CN108250985B - High-temperature-resistant adhesive capable of being rapidly cured at room temperature and preparation method thereof - Google Patents
High-temperature-resistant adhesive capable of being rapidly cured at room temperature and preparation method thereof Download PDFInfo
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- CN108250985B CN108250985B CN201810087689.4A CN201810087689A CN108250985B CN 108250985 B CN108250985 B CN 108250985B CN 201810087689 A CN201810087689 A CN 201810087689A CN 108250985 B CN108250985 B CN 108250985B
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
The invention belongs to the field of adhesives, and particularly relates to a high-temperature-resistant adhesive capable of being rapidly cured at room temperature and a preparation method thereof. A high-temperature-resistant adhesive capable of being rapidly cured at room temperature comprises a component A and a component B in a mass ratio of 100:150, wherein the component A is a magnesium oxide and iron oxide modified aluminum dihydrogen phosphate solution; the component B comprises the following raw materials in parts by mass: 50-90 parts of aluminum oxide, 0.1-25 parts of aluminum nitride, 0.1-10 parts of calcium fluoride, 0.2-15 parts of high-temperature resistant filler and 0.1-5 parts of toughening agent. The adhesive prepared by using the modified aluminum dihydrogen phosphate has low viscosity, is easy to coat, and is improved in curing speed, water resistance, thermal shock resistance and bonding strength; the curing accelerator with mild addition is added into the curing agent, and the addition proportion is adjusted, so that the whole curing process is mild, the porosity of the cured product is low, and the structure of the cured product is more compact, thereby improving the mechanical property and the water resistance of the cured product of the adhesive, and simultaneously solving the contradiction between the room-temperature rapid curing and the application period.
Description
Technical Field
The invention belongs to the field of adhesives, and particularly relates to a high-temperature-resistant adhesive capable of being rapidly cured at room temperature and a preparation method thereof.
Background
According to the difference of chemical components, adhesives can be classified into organic adhesives and inorganic adhesives. Compared with organic adhesives, the inorganic adhesive has the advantages of low cost, convenient use, excellent temperature resistance, small thermal expansion coefficient, room-temperature curing, no shrinkage, oil resistance, radiation resistance, good durability and the like, plays an irreplaceable role in the fields of aviation, aerospace, machinery, electronics, chemical industry, buildings and the like, and has increasingly remarkable importance.
Phosphate adhesives are the most important and promising inorganic adhesives. The high-temperature-resistant adhesive is prepared by taking aluminum phosphate or modified phosphate as curing main resin and adding a proper amount of curing agent, framework material and the like, and has the characteristics of environmental protection, rich resources, strong adhesive force, simple preparation, excellent heat resistance, fire resistance, durability and the like. In order to realize normal-temperature curing of the inorganic phosphate adhesive, alkaline metal oxide is often added into an adhesive curing agent, and due to violent reaction, agglomeration is easily caused, so that the number of holes of a cured product is increased, and the technical problems of reduced mechanical property, poor manufacturability and the like of the adhesive are easily caused.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a high-temperature-resistant adhesive capable of being rapidly cured at room temperature and a preparation method thereof.
The technical scheme of the invention is as follows:
a high-temperature-resistant adhesive capable of being rapidly cured at room temperature comprises a component A and a component B in a mass ratio of 100:150, wherein the component A is a magnesium oxide and iron oxide modified aluminum dihydrogen phosphate solution; the component B comprises the following raw materials in parts by mass:
further, the modified aluminum dihydrogen phosphate solution is prepared by reacting 100 parts by mass of 85% phosphoric acid solution with 20-45 parts by mass of aluminum hydroxide to obtain an aluminum dihydrogen phosphate solution, and modifying the aluminum dihydrogen phosphate solution by 0.1-10 parts by mass of magnesium oxide and 0.1-10 parts by mass of iron oxide.
Further, the high-temperature-resistant filler in the component B is prepared from the following raw materials in parts by mass:
0.1-10 parts of titanium carbide
0.1-5 parts of zirconium oxide or yttrium oxide.
Further, the toughening agent in the component B is silicon carbide chopped fibers or silicon carbide whiskers.
Further, the curing temperature of the adhesive is 21-25 ℃, and the curing time is 24 hours.
