CN114644891A - Preparation method and application of ethyl silicate high-temperature strain adhesive - Google Patents
Preparation method and application of ethyl silicate high-temperature strain adhesive Download PDFInfo
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- CN114644891A CN114644891A CN202210332723.6A CN202210332723A CN114644891A CN 114644891 A CN114644891 A CN 114644891A CN 202210332723 A CN202210332723 A CN 202210332723A CN 114644891 A CN114644891 A CN 114644891A
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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
- 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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
- C09J5/02—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving pretreatment of the surfaces to be joined
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
- C09J5/06—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving heating of the applied adhesive
Abstract
A preparation method and application of ethyl silicate high-temperature strain adhesive belong to the field of strain adhesive. Adding ethyl silicate and ethanol into a glass flask, stirring and mixing to form ethyl silicate-ethanol solution, standing at room temperature, dripping a catalyst solution into the ethyl silicate-ethanol solution, dripping the catalyst and fully stirring to obtain partially hydrolyzed ethyl silicate hydrolysate, checking whether the hydrolysate is colorless and transparent, and measuring SiO of the hydrolysate2Content, viscosity, density index; transferring the obtained hydrolyzed solution into clean and dry glass container, sealing, storing for a certain period, adding hardener, stirring to transparent colorless, adding filler, stirringAnd uniformly stirring and sealing to obtain the ethyl silicate high-temperature strain adhesive. The ethyl silicate high-temperature strain adhesive disclosed by the invention has the advantages of high tolerance temperature, small brittleness, greenness, environmental friendliness, no toxicity, no peculiar smell and high bonding strength, and can firmly adhere a strain gauge to resist the high temperature below 1000 ℃.
Description
Technical Field
The invention belongs to the field of strain adhesives, and particularly relates to an ethyl silicate high-temperature strain adhesive capable of firmly adhering a strain gauge and resisting a high temperature below 1000 ℃, and a preparation method and an application method thereof.
Background
The strain adhesive is an adhesive with special mechanical properties, and not only can firmly adhere the strain gauge, but also can accurately transfer strain. In recent years, as the requirement of high-temperature test of strain gauges develops, the high-temperature resistance of strain gauges is also challenged greatly. The high-temperature resistant strain adhesive commonly used at present mainly comprises organic silicon resin strain adhesive and phosphate strain adhesive. Although the organic silicon resin strain adhesive has high bonding strength and good toughness, the maximum service temperature is generally 400 ℃, and the strain test at higher temperature cannot be met. For example, chinese invention patent CN108148539A discloses a medium-temperature-cured high-temperature-resistant wave-transmitting adhesive which is prepared from epoxy modified silicone resin, mica powder and the like as raw materials and can resist the high temperature of 450 ℃. Phosphate strain adhesives, although able to withstand higher temperatures, have the problem of being brittle and lacking in bond strength (chemical bonding, 2017,39(01): 18).
Disclosure of Invention
The invention provides ethyl silicate high-temperature strain adhesive and a preparation method and application thereof.
A preparation method of ethyl silicate high-temperature strain adhesive comprises the following raw materials in parts by weight:
ethyl silicate: 100 portions of
Ethanol: 10-15 parts of
Catalyst: 8 to 13 portions of
Hardening agent: 50-70 parts of
Filling: 90-110 parts.
The preparation process comprises the following steps: adding ethyl silicate and ethanol into a glass flask according to the parts by weight, fully stirring to mix the ethyl silicate and the ethanol to form ethyl silicate-ethanol solution, and standing at room temperature for 80-100 min; dropwise adding the catalyst solution into the ethyl silicate-ethanol solution while stirring, wherein the rotating speed is 500-600 r/min; dripping catalyst and stirring to obtain partially hydrolyzed ethyl silicate hydrolysate, checking whether the hydrolysate is colorless and transparent, and measuring SiO of the hydrolysate2Content, viscosity, density index. Transferring the prepared hydrolyzed ethyl silicate solution into a clean and dry glass container, sealing, storing for 12-16 days at 20-25 ℃, adding a hardening agent in parts by weight, stirring until the mixture is transparent and colorless, and storing for 5-7 days at not less than 22 ℃ in a sealing way; and adding the filler according to the weight part, uniformly stirring, sealing, standing at 21-23 ℃ for 20-40min, uncovering, stirring for a plurality of times, immediately sealing, and uniformly stirring to obtain the ethyl silicate high-temperature strain adhesive.
