CN107337230A - A kind of high-activity nano zinc oxide and preparation method thereof - Google Patents
A kind of high-activity nano zinc oxide and preparation method thereof Download PDFInfo
- Publication number
- CN107337230A CN107337230A CN201710799405.XA CN201710799405A CN107337230A CN 107337230 A CN107337230 A CN 107337230A CN 201710799405 A CN201710799405 A CN 201710799405A CN 107337230 A CN107337230 A CN 107337230A
- Authority
- CN
- China
- Prior art keywords
- solution
- preparation
- zinc
- zinc oxide
- activity nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 230000000694 effects Effects 0.000 title claims abstract description 53
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [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 claims abstract description 62
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 44
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 44
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 44
- 238000001914 filtration Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 24
- 239000012065 filter cake Substances 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 16
- 239000011701 zinc Substances 0.000 claims abstract description 15
- 235000017550 sodium carbonate Nutrition 0.000 claims abstract description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 12
- 238000007701 flash-distillation Methods 0.000 claims abstract description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 13
- 238000011403 purification operation Methods 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 9
- 238000000746 purification Methods 0.000 claims description 8
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 2
- 241000722270 Regulus Species 0.000 claims 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- WQSRXNAKUYIVET-UHFFFAOYSA-N sulfuric acid;zinc Chemical compound [Zn].OS(O)(=O)=O WQSRXNAKUYIVET-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- 239000002893 slag Substances 0.000 description 9
- 239000011572 manganese Substances 0.000 description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 7
- 229910052748 manganese Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- 238000006386 neutralization reaction Methods 0.000 description 6
- 229910052725 zinc Inorganic materials 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000003345 natural gas Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- -1 into filter press Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a kind of high-activity nano zinc oxide and preparation method thereof, is related to nano oxygen agent preparing technical field.A kind of preparation method of high-activity nano zinc oxide includes：It is 1 by weight ratio:During 1.1~1.5 pure solution of zinc sulfate are carried out at a temperature of 70~80 DEG C after being mixed with soda ash solution and operation, and adjust the Zn in solution2+Content be less than 1.5g/L after obtain mixed liquor；Basic zinc carbonate is obtained by mixed liquor press filtration and after separating；The sulfate radical in basic zinc carbonate is washed away, and press filtration obtains the basic zinc carbonate filter cake of water content 25~35%；Basic zinc carbonate filtration cakes torrefaction is obtained into the basic zinc carbonate of powdery, flash distillation calcining is then carried out at a temperature of 600~700 DEG C.This preparation method is workable, and can effectively save preparing raw material.Meanwhile the high-activity nano zinc oxide that this preparation method is prepared has higher activity, uniform particle sizes, specific surface area is big, stable performance.
Description
Technical field
The present invention relates to a kind of nano zine oxide preparing technical field, and more particularly to a kind of high-activity nano zinc oxide and
Its preparation method.
Background technology
At present, high-activity nano zinc oxide of the zinc oxide content more than 95% is largely used.It is but big absolutely
The specific surface area of most high-activity nano zinc oxide is 40-50 ㎡/g, and performance is unstable.Such zinc oxide is applied to rubber
When in glue production, be easy to occur zinc oxide be difficult to disperse, conglomeration phenomena such as, and add the dosage of zinc oxide, make residual in sizing material
Stay zinc amount more, not only waste zinc resource, also greatly pollute environment.How the ratio surface of high-activity nano zinc oxide is improved
Product, turn into the emphasis of industry research.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high-activity nano zinc oxide, this preparation method operability
By force, and preparing raw material can be effectively saved, there is larger market popularization value.Meanwhile this preparation method is prepared
High-activity nano zinc oxide has higher activity, and uniform particle sizes, specific surface area is big, stable performance.
Another object of the present invention is to provide a kind of high-activity nano zinc oxide, by above-mentioned preparation method prepare and
Obtain.This high-activity nano zinc oxide has higher activity, and uniform particle sizes, specific surface area is big, stable performance.