The preparation method of the room-temperature fast-curing high-temperature-resistant adhesive comprises the following steps:
the method comprises the following steps: weighing the following raw materials in parts by mass:
100 parts of 85% phosphoric acid solution, 20-45 parts of aluminum hydroxide solid powder, 0.1-10 parts of magnesium oxide, 0.1-10 parts of ferric oxide, 50-90 parts of aluminum oxide, 0.1-25 parts of aluminum nitride, 0.1-10 parts of calcium fluoride, 0.1-10 parts of titanium carbide, 0.1-5 parts of zirconium oxide or yttrium oxide and 0.1-5 parts of silicon carbide chopped fibers or silicon carbide whiskers;
step two: preparing a component A:
slowly adding 20-45 parts of aluminum hydroxide solid powder into 100 parts of 85% phosphoric acid solution by mass, stirring for a certain time at a certain reaction temperature, adding 0.1-10 parts of magnesium oxide and 0.1-10 parts of ferric oxide, and keeping the original reaction temperature and continuously stirring for a certain time to prepare a modified aluminum dihydrogen phosphate solution;
step three: preparing a component B:
adding 50-90 parts of aluminum oxide, 0.1-25 parts of aluminum nitride, 0.1-10 parts of calcium fluoride, 0.1-10 parts of titanium carbide, 0.1-5 parts of zirconium oxide or yttrium oxide and 0.1-5 parts of silicon carbide chopped fibers or silicon carbide whiskers into a stirrer, and stirring and uniformly mixing;
step four: preparing a room-temperature fast-curing high-temperature-resistant adhesive:
and adding the component A and the component B into a mortar according to the mass ratio of 100:150, and uniformly mixing and grinding to obtain the room-temperature fast-curing high-temperature-resistant adhesive.
Further, the reaction temperature in the second step is 90-100 ℃, and the stirring speed is 80-100 rmp.
Further, the reaction time of the phosphoric acid solution and the aluminum hydroxide solid powder in the second step is 1 hour, and the reaction time after adding the magnesium oxide and the iron oxide is 1.5 hours.
The invention has the beneficial effects that:
firstly, magnesium oxide, iron oxide and other metal oxides are used for modifying aluminum dihydrogen phosphate to prepare resin, compared with common aluminum phosphate resin, the viscosity of the adhesive is greatly reduced, the coating is easy, the manufacturability is good, the curing speed can be improved by utilizing the magnesium oxide modified aluminum dihydrogen phosphate, the adhesive provided by the invention can be rapidly cured at room temperature under the combined action of the magnesium oxide modified aluminum dihydrogen phosphate and a curing accelerator, namely aluminum nitride, the maximum value of the bonding strength can be up to 50% after 1 hour of curing, and the adhesive can be nearly completely cured within 24 hours at room temperature; the iron oxide modified aluminum dihydrogen phosphate can improve the bonding strength of the adhesive; meanwhile, the waterproof performance, the thermal shock resistance, the bonding strength and the like of the adhesive are improved.
Secondly, the mild curing accelerator aluminum nitride is added into the curing agent aluminum oxide, and the adding proportion of the curing accelerator is adjusted, so that the viscosity of the adhesive is low after the resin and the curing agent are mixed, the whole curing process is mild, and the contradiction between room-temperature rapid curing and the pot life is solved.
The calcium fluoride is added into the adhesive system, and can act with the curing agent in a synergistic manner, so that the cured product structure is more compact by reducing the porosity of the cured product in a mild curing process, and the mechanical property and the water resistance of the cured product of the adhesive are improved.
Titanium carbide, zirconium oxide or yttrium oxide is added into the adhesive system to serve as high-temperature-resistant filler, so that the adhesive can still maintain certain bonding strength at the high temperature of 1600 ℃; the toughening agent is also added into the adhesive system, so that the toughness of the adhesive system is improved.
The high-temperature-resistant adhesive capable of being rapidly cured at room temperature and the preparation method thereof have the advantages of low cost of raw materials, simple process, easy operation and no environmental pollution.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1: a room-temperature fast-curing high-temperature-resistant adhesive and a preparation method thereof are disclosed:
a high-temperature-resistant adhesive capable of being rapidly cured at room temperature comprises a component A and a component B in a mass ratio of 100:150, wherein the component A is a magnesium oxide and iron oxide modified aluminum dihydrogen phosphate solution;
the component B comprises the following raw materials in parts by mass:
the modified aluminum dihydrogen phosphate solution in the component A is prepared by reacting 100 parts by mass of 85% phosphoric acid solution with 20-45 parts by mass of aluminum hydroxide to obtain an aluminum dihydrogen phosphate solution, and modifying the aluminum dihydrogen phosphate solution by 0.1-10 parts by mass of magnesium oxide and 0.1-10 parts by mass of iron oxide.
