CN112029474B - Organic silicon sealing adhesive capable of resisting temperature of 500 ℃ and preparation and use methods thereof - Google Patents

Organic silicon sealing adhesive capable of resisting temperature of 500 ℃ and preparation and use methods thereof Download PDF

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Publication number
CN112029474B
CN112029474B CN202010986037.1A CN202010986037A CN112029474B CN 112029474 B CN112029474 B CN 112029474B CN 202010986037 A CN202010986037 A CN 202010986037A CN 112029474 B CN112029474 B CN 112029474B
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sealing
ethyl silicate
organic silicon
epoxy
hydrolyzed
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CN112029474A (en
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王杰
徐琪
刘翔
邢彬
张丽娜
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AECC Shenyang Liming Aero Engine Co Ltd
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AECC Shenyang Liming Aero Engine Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • C09J183/06Polysiloxanes containing silicon bound to oxygen-containing groups
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/02Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving pretreatment of the surfaces to be joined

Abstract

The invention relates to an organic silicon sealing adhesive capable of resisting temperature of 500 ℃ and a preparation method and a use method thereof, wherein the sealing adhesive comprises epoxy organic silicon resin, hydrolyzed ethyl silicate-40, a filler, a pigment and a diluent in a mass ratio. During preparation, after the hydrolyzed ethyl silicate 40 is prepared and the epoxy organic silicon resin is thickened, the pigment is added into the hydrolyzed ethyl silicate to form B1 mixed liquid; adding hydrolyzed ethyl silicate 40 to form B2 mixed liquid; the filler is dissolved in the X-7 epoxy paint diluent to form B3 mixed liquid; and mixing the mixed solution B2 and B3, and oscillating to form the organic silicon sealing glue. When the sealing glue is used, after the surface to be bonded is wiped and dried, the viscosity of the sealing glue is adjusted and then the sealing glue is uniformly coated, and then parts are combined and assembled after being solidified. The sealing compound prepared by the method completely meets the sealing design requirements of relevant parts of the engine by performing examination tests on the appearance, dryness, heat resistance, sealing property, corrosivity, sealing effect of typical parts of the engine and the like of the material.

Description

Organic silicon sealing adhesive capable of resisting temperature of 500 ℃ and preparation and use methods thereof
The technical field is as follows:
the invention belongs to the technical field, particularly relates to sealing glue, and particularly relates to organic silicon sealing glue capable of resisting temperature of 500 ℃ as well as a preparation method and a use method thereof.
Background art:
the sealing compound related to the invention mainly aims at the special purpose of the engine, is a necessary material for engine overhaul, and is an imported material: the existing technical standard is not available, and the storage period is short, so that certain difficulty is brought to purchasing, and the production requirement cannot be guaranteed; in an aircraft engine, gaps always exist between the joint surfaces of parts of the aircraft engine, in order to ensure the normal operation of the engine and maintain the normal operating pressure and safety of a system, the joint surfaces must be sealed to prevent oil leakage, gas leakage, water leakage and the like, and a sealant is mainly used for parts with small sealing gaps, such as the joint surfaces of an installation edge of an engine combustion chamber casing and an installation edge in a high-pressure turbine guider (including an adjusting ring), the joint surfaces of a high-pressure guide inner ring and a swirler (including a sealing element), the joint surfaces of a heat exchanger shell and a heat exchange element, the joint surfaces of a shell and a joint of a pneumatic actuator cylinder, a fuel leakage valve (a shell, a gasket and a valve) of an adjustable nozzle, a thermocouple, a nozzle, a pressure sensor and other parts which are assembled in a general way; in the prior art, the imported sealant is adopted, so that the imported material needs time in ordering, production and customs, and the production progress and military requirements are influenced to different degrees by factors such as temperature difference and uncontrollable property; and the colloid belongs to fluid, and has hidden danger in the transportation process.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, provides the organic silicon sealing adhesive capable of resisting the temperature of 500 ℃ and the preparation and use methods thereof, aims at special purposes of an engine, solves the urgent need of production, meets the sealing performance design requirement of the engine, replaces import, and realizes the localization of materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
an organic silicon sealing adhesive capable of resisting temperature of 500 ℃ comprises epoxy organic silicon resin, ethyl silicate hydrate-40, filler, pigment and diluent in a mass ratio; the mass proportion relation of the components is that the epoxy organic silicon resin: hydrolysis of ethyl silicate: filling: pigment: diluent ═ (60-69): (7-11): (6.5-7.7): (10-16): (5-6.4).
