CN109897401A - A kind of siliceous high-temperature-resistant insulating paint and its preparation method and application - Google Patents
A kind of siliceous high-temperature-resistant insulating paint and its preparation method and application Download PDFInfo
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Abstract
本发明涉及一种含硅耐高温绝缘涂料及其制备方法。所述含硅耐高温绝缘涂料包含如下组分或者由如下组分组成：磷酸盐溶液、氧化硅、氧化铝、氧化锌、硅溶胶和稀释剂以及可选的硼酸。所述方法包括磷酸盐溶液的制备：将磷酸溶液和金属氢氧化物升温至煮沸状态并保持至反应体系透明，然后降温至室温并陈化12小时以上；含硅耐高温绝缘涂料的制备：加入磷酸盐溶液、氧化硅、氧化铝、氧化锌、硅溶胶和稀释剂以及可选的硼酸，搅拌均匀后球磨，从而得到所述含硅耐高温绝缘涂料。本发明还提供了涂料在制备耐高温和/或绝缘涂层中的应用。本发明涂料具有优异的耐高温性、绝缘性和附着性等性能。The invention relates to a silicon-containing high temperature resistant insulating paint and a preparation method thereof. The silicon-containing high temperature resistant insulating coating comprises or consists of the following components: phosphate solution, silica, alumina, zinc oxide, silica sol, diluent and optional boric acid. The method includes the preparation of a phosphate solution: the phosphoric acid solution and the metal hydroxide are heated to a boiling state and kept until the reaction system is transparent, then cooled to room temperature and aged for more than 12 hours; the preparation of the silicon-containing high temperature resistant insulating coating: adding Phosphate solution, silicon oxide, aluminum oxide, zinc oxide, silica sol, diluent and optional boric acid are mixed uniformly and then ball-milled to obtain the silicon-containing high temperature resistant insulating coating. The present invention also provides the application of the coating in the preparation of high temperature resistant and/or insulating coatings. The coating of the invention has excellent properties such as high temperature resistance, insulation and adhesion.
Description
Technical field
The present invention relates to paint fields, and in particular to a kind of siliceous high-temperature-resistant insulating paint and its preparation method and application.
Background technique
With the rapid development of the industries such as Aeronautics and Astronautics, automobile and weapons, the requirement for material protection is increasingly
Height, certain elements need the operations under high temperature and corrosive environment, at the same also to have the physical characteristics such as antifatigue, anti-thermal shock and
The functional properties such as insulation.Coatings have excellent electrical insulating property, are widely used in electrical property component field.It is organic exhausted
Edge coating is easy aging and does not have flame retarding function.Inorganic coating has the characteristics that high temperature resistant, corrosion-resistant, do not go mouldy can be to base
Body plays the role of long-effective protection.But existing inorganic coating there are still such as adhesive force, corrosion resistance, corrosivity, heat resistance,
The deficiency of middle one or more kinds of performances of the performances such as shock resistance, weatherability, foaming characteristic, stability.
Summary of the invention
Existing in the prior art above-mentioned one or more kinds of insufficient in order to solve, the present invention provides one in first aspect
The siliceous high-temperature-resistant insulating paint of kind, the siliceous high-temperature-resistant insulating paint include following component or are grouped as by following group: phosphorus
Acid salt solution, silica, aluminium oxide, zinc oxide, silica solution and diluent and optional boric acid.
The present invention additionally provides in second aspect and a kind of prepare siliceous high-temperature insulation described in first aspect present invention and apply
The method of material, described method includes following steps: (1) preparation of phosphate solution: phosphoric acid solution and metal hydroxides being set
It is mixed in reaction vessel and is warming up to boil condition and reacted, until the transparency of reaction system is not further added by；Then, will
Reaction system is cooled to room temperature, and at room temperature ageing 12 hours or more, is preferably aged 12 hours to 36 hours, obtains phosphate
Solution；(2) phosphate solution, silica, oxidation the preparation of siliceous high-temperature-resistant insulating paint: are added in Xiang Suoshu phosphate solution
Aluminium, zinc oxide, silica solution and diluent and optional boric acid, it is excellent after mixing evenly by ball milling method mixing 2 hours or more
First ball milling 2 hours to 8 hours, to obtain the siliceous high-temperature-resistant insulating paint.
