CN111826111A - Epoxy potting repair adhesive capable of being rapidly cured at room temperature and preparation method thereof - Google Patents
Epoxy potting repair adhesive capable of being rapidly cured at room temperature and preparation method thereof Download PDFInfo
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- CN111826111A CN111826111A CN202010775784.0A CN202010775784A CN111826111A CN 111826111 A CN111826111 A CN 111826111A CN 202010775784 A CN202010775784 A CN 202010775784A CN 111826111 A CN111826111 A CN 111826111A
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- epoxy
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- room temperature
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4215—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof cycloaliphatic
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
- C08G59/686—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used containing nitrogen
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to the field of valve maintenance, in particular to an epoxy potting repair adhesive capable of being rapidly cured at room temperature and a preparation method thereof. The composition comprises the following components in parts by weight: a main agent: 100 parts of acrylic acid modified epoxy resin, and a curing agent: 92-100 parts of acid anhydride, 0.5-5.0 parts of accelerator and 0.3-3.0 parts of tertiary amine, and the preparation method comprises the following steps: adding a reactive diluent, butyl acrylate, acrylonitrile, methyl methacrylate and benzoyl peroxide into a reaction bottle; stirring the reagent, heating to 90 ℃, reacting for four hours, and controlling the reaction temperature to be 90-95 ℃; after reacting for four hours, cooling the reagent in the reaction bottle to 60 ℃; adding epoxy resin and reactive diluent into a reaction bottle to prepare an epoxy pouring sealant main agent; preparation of the curing agent: adding anhydride and an accelerator into another container, and mixing for 30 minutes to prepare a curing agent; the epoxy pouring sealant main agent is mixed with the curing agent, and compared with the prior art, the epoxy pouring sealant main agent can be surface-dried for 1-2 hours at room temperature and completely cured for 2-4 hours.
Description
Technical Field
The invention relates to the field of valve maintenance, in particular to an epoxy potting repair adhesive capable of being rapidly cured at room temperature and a preparation method thereof.
Background
In the valve maintenance process, a plurality of problems such as valve body cracks, water leakage and the like can be encountered, the valve replacement cost is too high, the problems of complex process and long time consumption in the composition are solved by commonly using repair glue in daily life, and the curing time of the repair glue directly influences the maintenance efficiency.
Therefore, it is necessary to design an epoxy potting repair adhesive capable of being rapidly cured at room temperature and a preparation method thereof.
Disclosure of Invention
The invention breaks through the difficult problems in the prior art and designs the epoxy potting repairing adhesive capable of being rapidly cured at room temperature and the preparation method thereof.
In order to achieve the purpose, the invention designs an epoxy potting repair adhesive capable of being rapidly cured at room temperature, which comprises the following components in parts by weight: a main agent: 100 parts of acrylic acid modified epoxy resin, and a curing agent: 92-100 parts of acid anhydride, 0.5-5.0 parts of accelerator and 0.3-3.0 parts of tertiary amine,
a preparation method of epoxy potting repair adhesive capable of being rapidly cured at room temperature comprises the following steps:
step 1: adding reactive diluent, butyl acrylate, acrylonitrile, methyl methacrylate and benzoyl peroxide into a reaction bottle,
step 2: stirring and heating the reagent in the reaction bottle to 90 ℃, reacting for four hours, controlling the reaction temperature to be 90-95 ℃,
and step 3: after reacting for four hours, cooling the reagent in the reaction bottle to 60 ℃,
and 4, step 4: adding epoxy resin and reactive diluent into a reaction bottle to prepare an epoxy pouring sealant main agent,
and 5: preparation of the curing agent: adding anhydride and accelerator into another container, mixing for 30 min to obtain curing agent,
step 6: mixing the epoxy pouring sealant main agent with the curing agent.
The epoxy resin is one or a mixture of two of bisphenol A type liquid epoxy resin with an epoxy value of 0.54 and bisphenol F type liquid epoxy resin, and the dosage of the epoxy resin is 20-80 Wt% of the main agent of the epoxy pouring sealant.
The reactive diluent is one or a mixture of more than one of ethylene glycol diglycidyl ether and butanediol diglycidyl ether, and the dosage of the reactive diluent is 10-30 Wt% of the epoxy resin.
The using amount of butyl acrylate is 3-4 wt% of epoxy resin, acrylonitrile is 4-9 wt% of epoxy resin, methyl methacrylate is 5-9 wt% of epoxy resin, and benzoyl peroxide is 0.05-0.1 wt% of epoxy resin.
The proportion of the main agent to the curing agent of the epoxy potting repair adhesive is 1: 0.2-1, and the time required for normal-temperature curing is 2-4 hours.
