CN108997784A - A kind of carbon coating ZrW2O8An one step preparation method - Google Patents
A kind of carbon coating ZrW2O8An one step preparation method Download PDFInfo
- Publication number
- CN108997784A CN108997784A CN201810749727.8A CN201810749727A CN108997784A CN 108997784 A CN108997784 A CN 108997784A CN 201810749727 A CN201810749727 A CN 201810749727A CN 108997784 A CN108997784 A CN 108997784A
- Authority
- CN
- China
- Prior art keywords
- carbon coating
- zrw
- step preparation
- precipitating
- reaction
- 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.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention provides a kind of carbon coating ZrW2O8An one step preparation method, it is characterized in that, comprising steps of tungstates and zirconates are dissolved in hydrochloric acid according to atomic ratio Zr: W=1: 2, glucose stirring and dissolving is added, solution is moved into the hydrothermal reaction kettle with polytetrafluoroethylliner liner, sealing is tightened, is put into 180~220 DEG C of constant temperature ovens and stands reaction 8~12 hours；Filtering precipitating after reaction is cleaned with deionized water repeatedly until pH value 7~8；It is filtered using centrifuge precipitating or pumping and filtering device and isolates sediment, be put into drying in 50~70 DEG C of baking oven and obtain final product.The present invention uses one-step synthesis method carbon coating ZrW2O8Negative thermal expansion material, simple process, product can be used for the temperature compensation filler of polymer support plate, prepare zero thermal expansion electronic circuit board.
Description
Technical field
The invention belongs to material chemistry technical fields, are related to a kind of carbon coating ZrW2O8An one step preparation method.
Background technique
With the development of science and technology, the trend of miniaturization and multifunction is increasingly presented in each electronic product, can to it
Requirement by property is also higher and higher.The reliability of the thermal expansion character extreme influence electronic device of wiring board support plate.Many class bones
The molybdate of frame structure and with tungstate material have unique negative expansion effect.ZrW2O8It is a kind of widely used negative heat
Expanding material can be used for the temperature compensation filler of epoxy support plate or polyimides support plate, but organic-inorganic phase is compatible
Property can very big influence ZrW2O8Being evenly distributed in organic support plate, and then the thermal expansion character of entire support plate is influenced, negative heat is swollen
Swollen material carbon material cladding can be obviously improved compatibility in a polymer matrix.
Summary of the invention
The purpose of the present invention is to provide a kind of carbon coating ZrW2O8An one step preparation method, which is characterized in that including step
It is rapid: tungstates and zirconates being dissolved in hydrochloric acid according to atomic ratio Zr: W=1: 2, glucose stirring and dissolving is added, solution is moved
Enter in the hydrothermal reaction kettle with polytetrafluoroethylliner liner, tighten sealing, is put into 180~220 DEG C of constant temperature ovens and stands reaction 8
~12 hours；Filtering precipitating after reaction is cleaned with deionized water repeatedly until pH value 7~8；It is precipitated or is taken out using centrifuge
Filter equipment, which is filtered, isolates sediment, is put into drying in 50~70 DEG C of baking oven and obtains final product.
The tungstates includes one of ammonium tungstate, ammonium metatungstate, sodium tungstate, potassium tungstate or combinations thereof, and zirconates includes
One of zirconyl nitrate, zirconyl chloride or combinations thereof, the concentration of zirconates in the solution are 0.05~0.1mol/L.
0.2~the 0.4mol/L of equivalent concentration of the glucose in the solution, concentration of hydrochloric acid are 4~6mol/L.
The present invention uses one-step synthesis method carbon coating ZrW2O8Negative thermal expansion material, simple process, product can be used for polymer
The temperature compensation filler of support plate, prepares zero thermal expansion electronic circuit board.
The contents of the present invention and feature have revealed that as above, however the present invention that describes of front only briefly or pertains only to this
The specific part of invention, feature of the invention may be more than what content disclosed herein was related to.Therefore, protection model of the invention
The revealed content of embodiment should be not limited to by enclosing, and should include the combination of all the elements embodied in different piece, with
And it is various without departing substantially from replacement and modification of the invention, and covered by claims of the present invention.
Detailed description of the invention
Fig. 1 is to synthesize carbon coating ZrW using (embodiment 1) of the invention2O8SEM photograph.