The epoxy organic silicon resin is a component one of an epoxy organic silicon heat-resistant paint H61-1 for aviation, and the adopted technical standard is GJB 1590.
The hydrolyzed ethyl silicate is silicon-40.
The filler is talcum powder and gas-phase white carbon black, and the mass ratio of the talcum powder to the gas-phase white carbon black is (6.0-6.8): (0.5-0.9), the technical standard adopted by the talcum powder is GB/T15342, and the technical standard adopted by the fumed silica is Q/SHG.102.101.
The pigment is a component III of epoxy organosilicon heat-resistant paint H61-1, and the adopted technical standard is GJB 1590.
The diluent is epoxy paint diluent with the brand number of X-7, and the adopted technical standard is Q/12DT 0129.
Step 1, preparing materials
Preparing epoxy organic silicon resin, hydrolyzed ethyl silicate, a filler, a pigment and a diluent according to a mass ratio;
step 2, preparation of Ethyl silicate hydrolysate 40
(1) According to the volume ratio, ethyl silicate-40: alcohol hydrolysis: hydrochloric acid ═ (95-105): (65-75): (0.7-1.1), preparing materials;
(2) the ethyl silicate-40 is divided into ethyl silicate-40A and ethyl silicate-40B, and the volume ratio of the ethyl silicate to the ethyl silicate-40A is as follows: ethyl silicate-40B ═ 1.8-2.2: 1, the concentration percentage of the hydrolyzed alcohol is 89% -93%, the hydrolyzed alcohol is divided into a hydrolyzed alcohol A and a hydrolyzed alcohol B, and the volume ratio of the hydrolyzed alcohol A to the hydrolyzed alcohol B is as follows: hydrolyzed alcohol B ═ (0.8-1.2): (0.8-1.2);
(3) mixing ethyl silicate-40A and hydrolysis alcohol A to form a solution a, mixing hydrochloric acid and hydrolysis alcohol B, dissolving the mixture in ethyl silicate-40B to form a solution B, and uniformly mixing the solution a and the solution B to obtain hydrolysis ethyl silicate 40;
step 3, preparing a B2 mixed liquid:
taking epoxy silicone resin, thickening, and adding pigment into the thickened epoxy silicone resin to form B1 mixed liquid; adding hydrolyzed ethyl silicate 40 into B1 to form B2 mixed liquid;
step 4, preparing a B3 mixed liquid:
and (3) taking the filler, and dissolving the filler in the X-7 epoxy paint diluent to form B3 mixed liquid.
Step 5, preparing organic silicon sealing glue:
and mixing the mixed solution B2 with the mixed solution B3, and then uniformly shaking to form uniform silver fluid, namely the organic silicon sealing glue.
In the step 2(1), the technical standard adopted by the ethyl silicate-40 is HB 5345; the standard used for concentrated hydrochloric acid is GB/T622.
In the step 2(1), the concentration of the hydrolyzed alcohol is 91%, and the hydrolyzed alcohol is prepared by adding distilled water into absolute ethyl alcohol.
In the step 3, the thickening treatment process comprises the following steps: and (3) placing the epoxy organic silicon resin into a glass beaker, slowly evaporating at 90-95 ℃ in a water bath kettle to reduce the volume of the original paint by 1/4-2/5, completing thickening, and placing in a sealed container for later use.
