CN113830819A - Preparation method of skin-color zinc oxide - Google Patents
Preparation method of skin-color zinc oxide Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 13
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 29
- 238000002386 leaching Methods 0.000 claims description 28
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 11
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- 239000000843 powder Substances 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
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- 238000010438 heat treatment Methods 0.000 claims description 8
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
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- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 235000014692 zinc oxide Nutrition 0.000 description 42
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 239000004312 hexamethylene tetramine Substances 0.000 description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
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- 239000000126 substance Substances 0.000 description 4
- 241000209140 Triticum Species 0.000 description 3
- 235000021307 Triticum Nutrition 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical group [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- ZPEJZWGMHAKWNL-UHFFFAOYSA-L zinc;oxalate Chemical compound [Zn+2].[O-]C(=O)C([O-])=O ZPEJZWGMHAKWNL-UHFFFAOYSA-L 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 206010072170 Skin wound Diseases 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 206010052428 Wound Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229920003180 amino resin Polymers 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
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- 210000002257 embryonic structure Anatomy 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
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- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
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- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000000475 sunscreen effect Effects 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical compound [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/62—L* (lightness axis)
-
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/63—Optical properties, e.g. expressed in CIELAB-values a* (red-green axis)
-
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/64—Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a preparation method of skin-color zinc oxide, which belongs to the technical field of zinc oxide, wherein the prepared skin-color ZnO has small particle size, nitrogen atoms generated by decomposition enter zinc oxide lattices to be colored in the process of generating the zinc oxide by thermal decomposition of a zinc oxide precursor, after doping, the performance of the zinc oxide lattice is changed due to the change of a microstructure caused by doping, the nitrogen atoms enter the zinc oxide lattices to be colored, the absorbance in an ultraviolet region is superior to that of the white zinc oxide of the same type, the dispersibility is good, the appearance is spherical-like, the ultraviolet shielding is superior to that of common zinc oxide, and the zinc oxide is suitable for foundation cosmetics, medicines and skin-color-imitating plastics.
Description
Technical Field
The invention belongs to the technical field of zinc oxide, and particularly relates to a preparation method of skin-color zinc oxide.
Background
The wet metallurgy process generally comprises pretreatment, leaching, mass removal, extraction or electrodeposition and other processes. Leaching is also known as leaching, dissolution or wet decomposition. It is a wet metallurgy process which uses proper leaching agent to selectively react with some components in solid materials such as ore, calcine and the like and make them enter the leaching agent, and other insoluble components remain in the leaching residue. At present, the leaching process has more classification schemes, and the classification schemes are classified according to operation modes, or are divided into intermittent leaching, continuous leaching, fluidized leaching, percolation leaching, heap leaching and in-situ leaching. Classified according to the type of leaching agent, and can be classified into acid leaching and alkali leachingLeaching, oxygen leaching, chlorination leaching, cyanide leaching, thiourea leaching and bacterial leaching. Zinc oxide, commonly known as zinc white, is an important inorganic chemical product. The zinc oxide is widely applied to rubber, paint, ceramics, chemical industry, medicine, food and the like, and the common zinc oxide is hexagonal crystal white powder. The ZnO has the functions of sterilization, crease resistance, hemostasis, convergence and the like on skin, is used for preparing zinc paste, rubber, and the like in medicine and treating skin wounds because of being widely applied to the fields of pigments, medicines, plastics, ceramic glass and the like, and the zinc oxide has an excellent ultraviolet shielding function, is suitable for preparing sunscreen cream in cosmetics, and is required to be mixed with organic dye or inorganic vibration material for preparing colored products, so that the operation is troublesome, and the use performance of the zinc oxide can be influenced. Currently, skin-color or near-skin-color products, such as skin-color wound plasters, or skin-color handles, garments, tools, etc., are increasingly used, and for example, CN104610743A discloses skin-color coated simulated doll embryos, etc., formulated with non-toxic pigments. Conventionally, elements or compounds have been dissolved in a solid solution to make it colored: for example, Miss solid solution of small amount of manganese oxide in zinc oxide can make it turn yellow, but these heavy metal elements are harmful to human body, and are not suitable for general use in cosmetics and medicine industry, so that in the course of thermal decomposition of basic zinc carbonate, a proper quantity of ammonium hydrogen carbonate can be added to obtain the invented product with small grain size, good dispersibility and approximate spherical skin colour zinc oxide, and in the course of preparing nano zinc oxide by using ultragravity method, the nano skin colour ZnO can be prepared by adding small quantity of surfactant and in-situ modification method, and the addition of modifier can produce a certain promoting action for preparation process, and the invented product can be used as substitute for preparing nano skin colour ZnO3Method for preparing red zinc oxide by decomposing zinc oxalate in atmosphere, wherein nitrogen atom is solid-melted in zinc oxide crystal to make it colored, and prescription age is in NH3、H2The method for preparing the skin-color superfine powder ZnO by thermally decomposing the zinc oxalate in the mixed atmosphere needs expensive and impurity-loaded gas atmosphere equipment or a supergravity facility, has higher cost and complex operation process. Those skilled in the art are keen to develop a method for preparing skin-color zinc oxide to meet the existing application market and performance requirements.
