CN107162041B - A kind of preparation process of high quality nano zinc oxide - Google Patents
A kind of preparation process of high quality nano zinc oxide Download PDFInfo
- Publication number
- CN107162041B CN107162041B CN201710554616.7A CN201710554616A CN107162041B CN 107162041 B CN107162041 B CN 107162041B CN 201710554616 A CN201710554616 A CN 201710554616A CN 107162041 B CN107162041 B CN 107162041B
- Authority
- CN
- China
- Prior art keywords
- reaction kettle
- zinc oxide
- preparation process
- parts
- high quality
- 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.)
- Active
Links
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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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
- C01P2006/12—Surface area
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Composite Materials (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation process of high quality nano zinc oxide, include the following steps: for zinc sulfate and deionized water to be uniformly mixed jointly, adds carbonic acid nak response and Zn is made5(CO3)2(OH)6, then by Zn5(CO3)2(OH)6It mixes and is put into reaction kettle jointly with rare-earth stabilizer, silane coupling agent, methyl acrylate, heated up, pressurizeed, ultrasonic irradiation processing, finally added dehydrated alcohol into resulting reactant, get product nano zine oxide after being centrifuged, being dried.The present invention has carried out special improvement to the preparation process of nano zine oxide and has handled, effectively reduce the particle size of Zinc oxide particles, its partial size is not more than 10nm, its surface-active is improved again simultaneously, improves filling service performance, integrated quality is good, furthermore, this method is highly-safe, small to environmental hazard degree, and the market competitiveness is strong.
Description
Technical field
The invention belongs to the processing preparation fields of nano zine oxide, and in particular to a kind of preparation of high quality nano zinc oxide
Technique.
Background technique
Nano zine oxide is a kind of new inorganic material of multifunctionality, and granular size is about at 1~100 nanometer.Due to
The imperceptibility of crystal grain, Electronic Structure and crystal structure change, and produce the surface effect that macro object does not have
It answers, bulk effect, quantum size effect and macroscopical tunnel-effect and the features such as the high grade of transparency, polymolecularity.Discovered in recent years
It catalysis, optics, magnetics, in terms of show many specific functions, make it in ceramics, chemical industry, electronics, optics, life
There is important application value in many fields such as object, medicine, the particularity and purposes that can not compare with common zinc oxide.Nanometer
Zinc oxide can be used for ultraviolet light masking material, antibacterial agent, fluorescent material, catalysis material etc. in fields such as weaving, coating.Due to
The a series of superiority of nano zine oxide and very tempting application prospect, therefore research and develop nano zine oxide and have become many science and technology
Personnel's focus of attention.
Currently, preparing there are many kinds of the methods of nano zinc oxide material, such as vapour deposition process, sol-gel method, precipitating
Method, combustion method, water (solvent) thermal method, template etc..The nano granular of zinc oxide diameter that majority method obtains at present is thicker, than
Surface area is smaller, and size is inhomogenous, and dispersibility is also not good enough, to affect the application performance of nano zine oxide nanometer.
In other words, stablize the granular size of nano zine oxide, the granular size of diminution nano zine oxide as far as possible is to promote its use
The effective way of performance constantly improves this people to preparation process.Application No. is: 201610531155 .7 are disclosed
A kind of high-activity nano zinc oxide preparation method utilizes hydroxy propyl methacrylate, hydroxymethyl diethyl phosphonate, diethyl
Alkene triamine pentamethylene Alendronate limits zinc oxide nucleation size and the direction of growth, using dimethylamino sulfonic acid chloride as stabilizer
Deng, the partial size of final nano zine oxide obtained is 10 ~ 18nm, and particle size parameters and service performance have all well and good promotion, but
It can be seen that it still effectively cannot largely prepare 10nm nano particle below, it is equally limited in higher quality field
In application, and dimethylamino sulphonyl chlorine component used in it is more toxic (danger signal T+), to the health of operator
In the presence of very big security risk, while the chemical component that its addition utilizes is more, and generated waste liquid is less susceptible to purify, and is processed into
This is higher.Therefore, in order to enhance one's market competitiveness, this technique still needs to further improvement processing.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of preparation process of high quality nano zinc oxide is provided.
