CN112852363B - High-strength low-temperature-resistant adhesive and preparation method and application thereof - Google Patents
High-strength low-temperature-resistant adhesive and preparation method and application thereof Download PDFInfo
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- CN112852363B CN112852363B CN202110037434.9A CN202110037434A CN112852363B CN 112852363 B CN112852363 B CN 112852363B CN 202110037434 A CN202110037434 A CN 202110037434A CN 112852363 B CN112852363 B CN 112852363B
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/36—Hydroxylated esters of higher fatty acids
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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
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention provides a high-strength low-temperature-resistant adhesive, and a preparation method and application thereof, wherein the adhesive is a castor oil/polyurethane amine novel epoxy curing adhesive, the amine value of the epoxy curing adhesive is 200-300 mgKOH/g, the functionality is 7-13, the functionality is high, and the viscosity is high. The high-strength low-temperature-resistant adhesive provided by the invention has good bonding strength, high and low temperature resistance, performance of enduring large-scale rapid temperature change and impact resistance; wherein the bonding strength is more than 2MPa and can reach 12MPa; can bear low temperature below minus 30 ℃, can bear low temperature of minus 120 ℃, and can not be embrittled, separated and shrunk under ultralow temperature; the adhesive layer is not damaged when the temperature is changed between 120 ℃ below zero and 110 ℃; the retention rate of the bonding strength after high-frequency impact is more than 75%, can reach 97%, has excellent performance, and can bear high load and high-frequency vibration impact of rocket lifting and recovery for 5 times.
Description
Technical Field
The invention belongs to the technical field of aerospace materials, and particularly relates to a high-strength low-temperature-resistant adhesive as well as a preparation method and application thereof.
Background
The adhesive for aerospace is used for products such as carrier rockets, satellites and spacecrafts, and due to the special launching environment and space orbit environment, the rockets, the satellites and the spacecrafts need to bear the tests of ultralow temperature, ultrahigh temperature, high vacuum, ultraviolet rays and the like, so the adhesive for the aerospace field needs to have the characteristics of excellent high and low temperature resistance, high bonding strength and high bonding strength retention rate after high-frequency impact resistance. The aerospace adhesive in the prior art is a high-temperature-resistant epoxy resin adhesive which takes epoxy resin, a curing agent and an accelerant as raw materials, but in the using process, sand blasting treatment is needed on the surface of aerospace equipment, and the bonding strength is not ideal. In the prior art, low-temperature resistant adhesives prepared from polyurethane and epoxy resin are also used as raw materials, but the technical problem of low impact strength is solved.
Disclosure of Invention
In order to solve the technical problems, the invention provides the adhesive which has high bonding strength, does not need surface sand blasting in the using process, is resistant to high and low temperatures, can resist large-range temperature change and is impact-resistant.
The invention aims to provide a high-strength low-temperature-resistant adhesive.
The invention also aims to provide a preparation method of the high-strength low-temperature-resistant adhesive.
The invention further aims to provide application of the adhesive.
The high-strength low-temperature-resistant adhesive comprises 100-120 parts by weight of a component A and 80-100 parts by weight of a component B,
the component A is epoxy resin;
the component B is prepared from the following raw materials in parts by weight:
90-110 parts of castor oil, namely,
145-170 parts of polyisocyanate,
0.2 to 0.4 portion of defoaming agent,
0.1 to 0.3 portion of wetting agent,
350-450 parts of water.
The defoaming agent adopted by the invention is a defoaming agent without organic silicon, and the main components of the defoaming agent are defoaming polyacrylate and polymer solution, and the defoaming agent does not contain organic silicon.
The defoaming agent and the wetting agent adopted by the invention are both sold in the market, wherein the model of the defoaming agent is BYK-051N, and the model of the wetting agent is BYK-306. The defoaming agent adopted by the invention has good compatibility and does not generate shrinkage cavity; the wetting agent adopted by the invention can well wet the substrate and prevent shrinkage cavity.