Further, the ethyl silicate is a main raw material for preparing the high-temperature strain adhesive, wherein SiO is2The content is 28-40%. The ethanol is a cosolvent, the purity is analytically pure, and the ethanol has the function of promoting the ethyl silicate raw material and the catalyst aqueous solution to be fully mutually soluble.
Further, the catalyst is a hydrochloric acid-boric acid mixed aqueous solution or a sulfuric acid-boric acid mixed aqueous solution or a nitric acid-boric acid mixed aqueous solution, and is used for stably controlling the hydrolysis speed of the ethyl silicate, and improving the binding power and the binding strength of the prepared high-temperature strain adhesive at high temperature, so that the high-temperature strain adhesive can endure the high temperature of 700-1000 ℃ and keep good binding strength. According to the invention, a hydrochloric acid-boric acid mixed aqueous solution, a sulfuric acid-boric acid mixed aqueous solution or a nitric acid-boric acid mixed aqueous solution is used as a catalyst for hydrolysis reaction of ethyl silicate, and when the catalyst is the hydrochloric acid-boric acid mixed aqueous solution, the mass ratio of hydrochloric acid (mass fraction is 36%), boric acid (analytically pure) and water is 1:0.7: 16. When the catalyst is a sulfuric acid-boric acid mixed aqueous solution, the mass ratio of sulfuric acid (mass fraction is 98%), boric acid (analytically pure) and water is 1:1.5: 32. When the catalyst is a nitric acid-boric acid mixed aqueous solution, the mass ratio of nitric acid (mass fraction is 68%), boric acid (analytically pure) and water is 1:0.8: 18. The catalyst can stably prepare partially hydrolyzed ethyl silicate hydrolysate.
Furthermore, the hardening agent is ethyl cellosolve and is used for adjusting the hardness of the prepared high-temperature strain adhesive, so that the high-temperature strain adhesive can still maintain good hardness at the high-temperature stage of 700-1000 ℃.
Further, the filler is mixed corundum, is obtained by mixing corundum particles with the particle size of M7 and corundum particles with the particle size of M40 according to the mass ratio of 1:1, and is used for mixing with partially hydrolyzed ethyl silicate hydrolysate to prepare the ethyl silicate high-temperature strain adhesive.
Further, the prepared partially hydrolyzed ethyl silicate hydrolysate is characterized in that: the appearance is colorless and transparent; SiO 22The content is 23-25%; at 20 ℃, the viscosity is 2.0-3.0 cSt, and the density is 0.92-0.94 g/cm3。
The application of the ethyl silicate high-temperature strain adhesive is characterized in that the ethyl silicate high-temperature strain adhesive is used for adhering a strain gauge on a metal base material, and comprises the following steps:
step 1: surface treatment: and (3) pretreating the surface of the metal base material to be adhered to increase the surface roughness of the base material and remove impurities such as oil stains, dust and the like on the surface to obtain the surface-treated metal base material.
Step 2: pasting a strain gauge: firstly, uniformly coating a layer of high-temperature strain adhesive on a metal base material after surface treatment to serve as an insulating layer, and carrying out air drying and ammonia drying treatment on the insulating layer. And after the ammonia gas is fully volatilized, uniformly coating a second layer of high-temperature strain adhesive, flatly paving the strain gauge and the lead thereof on the second layer of high-temperature strain adhesive, compressing and fixing, continuously and uniformly coating a layer of high-temperature strain adhesive on the strain gauge and the lead thereof, and carrying out air drying and ammonia drying treatment on the strain gauge and the lead thereof.
And step 3: strengthening: after the ammonia drying is finished for 30 minutes, a layer of partially hydrolyzed ethyl silicate hydrolysate added with a small amount of water is uniformly coated, and after several minutes, the mixture is air-dried and ammonia-dried.
And 4, step 4: and (3) high-temperature curing, namely after the ammonia gas is fully volatilized, putting the materials into a heating furnace for heating and curing, firstly heating to 75-85 ℃, preserving the heat for 0.5-1.5 hours, then heating to 250-280 ℃, preserving the heat for 25-35 minutes, and finally heating to 340-360 ℃, preserving the heat for 25-35 minutes. If the adhered strain gauge needs to be tested or worked at a high temperature of over 700 ℃, the heating temperature of the last step is increased to 700 ℃ and kept for 13-17 minutes. And after the heat preservation is finished, opening the heating furnace to cool the material, and finishing the solidification to obtain the metal base material adhered with the strain gauge.