In the step 4, the talc powder in the filler is dissolved in X-7 epoxy paint diluent together with fumed silica after being calcined and screened, and the specific calcining and screening process is as follows: calcining the talcum powder at 300 +/-10 ℃ for 3-5 h, sieving the calcined talcum powder through a 320-mesh standard sieve with the aperture of 0.045mm, keeping the talcum powder at the part under the sieve in a sealed container, finishing calcining and sieving, and storing for later use.
In the step 5, the oscillation time is 10-15 min.
In the step 5, the prepared organic silicon sealing adhesive is subjected to a heat resistance test, and after being heated for 48 hours at the high temperature of 500 +/-10 ℃, the adhesive does not fall off and has no cracks through detection.
In the step 5, the prepared organic silicon sealing compound is subjected to a sealing test, the sealing test is carried out according to the standard HB5388, the sealing test is carried out at 500 +/-10 ℃ for 48 hours, the sealing test is carried out after 1.2MPA is pressed and kept for 3 minutes, the pressure drop is not more than 0.2MPa, and the pressure drop is not more than 0.1MPa through detection.
In the step 5, after the prepared organosilicon sealing adhesive is adhered to the part, a sealing performance test is carried out, 0.5MPA is kept for 7.5min, the pressure drop is not more than 0.15MPA, and the pressure drop is not more than 0.1MPa after the test.
In the step 5, the prepared organic silicon sealing glue is free from corrosion through a corrosion experiment.
In the step 5, the prepared organic silicon sealing glue is uniform silver viscous fluid.
The use method of the organic silicon sealing glue comprises the following steps:
(1) removing oil on the surface to be bonded by a wiping method by using a cloth block soaked with acetone, and drying in the air at room temperature for 10-15 min;
(2) adjusting the viscosity of the sealing glue to be 15-50 seconds (coating-4 viscometer) by adopting X-7 epoxy paint thinner according to the requirement of the coating thickness of the part coating part on the sealing glue;
(3) coating a layer of well-stirred sealing glue on the bonding surface in advance, and not coating glue on the peripheries of the gasket and the flange plate with the width of 3 mm;
(4) after the sealing glue is coated (redundant sealing glue is removed from the surface by a cloth block wiping method), keeping for 10-30 min, and combining parts;
(5) before the parts are assembled, curing operation is carried out, wherein the curing mode adopts one of the following two modes, (one) curing is carried out for 5-6 hours at 18-30 ℃; and (II) curing for 1.5-2 h at 150-200 ℃.
In the step (5), the curing mode is selected according to the size of the workpiece and specific working conditions, when the joint surface of the installation side of a large part (due to the large assembly and the fitting piece which cannot be heated) is cured at 18-30 ℃, and when the part is small and single (does not need to be assembled), the part can be heated and cured, and good sealing performance can be obtained.
In the step (5), if the sealing compound is cured at the temperature of 18-30 ℃, other work can be performed on the part in the curing process, but fuel oil, lubricating oil and the like cannot fall on the connecting part.
The invention has the beneficial effects that:
the organic silicon sealing adhesive capable of resisting the temperature of 500 ℃ prepared by the invention has excellent heat resistance and sealing performance, does not corrode metal base materials, and is used for sealing joints of engines at the temperature of 500 ℃ in air medium; aiming at the special application of the engine, the sealing ring is used in an air medium at the temperature of 0-500 ℃ and the pressure of 1.2MPa, and plays a role in sealing.
The invention is used for the combination surface (comprising an adjusting ring) of the rear mounting edge of the casing of a combustion chamber of an engine and the inner mounting edge of a high-pressure turbine guider and the combination surface (comprising a sealing element) of a high-pressure guide inner ring and a swirler; the combined surface of the heat exchanger shell and the heat exchange element, the combined surface of the shell and the joint of the pneumatic actuating cylinder, an oil leakage valve (shell, gasket and valve) of the adjustable nozzle, a thermocouple, a nozzle, a pressure sensor and the joint of the mixer shell, and the like. The application condition is good, the process is feasible, the quality is reliable, the sealing glue can replace the imported sealing glue, the urgent need of production is met, the situation of being restricted by people is eliminated, and a large amount of foreign exchange is saved.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to examples.