The curing temperature of the room temperature fast curing high temperature resistant adhesive is 21-25 ℃, the curing time is 24 hours, and the pot life is 40-60 min.
The preparation method of the room-temperature fast-curing high-temperature-resistant adhesive comprises the following steps:
the method comprises the following steps: weighing the following raw materials in parts by mass:
100 parts of 85% phosphoric acid solution, 20-45 parts of aluminum hydroxide solid powder, 0.1-10 parts of magnesium oxide, 0.1-10 parts of ferric oxide, 50-90 parts of aluminum oxide, 0.1-25 parts of aluminum nitride, 0.1-10 parts of calcium fluoride, 0.1-10 parts of titanium carbide, 0.1-5 parts of zirconium oxide or yttrium oxide and 0.1-5 parts of silicon carbide chopped fibers or silicon carbide whiskers;
step two: preparing a component A:
slowly adding 20-45 parts of aluminum hydroxide solid powder into 100 parts of 85% phosphoric acid solution by mass, stirring for a certain time at a certain reaction temperature, adding 0.1-10 parts of magnesium oxide and 0.1-10 parts of ferric oxide, and keeping the original reaction temperature and continuously stirring for a certain time to prepare a modified aluminum dihydrogen phosphate solution;
step three: preparing a component B:
adding 50-90 parts of aluminum oxide, 0.1-25 parts of aluminum nitride, 0.1-10 parts of calcium fluoride, 0.1-10 parts of titanium carbide, 0.1-5 parts of zirconium oxide or yttrium oxide and 0.1-5 parts of silicon carbide chopped fibers or silicon carbide whiskers into a stirrer, and stirring and uniformly mixing;
step four: preparing a room-temperature fast-curing high-temperature-resistant adhesive:
and adding the component A and the component B into a mortar according to the mass ratio of 100:150, and uniformly mixing and grinding to obtain the room-temperature fast-curing high-temperature-resistant adhesive.
Further, the reaction temperature in the second step is 90-100 ℃, the stirring speed is 80-100 rmp, the reaction time of the phosphoric acid solution and the aluminum hydroxide solid powder is 1 hour, and the reaction time after the magnesium oxide and the ferric oxide are added is 1.5 hours.
Example 2: a room-temperature fast-curing high-temperature-resistant adhesive and a preparation method thereof are disclosed:
a high-temperature-resistant adhesive capable of being rapidly cured at room temperature comprises a component A and a component B in a mass ratio of 100:150, wherein the component A is a magnesium oxide and iron oxide modified aluminum dihydrogen phosphate solution; the component B comprises the following raw materials in parts by mass:
the modified aluminum dihydrogen phosphate solution in the component A is prepared by reacting 100 parts by mass of 85% phosphoric acid solution with 25 parts by mass of aluminum hydroxide to obtain an aluminum dihydrogen phosphate solution, and modifying the aluminum dihydrogen phosphate solution by using 2 parts by mass of magnesium oxide and 2 parts by mass of iron oxide.
The curing temperature of the room temperature fast curing high temperature resistant adhesive is 21-25 ℃, the curing time is 24 hours, and the pot life is 40-60 min.
The preparation method of the room-temperature fast-curing high-temperature-resistant adhesive comprises the following steps:
the method comprises the following steps: weighing the following raw materials in parts by mass:
100 parts of 85% phosphoric acid solution, 25 parts of aluminum hydroxide solid powder, 2 parts of magnesium oxide, 2 parts of ferric oxide, 60 parts of aluminum oxide, 5 parts of aluminum nitride, 2 parts of calcium fluoride, 2 parts of titanium carbide, 1 part of zirconium oxide and 1 part of silicon carbide chopped fiber;
step two: preparing a component A:
slowly adding 25 parts of aluminum hydroxide solid powder into 100 parts of 85% phosphoric acid solution by mass, stirring for 1h at the stirring speed of 80rmp at the temperature of 92 ℃, adding 2 parts of magnesium oxide and 2 parts of iron oxide, and keeping the temperature of 92 ℃ and continuously stirring for 1.5h to prepare modified aluminum dihydrogen phosphate solution;
step three: preparing a component B:
adding 60 parts of alumina, 5 parts of aluminum nitride, 2 parts of calcium fluoride, 2 parts of titanium carbide, 1 part of zirconia and 1 part of silicon carbide chopped fibers into a stirrer for stirring, taking out the component B after stirring for 1 hour, manually crushing some blocks, pouring into the stirrer for stirring, and repeating the steps for three times to uniformly mix the raw materials in the component B;
step four: preparing a room-temperature fast-curing high-temperature-resistant adhesive:
adding the component A and the component B into a mortar according to the mass ratio of 100:150, uniformly mixing and grinding, and standing for 5-10 min, wherein the adhesive has no solid particles and no obvious interface, so that the finished product of the room-temperature fast-curing high-temperature-resistant adhesive is prepared.