Accelerator (b): one or more of DMP, imidazole and boron trifluoride amine complex, and the dosage of the complex is 0.5 to 5.0 parts per hundred parts of curing agent
Compared with the prior art, the valve can be surface-dried for 1-2 hours at room temperature, and completely cured for 2-4 hours, the valve can be put into normal use within 2-4 hours in the valve maintenance application, the bonding shear strength of stainless steel is not less than 10MPa, the problems of complex operation and long time consumption in the valve maintenance process are solved, and the requirement of the rapid filling and sealing repair material of the valve can be met.
Detailed Description
The invention designs an epoxy potting repair adhesive capable of being rapidly cured at room temperature, which comprises the following components in parts by weight: a main agent: 100 parts of acrylic acid modified epoxy resin, and a curing agent: 92-100 parts of acid anhydride, and an accelerator: 0.5 to 5.0 parts by weight of a tertiary amine and 0.3 to 3.0 parts by weight of a tertiary amine
A preparation method of epoxy potting repair adhesive capable of being rapidly cured at room temperature comprises the following steps:
step 1: reactive diluents, butyl acrylate, acrylonitrile, methyl methacrylate and benzoyl peroxide were added to the reaction flask. Wherein the reactive diluent is one or a mixture of more than one of ethylene glycol diglycidyl ether and butanediol diglycidyl ether, and the dosage of the reactive diluent is 10-30 Wt% of the epoxy resin; the using amount of butyl acrylate is 3-4 wt% of epoxy resin, acrylonitrile is 4-9 wt% of epoxy resin, methyl methacrylate is 5-9 wt% of epoxy resin, and benzoyl peroxide is 0.05-0.1 wt% of epoxy resin.
Step 2: stirring and heating the reagent in the reaction bottle to 90 ℃, reacting for four hours, controlling the reaction temperature to be 90-95 ℃,
and step 3: after reacting for four hours, cooling the reagent in the reaction bottle to 60 ℃, wherein the epoxy resin is one or a mixture of two of bisphenol A type liquid epoxy resin and bisphenol F type liquid epoxy resin with the epoxy value of 0.54, and the dosage of the epoxy resin is 20-80 wt% of the main agent of the epoxy pouring sealant.
And 4, step 4: adding epoxy resin and reactive diluent into a reaction bottle to prepare an epoxy pouring sealant main agent,
and 5: preparation of the curing agent: and adding the anhydride and then the accelerator into another container, and mixing for 30 minutes to prepare the curing agent. Wherein the accelerant is one or more than one of DMP, imidazole and boron trifluoride amine complex, and the dosage is 0.5-5 parts per hundred parts by weight of the curing agent.
Step 6: mixing the epoxy pouring sealant main agent with the curing agent. The proportion of the main agent to the curing agent of the epoxy potting repair adhesive is 1: 0.2-1, and the time required for normal-temperature curing is 2-4 hours.
Example 1
Charging a reactor with 30 grams of butyl acrylate, 50 grams of acrylonitrile, 50 grams of methyl methacrylate, and 0.5 grams of benzoyl peroxide; stirring and heating to 90 ℃, controlling the reaction temperature at 90-95 ℃, reacting for 4 hours, cooling to 60 ℃, adding 700g of bisphenol A epoxy resin E-51 and 169.5g of butanediol diglycidyl ether, stirring and reacting for 60 minutes to prepare the main agent of the epoxy potting repair adhesive.
In another reactor, 980 g of methylnadic anhydride, 10 g of DMP-30 and 10 g of imidazole were added and mixed for 30 minutes to obtain a curing agent.
The performance index of the adhesive is as follows (mixing ratio of main agent to curing agent is 2: 1)
(1) Viscosity: initial at 1000mPa s at 25 ℃, (2) gel time: 1 h; curing time: 3 hours; (3) the shear strength is more than or equal to 10MPa (the test material is 306 stainless steel); (4) tensile strength: not less than 25 MPa; (5) elongation at break: more than or equal to 10 percent; (6) endurance stress (at 16MP pressure): the time is more than or equal to 1000 hours.
Example 2
Adding 40 g of butyl acrylate, 40 g of acrylonitrile, 50g of methyl methacrylate and 0.5 g of benzoyl peroxide into a reactor, stirring and heating to 90 ℃, controlling the reaction temperature at 90-95 ℃, reacting for 4 hours, cooling to 60 ℃, adding 750g of bisphenol A type epoxy resin E-51 and 119.5g of butanediol diglycidyl ether, and stirring and reacting for 60 minutes to obtain the main agent of the epoxy potting repair adhesive.
In another reactor, 980 g of methylnadic anhydride, 5g of DMP-30 and 15 g of imidazole were added and mixed for 30 minutes to obtain a curing agent.