In the following examples, ethyl silicate-40 was used with the technical standard HB 5345; the standard adopted by concentrated hydrochloric acid is GB/T622; the concentration of the hydrolyzed alcohol is 91 percent, and the hydrolyzed alcohol is prepared by adding distilled water into absolute ethyl alcohol.
The thickening treatment process comprises the following steps: and (3) placing the epoxy organic silicon resin into a glass beaker, slowly evaporating at 90-95 ℃ in a water bath kettle to reduce the volume of the original paint by 1/4-1/3, completing thickening, and placing in a sealed container for later use.
The use method of the organic silicon sealing glue prepared in the following examples comprises the following steps:
(1) removing oil on the surface to be bonded by a wiping method by using a cloth block soaked with acetone, and drying in the air at room temperature for 10-15 min;
(2) coating a 4 viscometer according to the requirement of the coating thickness of the sealing glue on the coating part of the part, and adjusting the viscosity of the sealing glue to be 15-50 seconds by adopting an X-7 epoxy paint diluent;
(3) coating a layer of well-stirred sealing glue on the connecting surface in advance, and not coating glue on the peripheries of the gasket and the flange plate with the width of 3 mm;
(4) after the sealing glue is coated (redundant sealing glue is removed from the surface by a cloth block wiping method), keeping for 10-30 min, and combining parts;
(5) before the parts are assembled, curing operation is carried out, the curing mode is selected according to the size and the specific working condition of a workpiece, when a joint surface of a mounting side of a large part (a fitting part which cannot be heated due to the large assembly) is cured for 5-6h at 18-30 ℃, and when the part is a small and single part (which does not need to be combined), the part can be heated and cured, and good sealing performance can be obtained.
The prepared silicone sealing compound was subjected to a sealing test using the standard of reference HB 5388. The sealing performance is 500 ℃, after the heat resistance is kept for 48 hours, the pressure is increased by 1.2MPA and kept for 3min, and the pressure drop condition is judged according to the display data of a pressure gauge.
After the organic silicon sealing glue is used for part installation, the sealing performance is checked, the sealing performance is kept for 7.5min at 0.5MPA, and a pressure gauge displays data and judges the pressure drop condition.
Example 1:
(1) preparing hydrolyzed ethyl silicate silicon-40
Weighing 66ml of ethyl silicate-40 and 35ml of hydrolysis alcohol, and mixing; then measuring 0.92ml of hydrochloric acid, dissolving in the remaining 35ml of hydrolysis alcohol, and simultaneously adding into the remaining 34ml of ethyl silicate-40; and mixing the two mixed solutions together, and uniformly stirring to obtain the hydrolyzed ethyl silicate 40.
(2) Preparing organic silicon sealing glue
After preparing the hydrolyzed ethyl silicate silicon 40, taking 100g as an example, respectively weighing:
the epoxy organosilicon heat-resistant paint H61-1 comprises the following components: 64.5g
Hydrolysis of ethyl silicate silicon-40: 9g of
Talc powder: 6.4g
White carbon black by a gas phase method: 0.7g
Epoxy organosilicon heat-resistant paint H61-1 comprises the following three components: 13g
Epoxy paint diluent X-7: 6g of a mixture;
(3) thickening the epoxy organosilicon heat-resistant paint H61-1 component I, adding the thickened epoxy organosilicon heat-resistant paint H61-1 component III, and adding hydrolyzed ethyl silicate 40 to form a B2 mixed liquid;
(4) after calcining and screening, talcum powder and fumed silica are dissolved in X-7 epoxy paint diluent to form B3 mixed liquid;
(5) and mixing the mixed solution B2 with the mixed solution B3, and then shaking for 10-15 min to be uniform to form uniform silver fluid, namely the organic silicon sealing glue.