Example 3: a room-temperature fast-curing high-temperature-resistant adhesive and a preparation method thereof are disclosed:
a high-temperature-resistant adhesive capable of being rapidly cured at room temperature comprises a component A and a component B in a mass ratio of 100:150, wherein the component A is a magnesium oxide and iron oxide modified aluminum dihydrogen phosphate solution; the component B comprises the following raw materials in parts by mass:
the modified aluminum dihydrogen phosphate solution in the component A is prepared by reacting 100 parts by mass of 85% phosphoric acid solution with 30 parts by mass of aluminum hydroxide to obtain an aluminum dihydrogen phosphate solution, and modifying the aluminum dihydrogen phosphate solution by using 4 parts by mass of magnesium oxide and 4 parts by mass of iron oxide.
The curing temperature of the room temperature fast curing high temperature resistant adhesive is 21-25 ℃, the curing time is 24 hours, and the pot life is 40-60 min.
The preparation method of the room-temperature fast-curing high-temperature-resistant adhesive comprises the following steps:
the method comprises the following steps: weighing the following raw materials in parts by mass:
100 parts of 85% phosphoric acid solution, 30 parts of aluminum hydroxide solid powder, 4 parts of magnesium oxide, 4 parts of ferric oxide, 70 parts of aluminum oxide, 10 parts of aluminum nitride, 4 parts of calcium fluoride, 4 parts of titanium carbide, 2 parts of zirconium oxide and 2 parts of silicon carbide chopped fibers;
step two: preparing a component A:
slowly adding 30 parts of aluminum hydroxide solid powder into 100 parts of 85% phosphoric acid solution by mass, stirring for 1h at the stirring speed of 90rmp at 94 ℃, adding 4 parts of magnesium oxide and 4 parts of iron oxide, and keeping the temperature at 94 ℃ and continuously stirring for 1.5h to prepare modified aluminum dihydrogen phosphate solution;
step three: preparing a component B:
adding 70 parts of alumina, 10 parts of aluminum nitride, 4 parts of calcium fluoride, 4 parts of titanium carbide, 2 parts of zirconia and 2 parts of silicon carbide chopped fibers into a stirrer for stirring, taking out the component B after stirring for 1 hour, manually crushing some blocks, pouring into the stirrer for stirring, and repeating the steps for three times to uniformly mix the raw materials in the component B;
step four: preparing a room-temperature fast-curing high-temperature-resistant adhesive:
adding the component A and the component B into a mortar according to the mass ratio of 100:150, uniformly mixing and grinding, and standing for 5-10 min, wherein the adhesive has no solid particles and no obvious interface, so that the finished product of the room-temperature fast-curing high-temperature-resistant adhesive is prepared.
Example 4: a room-temperature fast-curing high-temperature-resistant adhesive and a preparation method thereof are disclosed:
a high-temperature-resistant adhesive capable of being rapidly cured at room temperature comprises a component A and a component B in a mass ratio of 100:150, wherein the component A is a magnesium oxide and iron oxide modified aluminum dihydrogen phosphate solution; the component B comprises the following raw materials in parts by mass:
the modified aluminum dihydrogen phosphate solution in the component A is prepared by reacting 100 parts by mass of 85% phosphoric acid solution with 35 parts by mass of aluminum hydroxide to obtain an aluminum dihydrogen phosphate solution, and modifying the aluminum dihydrogen phosphate solution by 6 parts by mass of magnesium oxide and 6 parts by mass of iron oxide.
The curing temperature of the room temperature fast curing high temperature resistant adhesive is 21-25 ℃, the curing time is 24 hours, and the pot life is 40-60 min.