Specific embodiment
Embodiment 1
0.1mol/L ammonium tungstate and 0.05mol/L zirconyl nitrate are dissolved in 4mol/L hydrochloric acid, the Portugal 0.3mol/L is added
Solution is moved into the hydrothermal reaction kettle with polytetrafluoroethylliner liner, tightens sealing, be put into 180 DEG C of perseverances by grape sugar stirring and dissolving
Reaction 12 hours are stood in warm baking oven；Filtering precipitating after reaction is cleaned with deionized water repeatedly until pH value 7~8；Using
Centrifuge precipitating or pumping and filtering device are filtered and isolate sediment, are put into drying in 50 DEG C of baking oven and obtain shown in Fig. 1 finally
Product carbon coating ZrW2O8。
Embodiment 2
0.1mol/L ammonium metatungstate and 0.05mol/L zirconyl chloride are dissolved in 6mol/L hydrochloric acid, 0.2mol/L is added
Solution is moved into the hydrothermal reaction kettle with polytetrafluoroethylliner liner, tightens sealing, be put into 220 DEG C by glucose stirring and dissolving
Reaction 8 hours are stood in constant temperature oven；Filtering precipitating after reaction is cleaned with deionized water repeatedly until pH value 7~8；It adopts
It is filtered with centrifuge precipitating or pumping and filtering device and is isolated sediment, be put into drying in 70 DEG C of baking oven and obtain final product carbon
Coat ZrW2O8。
Embodiment 3
0.2mol/L sodium tungstate and 0.1mol/L zirconyl nitrate are dissolved in 5mol/L hydrochloric acid, 0.3mol/L grape is added
Solution is moved into the hydrothermal reaction kettle with polytetrafluoroethylliner liner, tightens sealing, be put into 200 DEG C of constant temperature by sugared stirring and dissolving
Reaction 10 hours are stood in baking oven；Filtering precipitating after reaction is cleaned with deionized water repeatedly until pH value 7~8；Using from
Scheming precipitating or pumping and filtering device, which are filtered, isolates sediment, is put into drying in 60 DEG C of baking oven and obtains final product carbon coating
ZrW2O8。
Embodiment 4
0.2mol/L potassium tungstate and 0.1mol/L zirconyl chloride are dissolved in 5mol/L hydrochloric acid, 0.4mol/L grape is added
Solution is moved into the hydrothermal reaction kettle with polytetrafluoroethylliner liner, tightens sealing, be put into 220 DEG C of constant temperature by sugared stirring and dissolving
Reaction 10 hours are stood in baking oven；Filtering precipitating after reaction is cleaned with deionized water repeatedly until pH value 7~8；Using from
Scheming precipitating or pumping and filtering device, which are filtered, isolates sediment, is put into drying in 60 DEG C of baking oven and obtains final product carbon coating
ZrW2O8。
Claims (4)
1. a kind of carbon coating ZrW2O8An one step preparation method, which is characterized in that comprising steps of by tungstates and zirconates according to original
Son ratio Zr: W=1: 2 is dissolved in hydrochloric acid, and glucose stirring and dissolving is added, and solution is moved into the water for having polytetrafluoroethylliner liner
In thermal response kettle, sealing is tightened, is put into 180~220 DEG C of constant temperature ovens and stands reaction 8~12 hours；It filters after reaction
Precipitating is cleaned with deionized water repeatedly until pH value 7~8；Using centrifuge precipitating or pumping and filtering device be filtered isolate it is heavy
Starch is put into drying in 50~70 DEG C of baking oven and obtains final product.
2. a kind of carbon coating ZrW according to claim 12O8An one step preparation method, it is characterised in that: the tungstates packet
Include one of ammonium tungstate, ammonium metatungstate, sodium tungstate, potassium tungstate or combinations thereof, zirconates includes zirconyl nitrate, in zirconyl chloride
One kind or combinations thereof, the concentration of zirconates in the solution are 0.05~0.1mol/L.
3. a kind of carbon coating ZrW according to claim 12O8An one step preparation method, it is characterised in that: the glucose exists
0.2~0.4mol/L of equivalent concentration in solution, concentration of hydrochloric acid are 4~6mol/L.