The present invention has following beneficial technical effect:
(1) high temperature resistant.Coating of the invention is applied by phosphate solution as main film forming substance, therefore by coating of the present invention
The maximum operation (service) temperature of the coating of system can be up to 1000 DEG C.
(2) insulating properties.Coating of the invention can be applied to conductive surface and play the role of insulation.
(3) anticorrosive property.Excellent anticorrosive property is provided for coated substrate by the coating that coating of the invention coats.
(4) stability.In some preferred embodiments, coating of the invention is due to controlling phosphatic composition,
So that coating is not likely to produce precipitating, can be stored for a long time after preparation.
(5) Anti-bubble.In some preferred embodiments, coating of the invention is due to controlling phosphatic group
At, therefore reduce or prevent the appearance of foaming phenomena when coating coating using coating of the invention.
(6) coating surface slickness is good.In some preferred embodiments, coating of the invention is due to using spherical powder
Material, in particular by the spherical powder with a certain proportion of specific surface area combination in the case where, these spherical powders are solid
Can be in coating substrate surface self assembly before change, therefore smooth coating can be formed.
(7) adhesive force is strong.The adhesive force of the coating coated by coating of the present invention can achieve 2 grades.
(8) shock resistance is good.The coating coated by coating of the present invention does not also crack under conditions of 800 DEG C to air quenching,
It is not stratified with matrix surface.
(9) corrosivity.In some preferred embodiments, coating of the invention is due to controlling phosphatic ratio,
The acidity of coating is controlled, therefore can be reduced to coated substrate such as corrosion of metal.On the other hand, slight excess of phosphorus
Acid is conducive to combining closely for coating and basal body interface to the acid etching of coated substrate such as metal appropriateness.
Specific embodiment
As described above, the present invention provides a kind of siliceous high-temperature-resistant insulating paint, the siliceous high temperature resistant in first aspect
Coatings include following component or are grouped as by following group: phosphate solution, silica, aluminium oxide, zinc oxide, silica solution
With diluent and optional boric acid.
In some preferred embodiments, the phosphate solution is phosphoric acid magnesium salt solution, the more preferably phosphoric acid of magnesium
The hydrophosphate of dihydric salt and/or magnesium.The phosphate solution can also be phosphalugel solution, the more preferably di(2-ethylhexyl)phosphate of aluminium
The hydrophosphate of hydrogen salt and/or magnesium.It is further preferred that the phosphate solution is the phosphoric acid magnesium salt solution and the aluminum phosphate
The combination of salting liquid.
In some preferred embodiments, the phosphate solution is prepared as follows: by phosphoric acid solution and gold
Belong to hydroxide and be placed in reaction vessel and mix and be warming up to boil condition and reacted, until reaction system become it is transparent and
The transparency is not further added by.With the progress of reaction, reaction system can gradually become transparent and finally no longer become more transparent
(i.e. transparency is not further added by) it is transparent can to observe by the naked eye reaction system)；Then, reaction system is cooled to
Room temperature, and at room temperature ageing 12 hours or more, preferably it is aged 12 hours to 36 hours.If digestion time is insufficient, possible body
Be it is unstable, influence the uniformity and adhesion strength of coating.By ageing, the equal of coating obtained by the present invention can be significantly improved
Even property and adhesion strength, to avoid coating peeling, reason is also unknown at present, and mechanism is up for further studying.
In some preferred embodiments, the phosphoric acid solution is the phosphate aqueous solution of 85 mass % or more, such as dense
Degree is the phosphate aqueous solution of 85 mass %.If phosphoric acid solution concentration is too low, reaction speed may be excessively slow, and with metal hydrogen-oxygen
The reaction of compound may not be sufficient, it is also possible to which the stability of the coating finally obtained is insufficient, and curing rate is slow, and coating is taken
Between it is long.