The preparation method of the room-temperature fast-curing high-temperature-resistant adhesive comprises the following steps:
the method comprises the following steps: weighing the following raw materials in parts by mass:
100 parts of 85% phosphoric acid solution, 35 parts of aluminum hydroxide solid powder, 6 parts of magnesium oxide, 6 parts of ferric oxide, 80 parts of aluminum oxide, 15 parts of aluminum nitride, 6 parts of calcium fluoride, 6 parts of titanium carbide, 3 parts of yttrium oxide and 3 parts of silicon carbide whisker;
step two: preparing a component A:
slowly adding 35 parts of aluminum hydroxide solid powder into 100 parts of 85% phosphoric acid solution by mass, stirring for 1h at the stirring speed of 100rmp at 95 ℃, adding 6 parts of magnesium oxide and 6 parts of iron oxide, and keeping stirring for 1.5h at 95 ℃ to obtain modified aluminum dihydrogen phosphate solution;
step three: preparing a component B:
adding 80 parts of aluminum oxide, 15 parts of aluminum nitride, 6 parts of calcium fluoride, 6 parts of titanium carbide, 3 parts of yttrium oxide and 3 parts of silicon carbide whiskers into a stirrer for stirring, taking out the component B after stirring for 1 hour, manually crushing some blocks, pouring the blocks into the stirrer for stirring, and repeating the steps for three times to uniformly mix all the raw materials in the component B;
step four: preparing a room-temperature fast-curing high-temperature-resistant adhesive:
adding the component A and the component B into a mortar according to the mass ratio of 100:150, uniformly mixing and grinding, and standing for 5-10 min, wherein the adhesive has no solid particles and no obvious interface, so that the finished product of the room-temperature fast-curing high-temperature-resistant adhesive is prepared.
Example 5: a room-temperature fast-curing high-temperature-resistant adhesive and a preparation method thereof are disclosed:
a high-temperature-resistant adhesive capable of being rapidly cured at room temperature comprises a component A and a component B in a mass ratio of 100:150, wherein the component A is a magnesium oxide and iron oxide modified aluminum dihydrogen phosphate solution; the component B comprises the following raw materials in parts by mass:
the modified aluminum dihydrogen phosphate solution in the component A is prepared by reacting 100 parts by mass of 85% phosphoric acid solution with 40 parts by mass of aluminum hydroxide to obtain an aluminum dihydrogen phosphate solution, and modifying the aluminum dihydrogen phosphate solution by 8 parts by mass of magnesium oxide and 8 parts by mass of iron oxide.
The curing temperature of the room temperature fast curing high temperature resistant adhesive is 21-25 ℃, the curing time is 24 hours, and the pot life is 40-60 min.
The preparation method of the room-temperature fast-curing high-temperature-resistant adhesive comprises the following steps:
the method comprises the following steps: weighing the following raw materials in parts by mass:
100 parts of 85% phosphoric acid solution, 40 parts of aluminum hydroxide solid powder, 8 parts of magnesium oxide, 8 parts of ferric oxide, 85 parts of aluminum oxide, 20 parts of aluminum nitride, 8 parts of calcium fluoride, 8 parts of titanium carbide, 4 parts of yttrium oxide and 4 parts of silicon carbide whisker;
step two: preparing a component A:
slowly adding 40 parts of aluminum hydroxide solid powder into 100 parts of 85% phosphoric acid solution by mass, stirring for 1h at the stirring speed of 80rmp at 98 ℃, adding 8 parts of magnesium oxide and 8 parts of iron oxide, and keeping the temperature at 98 ℃ and continuously stirring for 1.5h to prepare modified aluminum dihydrogen phosphate solution;
step three: preparing a component B:
adding 85 parts of alumina, 20 parts of aluminum nitride, 8 parts of calcium fluoride, 8 parts of titanium carbide, 4 parts of yttrium oxide and 4 parts of silicon carbide whiskers into a stirrer for stirring, taking out the component B after stirring for 1 hour, manually crushing some blocks, pouring into the stirrer for stirring, and repeating the steps for three times to uniformly mix all the raw materials in the component B;
step four: preparing a room-temperature fast-curing high-temperature-resistant adhesive:
adding the component A and the component B into a mortar according to the mass ratio of 100:150, uniformly mixing and grinding, and standing for 5-10 min, wherein the adhesive has no solid particles and no obvious interface, so that the finished product of the room-temperature fast-curing high-temperature-resistant adhesive is prepared.