The present invention is solved its technical problem and realized using following technical scheme.
The present invention proposes a kind of preparation method of high-activity nano zinc oxide, and it includes：
It is 1 by weight ratio:1.1~1.5 pure solution of zinc sulfate mixed with soda ash solution after in 70~80 DEG C of temperature
Under carry out neutralization operation, and adjust neutralize the Zn2+ in post-job solution content be less than 1.5g/L after obtain mixed liquor；
Basic zinc carbonate is obtained by mixed liquor press filtration and after separating；
The sulfate radical in basic zinc carbonate is washed away, and press filtration obtains the basic zinc carbonate filter cake of water content 25~35%；
The basic zinc carbonate filter cake of water content 25~35% is dried to obtain the basic zinc carbonate of powdery, then to powder
The basic zinc carbonate of shape carries out flash distillation calcining at a temperature of 600~700 DEG C.
The present invention proposes a kind of high-activity nano zinc oxide, is prepared by the preparation method of high-activity nano zinc oxide
Obtain.
A kind of beneficial effect of high-activity nano zinc oxide of the embodiment of the present invention and preparation method thereof is：
The preparation method of a kind of high-activity nano zinc oxide provided, first, by being 1 by weight ratio:1.1~1.5 is pure
During net solution of zinc sulfate is carried out at a temperature of 70~80 DEG C after being mixed with soda ash solution and operation, and after adjusting and neutralizing operation
Solution in Zn2+Content be less than 1.5g/L after obtain mixed liquor.Zn in obtained mixed liquor2+Content obtain effectively
Ground controls, and the nano zine oxide that high activity is prepared for the later stage provides enough guarantees.Next, by mixed liquor press filtration and divides
Basic zinc carbonate is obtained from after.Eliminate the moisture and impurity being more than in solution.Then, the sulfuric acid in basic zinc carbonate is washed away
Root, and press filtration obtains the basic zinc carbonate filter cake of water content 25~35%.And by the basic zinc carbonate of this water content 25~35%
Filter cake is dried to obtain the basic zinc carbonate of powdery, and then the basic zinc carbonate of powdery is entered at a temperature of 600~700 DEG C
Row flash distillation calcining can obtain nano zine oxide.So design so that the high-activity nano zinc oxide being prepared has higher
Activity, uniform particle sizes, specific surface area is big, stable performance.Meanwhile the method is workable, and can the system of effectively saving
Standby raw material, has larger market popularization value.
The high-activity nano zinc oxide of offer, is prepared by above-mentioned preparation method.This high-activity nano aoxidizes
Zinc has higher activity, and uniform particle sizes, specific surface area is big, stable performance.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, it is the conventional production that can be obtained by commercially available purchase
Product.
High-activity nano zinc oxide of the embodiment of the present invention and preparation method thereof is specifically described below.
A kind of preparation method of high-activity nano zinc oxide, it includes：
First, it is 1 by weight ratio:1.1~1.5 pure solution of zinc sulfate mixed with soda ash solution after at 70~80 DEG C
At a temperature of carry out neutralization operation, and adjust the Zn neutralized in post-job solution2+Content be less than 1.5g/L after obtain mixed liquor.
Zn in obtained mixed liquor2+Content be effectively controlled, the nano zine oxide that high activity is prepared for the later stage provides
Enough guarantee.
As preferable scheme, also include before neutralization operation the concentration for adjusting pure solution of zinc sulfate to 100~
120g/L.Certainly, in other embodiments of the invention, the concentration of pure solution of zinc sulfate can also be selected according to demand
Select, the present invention does not limit.
