CN107325119A - A kind of method that complexing prepares yttrium colloidal sol - Google Patents
A kind of method that complexing prepares yttrium colloidal sol Download PDFInfo
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- CN107325119A CN107325119A CN201710460773.1A CN201710460773A CN107325119A CN 107325119 A CN107325119 A CN 107325119A CN 201710460773 A CN201710460773 A CN 201710460773A CN 107325119 A CN107325119 A CN 107325119A
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- yttrium
- colloidal sol
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- citric acid
- water bath
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- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 60
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 24
- 230000000536 complexating effect Effects 0.000 title abstract description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 99
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 58
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 38
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims abstract description 34
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 20
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 19
- 239000002244 precipitate Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 9
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims abstract description 8
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical class [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 6
- 239000011230 binding agent Substances 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 238000005266 casting Methods 0.000 claims description 7
- 239000008139 complexing agent Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 8
- 230000033228 biological regulation Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 5
- 230000008034 disappearance Effects 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 244000248349 Citrus limon Species 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000010406 interfacial reaction Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 2
- 238000003618 dip coating Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- KOESKPNTZNDMJP-UHFFFAOYSA-N yttrium(3+) hexanitrate Chemical compound [N+](=O)([O-])[O-].[Y+3].[Y+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] KOESKPNTZNDMJP-UHFFFAOYSA-N 0.000 description 1
- DEXZEPDUSNRVTN-UHFFFAOYSA-K yttrium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Y+3] DEXZEPDUSNRVTN-UHFFFAOYSA-K 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C1/00—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
- B22C1/16—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents
- B22C1/18—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of inorganic agents
- B22C1/183—Sols, colloids or hydroxide gels
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Colloid Chemistry (AREA)
Abstract
The present invention relates to a kind of method that complexing prepares yttrium colloidal sol；According to six water yttrium nitrates and citric acid 3:4‑4:3 ratio is dissolved in deionized water, and 60 80 DEG C of stirring in water bath obtain the 0.5mol/L of yttrium nitrate concentration 0.1 citric acid and the mixed solution of yttrium nitrate to dissolving；Addition is used as crosslinking agent polyethylene glycol 400；Citric acid is set fully to be complexed with yttrium nitrate；Under conditions of 60 80 DEG C of stirring in water bath, ammonia spirit is added drop-wise in the yttrium nitrate solution of citric acid complex, pH is to there is white precipitate suspension for regulation；Suspension continues that ammonia spirit is added dropwise, white precipitate gradually increases under stirring in water bath, is further continued for being added dropwise ammoniacal liquor up to white precipitate all disappears again, obtains the excessive yttrium colloidal sol of ammoniacal liquor；85 95 DEG C are warming up to, excess of ammonia water is evaporated, yttrium colloidal sols of the pH in the range of 7 11 is obtained.This method effectively reduces production cost, simplifies the preparation technology of yttrium colloidal sol, reduces the requirement to equipment.
Description
Technical field
The invention belongs to inorganic materials field, a kind of structural member surface protection sol bonded yttrium agent is specifically referred to
Preparation method.
Background technology
Inorganic coating, which has, can lift intensity, the hardness of matrix, the advantages of suppressing interfacial reaction, and with excellent height
Warm anti-oxidant, corrosion resistance, is widely used in the fields such as Aero-Space and electronic information.The method for preparing inorganic coating
Mainly there are the methods such as spraying process, dip-coating method, sol-gal process, vapour deposition process.Wherein spraying process is needed with dip-coating method
Indifferent oxide powder is dispersed in suitable dispersant or binding agent, indifferent oxide powder and dispersant or binding agent
After well mixed, that is, well mixed slurry is obtained, it is uniform then to can be prepared by surface using the method for spraying or Best-Effort request
Inorganic coating.Yttrium has good chemical inertness, does not occur with the element such as Hf, Cr, Ni, Nb, Ti in high temperature alloy
Reaction.Thus selection yttrium colloidal sol is used for as binding agent in the preparation of structural member coating material, and yttrium colloidal sol can be with after high-temperature process
Indifferent oxide reacts, and forms the compound containing yttrium, and then can effectively suppress interfacial reaction.
