CN113604180B - Low-temperature-resistant high-thixotropy epoxy daub and preparation method thereof - Google Patents
Low-temperature-resistant high-thixotropy epoxy daub and preparation method thereof Download PDFInfo
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- CN113604180B CN113604180B CN202110922876.1A CN202110922876A CN113604180B CN 113604180 B CN113604180 B CN 113604180B CN 202110922876 A CN202110922876 A CN 202110922876A CN 113604180 B CN113604180 B CN 113604180B
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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
- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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Abstract
A low temperature resistant high thixotropy epoxy daub and a preparation method thereof, belonging to the technical field of energy transportation and storage industrial adhesives; is a bi-component adhesive, which is prepared from the following components in percentage by weight of 1: (0.75-1.25) by mixing the component A and the component B. The component A comprises the following components: 15-50 parts of epoxy resin, 1-10 parts of diluent, 40-75 parts of filler, 0.5-5 parts of thixotropic agent and 0.1-1 part of pigment; the component B comprises: 30-50 parts of amine curing agent, 0.5-5 parts of curing accelerator, 40-65 parts of filler and 0.5-5 parts of diluent; the bi-component epoxy daub prepared by the invention has high viscosity, excellent mechanical property and adhesive property at low temperature, especially at-40 ℃ and-25 ℃, thixotropic index larger than or equal to 1.3 and high thixotropic index. The epoxy daub is applied to transportation and storage devices of clean energy, and comprises a liquefied oil gas ship, a shore tank and bonding of metal materials in a shore station liquid cargo containment system.
Description
Technical Field
The invention relates to the technical field of industrial adhesives for energy transportation and storage, in particular to low-temperature-resistant high-thixotropy epoxy daub and a preparation method and application thereof.
Background
In recent years, due to the increasing awareness of the environment, the application range of liquefied petroleum gas is becoming wider and wider. The number of imports for liquefied oil and gas in China has increased dramatically year by year, and thus there is an increasing demand for means for transporting and storing liquefied oil and gas. In the application process of liquefied oil gas transportation and storage devices including liquefied oil gas ships, shore tanks and pipelines, the device relates to the bonding of an outer plate of a foamed polyurethane thermal insulation plate and a cabin steel plate, and needs epoxy daub to have no sagging on a vertical surface, high thixotropy, bearing capacity, excellent compression creep property and easy mechanical mixing, and further requires the epoxy daub to have good mechanical property and bonding property under the low-temperature condition of (-40 ℃ to-25 ℃) in the ocean transportation process.
The cured epoxy daub is hard and brittle, is more prominent when used at low temperature, and has changed performance due to the slowing of the thermal motion of molecular chains, the reduction of the flexibility of the molecular chains, the reduction of the distance between molecules and the increase of the internal stress between molecules and molecules. In order to maintain good mechanical properties (shear strength and tensile strength) of the epoxy daub at low temperature: 1) The better the low temperature resistance, the lower the glass transition temperature (Tg) of the polymer; 2) The higher the group content of the soft chain segment is, the better the low temperature resistance is; 3) The cross-linking density of the three-dimensional cross-linking network is improved, and the better the mechanical property is. 4) The dosage, compatibility and dispersion uniformity of the nano particles are improved, and the maximization of mechanical and bonding properties is realized;
the innovation points of the invention are as follows:
(1) according to the structure-activity relationship between the structure and the performance of the epoxy daub, the main agent, the curing agent and the variety proportion among the components are reasonably selected, so that the epoxy daub has lower glass transition temperature, is suitable for the proportion of a hard chain segment and a soft chain segment, has high thixotropy, and has better adhesive property and mechanical property at low temperature;
(2) provides a preparation method of low-temperature-resistant high-thixotropy epoxy daub.
Disclosure of Invention
The invention aims to provide low-temperature-resistant high-thixotropy epoxy daub, a preparation method and application. The obtained low-temperature-resistant high-thixotropy epoxy daub has high thixotropy and low-temperature resistance, particularly the high-temperature and low-temperature performance in the temperature range of-40 ℃ and-25 ℃ is basically the same, the mechanical property and the adhesive property of the epoxy daub in the temperature range of-40 ℃ and-25 ℃ are not changed along with the change of the temperature, and the epoxy daub is very stable and can be considered to resist sudden change and gradual change of the temperature. Meanwhile, the cured product does not crack or droop.