Wherein, the metal hydroxides is aluminium hydroxide and/or magnesium hydroxide, it can it is aluminium hydroxide, it can also be with
For magnesium hydroxide, the more preferably combination of aluminium hydroxide and magnesium hydroxide.
In the case where the metal hydroxides is aluminium hydroxide, the phosphoric acid and hydrogen-oxygen of participation and the reaction of aluminium hydroxide
The mass ratio for changing aluminium is 4~5:1, for example, 4:1,4.5:1 or 5:1.If the amount of aluminium hydroxide is excessive, phosphoric acid and hydroxide
Reactive aluminum is insufficient, precipitating is precipitated after there is white size pellets or cooling, so that wanted coating can not be made.If phosphorus
The dosage of acid is excessive, then is easy to cause to corrode to coated substrate, especially in the case where coated substrate is metal, in coating
Large quantitative metal liquid body can be generated, the uniformity of coating is destroyed, causes solidification difficult.
In the case where the metal hydroxides is magnesium hydroxide, the phosphoric acid and hydrogen-oxygen of participation and the reaction of magnesium hydroxide
The mass ratio for changing magnesium is 3.5~4.5:1.If the amount of magnesium hydroxide is excessive, phosphoric acid reacts not exclusively with magnesium hydroxide, reaction
System is agglomerated.If the dosage of phosphoric acid is excessive, it is easy that coated substrate is caused to corrode, is especially gold in coated substrate
In the case where category, large quantitative metal liquid body can be generated in coating, destroys the uniformity of coating, cause solidification difficult.
In the case where the metal hydroxides is the combination of aluminium hydroxide and magnesium hydroxide, participate in and aluminium hydroxide
The mass ratio of the phosphoric acid of reaction and aluminium hydroxide is 4~5:1, for example, 4:1,4.5:1 or 5:1, and is participated in and magnesium hydroxide
Reaction phosphoric acid and magnesium hydroxide mass ratio be 3.5~4.5:1.It is further preferred that the matter of magnesium hydroxide and aluminium hydroxide
Amount is than being not more than 0.4:1, for example, 0.1:1 to 0.4:1.If the mass ratio of magnesium hydroxide and aluminium hydroxide is excessive, i.e. hydrogen-oxygen
The quality accounting for changing magnesium is excessive, then the shock resistance of the coating coated by coating especially thermal shock resistance is poor, and coating is easy out
It splits, causes the separation with coated substrate.Specific mechanism is also unknown at present, needs to be further analyzed research.
In some preferred embodiments, the silica is powder particle form, and the average grain of powder particle
Diameter is 0.1 μm~0.3 μm, for example, 0.2 μm.
In some preferred embodiments, the aluminium oxide is powder particle form, and the average grain of powder particle
Diameter is 0.8 μm~2 μm, such as 1,1.5 or 2 μm.
The presence of aluminium oxide can improve the temperature tolerance of coating, and can reduce the corruption of coating with extra phosphatase reaction
Corrosion.The presence of silica can reduce fusing point, and due to oxidation at the use temperature (such as 1000 DEG C) more than 800 DEG C
Silicon can occur recrystallization phenomenon and can obtain the finer and close coating of coating.
In some preferred embodiments, the zinc oxide is powder particle form, and the average grain of powder particle
Diameter is 0.1 μm~0.3 μm, for example, 0.2 μm.Zinc oxide is added as additive, can be played thickening reinforcement and be promoted crosslinking
Effect.If the average grain diameter of Zinc oxide powder particle is too small, it is excessive to may cause system viscosity；If Zinc oxide powder
The average grain diameter of grain is excessive, then may not have strengthening effect.
In some preferred embodiments, the dioxide-containing silica in the silica solution is 21~25 mass %, such as
For 22,23,24 or 25 mass %.If the concentration of the silica in silica solution is excessive, coating surface cracking may cause；
If concentration is too low, possible coating surface is not fine and close.In addition, sodium ion when further preferential, in the silica solution
Content is less than 0.006 mass %.If the concentration of the sodium ion wherein contained is excessive, the use temperature of coating may be reduced.