Testing the performance of the room temperature fast curing high temperature resistant adhesive:
the adhesives provided in examples 2-5 were subjected to a heat resistance test, and the results were as follows:
curing at room temperature for 24h, heating to 1300 ℃ at the speed of 10 ℃/min in an air environment, and controlling the thermal weight loss to be 7-8%.
(II) curing speed test:
comparative example 1: the adhesive I and the preparation method thereof comprise the following steps:
the adhesive I comprises a component A and a component B in a mass ratio of 100:150, wherein the component A is an aluminum dihydrogen phosphate solution; the component B comprises the following raw materials in parts by mass:
the aluminum dihydrogen phosphate solution in the component A is prepared by reacting 100 parts by mass of 85% phosphoric acid solution with 30 parts by mass of aluminum hydroxide.
The preparation method of the adhesive I comprises the following steps:
the method comprises the following steps: weighing the following raw materials in parts by mass:
100 parts of 85% phosphoric acid solution, 30 parts of aluminum hydroxide solid powder, 70 parts of aluminum oxide, 4 parts of calcium fluoride, 4 parts of titanium carbide, 2 parts of zirconium oxide and 2 parts of silicon carbide chopped fibers;
step two: preparing a component A:
slowly adding 30 parts of aluminum hydroxide solid powder into 100 parts of 85% phosphoric acid solution by mass, and stirring for 1h at the stirring speed of 90rmp at 94 ℃ to prepare aluminum dihydrogen phosphate solution;
step three: preparing a component B:
adding 70 parts of alumina, 4 parts of calcium fluoride, 4 parts of titanium carbide, 2 parts of zirconia and 2 parts of silicon carbide chopped fibers into a stirrer for stirring, taking out the component B after stirring for 1 hour, manually crushing some blocks, pouring into the stirrer for stirring, and repeating the steps for three times to uniformly mix all the raw materials in the component B;
step four: preparing an adhesive I:
adding the component A and the component B into a mortar according to the mass ratio of 100:150, uniformly mixing and grinding, and standing for 5-10 min, wherein the adhesive is free of solid particles and obvious interfaces, so that the adhesive I is prepared.
The room temperature fast curing high temperature resistant adhesive and adhesive I prepared in example 3 were used to bond C/SiC, C/C and high temperature resistant alloy materials, and the shear strength of the adhesive at different curing times was tested, with the results shown in Table 1:
table 1:
as can be seen from the comparison of the shear strength of the adhesives in the table 1, in the process of preparing the room-temperature fast-curing high-temperature-resistant adhesive, the curing speed is improved by using magnesium oxide and iron oxide modified aluminum dihydrogen phosphate, and the adhesive provided by the invention is fast cured under the room-temperature condition under the combined action of the magnesium oxide and the iron oxide modified aluminum dihydrogen phosphate and the curing accelerator aluminum nitride, wherein the maximum value of the shear strength can be up to 50% after 1 hour of curing, and the adhesive can be nearly completely cured after 24 hours at room temperature; the adhesive I provided by the comparative example 1 is relatively slow in curing speed because no curing accelerator aluminum nitride is added, the maximum shear strength can be achieved only after 5 to 7 days of curing at room temperature, and the maximum shear strength is far smaller than that of the adhesive in the example 3 after 48 hours of curing, which shows that the curing speed of the phosphate adhesive can be improved by the adhesive prepared in the example 3.
(III) high temperature resistance test:
comparative example 2: the adhesive II and the preparation method thereof are as follows:
the adhesive II comprises a component A and a component B in a mass ratio of 100:150, wherein the component A is a magnesium oxide and iron oxide modified aluminum dihydrogen phosphate solution; the component B comprises the following raw materials in parts by mass:
the modified aluminum dihydrogen phosphate solution in the component A is prepared by reacting 100 parts by mass of 85% phosphoric acid solution with 30 parts by mass of aluminum hydroxide to obtain an aluminum dihydrogen phosphate solution, and modifying the aluminum dihydrogen phosphate solution by using 4 parts by mass of magnesium oxide and 4 parts by mass of iron oxide.