In order to achieve the purpose, the invention provides the following technical scheme: the low-temperature-resistant high-thixotropy epoxy daub comprises two components in a weight ratio of 1: (0.75-1.25) mixing the component A and the component B.
The component A is prepared from the following raw materials in parts by weight: 15-50 parts of epoxy resin, 1-10 parts of diluent, 40-75 parts of filler, 0.5-5 parts of thixotropic agent and 0.1-1 part of pigment; preferably 30-45 parts of epoxy resin, 3-8 parts of diluent, 50-65 parts of filler, 1-3 parts of thixotropic agent and 0.1-1 part of pigment;
the component B comprises the following components in parts by weight: 30-50 parts of amine curing agent, 0.5-5 parts of curing accelerator, 40-65 parts of filler and 0.5-5 parts of diluent; 35-45 parts of preferable amine curing agent, 1-4 parts of curing accelerator, 45-60 parts of filler and 1-4 parts of diluent;
the low-temperature-resistant high-thixotropy epoxy mastic is characterized in that: the component A is bisphenol A epoxy resin, the epoxy equivalent is 0.13-0.60eq/100g, and the normal-temperature viscosity is 8000-20000mPa s; a preferred bisphenol A type epoxy resin having an epoxy equivalent of 0.40 to 0.56eq/100g and a viscosity of 12000 to 18000 mPas;
the component A diluent is C2-C16 glycidyl ether, preferably one or more than two of dodecyl glycidyl ether, ethylene glycol glycidyl ether and 1,4-butanediol diglycidyl ether;
the component A filler is at least one of fumed silica, wollastonite, heavy calcium carbonate, light calcium carbonate and quartz powder; preferred is at least one of fumed silica, wollastonite and ground calcium carbonate.
The thixotropic agent is one or more than two of hydrogenated castor oil, polyamide wax, fumed silica and light calcium carbonate. One or more of fumed silica and light calcium carbonate are preferable.
The pigment is azo pigment, preferably C.I pigment series;
the low-temperature-resistant high-thixotropy epoxy mastic is characterized in that: the amine curing agent is a polyamide curing agent, the active hydrogen equivalent is 90-250g/eq, the viscosity is 100-4000mPa & s, and the preferable active hydrogen equivalent is 200-240g/eq and the viscosity is 3000-4000mPa & s.
The curing accelerator is a micromolecular amine or piperazine accelerator, preferably one or more than two of triethanolamine, N-aminoethyl piperazine, 2-ethyl-4-methylimidazole, benzoyl peroxide and nonyl phenol. Preferably one or more of triethanolamine, N-aminoethylpiperazine and 2-ethyl-4-methylimidazole.
The component B filler is at least one of fumed silica, wollastonite, heavy calcium carbonate, light calcium carbonate and quartz powder; preferred is at least one of fumed silica, wollastonite and ground calcium carbonate.
The component B diluent is a low-volatility organic solvent, preferably one of benzyl alcohol, n-butanol and methanol.
The preparation method of the low-temperature-resistant high-thixotropy epoxy daub is characterized by comprising the following steps of:
(1) Sequentially adding epoxy resin, a diluent, a filler, a thixotropic agent and a pigment required by the component A into a reaction kettle, heating to 30-80 ℃, mixing and stirring for 1-2h, dispersing for 2-4 times by a three-roller machine, and discharging to obtain the component A;
(2) Sequentially adding the component B, namely the amine curing agent, the curing accelerator, the filler and the diluent into another reaction kettle, heating to 30-80 ℃, mixing and stirring for 1-2 hours, dispersing for 2-4 times by a three-roll machine, and then discharging to obtain a component B;
(3) Mixing the component A in the step (1) and the component B in the step (2) according to the weight ratio of 1: (0.75-1.25) and uniformly mixing to prepare the low-temperature-resistant high-thixotropy epoxy daub.