The invention provides a high-strength low-temperature-resistant adhesive which is prepared from castor oil, polyisocyanate, water, a defoaming agent and a wetting agent as raw materials to obtain a component B, wherein the component B is mixed with component A epoxy resin to obtain a novel epoxy curing adhesive, namely castor oil/polyurethane amine, wherein the amine value is 200-300 mgKOH/g, and the functionality is 7-13. The adhesive provided by the invention has high bonding strength which is more than 2MPa and can reach 12MPa; the low temperature resistance is good, the low temperature of below-30 ℃ can be resisted, and the ultra-low temperature is not embrittled, separated or shrunk; the adhesive has good performance of tolerating large-amplitude rapid temperature change, changes at-120-110 ℃, and the adhesive layer is not damaged; the shock resistance is good, and the high-load and high-frequency shock impact of 5 times of rocket launching and rocket recovery can be borne.
Preferably, the component B is prepared from the following raw materials in parts by weight:
100 parts of castor oil, namely 100 parts of castor oil,
167.5 parts of polyisocyanate,
0.3 part of a defoaming agent,
0.2 part of wetting agent is added,
and 400 parts of water.
Preferably, the A component is epoxy E-44. The epoxy resin E-44 adopted by the invention has proper viscosity and epoxy content, is low in viscosity, does not need to add a solvent, can realize 100 percent of solid content, avoids the swelling corrosion of the solvent to an adhered heat-insulating layer, has the epoxy value of 0.44mol/100g, is high in polymerization degree, good in glue line toughness and keeps adhesion reliability in a high-impact working environment.
Preferably, the polyisocyanate is polymethylene polyphenyl isocyanate having an-NCO content of 25 to 40wt%. The polyisocyanate used in the invention is a mixture of isocyanate and diphenylmethane diisocyanate, wherein the-NCO content is 25-40 wt%. Polyisocyanates can undergo addition reactions with castor oil for the preparation of intermediates. The polyisocyanate adopted by the invention is a mixture of 3-6 functionality isocyanate, has the characteristics of large molecular weight and high functionality, can react with water to obtain high molecular weight and high functionality organic amine, and can ensure high curing speed and high bonding strength, thereby ensuring the stability of a bonding layer.
The invention provides a preparation method of the high-strength low-temperature-resistant adhesive, which comprises the following steps:
(1) Taking castor oil and polyisocyanate, uniformly mixing at room temperature, heating to 70-80 ℃, reacting for 3-5 h, cooling to 45-55 ℃, and performing heat preservation and aging for 8-12h to obtain an intermediate product A;
preferably, the mixing time of the castor oil and the polyisocyanate is 45 to 75min.
In the preparation method of the adhesive, in the step (1), firstly, castor oil and polyisocyanate are fully mixed, and then, the castor oil contains hydroxyl and the polyisocyanate to carry out addition reaction;
the reaction is as follows:
R—(NCO)n+R’—OH→R’—O—CO—NH—R—(NCO)n
the invention can make the reaction product more uniform after aging.
(2) Weighing water, heating to 80-90 ℃, dropwise adding the intermediate product A obtained in the step (1) into water, reacting at 35-95 ℃ for 5-20 h, vacuumizing until the vacuum degree reaches-0.08 MPa, heating to 110-115 ℃, removing water, adjusting the vacuum degree to be more than 0.098MPa, keeping the temperature at 110-115 ℃ for 1.5-2.5 h, and dehydrating again to obtain an intermediate product B; in the step, the product obtained in the step (1) reacts with a large amount of water and excessive water is removed, so that an intermediate product B-organic amine is obtained. In the step, firstly, water is weighed, the water content is far greater than that of the intermediate product A, so that the intermediate product A is prevented from self-polymerization, and then the mixture is heated to 35-95 ℃ for heat preservation reaction for 5-20 hours, so that the water and the intermediate product A are ensured to have sufficient addition reaction; then vacuumizing until the vacuum degree reaches-0.08 MPa, gradually heating to 110-115 ℃, and removing water to realize a large amount of rough water removal; finally, the vacuum degree is adjusted to be more than 0.098MPa, and the temperature is kept at 110-115 ℃ for 1.5-2.5 h, so that fine dehydration is realized in a small amount, and the purity of the intermediate product B is ensured.
R’—O—CO—NH—R—(NCO)n+H2O (excess)
→R’—O—CO—NH—R—(NH2)m
Preferably, the dropping rate of the intermediate product A is 3-5 kg/min. The invention adopts the dropping speed to ensure that the intermediate product A is contacted with a large amount of water, thereby avoiding the self-polymerization of the intermediate product A and reducing the generation of byproducts.