It may further be preferable that pH value of the silica solution at 20 DEG C is 2~4.If pH is excessive, entire painting Material may cause
The instability problem of system.In coating system of the invention, due to the presence of phosphate and silica solution, so that coating was solidifying
Si-P-O key network can be formed in journey, improve coating to the intensity of the caking property and coating itself of matrix；Moreover, because silicon
Silica in colloidal sol can be filled in silica and aluminium oxide after paint solidification in the form of nano SiO 2 particle
In particulate interspaces, it is hereby achieved that very fine and close coating.
In some preferred embodiments, the diluent is dehydrated alcohol or ethanol water, and still, ethyl alcohol is water-soluble
The concentration of liquid preferably more than 50 volume % (such as 60,70,80 or 90 volume % or more), otherwise solution makes coating obtained
Comprising excessive moisture, the problem of causing excess moisture as described above to cause.
In some preferred embodiments, the concentration of each component in the siliceous high-temperature-resistant insulating paint is such as
Under: 20~40 mass % (the mass % of for example, 20,30 or 40) phosphate solution；0~1 mass % boric acid (for example, 0.1,0.5
Or 1 mass %)；2~10 mass % (the mass % of for example, 2,4,6,8 or 10) silica；15~40 mass % (for example, 20,
25,30,35 or 40 mass %) aluminium oxide；1~3 mass % (the mass % of for example, 1,2 or 3) zinc oxide；10~30 mass %
(the mass % of for example, 10,15,20,25 or 30) silica solution；With 10~50 mass % (matter of for example, 10,20,30,40 or 50
Measure %) diluent.Wherein, fusing point can be reduced and promote to form a film by adding a small amount of boric acid.
In some preferred embodiments, the solidification temperature of the siliceous high-temperature-resistant insulating paint is 100 DEG C~130
℃.Coating of the invention is coated on substrate, through 100 DEG C~130 DEG C at a temperature of solidify, coating of the invention can occur
The binding force of dehydration reaction, coating and matrix improves, and stable coatings can be formed on matrix.The use temperature of gained coating can
To be up to 1000 DEG C.In addition, at service temperatures, which plays the role of insulation, anticorrosion etc. to matrix such as metallic matrix.
The present invention filters in second aspect offer and a kind of prepare siliceous high-temperature insulation described in first aspect present invention and apply
The method of material, described method includes following steps:
(1) preparation of phosphate solution: phosphoric acid solution and metal hydroxides are placed in reaction vessel and mixes and heats up
It is reacted to boil condition, until reaction system becomes transparent and transparent is not further added by；Then, reaction system is cooled down
To room temperature, and be aged 12 hours in room temperature or more, it is preferably aged 12 hours to 36 hours, obtains phosphate solution；
(2) preparation of siliceous high-temperature-resistant insulating paint: in Xiang Suoshu phosphate solution be added phosphate solution, silica,
Aluminium oxide, zinc oxide, silica solution and diluent and optional boric acid, after mixing evenly by ball milling method mixing 2 hours with
On, preferential ball milling 2 hours to 8 hours, to obtain the siliceous high-temperature-resistant insulating paint.
Embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
Technical solution in the embodiment of the present invention is become apparent from, is fully described by.But described embodiment is of the invention
A part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
Embodiment 1: phosphalugel solution is prepared
Weigh 85% concentration phosphoric acid 230g, Al (OH)3Powder 50g, which is placed in reaction vessel, to stir evenly.It is stirred to react simultaneously
It is warming up to boil condition, stops heating after reaction system is transparent.Reaction system is aged 12 hours after being cooled to room temperature.
Embodiment 2: phosphoric acid magnesium salts and phosphalugel solution are prepared
Weigh 85% concentration phosphoric acid 290g, Al (OH)3Powder 50g, Mg (OH)2Powder 15g, is placed in reaction vessel and stirs
Uniformly.It is stirred to react and is warming up to boil condition, stops heating after reaction system is transparent.Reaction system is aged after being cooled to room temperature
16 hours.