Specifically, neutralization reaction is to adjust pure solution of zinc sulfate concentration in 100~120g/L, and with pump to squeeze into first
Solution of zinc sulfate measuring tank.Certain density soda ash solution is prepared simultaneously, and pours into soda ash solution measuring tank.After analysis,
Start solution of zinc sulfate feed pump and soda ash solution feed pump, two kinds of solution are pressed 1:1.1~1.5, pass through spinner flowmeter meter
Amount, into hypergravity rotatable reactor, under the centrifugal action of high speed rotation, two kinds of liquid are quickly reacted, through overweight
Power reactor liquid outlet, the material of reaction is added into neutralization reaction tank, after stirring 30 minutes, started to warm up to 70 DEG C~80 DEG C,
Then sample examination, determine the pH value of feed liquid, work as Zn2+Content<During 1.5g/l, reaction end is determined.Meanwhile in the reality of the present invention
Apply in example, all mixing speeds can be selected and adjusted according to demand, and the present invention does not limit.
Further, the secondary zinc powder that 1~2 part is added into mixture is to carry out at twice, and adds parts by weight every time
For 0.5~1 part of secondary zinc powder.Certainly, in other embodiments of the invention, the specific addition situation in batches of secondary zinc powder
It can also be selected according to demand, the present invention does not limit.
Specifically, pure solution of zinc sulfate is by the way that the solution of zinc sulfate that concentration is 90~110g/L is carried out into the successively
Obtained after one purification operation and the second purification operation, and the first purification operation is used to remove the metal in solution of zinc sulfate
Slag, the second purification operation are used to remove the precipitation in solution of zinc sulfate.
Wherein, concentration is that 90~110g/L solution of zinc sulfate is by by 1~2 part of dense sulphur in parts by weight
Slow acid is added in 5~8 parts of water and forms mixture, and after temperature rises to 55~65 DEG C, 1~2 part is added into mixture
Secondary zinc powder and be prepared after stirring 1~1.5h.Preferably, 6 parts of water is added.Meanwhile in an embodiment of the present invention,
All mixing speeds can be selected and adjusted according to demand, and the present invention does not limit.
Wherein, the first purification operation is that solution of zinc sulfate is warming up into 80~85 DEG C, and adjust the pH value of solution to 5.0~
After 5.5, the potassium permanganate that addition concentration is 0.1~0.15moL/L is until Mn2+Content be less than 1mg/L stop after filtering out gold
Belong to slag.
In detail, solution of zinc sulfate is squeezed into purification pot with pump, to liquid warming in purification pot until fluid temperature reaches
80 DEG C, adjustment solution ph is 5.0, is stirred, then continual to be continuously added into the potassium permanganate that concentration is 0.1mol/L
And combine to stir, and detect Mn with atomic absorption method every 3~5min2+Content, until Mn2+Content<Stop after 1mg/L, connect
, filtered out the iron in the solution in purification pot, manganese slag by filter press, the liquid after filtering is that primary purification zinc sulfate is molten
Liquid.Meanwhile in an embodiment of the present invention, all mixing speeds can be selected and adjusted according to demand, the present invention
Do not limit.
Wherein, the second purification operation will be carried out after the first post-job solution of purification is warmed to 50~52 DEG C, successively plus
Enter the pH to 3.5~4 of concentrated sulfuric acid regulation solution, add zinc powder and adjust pH to 5~5.4 again, filtered after then stirring 1~1.5h
Precipitation.Meanwhile in an embodiment of the present invention, all mixing speeds can be selected and adjusted, this hair according to demand
It is bright not limit.
In detail, solution of zinc sulfate is squeezed into displacement tank with pump, is warmed to 50~52 DEG C, constantly add dense sulphur afterwards
The pH value of acid adjustment solution, when pH value is 3.5~4, metal zinc is put into, when pH value is transferred to 5~5.4, stops addition, adds
Pure solution of zinc sulfate is made in stirring at least 1~1.5h, the precipitation for then filtering out precipitation after complete.
As preferable scheme, the preparation method of high-activity nano zinc oxide also includes adding 1~2 part into mixture
The secondary zinc powder and solution of zinc sulfate that is prepared is filtered before the first purification operation is carried out after stirring 1~1.5h.This time
Filtration operation can effectively go the removal of impurity.Meanwhile in an embodiment of the present invention, all mixing speeds can be according to demand
Selected and adjusted, the present invention does not limit.
