CN114231186A - Fast-curing modified dry-hanging adhesive and preparation method and application thereof - Google Patents
Fast-curing modified dry-hanging adhesive and preparation method and application thereof Download PDFInfo
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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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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Abstract
The invention discloses a fast curing modified dry-hanging adhesive as well as a preparation method and application thereof, and the fast curing modified dry-hanging adhesive comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 100 parts of multifunctional acrylate monomer, 10-30 parts of thickening reinforcing agent, 0-30 parts of first thixotropic agent, 1-3 parts of first coupling agent and 50-200 parts of first powder filler; the component B comprises the following raw materials in parts by weight: 80-100 parts of self-made modified amine curing agent, 0.5-5 parts of first accelerator, 2-5 parts of second accelerator, 1-3 parts of second coupling agent, 0-30 parts of second thixotropic agent and 50-250 parts of second powder filler. Compared with the rapid epoxy dry-hanging adhesive prepared by other means, the novel rapid curing modified dry-hanging adhesive prepared by the invention has the advantages of easily available raw materials, very obvious price advantage and good economic benefit.
Description
Technical Field
The invention belongs to the technical field of adhesive curing, and particularly relates to a fast-curing modified dry-hanging adhesive as well as a preparation method and application thereof.
Background
The epoxy dry-hanging adhesive is a well-known normal-temperature high-performance structural adhesive, has high strength and small shrinkage, has very good adhesion to most materials, and has excellent performances such as weather resistance, chemical resistance and the like, so the epoxy dry-hanging adhesive is widely applied by people and is often used as a stone structural adhesive.
The epoxy dry-hanging adhesive has the disadvantages that firstly, the viscosity of the epoxy resin in the component A is high, a diluent is often added in the application, secondly, the reaction activity of the epoxy resin is low, the epoxy resin can be cured for a relatively long time to obtain the required strength, and particularly in a low-temperature environment, the viscosity of the epoxy resin is obviously increased, the reaction activity is greatly reduced, even the situation of false curing or no curing occurs, and the practical application is limited by a high temperature.
Aiming at the defects of the epoxy dry-hanging adhesive, in the production and formula design of daily enterprises, the following methods are usually adopted for effectively solving the problems:
1. when in use, the dry hanging glue is heated to reduce the viscosity of the product and improve the reactivity. But the operation is troublesome, the energy consumption is large, and meanwhile, heating on a construction site has certain potential safety hazard.
2. A large amount of diluent is added, so that the viscosity of the resin is reduced, and the operability is improved, but the product body strength is greatly influenced. Meanwhile, amine or thiol curing agents with high activity are adopted to improve the reaction activity, but the reaction activity is still greatly influenced by the temperature, the operation is generally required to be carried out at the temperature of more than 5 ℃, and more harmful gases are released and the cost is greatly increased.
Through examining the literature, patent CN201410853728 "a room temperature fast curing low stress transparent epoxy resin adhesive" still adopts epoxy resin as the main body, and acrylate monomers as the diluent, and the principle of fast curing still adopts thiol curing agent to improve the curing activity of epoxy resin.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a quick-curing modified dry-hanging adhesive. The invention starts from the curing reaction activity of the two-component adhesive, adopts the reaction of the high-activity multifunctional acrylate monomer and the organic amine curing agent, has large reaction activity and small influence of temperature, can still quickly react and crosslink and cure at lower temperature (0 ℃), and simultaneously has low viscosity of the acrylate monomer and easy operation at low temperature.
The second purpose of the invention is to provide a preparation method of the fast curing modified dry-hanging adhesive, which improves the bonding performance of the system by means of physical and chemical aspects.
The third purpose of the invention is to provide the application of the rapid curing modified dry-hanging adhesive, when in use, A, B two components are uniformly mixed according to a certain proportion, and the rapid reaction curing can be realized.
