodecyl sulfate to dopamine is 15: 30: 8: 15.
and S3, cooling the reaction kettle after the reaction is finished, filtering, washing for 4 times by using distilled water, and drying in vacuum to obtain the zinc borate nano powder.
Example 4
A preparation method of high-dispersity nano flaky zinc borate powder specifically comprises the following steps:
s1: zinc nitrate hexahydrate is added into ammonia water (NH) with the concentration of 12mol/L3·H2O) stirring for 3 hours to fully dissolve the solid, then adding distilled water, raising the temperature to 70 ℃, and stirring for 5 hours for later use; wherein, zinc nitrate hexahydrate and ammonia (NH)3·H2O) and distilled water in a mass-to-volume ratio of 30g to 80mL to 250 mL.
S2: adding boric acid into distilled water, heating to 75 ℃, stirring for 2.5 hours to obtain a boric acid solution with the concentration of 3.8%, then adding cyclohexanol, ethanol, sodium dodecyl sulfate and dopamine, continuously stirring for 0.5-2 hours, then transferring to a polytetrafluoroethylene high-pressure reaction kettle, and reacting for 28 hours at 145 ℃; wherein the mass ratio of cyclohexanol to ethanol to sodium dodecyl sulfate to dopamine is 18: 45: 10: 28.
and S3, cooling the reaction kettle after the reaction is finished, filtering, washing for 5 times by using distilled water, and drying in vacuum to obtain the zinc borate nano powder.
Claims (5)
1. A preparation method of high-dispersity nano flaky zinc borate powder is characterized by comprising the following steps:
s1: adding zinc nitrate hexahydrate into ammonia water (NH 3. H2O), stirring for 1-4 hours to fully dissolve solids, then adding distilled water, raising the temperature to 50-80 ℃, and stirring for 2-6 hours for later use;
s2: adding boric acid into distilled water, heating to 60-80 ℃, stirring for 1-3 hours to obtain a boric acid solution, then adding cyclohexanol, ethanol, sodium dodecyl sulfate and dopamine, continuously stirring for 0.5-2 hours, then transferring to a polytetrafluoroethylene high-pressure reaction kettle, and reacting for 20-30 hours at 120-150 ℃;
and S3, cooling the reaction kettle after the reaction is finished, filtering, washing for 3-5 times by using distilled water, and drying in vacuum to obtain the zinc borate nano powder.
2. The method for preparing high-dispersibility nano flaky zinc borate powder according to claim 1, wherein the ammonia (NH) is3·H2O) concentration is 10-13.5 mol/L.
3. The method for preparing high-dispersibility nano flaky zinc borate powder according to claim 1, wherein the zinc nitrate hexahydrate and ammonia (NH) water are used3·H2The mass-volume ratio of O) to distilled water is (10-40) g, (20-90) mL, (50-400) mL.
4. The method for preparing high-dispersibility nano flaky zinc borate powder according to claim 1, wherein the solubility of the boric acid solution is 2.5-4.2%.
5. The preparation method of the high-dispersibility nano flaky zinc borate powder according to claim 1, wherein the mass ratio of cyclohexanol, ethanol, sodium dodecyl sulfate and dopamine in step S3 is (10-20): (20-50): (6-12): (12-20).
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5342553A (en) * | 1991-11-22 | 1994-08-30 | U. S. Borax Inc. | Process of making zinc borate and fire-retarding compositions thereof |
| CN1603237A (en) * | 2004-09-30 | 2005-04-06 | 武汉大学 | Preparation method for zinc borate |
| CN1789135A (en) * | 2005-12-12 | 2006-06-21 | 中国科学院青海盐湖研究所 | Hydrothermal method for preparation of shape-controllable low-hydrate zinc borate powder |
| CN103012809A (en) * | 2012-12-26 | 2013-04-03 | 海城精华矿产有限公司 | Method for preparing zinc borate coated wood powder |
-
2021
- 2021-10-13 CN CN202111191904.3A patent/CN113773671A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5342553A (en) * | 1991-11-22 | 1994-08-30 | U. S. Borax Inc. | Process of making zinc borate and fire-retarding compositions thereof |
| CN1603237A (en) * | 2004-09-30 | 2005-04-06 | 武汉大学 | Preparation method for zinc borate |
| CN1789135A (en) * | 2005-12-12 | 2006-06-21 | 中国科学院青海盐湖研究所 | Hydrothermal method for preparation of shape-controllable low-hydrate zinc borate powder |
| CN103012809A (en) * | 2012-12-26 | 2013-04-03 | 海城精华矿产有限公司 | Method for preparing zinc borate coated wood powder |
Non-Patent Citations (3)
| Title |
|---|
| 董新艳，等: "阻燃剂七水硼酸锌的合成及表征", 《青海大学学报（自然科学版）》 * |
| 袁光辉: "硼酸锌的阻燃机理及其纳米化制备研究进展", 《安康学院学报》 * |
| 陈婷: "配位均匀沉淀法合成纳米硼酸锌及其应用研究", 《工程科技I辑》 * |
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