The present invention is achieved by the following technical solutions:
A kind of preparation process of high quality nano zinc oxide, includes the following steps:
(1) 1 ~ 1.5 part of zinc sulfate and 150 ~ 170 parts of deionized waters are weighed by weight, its common mixing is put into stirring
It is spare that mixed liquor A is obtained in tank, after high-speed stirred to perfect solution；
(2) 0.5 ~ 1 part of potassium carbonate is added into mixed liquor A made from step (1), continue to be stirred to react after 1 ~ 1.5h from
The heart obtains white depositions Zn5(CO3)2(OH)6It is spare；
(3) step (2) resulting white depositions are put into reaction kettle, 6 ~ 9 parts of rare earths is then added into reaction kettle
Stabilizer, 6 ~ 8 parts of silane coupling agents, 4 ~ 7 parts of methyl acrylates obtain mixed liquor with 600 ~ 700 revs/min of revolving speed after mixing evenly
B is spare；
(4) vacuumize process is carried out to the reaction kettle of step (3), then heating keep the temperature in reaction kettle be 140 ~
150 DEG C, 40 ~ 50min of isothermal holding；
(5) step (4) treated reaction kettle shifting is put into ultrasonic irradiation case, at this time by the temperature liter in reaction kettle
To 340 ~ 350 DEG C, pressure rises to 0.6 ~ 0.7MPa, during which carries out ultrasonic irradiation processing to the solution in reaction kettle simultaneously, altogether
After 30 ~ 40min of processing, reaction kettle taking-up is cooled to room temperature, it is spare to obtain mixed liquor C；
(6) 90 ~ 100 parts of dehydrated alcohols are added into the resulting mixed liquor C of step (5), carry out at centrifugation after mixing evenly
Reason, obtains centrifugal sediment, gets product nano zine oxide after being finally dried.Added when preparation the raw material that uses at
Divide few, progress once flushing centrifugal treating.
Further, number described in step (1) to step (6) is parts by weight.
Further, its interior vacuum degree is -0.085 ~ -0.095 after reaction kettle vacuumize process described in step (4)
MPa。
It further, is nitrogen protection environment in ultrasonic irradiation case described in step (5).
Further, there are three ultrasonic wave emission sources for setting in ultrasonic irradiation case described in step (5), are arranged at
On the excircle of reaction kettle placement location, ultrasonic wave emission source two-by-two between angle be 120 °, the ultrasonic wave source position
It is fixed, reaction kettle under the drive of external force with the continuous rotation of 8 ~ 10 revs/min of revolving speed, ultrasonic wave when ultrasonic irradiation processing
Frequency be 66 ~ 70kHz.
Further, temperature control when drying process described in step (6) is 70 ~ 75 DEG C.
In the preparation process of nano zine oxide, in order to guarantee the granular size of finished product finished product zinc oxide, need preparing
The growth of nucleus is controlled in the process, nucleating surface absorption and control is carried out using a variety of chemical addition agents and is also easy to produce crystal point
Problem uneven, that waste liquid yield is big is dissipated, the present invention is added to rare-earth stabilizer during the preparation process, compared with dimethylamino sulphur
The toxicity of acyl chlorides is remarkably decreased, and improves the safety of preparation method, at the same the ionic bond of rare earth element again can with it is nano oxidized
The complexing of zinc surface group, can promote the surface characteristic of finished product nano zine oxide, it is more easy to reunite to improve the smaller bring of partial size
The methyl acrylate of problem, addition can be adsorbed effectively on zinc oxide surface, further improved finished product nano zine oxide and existed
Filling using effect in the materials such as rubber, plastics has carried out at pressurization in specific reaction process in reaction kettle
Reason and ultrasonication wherein pressurization can promote the speed of reaction, while defining the growth of nucleus from external force factor, apply
Ultrasonication improve nucleus dispersion uniformity, reduce mutual growth effect, at the same improve again effectively at
Divide the deposition combination difficulty on nucleus, it is suppressed that it grows, and places in ultrasonic irradiation case for reaction kettle in processing
Platform can drive reaction kettle to rotate, and continuous rotation can promote the uniformity of ultrasonic irradiation processing, improve each to nucleus
The growth inhibitory effect in direction, under high pressure and the collective effect of ultrasonic wave, the particle of nano zine oxide is effectively controlled,
Even property is promoted very well.