Secondly, basic zinc carbonate is obtained by mixed liquor press filtration and after separating.Because above-mentioned neutralization reaction tank generates alkali formula
The mixed material of zinc carbonate and sodium sulphate.Therefore, using filter press separating mixture material respectively after can form basic zinc carbonate
Slurry and sodium sulphate finished product.Sodium sulphate reclaims, and basic zinc carbonate slurry is stand-by.
Then, the sulfate radical in basic zinc carbonate is washed away, and press filtration obtains the basic zinc carbonate filter of water content 25~35%
Cake.
Specifically, washing is carried out in water washing tank, by washing, the sulfate ion in material is washed away, until thing
Sulfate ion in material is washed thoroughly, and washing thoroughly material, into filter press, water, which is drained, to be molded and moisture content is low
Basic zinc carbonate filter cake, wherein, thoroughly standard is for cleaning：Sampling filtering, use BaCl2Solution titrates, and no white precipitate is
Thoroughly.
Then, the basic zinc carbonate filter cake of water content 25~35% is dried to obtain the basic zinc carbonate of powdery, so
Flash distillation calcining is carried out at a temperature of 600~700 DEG C to the basic zinc carbonate of powdery afterwards.
Specifically, basic zinc carbonate filter cake is calcined by dynamic calcining furnace, the tail gas for calcining formation enters this DS drying machine
It is interior, the basic zinc carbonate filter cake of water content 25~35% is sent into drying machine, entered through breaing up the dry basic zinc carbonate for forming powdery
Enter in dynamic calcining furnace, the hot-air formed after combustion of natural gas is sent into calcining furnace, with the basic zinc carbonate being sent into stove
Contact heat transfer is carried out, through 600~700 DEG C of hot air, basic zinc carbonate is through being rapidly decomposed into zinc oxide, the oxygen after decomposition
Change zinc and enter warehouse through trap trapping, as finished activated nano zine oxide high, specific surface area is big.
Wherein, flash distillation calcining is carried out at this temperature, and on the one hand can be effectively prevented from basic zinc carbonate can not decompose completely
The problem of.On the other hand, moreover it is possible to it is effectively prevented from the nano zinc oxide particles caused by calcining heat is too high and mutually merges,
Reunion present situation is aggravated into appearance phenomena such as bulky grain.
Embodiments of the invention, which also provide a kind of high-activity nano zinc oxide, to be prepared by above-mentioned preparation method
's.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of high-activity nano zinc oxide is present embodiments provided, is prepared by the following method and forms：
First, it is 1 by weight ratio:1.1 pure solution of zinc sulfate enter after being mixed with soda ash solution at a temperature of 70 DEG C
Row neutralizes operation, and adjusts the Zn neutralized in post-job solution2+Content 1.4g/L after obtain mixed liquor.
Secondly, basic zinc carbonate is obtained by mixed liquor press filtration and after separating.
Then, the sulfate radical in basic zinc carbonate is washed away, and press filtration obtains the basic zinc carbonate filter cake of water content 25%.
Then, the basic zinc carbonate filter cake of water content 25% is dried to obtain the basic zinc carbonate of powdery, it is then right
The temperature that the basic zinc carbonate of powdery is formed after combustion of natural gas is to carry out flash distillation calcining under 600 DEG C of hot-air.
Embodiment 2
The high-activity nano that a kind of preparation method for high-activity nano zinc oxide that the present embodiment provides provides with embodiment 1
The difference of the preparation method of zinc oxide is：
First, 1~2 part of the concentrated sulfuric acid in parts by weight is slowly added to form mixture in 5~8 parts of water,
And after temperature rises to 55 DEG C, into mixture at twice, every time add 0.5 part secondary zinc powder and stir 1h be prepared it is pure
Solution of zinc sulfate.
Secondly, solution of zinc sulfate is warming up to 80 DEG C, and adjusts the pH value of solution to after 5.0, addition concentration is 0.1moL/
L potassium permanganate is until Mn2+Content for 0.9mg/L stop after filtering out scum, manganese slag.