The prepared organic silicon sealing compound is subjected to a heat resistance test, a sealing property test after parts are adhered, and a corrosion test, and specific results are shown in the following table 1.
TABLE 1 test results for silicone sealants
Figure BDA0002689249380000051
Example 2
(1) Preparing hydrolyzed ethyl silicate silicon-40
Weighing 66ml of ethyl silicate-40 and 35ml of hydrolysis alcohol, and mixing; then measuring 0.92ml of hydrochloric acid, dissolving in the remaining 35ml of hydrolysis alcohol, and simultaneously adding into the remaining 34ml of ethyl silicate-40; and mixing the two mixed solutions together, and uniformly stirring to obtain the hydrolyzed ethyl silicate 40.
(2) Preparing organic silicon sealing glue
After preparing the hydrolyzed ethyl silicate silicon-40, taking 100g as an example, respectively weighing:
the epoxy organosilicon heat-resistant paint H61-1 comprises the following components: 69g
Hydrolysis of ethyl silicate silicon-40: 11g
Talc powder: 6.8g
White carbon black by a gas phase method: 0.9g
Epoxy organosilicon heat-resistant paint H61-1 comprises the following three components: 16g
Epoxy paint diluent X-7: 6.4g
And (3) preparing the organic silicon sealing compound in the same way as in the example 1 in the steps (3) to (5).
The prepared organic silicon sealing compound is subjected to a heat resistance test, a sealing property test after parts are adhered, and a corrosion test, and specific results are shown in the following table 2, wherein the sealing property test and the sealing test after the parts are adhered are both 0.1 MPa.
TABLE 2 test results for silicone sealants
Figure BDA0002689249380000061
Example 3
(1) Preparing hydrolyzed ethyl silicate silicon-40
Weighing 66ml of ethyl silicate-40 and 35ml of hydrolysis alcohol, and mixing; then measuring 0.92ml of hydrochloric acid, dissolving in the remaining 35ml of hydrolysis alcohol, and simultaneously adding into the remaining 34ml of ethyl silicate-40; and mixing the two mixed solutions together, and uniformly stirring to obtain the hydrolyzed ethyl silicate 40.
(2) Preparing organic silicon sealing glue
After preparing the hydrolyzed ethyl silicate silicon-40, taking 100g as an example, respectively weighing:
the epoxy organosilicon heat-resistant paint H61-1 comprises the following components: 60g of
Hydrolysis of ethyl silicate silicon-40: 7g of
Talc powder: 6.0g
White carbon black by a gas phase method: 0.5g
Epoxy organosilicon heat-resistant paint H61-1 comprises the following three components: 10g
Epoxy paint diluent X-7: 5g
And (3) preparing the organic silicon sealing compound in the same way as in the example 1 in the steps (3) to (5).
The prepared organic silicon sealing compound is subjected to a heat resistance test, a sealing property test after parts are adhered, and a corrosion test, and specific results are shown in the following table 3, wherein the sealing property test and the sealing test after the parts are adhered are both 0.1 MPa.
TABLE 3 test results for silicone sealants
Figure BDA0002689249380000071
Comparative example 1, the same as example 1, except that:
taking a first component W61-31 (the technical standard is Q/12DT0283-2010) of the aluminum powder organosilicon heat-resistant paint and a first component W8932-31 (the technical standard is HG/T3362-2003) of the aluminum powder organosilicon heat-resistant paint, and mixing the two components according to the mass ratio of 1:1 to form a first mixed component which is used for equivalently replacing a first component H61-1 of the epoxy organosilicon heat-resistant paint in the embodiment 1;
taking an aluminum powder organosilicon heat-resistant paint W61-31 (the technical standard is Q/12DT0283-2010) component II and an aluminum powder organosilicon heat-resistant paint (the technical standard is HG/T3362-2003) component II, mixing the two components according to the mass ratio of 1:1 to form a mixed component II, and equivalently replacing an epoxy organosilicon heat-resistant paint H61-1 component III in the example 1;
the prepared organic silica gel does not pass the heat resistance and sealing performance detection.