The present invention has the advantage that compared with prior art
The present invention has carried out special improvement to the preparation process of nano zine oxide and has handled, and effectively reduces Zinc oxide particles
Particle size, partial size is not more than 10nm, while improving its surface-active again, improves filling service performance, comprehensive product
Matter is good, in addition, this method is highly-safe, small to environmental hazard degree, the market competitiveness is strong.
Specific embodiment
Embodiment 1
A kind of preparation process of high quality nano zinc oxide, includes the following steps:
(1) 1 part of zinc sulfate and 150 parts of deionized waters are weighed by weight, its common mixing are put into agitator tank, high speed
It is spare that mixed liquor A is obtained after stirring to perfect solution；
(2) 0.5 part of potassium carbonate is added into mixed liquor A made from step (1), continues to be centrifuged after being stirred to react 1h, obtain white
Color sediment Zn5(CO3)2(OH)6It is spare；
(3) step (2) resulting white depositions are put into reaction kettle, it is steady that 6 parts of rare earths is then added into reaction kettle
Determine agent, 6 parts of silane coupling agents, 4 parts of methyl acrylates, it is spare to obtain mixed liquid B after mixing evenly with 600 revs/min of revolving speed；
(4) vacuumize process is carried out to the reaction kettle of step (3), it is 140 DEG C that then heating, which keeps the temperature in reaction kettle,
Isothermal holding 40min；
(5) step (4) treated reaction kettle shifting is put into ultrasonic irradiation case, at this time by the temperature liter in reaction kettle
To 340 DEG C, pressure rises to 0.6MPa, during which carries out ultrasonic irradiation processing to the solution in reaction kettle simultaneously, is jointly processed by
After 30min, reaction kettle taking-up is cooled to room temperature, it is spare to obtain mixed liquor C；
(6) 90 parts of dehydrated alcohols are added into the resulting mixed liquor C of step (5), carries out centrifugal treating after mixing evenly, obtains
Centrifugal sediment gets product nano zine oxide after being finally dried.
Further, number described in step (1) to step (6) is parts by weight.
Further, its interior vacuum degree is -0.085MPa after reaction kettle vacuumize process described in step (4).
It further, is nitrogen protection environment in ultrasonic irradiation case described in step (5).
Further, there are three ultrasonic wave emission sources for setting in ultrasonic irradiation case described in step (5), are arranged at
On the excircle of reaction kettle placement location, ultrasonic wave emission source two-by-two between angle be 120 °, the ultrasonic wave source position
It is fixed, reaction kettle under the drive of external force with the continuous rotation of 8 revs/min of revolving speed, ultrasonic wave when ultrasonic irradiation processing
Frequency is 66kHz.
Further, temperature control when drying process described in step (6) is 70 DEG C.
Embodiment 2
A kind of preparation process of high quality nano zinc oxide, includes the following steps:
(1) 1.2 parts of zinc sulfate and 160 parts of deionized waters are weighed by weight, its common mixing is put into agitator tank, it is high
It is spare that mixed liquor A is obtained after speed stirring to perfect solution；
(2) 0.8 part of potassium carbonate is added into mixed liquor A made from step (1), continues to be centrifuged after being stirred to react 1.3h, obtain
White depositions Zn5(CO3)2(OH)6It is spare；
(3) step (2) resulting white depositions are put into reaction kettle, it is steady that 8 parts of rare earths is then added into reaction kettle
Determine agent, 7 parts of silane coupling agents, 6 parts of methyl acrylates, it is spare to obtain mixed liquid B after mixing evenly with 650 revs/min of revolving speed；
(4) vacuumize process is carried out to the reaction kettle of step (3), it is 145 DEG C that then heating, which keeps the temperature in reaction kettle,
Isothermal holding 45min；
(5) step (4) treated reaction kettle shifting is put into ultrasonic irradiation case, at this time by the temperature liter in reaction kettle
To 345 DEG C, pressure rises to 0.65MPa, during which carries out ultrasonic irradiation processing to the solution in reaction kettle simultaneously, is jointly processed by
After 35min, reaction kettle taking-up is cooled to room temperature, it is spare to obtain mixed liquor C；
(6) 95 parts of dehydrated alcohols are added into the resulting mixed liquor C of step (5), carries out centrifugal treating after mixing evenly, obtains
Centrifugal sediment gets product nano zine oxide after being finally dried.