Thirdly, after the solution for filter out after scum, manganese slag being warmed into 50 DEG C, it is molten to sequentially add concentrated sulfuric acid regulation
The pH of liquid to 3.5, add zinc powder and adjust pH to 5 again, then obtain pure solution of zinc sulfate after filtering precipitation after stirring 1h.
Then, the concentration of pure solution of zinc sulfate is adjusted to 100g/L.It is 1 by weight ratio:1.2 pure zinc sulfate are molten
During liquid is carried out at a temperature of 60 DEG C after being mixed with soda ash solution and operation, and adjust the Zn neutralized in post-job solution2+'s
Content obtains mixed liquor after being 1.3g/L.And obtain basic zinc carbonate by mixed liquor press filtration and after separating.
Then, the sulfate radical in basic zinc carbonate is washed away, and press filtration obtains the basic zinc carbonate filter cake of water content 30%.
Then, the basic zinc carbonate filter cake of water content 30% is dried to obtain the basic zinc carbonate of powdery, it is then right
The temperature that the basic zinc carbonate of powdery is formed after combustion of natural gas is to carry out flash distillation calcining under 650 DEG C of hot-air.
Embodiment 3
The high-activity nano that a kind of preparation method for high-activity nano zinc oxide that the present embodiment provides provides with embodiment 1
The difference of the preparation method of zinc oxide is：
First, 1.5 parts of the concentrated sulfuric acid in parts by weight is slowly added to form mixture in 7 parts of water, and treated
After temperature rises to 60 DEG C, 0.8 part of secondary zinc powder is added every time and stirs 1.2h 100g/L is prepared into mixture at twice
Solution of zinc sulfate.
Secondly, 100g/L solution of zinc sulfate is warming up to 82 DEG C, and adjusts the pH value of solution to after 5.3, add concentration
Potassium permanganate for 0.13moL/L is until Mn2+Content for 0.7mg/L stop after filtering out scum, manganese slag.
Thirdly, after the solution for filter out after scum, manganese slag being warmed into 51 DEG C, it is molten to sequentially add concentrated sulfuric acid regulation
The pH of liquid to 3.8, add zinc powder and adjust pH to 5.2 again, then obtain pure zinc sulfate after filtering precipitation after stirring 1.3h
Solution.
Then, the concentration of pure solution of zinc sulfate is adjusted to 120g/L.It is 1 by weight ratio:1.5 pure zinc sulfate are molten
During liquid is carried out at a temperature of 80 DEG C after being mixed with soda ash solution and operation, and adjust the Zn neutralized in post-job solution2+'s
Content obtains mixed liquor after being 1.1g/L.And obtain basic zinc carbonate by mixed liquor press filtration and after separating.
Then, the sulfate radical in basic zinc carbonate is washed away, and press filtration obtains the basic zinc carbonate filter cake of water content 35%.
Then, the basic zinc carbonate filter cake of water content 35% is dried to obtain the basic zinc carbonate of powdery, it is then right
The temperature that the basic zinc carbonate of powdery is formed after combustion of natural gas is to carry out flash distillation calcining under 680 DEG C of hot-air.
Embodiment 4
The high-activity nano that a kind of preparation method for high-activity nano zinc oxide that the present embodiment provides provides with embodiment 1
The difference of the preparation method of zinc oxide is：
First, 2 parts of the concentrated sulfuric acid in parts by weight is slowly added to form mixture in 8 parts of water, and treats temperature
After degree rises to 65 DEG C, 1 part of secondary zinc powder is added every time and stirs 1.5h pure sulfuric acid is prepared into mixture at twice
Zinc solution.
Secondly, solution of zinc sulfate is warming up to 85 DEG C, and adjusts the pH value of solution to after 5.5, adding concentration is
0.15moL/L potassium permanganate is until Mn2+Content for 0.7mg/L stop after filtering out scum, manganese slag.