Preferably, the water content of the intermediate product B is below 0.1%.
(3) Adding a defoaming agent and a wetting agent into the intermediate product B, uniformly mixing, and reacting for 1.5-2.5 h at the temperature of 80-90 ℃ to obtain the component B; according to the invention, the castor oil modified organic amine mixture is obtained through the reaction in the step.
(4) And uniformly mixing the component A and the component B to obtain the adhesive.
Preferably, the amine value of the adhesive is 200-300 mgKOH/g, and the functionality is 7-13.
According to the preparation method of the adhesive, firstly, castor oil and polyisocyanate are subjected to a crosslinking reaction to obtain an intermediate product A, then the intermediate product A is dripped into warm water for further reaction and vacuum dehydration to obtain an intermediate product B-organic amine, a defoaming agent and a wetting agent are added into the intermediate product B to obtain a component B-castor oil modified organic amine mixture, and the component B and the component A are mixed to obtain the adhesive with excellent performance for aerospace. The novel epoxy curing adhesive obtained by the preparation method provided by the invention, namely the castor oil/polyurethane amine, has an amine value of 200-300 mgKOH/g and a functionality of 7-13, and has high functionality and high viscosity, so that the high curing speed and the high bonding strength are ensured.
The adhesive obtained by the method provided by the invention has high bonding strength which is more than 2MPa and can reach 12MPa; the low temperature resistance is good, the low temperature of below-30 ℃ can be resisted, and the low temperature is not embrittled, separated and shrunk; the adhesive has good performance of enduring large-amplitude rapid temperature change, changes at-120 to 110 ℃, and the adhesive layer is not damaged; the shock resistance is good, and the high-load and high-frequency shock impact of 5 times of rocket launching and rocket recovery can be borne.
The high-strength low-temperature-resistant adhesive provided by the invention can be applied to a rocket storage tank and is used for bonding a metal layer and a heat-insulating layer of the rocket storage tank. The adhesive provided by the invention has good high and low temperature resistance, good performance of resisting large-amplitude rapid temperature change and good impact resistance, and can adapt to the running environment of rocket launching.
The beneficial effects of the invention are as follows:
1. the high-strength low-temperature-resistant adhesive provided by the invention is a novel castor oil/polyurethane amine epoxy curing adhesive, the amine value of the epoxy curing adhesive is 200-300 mgKOH/g, the functionality is 7-13, the functionality is high, the viscosity is high, and the curing speed and the bonding strength of the adhesive are ensured.
2. The high-strength low-temperature-resistant adhesive provided by the invention has good bonding strength, high and low temperature resistance, performance of enduring large-scale rapid temperature change and impact resistance. Wherein the bonding strength is more than 2MPa and can reach 12MPa; the paint can resist low temperature below minus 30 ℃, can resist low temperature of minus 120 ℃, and can not be embrittled, separated and shrunk at low temperature; the adhesive layer is not damaged when the temperature is changed between 120 ℃ below zero and 110 ℃; the retention rate of the bonding strength after high-frequency impact is more than 75%, and can reach 97%.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
The raw material castor oil in the following examples of the present invention is commercially available industrial refined castor oil; the polyisocyanate is available from Wanhua chemistry and has the model number of PM-200; the defoaming agent is commercially available and is BYK-051N in model number; the wetting agent is commercially available in a model of BYK-306 and the epoxy resin in a model of E-44.
Embodiments 1 to 10 of the present invention provide a high-strength low-temperature-resistant adhesive, which comprises a component A and a component B,
the component A is epoxy resin;
the component B is prepared from the following raw materials in parts by weight:
the reaction mixture of castor oil and water is,
a polyisocyanate,
a defoaming agent,
a wetting agent, a surfactant,
and (3) water. Wherein the specific weight compositions of the raw materials of examples 1 to 5 are shown in Table 1. The specific weight compositions of the starting materials for examples 6-10 are shown in Table 2.