Has the advantages that:
compared with organic silicon resin strain adhesives and phosphate strain adhesives, the ethyl silicate high-temperature strain adhesive has the advantages of high temperature resistance, small brittleness and high bonding strength, can firmly adhere a strain gauge to resist the high temperature below 1000 ℃, and is suitable for adhering the strain gauge on chromium-nickel, titanium alloy and other high-temperature steel substrates to develop high-temperature vibration stress tests. The ethyl silicate high-temperature strain adhesive also has the beneficial effects of environmental protection, no toxicity and no peculiar smell.
Detailed Description
The present invention is described in detail below with reference to specific examples:
example 1
The mass portion ratio is as follows:
ethyl silicate: 100
Ethanol: 12
Catalyst: 11
Hardening agent: 60
Filling: 100
The preparation method comprises the following steps:
mixing SiO2100 parts of ethyl silicate having a content of 28% and 12 parts of analytically pure ethanol are dissolved in a glass flask and stirred well. 0.6 part of concentrated hydrochloric acid with the mass fraction of 36 percent and 0.4 part of boric acid with analytical purity are mixed and dissolved in 10 parts of water and fully stirred to prepare 11 parts of hydrochloric acid-boric acid mixed aqueous solution catalyst. And (3) dropwise adding the 11 parts of the catalyst aqueous solution into a mixed solution of ethyl silicate and ethanol, and performing stable hydrolysis on the ethyl silicate, wherein the stirring is performed while dropwise adding, and the rotating speed is 500-600 r/min, so as to prepare a partially hydrolyzed ethyl silicate hydrolysate. And adding 60 parts of ethyl cellosolve hardener into the prepared partially hydrolyzed ethyl silicate hydrolysate, stirring to fully mix the ethyl cellosolve hardener and the partially hydrolyzed ethyl silicate hydrolysate, adding 100 parts of mixed corundum filler, fully stirring, sealing and storing to obtain the ethyl silicate high-temperature strain adhesive.
The application method comprises the following steps:
step 1: surface treatment: al having a diameter of 130 μm is used2O3Base material to be bonded (e.g. chrome-nickel, titanium alloy)) The sand blasting treatment was performed, and then the surface of the substrate was wiped with an alcohol cotton ball. The prepared ethyl silicate high-temperature strain adhesive is dipped by an organic glass rod, and a layer (an insulating layer) is coated on the surface of the base material. And naturally drying the insulating layer for 12-15 hours at the temperature of not less than 22 ℃.
Step 2: pasting a strain gauge: firstly, uniformly coating a layer of high-temperature strain adhesive on a metal base material after surface treatment to serve as an insulating layer, and carrying out air drying and ammonia drying treatment on the insulating layer. And after the ammonia gas is fully volatilized, uniformly coating a second layer of high-temperature strain adhesive, flatly paving the strain gauge and the lead thereof on the second layer of high-temperature strain adhesive, compressing and fixing, continuously and uniformly coating a layer of high-temperature strain adhesive on the strain gauge and the lead thereof, and carrying out air drying and ammonia drying treatment on the strain gauge and the lead thereof.
And step 3: strengthening: after the ammonia drying is finished for 30 minutes, a layer of partially hydrolyzed ethyl silicate hydrolysate added with a small amount of water is uniformly coated, and after several minutes, the mixture is air-dried and ammonia-dried.
And 4, step 4: and (3) high-temperature curing, namely after ammonia gas is fully volatilized, putting the materials into a heating furnace for heating and curing, firstly heating to 80 ℃, preserving heat for 1 hour, then heating to 250-280 ℃, preserving heat for 30 minutes, and finally heating to 350 ℃, and preserving heat for 30 minutes. If the adhered strain gauge needs to be tested at a high temperature of 700-1000 ℃, the heating temperature of the last step needs to be raised to 700 ℃ and kept for 15 minutes. And after the heat preservation is finished, opening the heating furnace to cool the material, and finishing the solidification to obtain the metal base material adhered with the strain gauge.