Embodiment 3: siliceous high-temperature-resistant insulating paint
Phosphate solution, the 1g boric acid, 8g silica, 26g aluminium oxide, 4g zinc oxide, 35g silicon for taking 40g embodiment 1 to prepare
Colloidal sol (wherein dioxide-containing silica is 25 mass %, and sodium ions content is 0.024 mass %, pH 2.4), 36g concentration
50% ethanol solution, it is uniform by ball milling method mixing, obtain high-temperature insulating paint.Coating solidifies institute on stainless steel base
Coating is obtained, 30h is not fallen off under 1000 DEG C of environment, tests 2 grades of adhesive force, average dielectric constant 3.42 (repeat number n=10).
Embodiment 4: siliceous high-temperature-resistant insulating paint
Phosphate solution, the 1g boric acid, 8g silica, 26g aluminium oxide, 4g zinc oxide, 35g silicon for taking 40g embodiment 2 to prepare
Colloidal sol (wherein dioxide-containing silica is 25 mass %, and sodium ions content is 0.024 mass %, pH 2.4), 36g concentration
50% ethanol solution, it is uniform by ball milling method mixing, obtain high-temperature insulating paint.Coating solidifies institute on stainless steel base
Coating is obtained, 30h is not fallen off under 1000 DEG C of environment, tests 2 grades of adhesive force, average dielectric constant 3.44 (repeat number n=10).
Embodiment 5 to 11
It controls phosphoric acid and magnesium hydroxide mass ratio is 4:1；The mass ratio of aluminium hydroxide and magnesium hydroxide is 3.5:1, as follows
Change the mass ratio of phosphoric acid and aluminium hydroxide shown in table, other according to phosphate solution is prepared described in embodiment 2, then according still further to
Coating is prepared described in embodiment 4.As a result as shown in the table.
Embodiment 12 to 17
It controls phosphoric acid and aluminium hydroxide mass ratio is 4.6:1；The mass ratio of aluminium hydroxide and magnesium hydroxide is 4:1, as follows
Change the mass ratio of phosphoric acid and magnesium hydroxide shown in table, other according to phosphate solution is prepared described in embodiment 2, then according still further to
Coating is prepared described in embodiment 4.As a result as shown in the table.
Embodiment 18 to 24
Phosphoric acid and aluminium hydroxide mass ratio are controlled as 4.6:1, the mass ratio of phosphoric acid and magnesium hydroxide is 4:1；Such as following table institute
Show change aluminium hydroxide and magnesium hydroxide mass ratio, other according to phosphate solution is prepared described in embodiment 2, then according still further to
Coating is prepared described in embodiment 4.As a result as shown in the table.
Embodiment 25 to 36
Other than the digestion time of content and embodiment 35 and 36 shown in the following table is respectively 4 hours and 0 hour,
He all in accordance with preparing phosphate solution described in embodiment 2, and prepare coating according to described in embodiment 4.
Note: each component is in terms of weight percentage.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of siliceous high-temperature-resistant insulating paint, which is characterized in that the siliceous high-temperature-resistant insulating paint include following component or
Person is grouped as by following group: phosphate solution, silica, aluminium oxide, zinc oxide, silica solution and diluent and optional boron
Acid.
2. siliceous high-temperature-resistant insulating paint according to claim 1, which is characterized in that the siliceous high-temperature-resistant insulating paint
In each component concentration it is as follows: 20~40 mass % phosphate solutions；0-1 mass % boric acid；2~10 mass % oxidation
Silicon；15~40 mass % aluminium oxide；1~3 mass % zinc oxide；10~30 mass % silica solution；It is diluted with 10~50 mass %
Agent.
3. siliceous high-temperature-resistant insulating paint according to claim 1 or 2, it is characterised in that:
The silica is powder particle form, and the average grain diameter of powder particle is 0.1 μm~0.3 μm；
The zinc oxide is powder particle form, and the average grain diameter of powder particle is 0.1 μm~0.3 μm；
The aluminium oxide is powder particle form, and the average grain diameter of powder particle is 0.8 μm~2 μm.