In order to solve the technical problems, the invention is realized by the following technical scheme:
in a first aspect, the invention provides a novel fast-curing modified dry-hanging adhesive, which comprises two components A and B, wherein the component A comprises the following raw materials in parts by weight: 100 parts of multifunctional acrylate monomer, 10-30 parts of thickening reinforcing agent, 0-30 parts of first thixotropic agent, 1-3 parts of first coupling agent and 50-200 parts of first powder filler; the component B comprises the following raw materials in parts by weight: 80-100 parts of self-made modified amine curing agent, 0.5-5 parts of first accelerator, 2-5 parts of second accelerator, 1-3 parts of second coupling agent, 0-30 parts of second thixotropic agent and 50-250 parts of second powder filler.
Preferably, the multifunctional acrylate monomer is selected from trimethylolpropane triacrylate (TMPTA), pentaerythritol tetraacrylate (PET4A), methoxylated trimethylolpropane triacrylate (TMP3EOTA) and ethoxylated pentaerythritol tetraacrylate (PPTTA).
Preferably, the thickening and reinforcing agent is selected from polyacrylate resin and solid bisphenol A type epoxy resin; the first coupling agent is selected from 3- (methacryloyloxy) propyltrimethoxysilane and 3- (2, 3-glycidoxy) propyltrimethoxysilane.
Preferably, the base amine raw material of the homemade modified amine curing agent is selected from the group consisting of m-xylylenediamine (MXDA), Isophoronediamine (IPDA), 1, 3-diaminomethylcyclohexane (1, 3-BAC), methylcyclohexanediamine (HTDA), 4' -diaminodicyclohexylmethane (HMDA), and 1, 2-cyclohexanediamine.
Preferably, the first accelerator is selected from the group consisting of 2, 4, 6-tris (dimethylaminomethyl) phenol, benzyldimethylamine, o-hydroxybenzyldimethylamine and triethylamine; the second promoter is benzyl alcohol; the second coupling agent is selected from the group consisting of 3-aminopropyltriethoxysilane and 3- (2-aminoethylamino) propyltrimethoxysilane.
Preferably, the first thixotropic agent and the second thixotropic agent are both selected from precipitated silica and fumed silica; the first powder filler and the second powder filler are selected from calcium carbonate, silicon micropowder, barium sulfate and glass beads.
In a second aspect, the invention provides a preparation method for preparing the above fast curing modified dry-hanging adhesive, which comprises the following steps:
preparation of the component A:
weighing raw materials of a multifunctional acrylate monomer, a thickening reinforcing agent, a first thixotropic agent, a first coupling agent and a first powder filler according to the weight part ratio, firstly putting the multifunctional acrylate monomer and the thickening reinforcing agent into a stirrer, heating to 70-80 ℃, fully stirring until the thickening reinforcing agent is completely dissolved at the rotating speed of 50-80 r/min, then adding the first coupling agent, premixing and stirring for 5-15 min, then adding the first thixotropic agent, stirring for 5-15 min until the thickening reinforcing agent is completely uniform, then adding the first powder filler, continuously stirring for 50-60 min until the thickening reinforcing agent is completely uniform, and simultaneously cooling to 50 ℃ and discharging;
b, preparation of a component:
the method comprises the steps of firstly preparing a self-made modified amine curing agent according to a modification method, then weighing the raw materials of the self-made modified amine curing agent, a first accelerator, a second coupling agent, a second thixotropic agent and a second powder filler according to the weight part ratio, then adding the self-made modified amine curing agent, the first accelerator, the second accelerator and the second coupling agent into a stirrer, stirring for 5-15 minutes at a rotating speed of 50-80 r/min, then adding the second thixotropic agent into the stirrer, premixing and stirring for 5-15 minutes till the mixture is completely uniform, then adding the second powder filler, continuously stirring for 50-60 minutes till the mixture is completely uniform, and then discharging.