4. a kind of carbon coating ZrW as described in claims 1 to 3 any one2O8An one step preparation method preparation carbon coating
ZrW2O8。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810749727.8A CN108997784A (en) | 2018-07-02 | 2018-07-02 | A kind of carbon coating ZrW2O8An one step preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810749727.8A CN108997784A (en) | 2018-07-02 | 2018-07-02 | A kind of carbon coating ZrW2O8An one step preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108997784A true CN108997784A (en) | 2018-12-14 |
Family
ID=64599603
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810749727.8A Withdrawn CN108997784A (en) | 2018-07-02 | 2018-07-02 | A kind of carbon coating ZrW2O8An one step preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108997784A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6183716B1 (en) * | 1997-07-30 | 2001-02-06 | State Of Oregon Acting By And Through The State Board Of Higher Education Of Behalf Of Oregon State University | Solution method for making molybdate and tungstate negative thermal expansion materials and compounds made by the method |
| CN103937293A (en) * | 2014-04-28 | 2014-07-23 | 北京化工大学 | Carbon-coated white carbon black |
| CN106179407A (en) * | 2016-07-11 | 2016-12-07 | 陕西科技大学 | A kind of microwave-hydrothermal method prepares the method for carbon cladding zinc sulfide microsphere |
-
2018
- 2018-07-02 CN CN201810749727.8A patent/CN108997784A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6183716B1 (en) * | 1997-07-30 | 2001-02-06 | State Of Oregon Acting By And Through The State Board Of Higher Education Of Behalf Of Oregon State University | Solution method for making molybdate and tungstate negative thermal expansion materials and compounds made by the method |
| CN103937293A (en) * | 2014-04-28 | 2014-07-23 | 北京化工大学 | Carbon-coated white carbon black |
| CN106179407A (en) * | 2016-07-11 | 2016-12-07 | 陕西科技大学 | A kind of microwave-hydrothermal method prepares the method for carbon cladding zinc sulfide microsphere |
Non-Patent Citations (1)
| Title |
|---|
| 孙秀娟: "化学法制备负热膨胀性ZrW2O8粉体及薄膜", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| DE112015003730T5 (en) | Process for the production of metal powder | |
| CN104119250A (en) | Production method of high-purity metformin hydrochloride | |
| CN104829572A (en) | Novel crystal form of dapagliflozin and preparation method thereof | |
| CN106824131B (en) | A kind of chitosan-modified mesoporous material and its preparation method and application | |
| CN108619325A (en) | Tea Polyphenols are extracted from fresh tea passes | |
| JP2010254548A (en) | Colloidal silica and method for producing the same | |
| CN108997784A (en) | A kind of carbon coating ZrW2O8An one step preparation method | |
| CN105585035B (en) | A kind of preparation method of hollow aluminum oxide microspheres | |
| CN106673986A (en) | Method for preparing platinum acetylacetonate | |
| CN110568123A (en) | Method for analyzing quality of titanium liquid after acidolysis leaching | |
| CN114272914A (en) | Lithium adsorbent, membrane element, preparation method of membrane element, and lithium extraction method and device | |
| CN104140131B (en) | A kind of preparation method of potassium chloroplatinite | |
| CN109439891A (en) | A method of the recovering rare earth from LED fluorescent powder silica gel waste material | |
| CN105665748A (en) | Method for preparing high-purity superfine silver powder | |
| CN108821343B (en) | Slice Y2W3O12Method of synthesis of | |
| CN108707082A (en) | A kind of choline bitartrate preparation method | |
| CN108479857B (en) | Preparation method of ionic liquid modified polyaniline/titanium dioxide composite material | |
| CN106397347A (en) | Method for producing irganox 565 | |
| CN105440088B (en) | Glucosamine mixes strontium salt and its preparation method and application | |
| CN108500255A (en) | A kind of three-dimensional composite nano silver and preparation method thereof | |
| CN105859608B (en) | A method of preparing half tartrate crystal form B of piperazine Ma Selin | |
| CN109928423A (en) | A kind of preparation method of the nano barium phthalate for lithium battery | |
| CN106622174B (en) | The method that amino functional mesoporous silicon oxide is prepared as organic backbone using Lauxite | |
| JP4939021B2 (en) | Coated magnesium hydroxide, method for producing the same, and resin composition for electronic component material containing the same | |
| CN106565581A (en) | A method for comprehensive recovery and utilization of lithium containing mixed salts in a polyphenylene sulfide production process |
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 | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20181214 |
|
| WW01 | Invention patent application withdrawn after publication |