The preparation method of the adhesive II comprises the following steps:
the method comprises the following steps: weighing the following raw materials in parts by mass:
100 parts of 85% phosphoric acid solution, 30 parts of aluminum hydroxide solid powder, 4 parts of magnesium oxide, 4 parts of ferric oxide, 70 parts of aluminum oxide, 10 parts of aluminum nitride, 4 parts of calcium fluoride and 2 parts of silicon carbide chopped fibers;
step two: preparing a component A:
slowly adding 30 parts of aluminum hydroxide solid powder into 100 parts of 85% phosphoric acid solution by mass, stirring for 1h at the stirring speed of 90rmp at 94 ℃, adding 4 parts of magnesium oxide and 4 parts of iron oxide, and keeping the temperature at 94 ℃ and continuously stirring for 1.5h to prepare modified aluminum dihydrogen phosphate solution;
step three: preparing a component B:
adding 70 parts of alumina, 10 parts of aluminum nitride, 4 parts of calcium fluoride and 2 parts of silicon carbide chopped fibers into a stirrer, stirring for 1 hour, taking out the component B, manually crushing some blocks, pouring the blocks into the stirrer, stirring, and repeating the steps for three times to uniformly mix the raw materials in the component B;
step four: preparing an adhesive II:
and adding the component A and the component B into a mortar according to the mass ratio of 100:150, uniformly mixing and grinding, and standing for 5-10 min, wherein the adhesive has no solid particles and no obvious interface, so as to obtain the adhesive II.
The room temperature fast curing high temperature resistant adhesive and the adhesive II prepared in the example 3 are used for bonding C/SiC, C/C and high temperature resistant alloy materials, the adhesive bonding performance of the adhesives at different temperatures is tested, the test result at the temperature of more than 1000 ℃ is the room temperature test result after the temperature is kept for 30min, and the rest are the online test results, and the results are shown in the table 2:
table 2:
as can be seen from the comparison of the data in table 2, the adhesive of the present invention has the advantages that titanium carbide, zirconium oxide or yttrium oxide as the high temperature resistant filler is added, and the fillers play a role of supporting the framework under the high temperature condition, and in addition, the addition of the fillers can make the structure of the cured product more compact, so that the adhesive can still maintain a certain bonding strength under the high temperature condition of 1600 ℃; and the adhesive II does not contain high-temperature-resistant filler, the structure of a cured product is not compact enough, and a supporting structure is lacked at high temperature, so that the bonding force is reduced more severely at the temperature of more than 1000 ℃.
(IV) testing the water resistance:
comparative example 3: adhesive III and preparation method thereof
The adhesive III comprises a component A and a component B in a mass ratio of 100:150, wherein the component A is a magnesium oxide and iron oxide modified aluminum dihydrogen phosphate solution; the component B comprises the following raw materials in parts by mass:
the modified aluminum dihydrogen phosphate solution in the component A is prepared by reacting 100 parts by mass of 85% phosphoric acid solution with 30 parts by mass of aluminum hydroxide to obtain an aluminum dihydrogen phosphate solution, and modifying the aluminum dihydrogen phosphate solution by using 4 parts by mass of magnesium oxide and 4 parts by mass of iron oxide.
The preparation method of the room-temperature fast-curing high-temperature-resistant adhesive comprises the following steps:
the method comprises the following steps: weighing the following raw materials in parts by mass:
100 parts of 85% phosphoric acid solution, 30 parts of aluminum hydroxide solid powder, 4 parts of magnesium oxide, 4 parts of ferric oxide, 70 parts of aluminum oxide, 10 parts of aluminum nitride, 4 parts of titanium carbide, 2 parts of zirconium oxide and 2 parts of silicon carbide chopped fibers;
step two: preparing a component A:
slowly adding 30 parts of aluminum hydroxide solid powder into 100 parts of 85% phosphoric acid solution by mass, stirring for 1h at the stirring speed of 90rmp at 94 ℃, adding 4 parts of magnesium oxide and 4 parts of iron oxide, and keeping the temperature at 94 ℃ and continuously stirring for 1.5h to prepare modified aluminum dihydrogen phosphate solution;
step three: preparing a component B:
adding 70 parts of alumina, 10 parts of aluminum nitride, 4 parts of titanium carbide, 2 parts of zirconia and 2 parts of silicon carbide chopped fibers into a stirrer for stirring, taking out the component B after stirring for 1 hour, manually crushing some blocks, pouring into the stirrer for stirring, and repeating the steps for three times to uniformly mix all the raw materials in the component B;
step four: preparing an adhesive III:
and adding the component A and the component B into a mortar according to the mass ratio of 100:150, uniformly mixing and grinding, and standing for 5-10 min, wherein the adhesive is free of solid particles and obvious interfaces, so that the adhesive III is prepared.