The adhesive has the following performance indexes: (Main agent and curing agent mixing ratio 2: 1)
(1) Viscosity: initially at 1000mPa s at 25 ℃; (2) gel time: 1 h; curing time: 2.8 hours; (3) shear strength: not less than 10MPa (the test material is 306 stainless steel); (4) tensile strength: not less than 25 MPa; (5) elongation at break: more than or equal to 10 percent; (6) endurance stress (at 16MP pressure): the time is more than or equal to 1000 hours.
Example 3
Adding 40 g of butyl acrylate, 40 g of acrylonitrile, 50g of methyl methacrylate and 0.5 g of benzoyl peroxide into a reactor, stirring and heating to 90 ℃, controlling the reaction temperature at 90-95 ℃, reacting for 4 hours, cooling to 60 ℃, adding 750g of bisphenol A type epoxy resin E-51 and 119.5g of butanediol diglycidyl ether, and stirring and reacting for 60 minutes to obtain the main agent of the epoxy potting repair adhesive.
In another reactor 970 g of methylnadic anhydride, 10 g of DMP-30, 20 g of imidazole were added and mixed for 30 minutes to obtain a curing agent.
The performance index of the adhesive is as follows (mixing ratio of main agent to curing agent is 2: 1)
(1) Viscosity: initially at 1000mPa s at 25 ℃; (2) gel time: 1 h; curing time: 2.5 hours; (3) shear strength: not less than 10MPa (the test material is 306 stainless steel); (4) tensile strength: not less than 25 MPa; (5) elongation at break: more than or equal to 10 percent; (6) endurance stress (at 16MP pressure): the time is more than or equal to 1000 hours.
Example 4
Charging a reactor with 40 grams of butyl acrylate, 40 grams of acrylonitrile, 50 grams of methyl methacrylate and 0.5 grams of benzoyl peroxide; stirring and heating to 90 ℃, controlling the reaction temperature at 90-95 ℃, reacting for 4 hours, cooling to 60 ℃, adding 750g of bisphenol A type epoxy resin E-51 and 119.5g of butanediol diglycidyl ether, stirring and reacting for 60 minutes to prepare the main agent of the epoxy potting repair adhesive.
In another reactor, 960 g of methylnadic anhydride, 20 g of DMP-30, and 20 g of imidazole were added and mixed for 30 minutes to obtain a curing agent.
The performance index of the adhesive is as follows (mixing ratio of main agent to curing agent is 2: 1)
(1) Viscosity: initially at 1000mPa s at 25 ℃; (2) gel time: 1 h; curing time: 2.0 hours; (3) shear strength: not less than 10MPa (the test material is 306 stainless steel); (4) tensile strength: not less than 25 MPa; (5) elongation at break: more than or equal to 10 percent; (6) endurance stress resistance: (at a pressure of 16 MP) 1000h or more.
The performance indexes of the fast curing epoxy pouring sealant disclosed by the invention are as follows (1): 900 to 2500 mPas at 25 ℃; (2) gel time: 1 h-2 h, which can be adjusted by the type and addition amount of the accelerator, and (3) the shear strength: not less than 10 MPa; (4) tensile strength: not less than 25MPa, (5) elongation at break: more than or equal to 10 percent; (6) endurance stress (16MP, h): the time is more than or equal to 1000 hours.
The fast-curing epoxy potting repair adhesive can realize non-disassembly repair of the valve, such as filling and repair between a sealing surface of a butterfly valve seat and a butterfly plate, and can greatly improve the reliability of a repaired part along with the use of the potting repair adhesive, thereby greatly reducing potential safety hazards in the use process and prolonging the service life of the valve; in order to overcome the defects of large brittleness and poor impact property of the common epoxy potting adhesive, the epoxy potting adhesive prepared by toughening the acrylic copolymer has the following advantages: the adhesive has low viscosity and impact resistance, and solves the problems of high viscosity and short pot life of the adhesive; and the curing time of the adhesive is adjusted by the accelerator, so that the target adhesive has the characteristic of quick curing.
Claims (7)
1. An epoxy potting repair adhesive capable of being rapidly cured at room temperature comprises the following components in parts by weight: a main agent: 100 parts of acrylic acid modified epoxy resin, and the curing agent comprises the following components: 92-100 parts of acid anhydride, 0.5-5.0 parts of accelerator and 0.3-3.0 parts of tertiary amine.
2. The preparation method of the room-temperature fast-curing epoxy potting repair adhesive according to claim 1, characterized by comprising the following steps: the preparation method comprises the following steps:
step 1: adding reactive diluent, butyl acrylate, acrylonitrile, methyl methacrylate and benzoyl peroxide into a reaction bottle,
step 2: stirring and heating the reagent in the reaction bottle to 90 ℃, reacting for four hours, controlling the reaction temperature to be 90-95 ℃,
and step 3: after reacting for four hours, cooling the reagent in the reaction bottle to 60 ℃,
and 4, step 4: adding epoxy resin and reactive diluent into a reaction bottle to prepare an epoxy pouring sealant main agent,
and 5: adding anhydride and accelerator into another container, mixing for 30 min to obtain curing agent,
step 6: mixing the epoxy pouring sealant main agent with the curing agent.