Disclosure of Invention
In view of the above, the invention provides a preparation method of skin-color zinc oxide.
A preparation method of skin-color zinc oxide comprises the following steps: firstly, putting ammonia water and urotropine into a reaction kettle, heating, adding hot galvanizing ash, adding dibenzoyl peroxide with the mass of 0.05-0.1% of the hot galvanizing ash under the condition of leaching temperature of 50-60 ℃, leaching for 2.5-3 hours, and filtering to obtain a zinc solution; dibenzoyl peroxide (BPO) has been used as a radical initiator for reactions that can oxidize to Fe2+Is oxidized into Fe3+Further form iron precipitate, and the divalent copper ions have catalytic action to realize separation. Step two, ammonia immersion zinc powder purification: purifying, aging and filtering zinc powder, and drying at 100-110 ℃ to obtain precursor powder; and finally, heating the precursor powder and then obtaining the active zinc oxide under the condition of a calcination process.
Urotropin, which is a condensation product of formaldehyde and ammonia, also known as hexamethylenetetramine, can be reacted in the gas phase or in aqueous solution or in an inert solvent. Urotropin has been used as a curing agent for phenolics, a catalyst for aminoplasts, an accelerator for rubber vulcanization, and a preservative for food processing.
Urotropine is easily dissolved in water, and is decomposed when the temperature is heated to about 260 ℃, the pH value of the aqueous solution is 8-9, hexamethylenetetramine generally has a monovalent alkaline reaction, and the aqueous solution establishes the following balance. C6H12N4+6H20 =6CH2O+4NH3By utilizing this property, hexamethylenetetramine can be used as a donor of formaldehyde or ammonia. The thermal decomposition of the substance can be used as a source of active nitrogen which is easily decomposed to generate nitrogen atoms or nitrogen hydrogen bonds in the calcining process of the zinc oxide.
Further, in the second step, the concentration of ammonia water is 6-7 mol/L, the concentration of urotropine is 0.6-0.62 mol/L, and the liquid-solid ratio is 6-7: 1, pH9.5-11.
Further, the third step of calcination process conditions include calcination temperature of 380-400 ℃ and calcination time of 1.5-2.0 h.
Furthermore, the aging time of the second step is 5-10 min, and the aging temperature is 180-200 ℃.
The zinc powder realizes the replacement of copper ion, cadmium ion impurities and the like.
Furthermore, the zinc powder in the second step is purified, wherein the using amount of the zinc powder is 1.0-1.1 g/L, the reaction time is 1.5-2 h, the reaction temperature is 25-30 ℃, and the zinc powder is zinc powder containing 3-4 mass percent of copper sulfate.
The invention has the beneficial effects that:
the invention firstly uses the alkalinity of hexamine and ammonia water to carry out ammonia leaching on the zinc-containing hot-dip ash, the alkalinity of urotropine reduces the using amount of the ammonia water, the urotropine is decomposed when being heated to about 260 ℃, the pH value of the aqueous solution is 8-9, the hexamine is generally in monovalent alkaline reaction, and by utilizing the property, the hexamine can be used as NH at high temperature4 +The donor of (1). The thermal decomposition of the substance can be used as a source of active nitrogen which is easily decomposed to generate nitrogen atoms or nitrogen hydrogen bonds in the calcining process of the zinc oxide. In the ammonia evaporation and precipitation process, nitrogen atoms or nitrogen hydrogen bonds are generated by the thermal decomposition of the adsorption of a precursor mainly comprising basic zinc carbonate, so that the amount of zinc oxide lattice nitrogen is increased, urotropine is uniformly distributed on the surfaces of precursor particles or is included in the precursor particles in a solution form, and NH4 is generated in the process of generating zinc oxide by thermal decomposition+The urotropine realizes simple nitrogen supply in high-temperature calcination, crystal lattice defects are formed by doping of nitrogen atoms or nitrogen hydrogen bonds in the skin color zinc oxide crystal lattice, electron holes are easier to form, and the performance of the urotropine is changed due to the change of a microstructure caused by doping, so that the absorbance in an ultraviolet region is better than that of white zinc oxide used in the current market.