The preparation method of the adhesive comprises the following steps:
(1) Adding castor oil and polyisocyanate into a reaction kettle F1, mixing for 45-75min at room temperature, gradually heating the reaction kettle F1 to 70-80 ℃, reacting for 3-5 h, cooling to 45-55 ℃, preserving heat and aging for 8-12h to obtain an intermediate product A;
(2) Weighing water and adding the water into a reaction kettle F2, gradually heating the reaction kettle F2 to 35-95 ℃, dropwise adding the intermediate product A obtained in the step (1), wherein the dropwise adding speed is 3-5 kg/min, carrying out heat preservation reaction at 35-95 ℃ for 5-20 h, vacuumizing the reaction kettle F2 until the vacuum degree reaches-0.08 MPa, gradually heating to 110-115 ℃, removing the water, adjusting the vacuum degree to be more than 0.098MPa, and carrying out heat preservation at 110-115 ℃ for 1.5-2.5 h to obtain an intermediate product B; the water content of the intermediate product B is below 0.1%;
(3) Adding a defoaming agent and a wetting agent into the reaction kettle F2, uniformly mixing the defoaming agent and the wetting agent with the intermediate product B, controlling the temperature of the reaction kettle F2 to be 80-90 ℃, and reacting for 1.5-2.5 hours to obtain the component B;
(4) And uniformly mixing the component A and the component B according to a ratio to obtain the adhesive.
TABLE 1 raw Material compositions of examples 1 to 5
TABLE 2 raw material compositions of examples 6 to 10
The preparation method of the adhesive of the embodiments 1 to 5 is the same, and comprises the following steps:
(1) Adding castor oil and polyisocyanate into a reaction kettle F1, mixing for 1h at room temperature, gradually heating the reaction kettle F1 to 70-80 ℃, reacting for 4h, cooling to 50 ℃, and preserving heat and aging for 10h to obtain an intermediate product A;
(2) Weighing water and adding the water into a reaction kettle F2, gradually heating the reaction kettle F2 to 35-95 ℃, dropwise adding the intermediate product A obtained in the step (1), wherein the dropwise adding speed is 4kg/min, carrying out heat preservation reaction at 35-95 ℃ for 20 hours, vacuumizing the reaction kettle F2 until the vacuum degree reaches-0.08 MPa, gradually heating to 110-115 ℃, removing the water, adjusting the vacuum degree to be more than 0.098MPa, carrying out heat preservation at 110-115 ℃ for 2 hours, and dehydrating again to obtain an intermediate product B; the water content of the intermediate product B is below 0.1%;
(3) Adding a defoaming agent and a wetting agent into the reaction kettle F2, uniformly mixing the defoaming agent and the wetting agent with the intermediate product B, controlling the temperature of the reaction kettle F2 to be 80-90 ℃, and reacting for 2 hours to obtain the component B;
(4) And uniformly mixing the component A and the component B according to a ratio to obtain the adhesive.
The preparation method of the adhesives of the embodiments 6 to 8 is the same, and comprises the following steps:
(1) Adding castor oil and polyisocyanate into a reaction kettle F1, mixing for 45 hours at room temperature, gradually heating the reaction kettle F1 to 70-75 ℃, reacting for 5 hours, cooling to 45 ℃, and preserving heat and aging for 12 hours to obtain an intermediate product A;
(2) Weighing water, adding the water into a reaction kettle F2, gradually heating the reaction kettle F2 to 35-40 ℃, dropwise adding the intermediate product A obtained in the step (1), wherein the dropwise adding speed is 3kg/min, keeping the temperature at 35-40 ℃ for reaction for 20 hours, vacuumizing the reaction kettle F2 until the vacuum degree reaches-0.08 MPa, gradually heating to 110-115 ℃, removing the water, adjusting the vacuum degree to be more than 0.098MPa, keeping the temperature at 110-115 ℃ for 1.5 hours, and dehydrating again to obtain an intermediate product B; the water content of the intermediate product B is below 0.1 percent;
(3) Adding a defoaming agent and a wetting agent into the reaction kettle F2, uniformly mixing with the intermediate product B, controlling the temperature of the reaction kettle F2 at 80-85 ℃, and reacting for 1.5h to obtain the component B;
(4) And uniformly mixing the component A and the component B according to a ratio to obtain the adhesive.