Preferably, the modification method of the homemade modified amine curing agent comprises addition modification or Mannich modification;
when the modification method is addition modification, the addition modification method includes:
adding a basic amine raw material into a reaction device, heating to 50-70 ℃ under stirring, adding liquid epoxy resin in batches every 20-30 minutes under continuous stirring, heating to 70-80 ℃ after adding the materials, carrying out heat preservation reaction for 1.5-2 hours, cooling to normal temperature, and discharging to obtain a self-made addition modified amine curing agent; wherein the liquid epoxy resin and the basic amine raw material are added in the following weight ratio: 1: 1.5 to 3.5.
When the modification method is a mannich modification, the mannich modification method comprises:
adding basic amine and phenol raw materials into reaction equipment, heating to 80-85 ℃ under the stirring condition, adding paraformaldehyde in batches every 20-30 minutes under continuous stirring, heating to 95-105 ℃ after adding the materials, carrying out heat preservation reaction for 3-5 hours, finally controlling the temperature to be 100-105 ℃, removing water in the system through vacuum, collecting through a condensation reflux mode until no water is evaporated, and cooling and discharging to obtain the self-made Mannich modified amine curing agent. Wherein the adding weight ratio of phenol to paraformaldehyde and basic amine raw materials is as follows: 1: 0.64: 3.0 to 4.5.
It is further preferred that the liquid epoxy resin is selected from the group consisting of bisphenol a type epoxy resins and bisphenol F type epoxy resins.
In a third aspect, the invention also provides an application of the novel fast curing modified dry-hanging adhesive, wherein when the component A and the component B are used, the weight ratio of the component A to the component B is 1: 1, mixing uniformly, and then realizing rapid reaction and solidification.
The thickening and reinforcing agent disclosed by the invention has the functions of thickening (viscosity increasing) and improving the system strength. The multifunctional acrylate monomer has good solubility in the multifunctional acrylate monomer of the component A, the resin viscosity can be improved by adding the multifunctional acrylate monomer, the sedimentation condition of the multifunctional acrylate monomer is greatly improved after various fillers are added, and meanwhile, an interpenetrating network can be formed with main resin or even cross-linked with amine components during later-stage curing, so that the bulk strength of a cured product is further improved.
The accelerator selected by the invention is a tertiary amine accelerator and benzyl alcohol, the first accelerator is a tertiary amine accelerator which can accelerate the gelling process, and the second accelerator is benzyl alcohol which can improve the post-curing speed of the reaction and further reduce the mixing initial viscosity of the system, so that the operability is improved. The component A is the coupling agent with epoxy group or double bond to ensure the stable coexistence of the system, and the component B is the coupling agent with amido group to ensure the stable coexistence of the system. The invention relates to two modification methods of a self-made modified amine curing agent, which mainly aim to increase a rigid chain segment structure in a curing system through modification so as to improve the strength of a cured product.
Compared with the prior art, the low-temperature fast curing composition prepared by the invention has the following beneficial effects:
the fast curing modified dry-hanging adhesive prepared by the invention has the advantages that the double components have low viscosity at normal temperature, can have good blending hand feeling at low temperature of 0 ℃, are far lower than an epoxy system, are very easy to operate, and are very convenient to operate even at lower temperature in winter. The curing speed is high, the gel time at normal temperature is only a few minutes to more than ten minutes according to different raw materials and formulas, and the gel can be cured in a short time at low temperature of 0-5 ℃. Meanwhile, compared with the fast epoxy dry-hanging adhesive prepared by other means, the fast curing modified dry-hanging adhesive prepared by the invention has the advantages of easily available raw materials, very obvious price advantage and good economic benefit.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the following description of the preferred embodiments of the present invention is provided in connection with specific examples, which should not be construed as limiting the present patent.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are conventionally obtained commercially or prepared by conventional methods.