Thirdly, after the solution for filter out after scum, manganese slag being warmed into 52 DEG C, it is molten to sequentially add concentrated sulfuric acid regulation
The pH of liquid to 4, add zinc powder and adjust pH to 5.4 again, it is molten then to obtain pure zinc sulfate after filtering precipitation after stirring 1.5h
Liquid.
Then, the concentration of pure solution of zinc sulfate is adjusted to 120g/L.It is 1 by weight ratio:1.5 pure zinc sulfate are molten
During liquid is carried out at a temperature of 80 DEG C after being mixed with soda ash solution and operation, and adjust the Zn neutralized in post-job solution2+'s
Content obtains mixed liquor after being 1.2g/L.And obtain basic zinc carbonate by mixed liquor press filtration and after separating.
Subsequently, the sulfate radical in basic zinc carbonate is washed away, and press filtration obtains the basic zinc carbonate filter cake of water content 35%.
Then, the basic zinc carbonate filter cake of water content 35% is dried to obtain the basic zinc carbonate of powdery, it is then right
The temperature that the basic zinc carbonate of powdery is formed after combustion of natural gas is to carry out flash distillation calcining under 700 DEG C of hot-air.
In summary, the high-activity nano zinc oxide that embodiments of the invention provide has a higher activity, uniform particle sizes,
Specific surface area is big, stable performance.
Embodiments described above is part of the embodiment of the present invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of preparation method of high-activity nano zinc oxide, it is characterised in that it includes：
It is 1 by weight ratio:1.1~1.5 pure solution of zinc sulfate enter after being mixed with soda ash solution at a temperature of 70~80 DEG C
Row neutralizes operation, and adjusts the Zn neutralized in post-job solution2+Content be less than 1.5g/L after obtain mixed liquor；
Basic zinc carbonate is obtained by the mixed liquor press filtration and after separating；
The sulfate radical in the basic zinc carbonate is washed away, and press filtration obtains the basic zinc carbonate filter cake of water content 25~35%；
The basic zinc carbonate filter cake of water content 25~35% is dried to obtain the basic zinc carbonate of powdery, then to powder
The basic zinc carbonate of shape carries out flash distillation calcining at a temperature of 600~700 DEG C.
2. the preparation method of high-activity nano zinc oxide according to claim 1, it is characterised in that the pure sulfuric acid
Zinc solution is by the way that the solution of zinc sulfate that concentration is 90~110g/L is carried out into the first purification operation and second net successively
It is turned into what is obtained after industry, and the first purification operation is used to remove the regulus in the solution of zinc sulfate, described second is net
It is turned into industry to be used to remove the precipitation in the solution of zinc sulfate.
3. the preparation method of high-activity nano zinc oxide according to claim 2, it is characterised in that concentration be 90~
The 110g/L solution of zinc sulfate is by the way that 1~2 part of the concentrated sulfuric acid in parts by weight is slowly added into 5~8 parts
Mixture is formed in water, and after temperature rises to 55~65 DEG C, 1~2 part of secondary zinc powder and stirring 1 are added into the mixture
It is prepared after~1.5h；Preferably, 6 parts of water is added.
4. the preparation method of high-activity nano zinc oxide according to claim 3, it is characterised in that into the mixture
The secondary zinc powder for adding 1~2 part is to carry out at twice, and adds the secondary zinc powder that parts by weight are 0.5~1 part every time.
5. the preparation method of high-activity nano zinc oxide according to claim 3, it is characterised in that the high-activity nano
The preparation method of zinc oxide is additionally included in molten to the zinc sulfate before the solution of zinc sulfate carries out the first purification operation
Liquid is filtered.
6. the preparation method of high-activity nano zinc oxide according to claim 2, it is characterised in that first purification is made
Industry is that the solution of zinc sulfate is warming up into 80~85 DEG C, and adjusts the pH value of solution to after 5.0~5.5, and it is 0.1 to add concentration
~0.15moL/L potassium permanganate is until Mn2+Content be less than 1mg/L stop after filtering out regulus.