The low-temperature-resistant high-thixotropy epoxy daub is applied to a transportation and storage device of liquefied oil gas with the temperature range of-40 ℃ to 23 ℃, and comprises a liquefied oil gas ship, a shore tank and a metal material bonding in a shore station liquid cargo containment system.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described in the following combined with the specific embodiments. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The performance test method comprises the following steps:
1: low temperature resistance mechanical properties: manufacturing dumbbell-shaped sample bars according to ISO 604 standard, curing for 1h at 100 ℃, performing mechanical property test at-40 ℃, 25 ℃ and 23 ℃, and collecting data of tensile strength, elongation at break and tensile modulus;
2: low temperature resistant adhesive property: according to the ISO 4587 standard, bonding the epoxy daub on a stainless steel plate, curing for 1h at 100 ℃, then testing the shearing performance of the bonded sample strip at-40 ℃ and 23 ℃, and collecting the shearing performance data;
3: thixotropy testing: the viscosities, η 1 (viscosity at 1 RPM) and η 2 (viscosity at 10 RPM) were measured at a prescribed temperature (typically 23 ℃) using a rotary viscometer using a # 6 spindle at 1RPM and 10RPM, respectively, and the thixotropic index, it = η 1/η 2.
Example 1
The component A comprises the following components in parts by weight:
| raw materials | Epoxy equivalent eq/100g | Number of parts |
| Bisphenol A epoxy resin | 0.51 | 35 |
| Ground calcium carbonate | 60 | |
| 1,4 butanediol diglycidyl ether | 5 | |
| Fumed silica | 2 | |
| C.I Pigment Red | 0.5 |
The component B comprises the following components in parts by weight:
| raw materials | Equivalent g/eq of active hydrogen | Number of parts |
| Polyamide resin | 230 | 45 |
| Ground calcium carbonate | 55 | |
| N-aminoethylpiperazines | 3 | |
| Benzyl alcohol | 2 |
The preparation method of the low-temperature-resistant high-thixotropy epoxy daub comprises the following steps:
(1) Sequentially adding bisphenol A epoxy resin, heavy calcium carbonate, 1,4-butanediol diglycidyl ether, fumed silica and C.I Pigment Red into a reaction kettle, heating to 50 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component A;
(2) Sequentially adding polyamide resin, N-aminoethyl piperazine, heavy calcium carbonate and benzyl alcohol into a reaction kettle, heating to 50 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component B;
(3) And (3) uniformly mixing the component A in the step (1) and the component B in the step (2) according to the weight ratio of 1.
Example 2
The component A comprises the following components in parts by weight:
| raw materials | Epoxy equivalent eq/100g | Number of parts |
| Bisphenol A epoxy resin | 0.55 | 35 |
| Ground calcium carbonate | 65 | |
| Dodecyl glycidyl Ether | 5 | |
| Fumed silica | 3 | |
| C.I Pigment Green | 0.5 |
The component B comprises the following components in parts by weight:
| raw materials | Equivalent g/eq of active hydrogen | Number of copies |
| Polyamide resin | 240 | 40 |
| Ground calcium carbonate | 55 | |
| N-aminoethylpiperazines | 3 | |
| Methanol | 2 |
The preparation method of the low-temperature-resistant high-thixotropy epoxy daub comprises the following steps:
(1) Sequentially adding bisphenol A epoxy resin, heavy calcium carbonate, dodecyl glycidyl ether, fumed silica and C.I Pigment Green into a reaction kettle, heating to 50 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component A;
(2) Sequentially adding polyamide resin, N-aminoethyl piperazine, heavy calcium carbonate and methanol into a reaction kettle, heating to 50 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component B;
(3) And (3) uniformly mixing the component A in the step (1) and the component B in the step (2) according to the weight ratio of 1:1 to prepare the low-temperature-resistant high-thixotropy epoxy cement.
Example 3
The component A comprises the following components in parts by weight:
the component B comprises the following components in parts by weight:
| raw materials | Active hydrogenEquivalent g/eq | Number of parts |
| Polyamide resin | 240 | 40 |
| Ground calcium carbonate | 55 | |
| N-aminoethylpiperazines | 3 | |
| Methanol | 2 |
The preparation method of the low-temperature-resistant high-thixotropy epoxy daub comprises the following steps:
(1) Sequentially adding bisphenol A epoxy resin, heavy calcium carbonate, 1,4-butanediol diglycidyl ether, fumed silica and C.I Pigment Green into a reaction kettle, heating to 50 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component A;
(2) Sequentially adding polyamide resin, N-aminoethyl piperazine, heavy calcium carbonate and methanol into a reaction kettle, heating to 50 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component B;
(3) And (3) uniformly mixing the component A in the step (1) and the component B in the step (2) according to the weight ratio of 1:1 to prepare the low-temperature-resistant high-thixotropy epoxy cement.