The preparation method of the adhesive of the embodiments 9 to 10 is the same, and comprises the following steps:
(1) Adding castor oil and polyisocyanate into a reaction kettle F1, mixing for 75 hours at room temperature, gradually heating the reaction kettle F1 to 75-80 ℃, reacting for 3 hours, cooling to 55 ℃, preserving heat and aging for 8 hours to obtain an intermediate product A;
(2) Weighing water and adding the water into a reaction kettle F2, gradually heating the reaction kettle F2 to 90-95 ℃, dropwise adding the intermediate product A obtained in the step (1), wherein the dropwise adding speed is 5kg/min, keeping the temperature at 90-95 ℃ for 5h for reaction, vacuumizing the reaction kettle F2 until the vacuum degree reaches-0.08 MPa, heating to 110-115 ℃, removing the water, adjusting the vacuum degree to be more than 0.098MPa, keeping the temperature at 110-115 ℃ for 2.5h, and dehydrating again to obtain an intermediate product B; the water content of the intermediate product B is below 0.1%;
(3) Adding a defoaming agent and a wetting agent into the reaction kettle F2, uniformly mixing with the intermediate product B, controlling the temperature of the reaction kettle F2 at 85-90 ℃, and reacting for 1.5h to obtain the component B;
(4) And uniformly mixing the component A and the component B according to a ratio to obtain the adhesive.
The adhesive provided by the invention is used as an adhesive for a metal layer/a heat-insulating layer of a rocket tank, and in the application process, the operation time is less than 2h, and the actual drying time is more than 48 h.
The adhesive of comparative example 1 was prepared in the same manner as in examples 9 to 10.
Test examples
1. The viscosity of the intermediate product A obtained in step (1) of examples 1 to 10 and comparative example 1, the viscosity of the intermediate product B obtained in step (2) and the appearance, amine number and functionality of the adhesive finally obtained were measured and the results are shown in Table 3.
TABLE 3 test results
The results in table 3 show that, in the preparation process of the high-strength low-temperature-resistant adhesive provided by the invention, the viscosity of the obtained intermediate product a is about 2700mpa.s, the viscosity of the intermediate product B is about 3200mpa.s, and the viscosity is high, so that the excellent adhesive property of the finally obtained adhesive is ensured. The adhesive obtained by the invention is light yellow liquid, has an amine value of 200-300 mgKOH/g, an average functionality of 7-13, high functionality and high viscosity, and ensures good curing performance and bonding performance. In contrast, in comparative example 1, the weight ratio of the raw materials is out of the range of the present invention, because the viscosity of the intermediate product A is low, the viscosity of the obtained intermediate product B is low, the adhesive property is poor, and the adhesive property is poor.
2. The adhesives obtained in examples 1 to 10 and comparative example 1 were subjected to a performance test. The bonding strength test is carried out according to GB1742-1979 & lt & gt adhesive strength measurement method & gt, the low temperature resistance test is carried out according to GB/T2423.1-2001 & lt & gt environmental test for electrical and electronic products, the high temperature resistance test is carried out according to GB/T2423.2-2001 & lt & gt environmental test for electrical and electronic products, and the impact resistance test is carried out according to GB/T1843-2008 & lt & gt measurement method & gt impact strength of plastic cantilever beams, and the results are shown in Table 4.