Example 2
The mass portion ratio is as follows:
ethyl silicate: 100
Ethanol: 12
Catalyst: 10
Hardening agent: 60
Filling: 100
The preparation method comprises the following steps:
mixing SiO2100 parts of ethyl silicate having a content of 28% and 12 parts of analytically pure ethanol are dissolved in a glass flask and stirred well. 0.4 part of concentrated sulfuric acid with the mass fraction of 98 percent and 0.6 part of analytically pureThe boric acid was mixed and dissolved in 9 parts of water, and stirred sufficiently to prepare 10 parts of a sulfuric acid-boric acid mixed aqueous solution catalyst. And (3) dropwise adding the 10 parts of catalyst aqueous solution into a mixed solution of ethyl silicate and ethanol, and performing stable hydrolysis on the ethyl silicate, wherein the stirring is performed while dropwise adding, and the rotating speed is 500-600 r/min, so as to prepare a partially hydrolyzed ethyl silicate hydrolysate. And adding 60 parts of ethyl cellosolve hardener into the prepared partially hydrolyzed ethyl silicate hydrolysate, stirring to fully mix the ethyl cellosolve hardener and the partially hydrolyzed ethyl silicate hydrolysate, adding 100 parts of mixed corundum filler, fully stirring, sealing and storing to obtain the ethyl silicate high-temperature strain adhesive.
The application method of the ethyl silicate high-temperature strain adhesive in the embodiment is the same as that in the embodiment 1.
Example 3
The mass portion ratio is as follows:
ethyl silicate: 100
Ethanol: 12
Catalyst: 11
Hardening agent: 60
Filling: 100
The preparation method comprises the following steps:
mixing SiO2100 parts of ethyl silicate having a content of 28% and 12 parts of analytically pure ethanol are dissolved in a glass flask and stirred well. 0.6 part of nitric acid with the mass fraction of 68% and 0.4 part of boric acid with analytical purity are mixed and dissolved in 10 parts of water, and the mixture is fully stirred to prepare 11 parts of nitric acid-boric acid mixed aqueous solution catalyst. And (3) dropwise adding the 11 parts of the catalyst aqueous solution into a mixed solution of ethyl silicate and ethanol, and performing stable hydrolysis on the ethyl silicate, wherein the stirring is performed while dropwise adding, and the rotating speed is 500-600 r/min, so as to prepare a partially hydrolyzed ethyl silicate hydrolysate. And adding 60 parts of ethyl cellosolve hardener into the prepared partially hydrolyzed ethyl silicate hydrolysate, stirring to fully mix the ethyl cellosolve hardener and the partially hydrolyzed ethyl silicate hydrolysate, adding 100 parts of mixed corundum filler, fully stirring, sealing and storing to obtain the ethyl silicate high-temperature strain adhesive.
The application method of the ethyl silicate high-temperature strain adhesive in the embodiment is the same as that in the embodiment 1.
Claims (7)
1. A preparation method of ethyl silicate high-temperature strain adhesive is characterized by comprising the following raw materials in parts by weight:
ethyl silicate: 100 portions of
Ethanol: 10-15 parts of
Catalyst: 8-13 parts of
Hardening agent: 50-70 parts of
Filling: 90-110 parts;
the preparation process comprises the following steps: adding ethyl silicate and ethanol into a glass flask according to the parts by weight, fully stirring to mix the ethyl silicate and the ethanol to form ethyl silicate-ethanol solution, and standing at room temperature for 80-100 min; dropwise adding the catalyst solution into the ethyl silicate-ethanol solution while stirring, wherein the rotating speed is 500-600 r/min; dripping catalyst and stirring to obtain partially hydrolyzed ethyl silicate hydrolysate, checking whether the hydrolysate is colorless and transparent, and measuring SiO of the hydrolysate2Content, viscosity, density index; transferring the prepared hydrolyzed ethyl silicate solution into a clean and dry glass container, sealing, storing for 12-16 days at 20-25 ℃, adding a hardening agent in parts by weight, stirring until the mixture is transparent and colorless, and storing for 5-7 days at not less than 22 ℃ in a sealing way; and adding the filler according to the weight part, uniformly stirring, sealing, standing at 21-23 ℃ for 20-40min, uncovering, stirring for a plurality of times, immediately sealing, and uniformly stirring to obtain the ethyl silicate high-temperature strain adhesive.