The room temperature fast curing high temperature resistant adhesive and adhesive II prepared in example 3 were used to bond C/SiC, C/C and high temperature resistant alloy materials, the bonded test piece was immersed in tap water at room temperature, and the shear strength of the adhesive at the immersion time was measured, the results are shown in Table 3:
table 3:
the data comparison in the table 3 shows that the shear strength of the adhesive disclosed by the invention is only reduced by 8-10% when the adhesive is soaked in tap water for 30 days, and the shear strength of the adhesive III is reduced by more than 60% when the adhesive is soaked in tap water for 30 days, which indicates that the calcium fluoride is added into an adhesive system, and can act synergistically with a curing agent, so that the structure of a cured product is more compact by reducing the porosity of the cured product, and the mechanical property and the water resistance of the cured product of the adhesive are improved.
Claims (4)
1. The high-temperature-resistant adhesive capable of being rapidly cured at room temperature is characterized by comprising a component A and a component B in a mass ratio of 100:150, wherein the component A is a magnesium oxide and iron oxide modified aluminum dihydrogen phosphate solution; the component B comprises the following raw materials in parts by mass:
the curing temperature of the adhesive is 21-25 ℃, and the curing time is 24 hours; the modified aluminum dihydrogen phosphate solution is prepared by reacting 100 parts by mass of 85% phosphoric acid solution with 30 parts by mass of aluminum hydroxide to obtain an aluminum dihydrogen phosphate solution, and modifying the aluminum dihydrogen phosphate solution by using 4 parts by mass of magnesium oxide and 4 parts by mass of iron oxide.
2. A preparation method of a high-temperature-resistant adhesive capable of being rapidly cured at room temperature is characterized by comprising the following steps:
the method comprises the following steps: weighing the following raw materials in parts by mass:
100 parts of 85% phosphoric acid solution, 30 parts of aluminum hydroxide solid powder, 4 parts of magnesium oxide, 4 parts of ferric oxide, 70 parts of aluminum oxide, 10 parts of aluminum nitride, 4 parts of calcium fluoride, 4 parts of titanium carbide, 2 parts of zirconium oxide and 2 parts of silicon carbide chopped fibers;
step two: preparing a component A:
slowly adding 30 parts of aluminum hydroxide solid powder into 100 parts of 85 mass percent phosphoric acid solution, stirring for a certain time at a certain reaction temperature, adding 4 parts of magnesium oxide and 4 parts of iron oxide, keeping the original reaction temperature, and continuously stirring for a certain time to obtain a modified aluminum dihydrogen phosphate solution;
step three: preparing a component B:
adding 70 parts of alumina, 10 parts of aluminum nitride, 4 parts of calcium fluoride, 4 parts of titanium carbide, 2 parts of zirconia and 2 parts of silicon carbide chopped fibers into a stirrer, and uniformly stirring;
step four: preparing a room-temperature fast-curing high-temperature-resistant adhesive:
and adding the component A and the component B into a mortar according to the mass ratio of 100:150, and uniformly mixing and grinding to obtain the room-temperature fast-curing high-temperature-resistant adhesive.
3. The method for preparing the room-temperature fast curing high-temperature-resistant adhesive according to claim 2, wherein the reaction temperature in the second step is 90-100 ℃, and the stirring speed is 80-100 rpm.
4. The method for preparing the room temperature fast curing high temperature resistant adhesive according to claim 2 or 3, wherein the reaction time of the phosphoric acid solution and the aluminum hydroxide solid powder in the second step is 1 hour, and the reaction time after adding the magnesium oxide and the iron oxide is 1.5 hours.
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| CN109456073A (en) * | 2018-12-24 | 2019-03-12 | 宁波虔东科浩光电科技有限公司 | A kind of patching material in burner hearth gap and the method for repairing burner hearth gap with it |
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| CN101358111B (en) * | 2008-08-27 | 2011-09-21 | 黑龙江省科学院石油化学研究院 | Phosphates adhesive and preparation method thereof |
| CN101724352B (en) * | 2009-12-11 | 2012-09-05 | 北京培尔茂森科技推广有限责任公司 | Inorganic adhesive for artificial board and preparation method thereof |
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