7. the preparation method of high-activity nano zinc oxide according to claim 6, it is characterised in that second purification is made
Industry will be carried out after the post-job solution of first purification is warmed to 50~52 DEG C, add the pH of concentrated sulfuric acid regulation solution to
3.5~4, add zinc powder and adjust pH to 5~5.4 again, precipitation is filtered after then stirring 1~1.5h.
8. the preparation method of high-activity nano zinc oxide according to any one of claim 1 to 7, it is characterised in that enter
Row is described, which to be neutralized, also includes the concentration for adjusting the pure solution of zinc sulfate before operation to 100~120g/L.
9. the preparation method of high-activity nano zinc oxide according to claim 1, it is characterised in that flash distillation calcining is in day
The temperature formed after right gas burning is what is carried out in 600~700 DEG C of hot-air.
10. a kind of high-activity nano zinc oxide, it is characterised in that received by the high activity any one of claim 1 to 9
The preparation method of rice zinc oxide is prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710799405.XA CN107337230A (en) | 2017-09-07 | 2017-09-07 | A kind of high-activity nano zinc oxide and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710799405.XA CN107337230A (en) | 2017-09-07 | 2017-09-07 | A kind of high-activity nano zinc oxide and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107337230A true CN107337230A (en) | 2017-11-10 |
Family
ID=60214903
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710799405.XA Pending CN107337230A (en) | 2017-09-07 | 2017-09-07 | A kind of high-activity nano zinc oxide and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107337230A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108455656A (en) * | 2018-06-08 | 2018-08-28 | 广州科城环保科技有限公司 | A kind of preparation method of activated zinc oxide |
| CN108607356A (en) * | 2018-03-30 | 2018-10-02 | 徐玉玉 | A kind of multi-functional environment-protection air purification composite material and preparation method thereof |
| CN109399693A (en) * | 2018-12-20 | 2019-03-01 | 兴化金孔雀实业发展有限公司 | A kind of preparation process of high-purity nano-zinc oxide |
| CN111333101A (en) * | 2020-03-09 | 2020-06-26 | 济源市鲁泰纳米材料有限公司 | Nano zinc oxide, preparation method thereof and desulfurizer |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR678614A (en) * | 1928-11-09 | 1930-04-02 | Kalk Chemische Fabrik Gmbh | Process for the preparation of zinc oxide products |
| JPH04280814A (en) * | 1991-03-11 | 1992-10-06 | Hayashi Kinzoku Kogyosho:Kk | Production of ultrafine particulate zinc white |
| CN1418972A (en) * | 2002-11-28 | 2003-05-21 | 王树楷 | Method for preparing nano active zinc oxide from low grade zinc containing material |
| CN103145174A (en) * | 2012-06-25 | 2013-06-12 | 唐山海港合缘锌业有限公司 | Method for producing zinc oxide from low-grade zinc-containing mineral |
| CN103818945A (en) * | 2013-11-15 | 2014-05-28 | 洛阳市蓝天化工科技有限公司 | Production method of efficient zinc oxide |
| CN104591259A (en) * | 2015-02-09 | 2015-05-06 | 黄有余 | Engraftment type nano-zinc oxide and production process thereof |
| CN104671278A (en) * | 2015-02-10 | 2015-06-03 | 济源市鲁泰纳米材料有限公司 | Method for preparing high-activity nano zinc oxide |
-
2017
- 2017-09-07 CN CN201710799405.XA patent/CN107337230A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR678614A (en) * | 1928-11-09 | 1930-04-02 | Kalk Chemische Fabrik Gmbh | Process for the preparation of zinc oxide products |
| JPH04280814A (en) * | 1991-03-11 | 1992-10-06 | Hayashi Kinzoku Kogyosho:Kk | Production of ultrafine particulate zinc white |
| CN1418972A (en) * | 2002-11-28 | 2003-05-21 | 王树楷 | Method for preparing nano active zinc oxide from low grade zinc containing material |