Yttrium colloidal sol is the uniform dispersion of nanometer yttrium hydroxide or yittrium oxide micelle in water, is commonly used for high temperature alloy casting
With binder material, it is widely used in model casting field.The main metal alkoxide, oxide or inorganic salts by yttrium of yttrium colloidal sol
To prepare.The metal alkoxide of wherein yttrium is expensive, and yttrium colloidal sol is typically prepared using the oxide or inorganic salts of yttrium.But mesh
The preparation technology that the oxide or inorganic salts of preceding use yttrium prepare yttrium colloidal sol is complicated, and the cycle is long, high to equipment requirement；And prepare
Yttrium colloidal sol harsh, be easily gelled the problems such as short using the term of validity that there is preservation condition.
This patent is related to a kind of yttrium colloidal sol preparation method of use citric acid complex.Preparation method is simple, and the cycle is short.It is made
Standby yttrium Stability of Sols, viscosity is adjustable, and pH is adjustable in the range of 7-11 in addition.
The content of the invention
The purpose of the present invention is for existing yttrium colloidal sol preparation technology at present is complicated, preservation condition is harsh, effective life
It is short, easily the defect such as gelling there is provided a kind of technique it is simple, be easy to storage, steady in a long-term, viscosity is adjustable, the adjustable yttrium colloidal sols of pH
Preparation method.During the present invention is the yttrium nitrate solution by the citric acid complex into heating water bath, ammoniacal liquor regulation pH is added dropwise and obtains
Obtain citric acid complex, and then the yttrium colloidal sol stablized.
Invention is achieved through the following technical solutions.
A kind of method that complexing prepares yttrium colloidal sol, using citric acid as complexing agent, is prepared using water bath heating with yttrium nitrate
Yttrium colloidal sol.
Method of the present invention, including step are as follows：
(1) according to six water yttrium nitrates and citric acid mol ratio with 3:4-4:3 ratio is dissolved in deionized water, 60-80 DEG C
Stirring in water bath obtains yttrium nitrate concentration 0.1-0.5mol/L citric acid and the mixed solution of yttrium nitrate to dissolving；Add conduct
Crosslinking agent polyethylene glycol 400；Citric acid is set fully to be complexed with yttrium nitrate；
(2) under conditions of 60-80 DEG C of stirring in water bath, ammonia spirit is added drop-wise to the yttrium nitrate solution of citric acid complex
In, pH is to there is white precipitate suspension for regulation；
(3) suspension continues that ammonia spirit is added dropwise, white precipitate gradually increases under stirring in water bath, is further continued for that ammonia is added dropwise
Water is until white precipitate all disappearances again, obtain the excessive yttrium colloidal sol of ammoniacal liquor；
(4) 85-95 DEG C is warming up to, excess of ammonia water is evaporated, yttrium colloidal sols of the pH in the range of 7-11 is obtained.
During step (4) the evaporation ammoniacal liquor, the viscosity of yttrium colloidal sol is adjusted, when being warming up to 85-95 DEG C, passes through control
Water bath time processed increases viscosity, or adding deionized water reduces viscosity, obtains viscosity in the range of 10-80MPas
Yttrium colloidal sol.
The mass ratio of the crosslinking agent polyethylene glycol 400 and six water yttrium nitrates in colloidal sol is 1:200-1:40.
The ammonia spirit concentration is 25-28wt%；Add in the deionized water of equivalent and dilute.
The inorganic oxide coating yttrium colloidal sol that the yttrium colloidal sol of the present invention is prepared as binding agent is applied in model casting
Core and wax pattern surface.
The yttrium colloidal sol of stabilization prepared by the present invention, dissolved adhesiveness is adjustable in the range of 10-80MPas；PH is in 7-11 scopes
It is interior adjustable.This preparation method is that yttrium nitrate prepares yttrium colloidal sol using the inorganic salts of yttrium, can effectively reduce production cost, in addition
Using citric acid as complexing agent, yttrium colloidal sol is prepared using water bath heating, the preparation technology of yttrium colloidal sol can be simplified, is reduced to equipment
Requirement.