Example 4
The component A comprises the following components in parts by weight:
the component B comprises the following components in parts by weight:
| raw materials | Equivalent g/eq of active hydrogen | Number of parts |
| Polyamide resin | 180 | 45 |
| Ground calcium carbonate | 55 | |
| 2-ethyl-4-methylimidazole | 3 | |
| Benzyl alcohol | 2 |
The preparation method of the low-temperature-resistant high-thixotropy epoxy daub comprises the following steps:
(1) Sequentially adding bisphenol A epoxy resin, heavy calcium carbonate, 1,4-butanediol diglycidyl ether, fumed silica, light calcium carbonate and C.I Pigment Red into a reaction kettle, heating to 50 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component A;
(2) Sequentially adding polyamide resin, 2-ethyl-4-methylimidazole, heavy calcium carbonate and benzyl alcohol into a reaction kettle, heating to 50 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component B;
(3) And (3) uniformly mixing the component A in the step (1) and the component B in the step (2) according to the weight ratio of 1.
Example 5
The component A comprises the following components in parts by weight:
| raw materials | Epoxy equivalent eq/100g | Number of copies |
| Bisphenol A epoxy resin | 0.51 | 35 |
| Ground calcium carbonate | 60 | |
| 1,4 butanediol diglycidyl ether | 5 | |
| Fumed silica | 2.5 | |
| C.I Pigment Red | 0.5 |
The component B comprises the following components in parts by weight:
| raw materials | Equivalent g/eq of active hydrogen | Number of copies |
| Polyamide resin | 210 | 45 |
| Ground calcium carbonate | 55 | |
| 2-ethyl-4-methylimidazole | 3 | |
| Methanol | 2 |
The preparation method of the low-temperature-resistant high-thixotropy epoxy daub comprises the following steps:
(1) Sequentially adding bisphenol A epoxy resin, heavy calcium carbonate, 1,4-butanediol diglycidyl ether, fumed silica and C.I Pigment Red into a reaction kettle, heating to 50 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component A;
(2) Sequentially adding polyamide resin, 2-ethyl-4-methylimidazole, heavy calcium carbonate and methanol into a reaction kettle, heating to 50 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component B;
(3) And (3) uniformly mixing the component A in the step (1) and the component B in the step (2) according to the weight ratio of 1.
Example 6
The component A comprises the following components in parts by weight:
| raw materials | Epoxy equivalent eq/100g | Number of copies |
| Bisphenol A epoxy resin | 0.35 | 40 |
| Ground calcium carbonate | 60 | |
| 1,4 butanediol diglycidyl ether | 5 | |
| Fumed silica | 2.5 | |
| C.I Pigment Red | 1 |
The component B comprises the following components in parts by weight:
the preparation method of the low-temperature-resistant high-thixotropy epoxy daub comprises the following steps:
(1) Sequentially adding bisphenol A epoxy resin, heavy calcium carbonate, 1,4-butanediol diglycidyl ether, fumed silica and C.I Pigment Red into a reaction kettle, heating to 40 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component A;
(2) Sequentially adding polyamide resin, 2-ethyl-4-methylimidazole, heavy calcium carbonate and methanol into a reaction kettle, heating to 50 ℃, mixing and stirring for 1h, dispersing for 4 times by a three-roller machine, and discharging to obtain a component B;
(3) And (3) uniformly mixing the component A in the step (1) and the component B in the step (2) according to the weight ratio of 1:1 to prepare the low-temperature-resistant high-thixotropy epoxy cement.