Further, number described in step (1) to step (6) is parts by weight.
Further, its interior vacuum degree is -0.090 MPa after reaction kettle vacuumize process described in step (4).
It further, is nitrogen protection environment in ultrasonic irradiation case described in step (5).
Further, there are three ultrasonic wave emission sources for setting in ultrasonic irradiation case described in step (5), are arranged at
On the excircle of reaction kettle placement location, ultrasonic wave emission source two-by-two between angle be 120 °, the ultrasonic wave source position
It is fixed, reaction kettle under the drive of external force with the continuous rotation of 9 revs/min of revolving speed, ultrasonic wave when ultrasonic irradiation processing
Frequency is 68kHz.
Further, temperature control when drying process described in step (6) is 73 DEG C.
Embodiment 3
A kind of preparation process of high quality nano zinc oxide, includes the following steps:
(1) 1.5 parts of zinc sulfate and 170 parts of deionized waters are weighed by weight, its common mixing is put into agitator tank, it is high
It is spare that mixed liquor A is obtained after speed stirring to perfect solution；
(2) 1 part of potassium carbonate is added into mixed liquor A made from step (1), continues to be centrifuged after being stirred to react 1.5h, obtain white
Color sediment Zn5(CO3)2(OH)6It is spare；
(3) step (2) resulting white depositions are put into reaction kettle, it is steady that 9 parts of rare earths is then added into reaction kettle
Determine agent, 8 parts of silane coupling agents, 7 parts of methyl acrylates, it is spare to obtain mixed liquid B after mixing evenly with 700 revs/min of revolving speed；
(4) vacuumize process is carried out to the reaction kettle of step (3), it is 150 DEG C that then heating, which keeps the temperature in reaction kettle,
Isothermal holding 50min；
(5) step (4) treated reaction kettle shifting is put into ultrasonic irradiation case, at this time by the temperature liter in reaction kettle
To 350 DEG C, pressure rises to 0.7MPa, during which carries out ultrasonic irradiation processing to the solution in reaction kettle simultaneously, is jointly processed by
After 40min, reaction kettle taking-up is cooled to room temperature, it is spare to obtain mixed liquor C；
(6) 100 parts of dehydrated alcohols are added into the resulting mixed liquor C of step (5), carry out centrifugal treating after mixing evenly,
Centrifugal sediment is obtained, gets product nano zine oxide after being finally dried.
Further, number described in step (1) to step (6) is parts by weight.
Further, its interior vacuum degree is -0.095 MPa after reaction kettle vacuumize process described in step (4).
It further, is nitrogen protection environment in ultrasonic irradiation case described in step (5).
Further, there are three ultrasonic wave emission sources for setting in ultrasonic irradiation case described in step (5), are arranged at
On the excircle of reaction kettle placement location, ultrasonic wave emission source two-by-two between angle be 120 °, the ultrasonic wave source position
It is fixed, reaction kettle under the drive of external force with the continuous rotation of 10 revs/min of revolving speed, ultrasonic wave when ultrasonic irradiation processing
Frequency is 70kHz.
Further, temperature control when drying process described in step (6) is 75 DEG C.
Comparative example 1
This comparative example 1 compared with Example 2, the pressurized treatment to reaction kettle is saved in step (5) processing, removes this
Outer method and step is all the same.
Comparative example 2
This comparative example 2 compared with Example 2, keeps reaction kettle fixed, in addition to this in step (5) processing
Method and step is all the same.
Comparative example 3
This comparative example 3 compared with Example 2, saves ultrasonic irradiation processing, in addition to this in step (5) processing
Method and step is all the same.
Control group
Existing conventional nano zine oxide preparation method (application No. is: the preparation method of 201610531155 .7).