2. The method for preparing ethyl silicate high-temperature strain adhesive according to claim 1, wherein SiO in the ethyl silicate2The content is 28 to 40 percent; the ethanol is a cosolvent, and the purity is analytically pure.
3. The method for preparing ethyl silicate high-temperature strain gel according to claim 1, wherein the catalyst is hydrochloric acid-boric acid mixed aqueous solution, sulfuric acid-boric acid mixed aqueous solution or nitric acid-boric acid mixed aqueous solution; when the catalyst is a hydrochloric acid-boric acid mixed aqueous solution, the mass ratio of the hydrochloric acid to the boric acid to the water is 1:0.7: 16; when the catalyst is a sulfuric acid-boric acid mixed aqueous solution, the mass ratio of sulfuric acid to boric acid to water is 1:1.5: 32; when the catalyst is a nitric acid-boric acid mixed aqueous solution, the mass ratio of nitric acid to boric acid to water is 1:0.8: 18.
4. The method for preparing ethyl silicate high-temperature strain adhesive according to claim 1, wherein the filler is mixed corundum Al2O3The corundum particles are obtained by mixing corundum particles with a particle size of M7 and corundum particles with a particle size of M40 in a mass ratio of 1:1.
5. The method for preparing ethyl silicate high temperature strain adhesive according to claim 1, wherein the hardening agent is ethyl cellosolve.
6. The method for preparing ethyl silicate high-temperature strain adhesive according to claim 1, wherein the hydrolyzed solution of partially hydrolyzed ethyl silicate obtained by catalytic hydrolysis of ethyl silicate is colorless and transparent in appearance; SiO 22The content is 23-25%; at 20 ℃, the viscosity is 2.0-3.0 cSt, and the density is 0.92-0.94 g/cm3。
7. The application of the ethyl silicate high-temperature strain adhesive prepared by the method of claim 1, wherein the ethyl silicate high-temperature strain adhesive is used for adhering a strain gauge on a metal substrate, and comprises the following steps:
step 1: surface treatment: and (3) pretreating the surface of the metal base material to be adhered to increase the surface roughness of the base material and remove oil stains and dust impurities on the surface to obtain the surface-treated metal base material.
Step 2: pasting a strain gauge: firstly, uniformly coating a layer of high-temperature strain adhesive on a metal substrate after surface treatment to serve as an insulating layer, and carrying out air drying and ammonia drying treatment on the insulating layer; after the ammonia gas is fully volatilized, uniformly coating a second layer of high-temperature strain adhesive, flatly paving the strain gauge and the lead thereof on the second layer of high-temperature strain adhesive, pressing and fixing, continuously and uniformly coating a layer of high-temperature strain adhesive on the strain gauge and the lead thereof, and carrying out air drying and ammonia drying treatment on the strain gauge and the lead thereof;
and step 3: strengthening: after ammonia drying is finished for 30 minutes, uniformly coating a layer of partially hydrolyzed ethyl silicate hydrolysate added with a small amount of water, and after several minutes, air-drying and ammonia drying the hydrolysate;
and 4, step 4: high-temperature curing, namely after ammonia gas is fully volatilized, putting the materials into a heating furnace for heating and curing, firstly heating to 75-85 ℃, preserving heat for 0.5-1.5 hours, then heating to 250-280 ℃, preserving heat for 25-35 minutes, and finally heating to 360 ℃ of temperature of 340-; if the adhered strain gauge needs to be tested or operated at a high temperature of more than 700 ℃, the heating temperature of the last step needs to be increased to 700 ℃ and the temperature is kept for 13-17 minutes; and after the heat preservation is finished, opening the heating furnace to cool the material, and finishing the solidification to obtain the metal base material adhered with the strain gauge.
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2022
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| GB1292938A (en) * | 1970-09-25 | 1972-10-18 | Anderson Dev Co | Improvements in or relating to compositions containing hydrocarbonether polysilicates |
| CN85100057A (en) * | 1985-04-01 | 1986-07-23 | 清华大学 | High-temperature strain sustainable adhesive |
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| CN109059747A (en) * | 2018-07-04 | 2018-12-21 | 北京科技大学 | A kind of temporary frame work wire grid formula high temperature strain gauge and its manufacture and use method |
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