4. siliceous high-temperature-resistant insulating paint according to any one of claim 1 to 3, it is characterised in that:
Dioxide-containing silica in the silica solution is 21~25 mass %, and sodium ions content is less than 0.006 mass %；
Preferably, pH value of the silica solution at 20 DEG C is 2~4.
5. siliceous high-temperature-resistant insulating paint according to any one of claim 1 to 4, which is characterized in that the diluent
For dehydrated alcohol or ethanol water, the ethanol water is preferably the ethanol water of 50 volume %.
6. siliceous high-temperature-resistant insulating paint according to any one of claim 1 to 5, which is characterized in that the phosphate
Solution is phosphoric acid magnesium salt solution and/or phosphalugel solution；Preferably, the phosphate solution is phosphoric acid magnesium salt solution and phosphorus
The combination of sour aluminum salt solution.
7. siliceous high-temperature-resistant insulating paint according to claim 6, which is characterized in that the phosphate solution presses such as lower section
Formula preparation:
Phosphoric acid solution and metal hydroxides are placed in reaction vessel and mixes and is warming up to boil condition and react, until anti-
It answers system to become transparent and transparent is not further added by；Then, reaction system is cooled to room temperature, and is aged 12 hours in room temperature
More than, preferably it is aged 12 hours to 36 hours；Wherein, the metal hydroxides be aluminium hydroxide and/or magnesium hydroxide, preferably
For the combination of aluminium hydroxide and magnesium hydroxide.
8. high temperature resistant fluorescent paint according to any one of claim 1 to 7, which is characterized in that the phosphoric acid solution is
The phosphate aqueous solution of 85 mass % or more, and:
In the case where the metal hydroxides is aluminium hydroxide, the phosphoric acid and aluminium hydroxide of participation and the reaction of aluminium hydroxide
Mass ratio be 4~5:1；
In the case where the metal hydroxides is magnesium hydroxide, the phosphoric acid and magnesium hydroxide of participation and the reaction of magnesium hydroxide
Mass ratio be 3.5~4.5:1；
In the case where the metal hydroxides is the combination of aluminium hydroxide and magnesium hydroxide, magnesium hydroxide and aluminium hydroxide
Mass ratio is not more than 2:5.
9. a kind of method for preparing siliceous high-temperature-resistant insulating paint described in any item of the claim 1 to 8, which is characterized in that
Described method includes following steps:
(1) preparation of phosphate solution: phosphoric acid solution and metal hydroxides are placed in reaction vessel to mix and be warming up to and boiled
Boiling state is reacted, until reaction system becomes transparent and transparent is not further added by；Then, reaction system is cooled to room
Temperature, and at room temperature ageing 12 hours or more, it is preferably aged 12 hours to 36 hours, obtains phosphate solution；
(2) phosphate solution, silica, oxidation the preparation of siliceous high-temperature-resistant insulating paint: are added in Xiang Suoshu phosphate solution
Aluminium, zinc oxide, silica solution and diluent and optional boric acid, it is excellent after mixing evenly by ball milling method mixing 2 hours or more
First ball milling 2 hours to 8 hours, to obtain the siliceous high-temperature-resistant insulating paint.
10. siliceous high-temperature-resistant insulating paint according to any one of claim 1 to 8 or side as claimed in claim 9
Application of the siliceous high-temperature-resistant insulating paint made from method in preparation high temperature resistant and/or insulating coating.
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| CN111073356A (en) * | 2019-12-02 | 2020-04-28 | 中昊北方涂料工业研究设计院有限公司 | Single-component chromium-free silicon steel sheet protective coating and preparation thereof |
| CN112239863A (en) * | 2020-09-11 | 2021-01-19 | 武汉圆融科技有限责任公司 | An insulating coating solution for improving cracks in surface coating of grain-oriented silicon steel and preparation method thereof, and grain-oriented silicon steel sheet |
| CN112341845A (en) * | 2020-09-27 | 2021-02-09 | 中昊北方涂料工业研究设计院有限公司 | Chromium-free aluminum-containing phosphate composition and coating |
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