Yttrium colloidal sol is mainly used in the preparation of shell generally as the binding agent in high temperature alloy model casting, and this is specially
Core and wax pattern surface that yttrium colloidal sol prepared by profit has been supplied in model casting at present, are prepared using yttrium colloidal sol as binding agent
Inorganic oxide coating refer specifically to aluminum oxide and yttria coating, can effectively suppress high temperature alloy and core and type
Interfacial reaction between shell, lifts the surface quality and surface of internal cavity quality of high-temperature alloy casting.
Brief description of the drawings
Fig. 1 is the experiment flow figure of present example 1.
Embodiment
Embodiment 1：
Experiment flow figure is as shown in Figure 1.Specific implementation step is as follows：
(1) by six water yttrium nitrates and citric acid mol ratio 3:4 ratio, weighs six water yttrium nitrate 38.301g, lemon respectively
Sour 25.019g, is added in deionized water, is uniformly mixed, and obtains citric acid and nitre that yttrium nitrate concentration is 0.1mol/L
The mixed solution of sour yttrium, will be with six water yttrium nitrate mass ratioes 1:200 polyethylene glycol 400 is added to above-mentioned match somebody with somebody as crosslinking agent
In the citric acid of system and the mixed solution of yttrium nitrate, 60 DEG C of stirring in water bath 2h make citric acid be fully complexed with yttrium nitrate；
(2) concentrated ammonia liquor of 200ml mass ratioes 25% is taken, it is slow to add in the deionized water of equivalent, it is standby after stirring
With；Into the yttrium nitrate solution under 60 DEG C of water bath conditions, the ammonia spirit prepared is slowly instilled, pH is adjusted, is 6 to pH
During left and right, start white precipitate occur；
(3) suspension continues that ammonia spirit is added dropwise, white precipitate gradually increases under stirring in water bath, is further continued for that ammonia is added dropwise
Water is until white precipitate all disappearances again, obtain the excessive yttrium colloidal sol of ammoniacal liquor；
(4) rise bath temperature evaporates excess of ammonia water, you can the yttrium colloidal sol stablized to 85 DEG C.Pass through control
The ammonia vol control pH that 85 DEG C of water bath time controls are evaporated, and appropriate deionized water regulation viscosity is added, finally obtain pH
For 7, viscosity for 10MPas citric acid complex stable yttrium colloidal sol.
Embodiment 2：
(1) by six water yttrium nitrates and citric acid mol ratio 1:1 ratio, weighs six water yttrium nitrate 76.602g, lemon respectively
Sour 41.028g, is added in deionized water, is uniformly mixed, and obtains citric acid and nitre that yttrium nitrate concentration is 0.3mol/L
The mixed solution of sour yttrium, will be with six water yttrium nitrate mass ratioes 3:200 polyethylene glycol 400 is added to above-mentioned match somebody with somebody as crosslinking agent
In the citric acid of system and the mixed solution of yttrium nitrate；70 DEG C of stirring in water bath 2.5h, make citric acid be fully complexed with yttrium nitrate；
(2) concentrated ammonia liquor of 200ml mass ratioes 25% is taken, it is slow to add in the deionized water of equivalent, it is standby after stirring
With；Into the yttrium nitrate solution under 70 DEG C of water bath conditions, the ammonia spirit prepared is slowly instilled, pH is adjusted, is 6 to pH
During left and right, start white precipitate occur；
(3) suspension continues that ammonia spirit is added dropwise, white precipitate gradually increases under stirring in water bath, is further continued for that ammonia is added dropwise
Water is until white precipitate all disappearances again, obtain the excessive yttrium colloidal sol of ammoniacal liquor；
(4) obtain after yttrium colloidal sol, be warming up to 90 DEG C of water-baths, evaporate excess of ammonia water, by controlling 90 DEG C of water bath times,
It is 10 to finally obtain pH, and viscosity is the stable yttrium colloidal sol of 45MPas citric acid complex.