| CN103145174A (en) * | 2012-06-25 | 2013-06-12 | 唐山海港合缘锌业有限公司 | Method for producing zinc oxide from low-grade zinc-containing mineral |
| CN103818945A (en) * | 2013-11-15 | 2014-05-28 | 洛阳市蓝天化工科技有限公司 | Production method of efficient zinc oxide |
| CN104591259A (en) * | 2015-02-09 | 2015-05-06 | 黄有余 | Engraftment type nano-zinc oxide and production process thereof |
| CN104671278A (en) * | 2015-02-10 | 2015-06-03 | 济源市鲁泰纳米材料有限公司 | Method for preparing high-activity nano zinc oxide |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108607356A (en) * | 2018-03-30 | 2018-10-02 | 徐玉玉 | A kind of multi-functional environment-protection air purification composite material and preparation method thereof |
| CN108607356B (en) * | 2018-03-30 | 2021-04-23 | 杭州恒清科技有限公司 | Multifunctional environment-friendly air purification composite new material and preparation method thereof |
| CN108455656A (en) * | 2018-06-08 | 2018-08-28 | 广州科城环保科技有限公司 | A kind of preparation method of activated zinc oxide |
| CN109399693A (en) * | 2018-12-20 | 2019-03-01 | 兴化金孔雀实业发展有限公司 | A kind of preparation process of high-purity nano-zinc oxide |
| CN111333101A (en) * | 2020-03-09 | 2020-06-26 | 济源市鲁泰纳米材料有限公司 | Nano zinc oxide, preparation method thereof and desulfurizer |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107337230A (en) | A kind of high-activity nano zinc oxide and preparation method thereof | |
| CN104402031B (en) | A kind of polyaluminium chloride filter residue recycling technique | |
| CN106734072B (en) | Treatment method of cyanogen-containing waste residue | |
| CN101397181A (en) | Inorganic composite conditioner and sludge dewatering method thereof | |
| CN103011079B (en) | Method for treating waste carbide slag and waste hydrochloric acid | |
| CN106221849A (en) | Stalk fuel containing biomass sludge and preparation method thereof | |
| CN102139881B (en) | Method for producing hydrated silicon dioxide and aluminum-iron water treatment agent by using coal ash | |
| CN108998658A (en) | A method of roasting vanadium extraction | |
| CN103014361B (en) | Process for preparing vanadium pentoxide through leaching vanadium slag roasting clinker in metatitanic acid washing water | |
| CN110330439A (en) | A kind of zinc-glycine complex and preparation method thereof not introducing foreign ion | |
| CN107434315A (en) | A kind of leaded zinc steel wire rope sludge and the method for leaded waste hydrochloric acid integrated treatment | |
| WO2024051103A1 (en) | Phosphogypsum recovery method | |
| CN103351089A (en) | Method for preparing autoalkalization chromium tanning agent through utilizing leather making chromium-rich sludge | |
| CN111439765B (en) | Decalcification method for producing magnesium hydroxide suspension and application thereof | |
| CN107903166B (en) | Preparation method of feed-grade copper citrate | |
| CN107162040B (en) | The production method of feed zinc oxide | |
| CN209722238U (en) | A kind of processing system of the earth of positive pole containing arsenic | |
| CN100500867C (en) | Method for clarifying sugar liquid using quick lime | |
| CN106186017A (en) | A kind of purification process of aluminium hydroxide powder | |
| CN209155822U (en) | Lead sulfate tribasic continuous production device | |
| CN108101106B (en) | The Sewage treatment of zirconium carbonate process units discharge utilizes method | |
| CN104402058A (en) | Recycling process of polymeric aluminum ferric chlorine sulfate filter residue | |
| CN102092732A (en) | Method for preparing water glass and precipitated silica from treatment waste residues of sulfuric acid residues | |
| CN207361806U (en) | A kind of preparation system of high-activity nano zinc oxide | |
| CN108946778A (en) | A kind of polyaluminium chloride and its cleanly production technique |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171110 |
|
| RJ01 | Rejection of invention patent application after publication |