3. The preparation method of the epoxy potting repair adhesive capable of being rapidly cured at room temperature according to claim 2, which is characterized by comprising the following steps: the epoxy resin is one or a mixture of two of bisphenol A type liquid epoxy resin and bisphenol F type liquid epoxy resin with the epoxy value of 0.54, and the dosage of the epoxy resin is 20-80 wt% of the main agent of the epoxy pouring sealant.
4. The preparation method of the epoxy potting repair adhesive capable of being rapidly cured at room temperature according to claim 2, which is characterized by comprising the following steps: the reactive diluent is one or a mixture of more than one of ethylene glycol diglycidyl ether and butanediol diglycidyl ether, and the dosage of the reactive diluent is 10-30 wt% of the epoxy resin.
5. The preparation method of the epoxy potting repair adhesive capable of being rapidly cured at room temperature according to claim 2, which is characterized by comprising the following steps: the using amount of the butyl acrylate is 3-4 wt% of the epoxy resin, the acrylonitrile is 4-9 wt% of the epoxy resin, the methyl methacrylate is 5-9 wt% of the epoxy resin, and the benzoyl peroxide is 0.05-0.1 wt% of the epoxy resin.
6. The preparation method of the epoxy potting repair adhesive capable of being rapidly cured at room temperature according to claim 2, which is characterized by comprising the following steps: the proportion of the main agent to the curing agent of the epoxy potting repair adhesive is 1: 0.2-1, and the time required for normal-temperature curing is 2-4 hours.
7. The preparation method of the epoxy potting repair adhesive capable of being rapidly cured at room temperature according to claim 2, which is characterized by comprising the following steps: the accelerant is one or more than one of DMP, imidazole and boron trifluoride amine complex, and the using amount of the accelerant is 0.5-5 parts per hundred parts by weight of the curing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010775784.0A CN111826111A (en) | 2020-08-05 | 2020-08-05 | Epoxy potting repair adhesive capable of being rapidly cured at room temperature and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010775784.0A CN111826111A (en) | 2020-08-05 | 2020-08-05 | Epoxy potting repair adhesive capable of being rapidly cured at room temperature and preparation method thereof |
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| CN111826111A true CN111826111A (en) | 2020-10-27 |
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| CN202010775784.0A Pending CN111826111A (en) | 2020-08-05 | 2020-08-05 | Epoxy potting repair adhesive capable of being rapidly cured at room temperature and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112300740A (en) * | 2020-11-16 | 2021-02-02 | 上海汉司实业有限公司 | Room-temperature-cured high-heat-resistance high-peel-strength bi-component epoxy adhesive |
| CN112694855A (en) * | 2020-12-24 | 2021-04-23 | 苏州赛伍应用技术股份有限公司 | Modified acrylate adhesive, adhesive tape, and preparation method and application method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827566A (en) * | 2012-09-19 | 2012-12-19 | 三友（天津）高分子技术有限公司 | Single-component high/low-temperature-resistant epoxy resin composition |
| CN104119827A (en) * | 2014-07-25 | 2014-10-29 | 中国工程物理研究院化工材料研究所 | Room-temperature-curing epoxy-acid anhydride adhesive and preparation method thereof |
| CN104962224A (en) * | 2015-07-06 | 2015-10-07 | 深圳先进技术研究院 | Underfill adhesive and preparation method thereof |
-
2020
- 2020-08-05 CN CN202010775784.0A patent/CN111826111A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827566A (en) * | 2012-09-19 | 2012-12-19 | 三友（天津）高分子技术有限公司 | Single-component high/low-temperature-resistant epoxy resin composition |
| CN104119827A (en) * | 2014-07-25 | 2014-10-29 | 中国工程物理研究院化工材料研究所 | Room-temperature-curing epoxy-acid anhydride adhesive and preparation method thereof |
| CN104962224A (en) * | 2015-07-06 | 2015-10-07 | 深圳先进技术研究院 | Underfill adhesive and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112300740A (en) * | 2020-11-16 | 2021-02-02 | 上海汉司实业有限公司 | Room-temperature-cured high-heat-resistance high-peel-strength bi-component epoxy adhesive |
| CN112694855A (en) * | 2020-12-24 | 2021-04-23 | 苏州赛伍应用技术股份有限公司 | Modified acrylate adhesive, adhesive tape, and preparation method and application method thereof |
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