In order to compare effect of the present invention, to above-described embodiment 2, comparative example 1, comparative example 2, comparative example 3,
The corresponding nano zine oxide obtained of control group the method carries out Quality Detection, and specific correlation data is as shown in table 1 below:
Table 1
| Average grain diameter (nm) | Specific surface area (m2/ g) | |
| Embodiment 2 | 6 | 102 |
| Comparative example 1 | 18 | 75 |
| Comparative example 2 | 13 | 83 |
| Comparative example 3 | 22 | 62 |
| Control group | 14 | 86 |
Processing method of the present invention can effectively promote the specific surface area of nano zine oxide it can be seen from upper table 1, can be into one
Step reduces grain diameter size, convenient for its application in the technology field of higher requirement.
Claims (5)
1. a kind of preparation process of high quality nano zinc oxide, which comprises the steps of:
(1) 1 ~ 1.5 part of zinc sulfate and 150 ~ 170 parts of deionized waters are weighed by weight, its common mixing is put into agitator tank,
It is spare that mixed liquor A is obtained after high-speed stirred to perfect solution；
(2) 0.5 ~ 1 part of potassium carbonate is added into mixed liquor A made from step (1), continues to be centrifuged after being stirred to react 1 ~ 1.5h, obtain
White depositions Zn5(CO3)2(OH)6It is spare；
(3) step (2) resulting white depositions are put into reaction kettle, then into reaction kettle, 6 ~ 9 parts of addition is rare earth-stabilized
It is standby to obtain mixed liquid B with 600 ~ 700 revs/min of revolving speed after mixing evenly for agent, 6 ~ 8 parts of silane coupling agents, 4 ~ 7 parts of methyl acrylates
With；
(4) vacuumize process is carried out to the reaction kettle of step (3), it is 140 ~ 150 DEG C that then heating, which keeps the temperature in reaction kettle,
40 ~ 50min of isothermal holding；
(5) step (4) treated reaction kettle shifting is put into ultrasonic irradiation case, at this time rises to the temperature in reaction kettle
340 ~ 350 DEG C, pressure rises to 0.6 ~ 0.7MPa, during which carries out ultrasonic irradiation processing to the solution in reaction kettle simultaneously, jointly
After handling 30 ~ 40min, reaction kettle taking-up is cooled to room temperature, it is spare to obtain mixed liquor C；
(6) 90 ~ 100 parts of dehydrated alcohols are added into the resulting mixed liquor C of step (5), carries out centrifugal treating after mixing evenly, obtains
Centrifugal sediment gets product nano zine oxide after being finally dried；
Number described in above-mentioned steps (1) to step (6) is parts by weight.
2. a kind of preparation process of high quality nano zinc oxide according to claim 1, which is characterized in that in step (4)
Its interior vacuum degree is -0.085 ~ -0.095MPa after the reaction kettle vacuumize process.
3. a kind of preparation process of high quality nano zinc oxide according to claim 1, which is characterized in that in step (5)
It is nitrogen protection environment in the ultrasonic irradiation case.
4. a kind of preparation process of high quality nano zinc oxide according to claim 1, which is characterized in that in step (5)
There are three ultrasonic wave emission sources for setting in the ultrasonic irradiation case, are arranged on the excircle of reaction kettle placement location,
Ultrasonic wave emission source two-by-two between angle be 120 °, the ultrasonic wave source position is fixed, and reaction kettle is under the drive of external force
With the continuous rotation of 8 ~ 10 revs/min of revolving speed, the frequency of ultrasonic wave is 66 ~ 70kHz when the ultrasonic irradiation is handled.