Compared with the prior art, the invention has the following advantages:
the invention adopts hot-dip galvanized ash, hexamethylenetetramine and ammonia water as raw materials to prepare the skin color zinc oxide, has very simple operation, very low requirement on equipment, wide and cheap raw material sources, does not need additional gas reaction atmosphere for the agglomeration problem of precursor particles, ensures that dried precursor powder has good dispersibility, is uniformly heated during calcination and has high efficiency, the precursor can be quickly decomposed into zinc oxide, small particles are easily generated, the nano skin color zinc oxide product is prepared by the action of hexamethylenetetramine, has high yield and good skin color effect, can be in wheat color, and is suitable for foundation cosmetics, medicines and skin color imitation plastics.
Drawings
The invention is described in detail with reference to the accompanying drawings, wherein fig. 1 is an XRD (X-ray diffraction) spectrum of skin-color zinc oxide in example 1; FIG. 2 is an infrared spectrum of skin-tone zinc oxide of example 1; FIG. 3 is a graph comparing UV absorption curves of comparative example 1, and example 2, wherein a is example 1, b is example 2, and c is comparative example 1.
Detailed Description
Example 1
Firstly, putting ammonia water and urotropine into a reaction kettle, and heating, wherein the concentration of the ammonia water is 7mol/L, the concentration of the urotropine is 0.62mol/L, the pH value is 9.5, and the liquid-solid ratio is 7: 1, adding dibenzoyl peroxide with the mass of 0.1 percent of hot galvanizing ash to leach for 3 hours at the leaching temperature of 60 ℃ and filtering to obtain a zinc solution; secondly, purifying zinc powder by using ammonia immersion liquid, reducing the using amount of the zinc powder by 1.1g/L, reacting for 2h at the reaction temperature of 30 ℃, wherein the zinc powder is 325-mesh zinc powder containing copper sulfate with the mass fraction of 4 percent, ageing for 10min at the ammonia evaporation temperature of 120 ℃, calcining for 400 ℃, filtering, and drying at the temperature of 110 ℃ to obtain precursor powder; and finally, heating the JH-598 horizontal type muffle reverberatory furnace to 400 ℃ at the speed of 4 ℃/min, and calcining for 1.5h to obtain the active zinc oxide. Wherein the hot galvanizing ash comprises the main components of Zn95.89 percent, Fe2.53 percent, Cl0.05 percent, Cd0.0074 percent and Al2O30.0044、MgO0.004、CaO0.02。
The product is as follows: appearance near wheat skin color, colorimeter color measurement L =89.4, a =3.5, b = 24.0.
Example 2
Firstly, putting ammonia water and urotropine into a reaction kettle, and heating, wherein the concentration of the ammonia water is 6mol/L, the concentration of the urotropine is 0.6mol/L, and the liquid-solid ratio is 6: 1, under the conditions of pH11 and leaching temperature of 50 ℃, adding dibenzoyl peroxide with the mass of 0.05 percent of hot galvanizing ash for leaching for 2.5 hours and filtering to obtain a zinc solution; secondly, purifying the zinc powder by ammonia immersion to reduce the dosage of the zinc powder to 1.0g/L, reacting for 1.5h at the temperature of 30 ℃, wherein the zinc powder is 400-mesh zinc powder containing copper sulfate with the mass fraction of 4%; aging for 10min at 180 deg.C, filtering, and drying at 100 deg.C to constant weight to obtain precursor powder; and finally, heating the JH-598 horizontal type flame-proof reverberatory furnace to the calcining temperature of 380 ℃ at the speed of 5 ℃/min, and obtaining the active zinc oxide under the process condition of calcining time of 2h, wherein the hot galvanizing ash is the same as that in the example 1.
The product is as follows: appearance wheat skin color, colorimeter color measurement L =89.5, a =3.6, b = 24.2.
Comparative example 1
Commercial product GB/T3185-2016-BA 01-05 (type II) indirect method zinc oxide of Jinhua zinc oxide factory in Shanxi province, Anhui province, wherein the appearance is nearly pure white L =98.4, a =2.2 and b = 0.3.
Note: weighing 13g of sample, taking a fully-filled and compacted sample box (phi 40mm, H10 mm) as a standard, drying the sample at 105 ℃ for 2H under the condition that the weight of the sample is the same during each detection, taking 10 parts of sample, and taking the average value of the sample, wherein the average value is used for testing Lab value by a Konika Mengta portable color difference meter CR-10PLUS phi 8 mm; the product was analyzed with a DISCOVER type D8X-ray diffractometer under the following conditions: the method comprises the following steps of using a Cu target, wherein the tube voltage is 30kv, the tube current is 20mA, the scanning speed is 1 DEG/min, and the scanning range 2 theta is 30-60 deg.