Comparative example 2, like example 1, differs in that:
taking a component I of the aluminum powder organic silicon heat-resistant paint (the technical standard is HG/T3362-2003) to replace a component I of the epoxy organic silicon heat-resistant paint H61-1 in the example 1 in an equal amount;
taking a second component equivalent of aluminum powder organosilicon heat-resistant paint (the technical standard is HG/T3362-2003) to replace a third component H61-1 of the epoxy organosilicon heat-resistant paint in example 1;
the prepared organic silica gel does not pass the heat resistance and sealing performance detection.

Claims (4)

1. A preparation method of organic silicon sealing glue capable of resisting temperature of 500 ℃ is characterized in that the sealing glue is used for sealing an engine and comprises the following components, by mass, epoxy organic silicon resin, ethyl silicate hydrate-40, a filler, a pigment and a diluent; the mass proportion relation of the components is that the epoxy organic silicon resin: hydrolysis of ethyl silicate-40: filling: pigment: diluent = (60-69): (7-11): (6.5-7.7): (10-16): (5-6.4); the epoxy organic silicon resin is a component I of an epoxy organic silicon heat-resistant paint H61-1 for aviation, the filler is talcum powder and gas-phase white carbon black, and the mass ratio of the talcum powder to the gas-phase white carbon black is (6.0-6.8): (0.5-0.9), wherein the pigment is a component III of epoxy organosilicon heat-resistant paint H61-1, the diluent is epoxy paint diluent, and the brand is X-7;
the method comprises the following steps:
step 1, preparing materials
Preparing epoxy organic silicon resin, hydrolyzed ethyl silicate, a filler, a pigment and a diluent according to a mass ratio;
step 2, preparation of hydrolyzed ethyl silicate-40
(1) According to the volume ratio, ethyl silicate-40: alcohol hydrolysis: hydrochloric acid = (95-105): (65-75): (0.7-1.1), preparing materials;
(2) the ethyl silicate-40 is divided into ethyl silicate-40A and ethyl silicate-40B, and the volume ratio of the ethyl silicate to the ethyl silicate-40A is as follows: ethyl silicate-40B = (1.8-2.2): 1, the hydrolyzed alcohol is divided into a hydrolyzed alcohol A and a hydrolyzed alcohol B, and the volume ratio of the hydrolyzed alcohol A to the hydrolyzed alcohol B is as follows: hydrolyzed alcohol B = (0.8-1.2): (0.8-1.2);
(3) mixing ethyl silicate-40A and hydrolysis alcohol A to form a solution a, mixing hydrochloric acid and hydrolysis alcohol B, dissolving the mixture in ethyl silicate-40B to form a solution B, and uniformly mixing the solution a and the solution B to obtain hydrolysis ethyl silicate-40;
step 3, preparing a B2 mixed liquid:
taking epoxy silicone resin, thickening, adding pigment into the thickened epoxy silicone resin to form a B1 mixed solution, and adding hydrolyzed ethyl silicate-40 into B1 to form a B2 mixed liquid;
step 4, preparing a B3 mixed liquid:
dissolving a filler in an X-7 epoxy paint diluent to form a B3 mixed liquid;
step 5, preparing organic silicon sealing glue:
mixing the mixed solution B2 with the mixed solution B3, vibrating uniformly to form uniform silver fluid, namely the organic silicon sealing adhesive, performing a heat resistance test on the prepared organic silicon sealing adhesive, and detecting that the adhesive does not fall off and has no cracks after being heated for 48 hours in a high-temperature environment of 500 +/-10 ℃; performing a sealing test, heating at 500 + -10 deg.C for 48h, pressing 1.2MPA, and keeping for 3min, and detecting to reduce pressure drop to 0.1MPa or below; after the prepared organosilicon sealing glue is adhered to the part, the sealing performance test is carried out, 0.5MPA is kept for 7.5min, and the pressure drop is less than or equal to 0.1MPa through detection; the prepared organic silicon sealing adhesive has no corrosion through corrosion experiments.