Table 4 results of performance testing
The results in table 4 show that the adhesive provided by the invention has an adhesive strength of more than 2MPa, can reach 12MPa, and has excellent adhesive performance; the low-temperature resistance is excellent, wherein the low-temperature resistance is below minus 30 ℃ and can reach minus 120 ℃, and the adhesive layer is not embrittled, separated and shrunk at ultralow temperature; the high temperature resistance temperature is above 110 ℃; the retention rate of the bonding strength after high-frequency impact is more than 75%, and can reach 97%; the adhesive provided by the comparative example 1 has the adhesive strength of 0.5MPa and low adhesive strength; the low temperature resistance is-20 ℃, and the low temperature resistance is far inferior to that of the adhesives of examples 1-10; the high temperature resistance is only 90 ℃; the retention of the bond strength after high frequency impact was 50%. The high-strength low-temperature-resistant adhesive provided by the invention has excellent bonding strength, high-low temperature resistance and impact resistance, can adapt to the launching and running environment of a rocket, can bear high-load and high-frequency vibration impact of lifting off and recycling the rocket for 5 times, and has excellent performance and strong application performance.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (8)
1. The high-strength low-temperature-resistant adhesive is characterized by comprising 100 to 120 parts by weight of a component A and 80 to 100 parts by weight of a component B,
the component A is epoxy resin;
the component B is prepared from the following raw materials in parts by weight:
90 to 110 portions of castor oil, namely,
145 to 170 parts of polyisocyanate,
0.2 to 0.4 portion of defoaming agent,
0.1 to 0.3 portion of wetting agent,
350-450 parts of water;
the polyisocyanate is polymethylene polyphenyl isocyanate, wherein the-NCO content is 25 to 40wt%, and the polyisocyanate is a mixture of 3-6 functionality isocyanate;
the preparation method of the adhesive comprises the following steps:
(1) Uniformly mixing castor oil and polyisocyanate at room temperature, heating to 70-80 ℃, reacting for 3-5 h, cooling to 45-55 ℃, preserving heat and aging for 8-12h to obtain an intermediate product A, wherein the castor oil contains hydroxyl and the polyisocyanate for addition reaction;
(2) Weighing water, heating to 80-90 ℃, dropwise adding the intermediate product A obtained in the step (1) into water, carrying out heat preservation reaction at 35-95 ℃ for 5-20h, vacuumizing until the vacuum degree reaches-0.08 MPa, heating to 110-115 ℃, removing the water, adjusting the vacuum degree to be more than 0.098MPa, carrying out heat preservation at 110-115 ℃ for 1.5-2.5h, and dehydrating again to obtain an intermediate product B;
(3) Adding a defoaming agent and a wetting agent into the intermediate product B, uniformly mixing, and reacting for 1.5 to 2.5 hours at the temperature of 80 to 90 ℃ to obtain the component B;
(4) And uniformly mixing the component A and the component B according to a ratio to obtain the adhesive.
2. The high-strength low-temperature-resistant adhesive according to claim 1, wherein the component B is prepared from the following raw materials in parts by weight:
100 parts of castor oil, namely 100 parts of castor oil,
167.5 parts of polyisocyanate,
0.3 part of defoaming agent, 0.3 part of,
0.2 part of wetting agent is added,
and 400 parts of water.
3. The high strength, low temperature resistant adhesive of claim 1 or 2, wherein the A component is epoxy E-44.
4. The high strength low temperature resistant adhesive according to claim 1, wherein in the step (1), the mixing time of the castor oil and the polyisocyanate is 45-75min.
5. The high-strength low-temperature-resistant adhesive according to claim 4, wherein in the step (2), the dropping rate of the intermediate product A is 3 to 5kg/min.
6. The high-strength low-temperature-resistant adhesive according to claim 1, wherein in the step (2), the water content of the intermediate product B is less than or equal to 0.1%.
7. The high-strength low-temperature-resistant adhesive according to claim 1, wherein in the step (4), the amine value of the adhesive is 200 to 300mgKOH/g, and the functionality is 7 to 13.
8. Use of the high-strength low-temperature-resistant adhesive according to any one of claims 1 to 7 in a rocket tank.
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| EP1741734A1 (en) * | 2005-07-05 | 2007-01-10 | Sika Technology AG | Heat curable epoxy resin composition having low temperature impact strength comprising solid epoxy resins |
| US8076395B2 (en) * | 2009-09-11 | 2011-12-13 | Air Products And Chemicals, Inc. | Low temperature curable epoxy compositions containing urea curatives |
| CN103387648B (en) * | 2013-07-12 | 2015-07-15 | 浙江华宝油墨有限公司 | Preparation method and applications of hydrophilically modified polyisocyanate curing agent for waterborne polyurethane |
| CN105419714B (en) * | 2014-09-09 | 2018-04-27 | 贵阳时代沃顿科技有限公司 | A kind of epoxy resin dual-component polyurethane adhesive and preparation method thereof |
| CN105885754B (en) * | 2016-05-03 | 2019-10-11 | 上海大学 | Low form fire retarding epoxide resin adhesive and preparation method thereof |
| CN110272705B (en) * | 2019-05-20 | 2021-10-26 | 烟台大学 | Bi-component aqueous adhesive for automotive interior and preparation method thereof |
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