In conclusion, it can be seen from the infrared spectrum of the skin color zinc oxide that nitrogen atoms or nitrogen hydrogen bonds enter zinc oxide lattices, the skin color zinc oxide maintains strong absorption of ultraviolet light in an ultraviolet region of 200-380 mm, the absorbance is superior to that of the same type of white zinc oxide, and the absorption of visible light in a visible light range with the wavelength of 380-550 nm is obviously greater than that of the most widely used white zinc oxide at present, such as indirect zinc oxide.
Claims (5)
1. The preparation method of the skin color zinc oxide is characterized by comprising the following steps: firstly, putting ammonia water and urotropine into a reaction kettle, heating, adding hot galvanizing ash, adding dibenzoyl peroxide with the mass of 0.05-0.1% of the hot galvanizing ash under the condition of leaching temperature of 50-60 ℃, leaching for 2.5-3 hours, and filtering to obtain a zinc solution; step two, ammonia immersion zinc powder purification: purifying, aging and filtering zinc powder, and drying at 100-110 ℃ to obtain precursor powder; and thirdly, heating the precursor powder and then obtaining the active zinc oxide under the condition of a calcining process.
2. The preparation method of skin-color zinc oxide according to claim 1, wherein the ammonia water concentration in the first step is 6-7 mol/L, the urotropine concentration is 0.6-0.62 mol/L, and the liquid-solid ratio is 6-7: 1, pH9.5-11.
3. The preparation method of skin-color zinc oxide according to claim 1, wherein the calcination process conditions in the third step are that the calcination temperature is 380-400 ℃ and the calcination time is 1.5-2.0 h.
4. The method for preparing skin-color zinc oxide according to claim 1, wherein the aging time of the second step is 5-10 min, and the aging temperature is 180-200 ℃.
5. The preparation method of skin color zinc oxide according to claim 1, wherein the amount of zinc powder in the second step of zinc powder purification is 1.0-1.1 g/L, the reaction time is 1.5-2 h, the reaction temperature is 25-30 ℃, and the zinc powder is 3-4% by mass of copper sulfate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111218640.6A CN113830819A (en) | 2021-10-20 | 2021-10-20 | Preparation method of skin-color zinc oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202111218640.6A CN113830819A (en) | 2021-10-20 | 2021-10-20 | Preparation method of skin-color zinc oxide |
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| CN115028190A (en) * | 2022-06-16 | 2022-09-09 | 安徽锦华氧化锌有限公司 | Preparation method of active zinc oxide |
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| JP2008285345A (en) * | 2007-05-15 | 2008-11-27 | Sakai Chem Ind Co Ltd | Nitrogen-containing zinc oxide powder and its production method |
| CN102515252A (en) * | 2011-12-28 | 2012-06-27 | 韶关凯鸿纳米材料有限公司 | Film-coating production technology for nano zinc oxide |
| JP2014221708A (en) * | 2013-05-14 | 2014-11-27 | テイカ株式会社 | Zinc oxide and production method of zinc oxide as well as cosmetic, resin composition, coating composition, and inorganic powder using zinc oxide |
| CN110817935A (en) * | 2019-07-25 | 2020-02-21 | 重庆东群科技有限公司 | Method for preparing high-purity zinc oxide by utilizing zinc renewable resources |
| CN111001429A (en) * | 2019-12-27 | 2020-04-14 | 吉林师范大学 | Preparation method of nitrogen-doped modified zinc oxide visible-light-driven photocatalyst |
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| JP2008285345A (en) * | 2007-05-15 | 2008-11-27 | Sakai Chem Ind Co Ltd | Nitrogen-containing zinc oxide powder and its production method |
| CN102515252A (en) * | 2011-12-28 | 2012-06-27 | 韶关凯鸿纳米材料有限公司 | Film-coating production technology for nano zinc oxide |
| JP2014221708A (en) * | 2013-05-14 | 2014-11-27 | テイカ株式会社 | Zinc oxide and production method of zinc oxide as well as cosmetic, resin composition, coating composition, and inorganic powder using zinc oxide |
| CN110817935A (en) * | 2019-07-25 | 2020-02-21 | 重庆东群科技有限公司 | Method for preparing high-purity zinc oxide by utilizing zinc renewable resources |
| CN111001429A (en) * | 2019-12-27 | 2020-04-14 | 吉林师范大学 | Preparation method of nitrogen-doped modified zinc oxide visible-light-driven photocatalyst |
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| CN115028190A (en) * | 2022-06-16 | 2022-09-09 | 安徽锦华氧化锌有限公司 | Preparation method of active zinc oxide |
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Application publication date: 20211224 |