Embodiment 3：
(1) by six water yttrium nitrates and citric acid mol ratio 4:3 ratio, weighs six water yttrium nitrate 76.602g, lemon respectively
Sour 31.521g, is added in deionized water, after being uniformly mixed, obtain yttrium nitrate concentration be 0.5mol/L citric acid with
The mixed solution of yttrium nitrate；Will be with six water yttrium nitrate mass ratioes 1:40 polyethylene glycol 400 is added to above-mentioned match somebody with somebody as dispersant
In the citric acid of system and the mixed solution of yttrium nitrate；80 DEG C of stirring in water bath 3h, make citric acid be fully complexed with yttrium nitrate；
(2) concentrated ammonia liquor of 200ml mass ratioes 25% is taken, it is slow to add in the deionized water of equivalent, it is standby after stirring
With；Into the yttrium nitrate solution under 80 DEG C of water bath conditions, the ammonia spirit prepared is slowly instilled, pH is adjusted, is 6 to pH
During left and right, start white precipitate occur；
(3) suspension continues that ammonia spirit is added dropwise, white precipitate gradually increases under stirring in water bath, is further continued for that ammonia is added dropwise
Water is until white precipitate all disappearances again, obtain the excessive yttrium colloidal sol of ammoniacal liquor；
(4) obtain after yttrium colloidal sol, be warming up to 95 DEG C of water-baths, evaporate excess of ammonia water, adjusted by controlling water bath time
The viscosity of solution is saved, pH=11 is finally obtained, viscosity is the stable yttrium colloidal sol of 80MPas citric acid complex.
According to technique described in this patent, long-term room-temperature preservation, stable chemical performance can be made, viscosity is adjustable, pH is adjustable
Yttrium colloidal sol, no longer list one by one.
All methods and technology of preparing that the present invention is disclosed and proposed, those skilled in the art can be by using for reference in herein
Hold, the link such as appropriate feed change and process route is realized, although the method and technology of preparing of the present invention are by preferably implementing
Example is described, and person skilled substantially can be not departing from present invention, in spirit and scope to as described herein
Methods and techniques route is modified or reconfigured, to realize final technology of preparing.In particular, Suo Youxiang
Similar replacement and change is apparent to those skilled in the art, and they are considered as being included in essence of the invention
In god, scope and content.
Claims (6)
1. a kind of preparation method of yttrium colloidal sol, using citric acid as complexing agent, yttrium colloidal sol is prepared with yttrium nitrate using water bath heating.
2. the method as described in claim 1, it is characterized in that step is as follows：
(1) according to six water yttrium nitrates and citric acid mol ratio with 3:4-4:3 ratio is dissolved in deionized water, 60-80 DEG C of water-bath
Stirring obtains yttrium nitrate concentration 0.1-0.5mol/L citric acid and the mixed solution of yttrium nitrate to dissolving；Add as crosslinking
Agent polyethylene glycol 400；Citric acid is set fully to be complexed with yttrium nitrate；
(2) under conditions of 60-80 DEG C of stirring in water bath, ammonia spirit is added drop-wise in the yttrium nitrate solution of citric acid complex, adjusted
Section pH is to there is white precipitate suspension；
(3) suspension continues that ammonia spirit is added dropwise, white precipitate gradually increases under stirring in water bath, is further continued for dropwise addition ammoniacal liquor straight
All disappeared again to white precipitate, obtain the excessive yttrium colloidal sol of ammoniacal liquor；
(4) 85-95 DEG C is warming up to, excess of ammonia water is evaporated, yttrium colloidal sols of the pH in the range of 7-11 is obtained.
3. method as claimed in claim 2, it is characterized in that during step (4) evaporation ammoniacal liquor, the viscosity of yttrium colloidal sol is adjusted,
When being warming up to 85-95 DEG C, by controlling water bath time to increase viscosity, or adding deionized water reduces viscosity, obtains
Yttrium colloidal sol of the viscosity in the range of 10-80MPas.
4. method as claimed in claim 2, it is characterized in that the mass ratio of polyethylene glycol 400 and six water yttrium nitrates in colloidal sol is 1:
200-1:40。
5. method as claimed in claim 2, it is characterized in that ammonia spirit concentration is 25-28wt%, adds the deionization of equivalent
Diluted in water.
6. the inorganic oxide coating yttrium colloidal sol that yttrium colloidal sol is prepared as binding agent applies core and wax-pattern in model casting
Surface.
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