5. a kind of preparation process of high quality nano zinc oxide according to claim 1, which is characterized in that in step (6)
Temperature control when the described drying process is 70 ~ 75 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710554616.7A CN107162041B (en) | 2017-07-10 | 2017-07-10 | A kind of preparation process of high quality nano zinc oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710554616.7A CN107162041B (en) | 2017-07-10 | 2017-07-10 | A kind of preparation process of high quality nano zinc oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107162041A CN107162041A (en) | 2017-09-15 |
| CN107162041B true CN107162041B (en) | 2019-04-02 |
Family
ID=59823534
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710554616.7A Active CN107162041B (en) | 2017-07-10 | 2017-07-10 | A kind of preparation process of high quality nano zinc oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107162041B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108906064A (en) * | 2018-07-26 | 2018-11-30 | 安徽锦华氧化锌有限公司 | A kind of preparation method for the modified nano zinc oxide that photocatalytic degradation is strong |
| 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 |
| CN112142095A (en) * | 2020-11-19 | 2020-12-29 | 安徽泰龙锌业有限责任公司 | Preparation method of high-performance nano zinc oxide |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323948C (en) * | 2005-02-02 | 2007-07-04 | 苏州大学 | Preparation method of nanometer zinc oxide |
| US20090017303A1 (en) * | 2007-06-12 | 2009-01-15 | Fas Alliances, Inc. | Zinc oxide having enhanced photocatalytic activity |
| CN106006714B (en) * | 2016-07-07 | 2017-05-17 | 安徽省含山县锦华氧化锌厂 | Method for preparing high-activity nano-zinc oxide |
-
2017
- 2017-07-10 CN CN201710554616.7A patent/CN107162041B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107162041A (en) | 2017-09-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107162041B (en) | A kind of preparation process of high quality nano zinc oxide | |
| CN107011783A (en) | A kind of graphene/TiO2The preparation method of composite | |
| CN102515252B (en) | Film-coating production technology for nano zinc oxide | |
| CN106904623B (en) | A kind of purifying modified method of attapulgite | |
| TWI760244B (en) | Nano zirconia powder, preparation method thereof and dispersion liquid and optical film prepared therefrom | |
| CN105131806B (en) | Aqueous fluorescent polyurethane coating and its prepolymer blend method preparation method | |
| CN108585048A (en) | A kind of preparation method of the caesium doping tungsten bronze nano-powder with near-infrared shielding properties | |
| CN103752330B (en) | A kind of preparation method of ZnO/ZnS composite photocatalyst thin-film | |
| CN107500303B (en) | A kind of mesoporous magnesium silicate microballoon and its hydro-thermal-thermal transition preparation method | |
| CN107915257A (en) | A kind of preparation method and applications of tungsten bronze Nanodispersion | |
| CN106430137B (en) | A kind of preparation method of spherical nano hydroxyapatite particle | |
| CN106006711A (en) | Preparing method for nanometer zinc oxide | |
| CN104591259A (en) | Engraftment type nano-zinc oxide and production process thereof | |
| CN106928763A (en) | A kind of preparation method of antibacterial aqueous polyurethane coating | |
| CN108410017A (en) | A kind of preparation method for the high-dispersion barium sulfate composite material in plastic matrix | |
| CN104998629A (en) | SiO2-TiO2 composite nanomaterial of core-shell structure and preparation method and application thereof | |
| CN106947344B (en) | A kind of reflective heat-insulation paint and preparation method thereof | |
| CN105110362B (en) | A kind of preparation method based on the flower cluster-shaped zinc oxide hybrid material that cellulose nanospheres crystalline substance is template | |
| CN102910662A (en) | Preparation method of granularity-controllable CaCO3 | |
| CN110054222A (en) | It is a kind of to prepare mesoporous single crystals TiO2The method of nanoparticle | |
| CN106006714B (en) | Method for preparing high-activity nano-zinc oxide | |
| CN109455686A (en) | A kind of preparation method and product of Fluorescence Grade strontium monophosphate | |
| CN108455665A (en) | The method that successive reaction prepares rutile type nano titanic oxide | |
| CN107418432A (en) | A kind of method that leather stability and durability are improved based on nano titanium oxide | |
| CN108862373A (en) | A kind of preparation method of little particle nano zine oxide |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Process for preparing high-quality nanometer zinc oxide Effective date of registration: 20200622 Granted publication date: 20190402 Pledgee: Ma'anshan Pubang financing Limited by Share Ltd. Pledgor: ANHUI JINHUA ZINC OXIDE Co.,Ltd. Registration number: Y2020980003307 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20220817 Granted publication date: 20190402 Pledgee: Ma'anshan Pubang financing Limited by Share Ltd. Pledgor: ANHUI JINHUA ZINC OXIDE Co.,Ltd. Registration number: Y2020980003307 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20170915 Assignee: Xinghua Hongda zinc products factory Assignor: ANHUI JINHUA ZINC OXIDE Co.,Ltd. Contract record no.: X2023980032816 Denomination of invention: Preparation process of high-quality nanometer zinc oxide Granted publication date: 20190402 License type: Common License Record date: 20230223 |
|
| EE01 | Entry into force of recordation of patent licensing contract |