The results of testing the thixotropy, viscosity, mechanical properties and adhesion properties of the two-component epoxy mastic obtained in the above embodiments according to the corresponding test standards and methods are shown in the following table:
Claims (7)
1. the low-temperature-resistant high-thixotropy epoxy daub is characterized by comprising two components in a weight ratio of 1: (0.75-1.25) mixing the component A and the component B;
the component A is prepared from the following raw materials in parts by weight: 15-50 parts of epoxy resin, 1-10 parts of diluent, 40-75 parts of filler, 0.5-5 parts of thixotropic agent and 0.1-1 part of pigment;
the component B is prepared from the following components in parts by weight: 30-50 parts of amine curing agent, 0.5-5 parts of curing accelerator, 40-65 parts of filler and 0.5-5 parts of diluent;
the component A is bisphenol A epoxy resin, the epoxy equivalent is 0.13-0.60eq/100g, and the normal-temperature viscosity is 8000-20000mPa s;
the component A diluent is one or more than two of dodecyl glycidyl ether, ethylene glycol glycidyl ether and 1,4-butanediol diglycidyl ether;
the amine curing agent is a polyamide curing agent, the equivalent weight of active hydrogen is 90-250g/eq, and the viscosity is 100-4000mPa & s;
the curing accelerator is one or more than two of triethanolamine, N-aminoethyl piperazine, 2-ethyl-4-methylimidazole, benzoyl peroxide and nonyl phenol;
the component B diluent is a low-volatility organic solvent.
2. The low temperature resistant high thixotropy epoxy mastic of claim 1, characterized in that,
the component A is prepared from the following raw materials in parts by weight: 30-45 parts of epoxy resin, 3-8 parts of diluent, 50-65 parts of filler, 1-3 parts of thixotropic agent and 0.1-1 part of pigment;
the component B is prepared from the following components in parts by weight: 35-45 parts of amine curing agent, 1-4 parts of curing accelerator, 45-60 parts of filler and 1-4 parts of diluent.
3. The low temperature resistant high thixotropy epoxy mastic according to claim 1, wherein said low temperature resistant high thixotropy epoxy mastic is characterized by: the component A is bisphenol A epoxy resin, the epoxy equivalent is 0.40-0.56eq/100g, and the viscosity is 12000-18000mPa s;
the component A filler is at least one of fumed silica, wollastonite, heavy calcium carbonate, light calcium carbonate and quartz powder;
the thixotropic agent is one or more than two of hydrogenated castor oil, polyamide wax, fumed silica and light calcium carbonate;
the pigment is azo pigment.
4. The low temperature-resistant high thixotropy epoxy mastic according to claim 3, characterized in that,
the component A filler is at least one of fumed silica, wollastonite and heavy calcium carbonate;
the thixotropic agent is one or more than two of fumed silica and light calcium carbonate;
the pigment is C.I pigment series.
5. The low temperature-resistant high thixotropy epoxy mastic of claim 1, wherein said polyamide curing agent has an active hydrogen equivalent of 200-240g/eq and a viscosity of 3000-4000 mPa-s;
the curing accelerator is one or more than two of triethanolamine, N-aminoethyl piperazine and 2-ethyl-4-methylimidazole;
the component B filler is at least one of fumed silica, wollastonite, heavy calcium carbonate, light calcium carbonate and quartz powder;
the diluent of the component B is one of benzyl alcohol, n-butyl alcohol and methanol.
6. A method for preparing the low temperature resistant high thixotropy epoxy mastic according to any one of claims 1 to 5, characterized by the following steps:
(1) Sequentially adding epoxy resin, a diluent, a filler, a thixotropic agent and a pigment required by the component A into a reaction kettle, heating to 30-80 ℃, mixing and stirring for 1-2h, dispersing for 2-4 times by a three-roller machine, and discharging to obtain the component A;
(2) Sequentially adding the component B, namely the amine curing agent, the curing accelerator, the filler and the diluent into another reaction kettle, heating to 30-80 ℃, mixing and stirring for 1-2 hours, dispersing for 2-4 times by a three-roll machine, and then discharging to obtain a component B;
(3) Mixing the component A in the step (1) and the component B in the step (2) according to a weight ratio of 1: (0.75-1.25) and uniformly mixing to prepare the low-temperature-resistant high-thixotropy epoxy daub.
7. The use of the low temperature resistant high thixotropy epoxy mastic according to any one of claims 1-5 in transportation and storage devices for liquefied oil and gas at a temperature in the range of-40 ℃ to 23 ℃, including bonding of metal materials in liquefied oil and gas ships, shore tanks, shore station liquid cargo containment systems.
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