2. The method for preparing the silicone sealing compound resistant to the temperature of 500 ℃ according to claim 1, wherein in the step 2(1), the concentration of the hydrolyzed alcohol is 89% -93%.
3. The method for preparing the silicone sealing compound resistant to the temperature of 500 ℃ according to claim 1, wherein in the step 3, the thickening treatment process comprises: and (3) placing the epoxy organic silicon resin into a glass beaker, slowly evaporating at 90-95 ℃ in a water bath kettle to reduce the volume of the original paint by 1/4-2/5, completing thickening, and placing in a sealed container for later use.
4. The method for using the silicone sealing compound prepared by the method according to claim 1, comprising the following steps:
(1) removing oil on the surface to be bonded by a wiping method by using a cloth block soaked with acetone, and drying in the air at room temperature for 10-15 min;
(2) adjusting the viscosity of the sealing glue to be 15-50 seconds by adopting X-7 epoxy paint thinner according to the requirement of the coating thickness of the part coating part on the sealing glue;
(3) uniformly coating a layer of stirred sealing glue on the bonding surface in advance;
(4) after the sealing glue is coated, keeping for 10-30 min, and combining parts;
(5) before the parts are assembled, curing operation is carried out, and one of the following two curing modes is selected according to the actual conditions of the parts, wherein the curing mode is that (one) curing is carried out for 5-6h at 18-30 ℃; and (II) curing for 1.5-2 h at 150-200 ℃.
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3562124A (en) * 1968-08-02 1971-02-09 Hooker Chemical Corp Composition for corrosion protection
CN1654583A (en) * 2005-01-19 2005-08-17 山东大学 Multifunctional ablation-resistant adhesive for thermal protection and method for preparing same
CN101440268A (en) * 2008-12-30 2009-05-27 黑龙江省科学院石油化学研究院 Low temperature curing high temperature resistant inorganic / organic hybridization epoxy adhesive and preparation thereof
CN102277090A (en) * 2011-06-20 2011-12-14 山东大学 High-temperature inorganic composite adhesive and preparation method thereof
CN103421464A (en) * 2013-08-23 2013-12-04 中国人民解放军第五七一九工厂 Anti-vibration adhesive resistant to high and low temperature
CN104031601A (en) * 2014-05-28 2014-09-10 浙江大学 Insulative adhesive for preparing metallic and soft magnetic composite material and using method thereof
CN105753333A (en) * 2016-01-25 2016-07-13 山东中信能源联合装备股份有限公司 Reflection reducing film on basis of silica sol for glass for heat collecting cover tubes and method for preparing reflection reducing film

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3562124A (en) * 1968-08-02 1971-02-09 Hooker Chemical Corp Composition for corrosion protection
CN1654583A (en) * 2005-01-19 2005-08-17 山东大学 Multifunctional ablation-resistant adhesive for thermal protection and method for preparing same
CN101440268A (en) * 2008-12-30 2009-05-27 黑龙江省科学院石油化学研究院 Low temperature curing high temperature resistant inorganic / organic hybridization epoxy adhesive and preparation thereof
CN102277090A (en) * 2011-06-20 2011-12-14 山东大学 High-temperature inorganic composite adhesive and preparation method thereof
CN103421464A (en) * 2013-08-23 2013-12-04 中国人民解放军第五七一九工厂 Anti-vibration adhesive resistant to high and low temperature
CN104031601A (en) * 2014-05-28 2014-09-10 浙江大学 Insulative adhesive for preparing metallic and soft magnetic composite material and using method thereof
CN105753333A (en) * 2016-01-25 2016-07-13 山东中信能源联合装备股份有限公司 Reflection reducing film on basis of silica sol for glass for heat collecting cover tubes and method for preparing reflection reducing film

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
GJB 1590-1993 H61-1航空用环氧有机硅耐热漆规范;国防科学技术工业委员会;《中华人民共和国国家军用标准》;19930308;全文 *

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