The invention relates to a fast curing modified dry-hanging adhesive which comprises two components A and B, wherein the component A comprises 100 parts of multifunctional acrylate monomer, 10-30 parts of thickening reinforcing agent, 1-3 parts of first coupling agent, 0-30 parts of first thixotropic agent and 50-200 parts of first powder filler; the component B comprises 80-100 parts of self-made modified amine curing agent, 0.5-5 parts of first accelerator, 2-5 parts of second accelerator, 1-3 parts of second coupling agent, 0-30 parts of second thixotropic agent and 50-250 parts of second powder filler.
A fast curing modified dry-hanging adhesive is prepared by the following preparation process:
the preparation method of the component A comprises the following steps:
weighing raw materials of a multifunctional acrylate monomer, a thickening reinforcing agent, a first thixotropic agent, a first coupling agent and a first powder filler according to the weight part ratio, firstly putting the multifunctional acrylate monomer and the thickening reinforcing agent into a stirrer, heating to 70-80 ℃, fully stirring until the thickening reinforcing agent is completely dissolved at the rotating speed of 50-80 r/min, then adding the first coupling agent, premixing and stirring for 5-15 min, then adding the first thixotropic agent, stirring for 5-15 min until the thickening reinforcing agent is completely uniform, then adding the first powder filler, continuously stirring for 50-60 min until the thickening reinforcing agent is completely uniform, and simultaneously cooling to 50 ℃ and discharging.
The preparation method of the component B comprises the following steps:
firstly, self-made modified amine curing agent is prepared by two modification methods, specifically:
the first method, the addition modification method:
adding a basic amine raw material into a reaction device, heating to 50-70 ℃ under stirring, adding liquid epoxy resin in batches every 20-30 minutes under continuous stirring, heating to 70-80 ℃ after adding the materials, carrying out heat preservation reaction for 1.5-2 hours, cooling to normal temperature, and discharging to obtain a self-made addition modified amine curing agent; the liquid epoxy resin is selected from bisphenol A type epoxy resin and bisphenol F type epoxy resin. Wherein the liquid epoxy resin and the basic amine raw material are added in the following weight ratio: 1: 1.5 to 3.5.
Second method, mannich modification method:
adding basic amine and phenol raw materials into reaction equipment, heating to 80-85 ℃ under the stirring condition, adding paraformaldehyde in batches every 20-30 minutes under continuous stirring, heating to 95-105 ℃ after adding the materials, carrying out heat preservation reaction for 3-5 hours, finally controlling the temperature to be 100-105 ℃, removing water in the system through vacuum, collecting through a condensation reflux mode until no water is evaporated, and cooling and discharging to obtain the self-made Mannich modified amine curing agent. Wherein the adding weight ratio of phenol to paraformaldehyde and basic amine raw materials is as follows: 1: 0.64: 3.0 to 4.5.
And then, after the self-made modified amine curing agent is synthesized, weighing the raw materials of the self-made modified amine curing agent, a first accelerator, a second coupling agent, a second thixotropic agent and a second powder filler according to the weight part ratio, then adding the self-made modified amine curing agent, the first accelerator, the second accelerator and the second coupling agent into a stirrer at the rotating speed of 50-80 r/min, stirring for 5-15 min, then adding the second thixotropic agent, premixing and stirring for 5-15 min to be completely uniform, then adding the second powder filler, continuously stirring for 50-60 min to be completely uniform, and discharging.
A modified fast-curing dry-hanging adhesive comprises the following specific embodiments:
step one, self-preparing a modified amine curing agent, wherein the specific method comprises the following steps of:
table-one self-made modified amine curing agent raw material and its proportioning
| Examples of self-made modified amine curing agents | Raw material feeding weight ratio |
| Self-made modified amine curing agent 1 | Epoxy 128: m-xylylenediamine ═ 1: 2 |
| Self-made modified amine curing agent 2 | And (3) epoxy 170: methylcyclohexanediamine ═ 1: 1.88 |
| Self-made modified amine curing agent 3 | And (3) epoxy 170: HMDA is 1: 3.5 |
| Self-made modified amine curing agent 4 | Epoxy 128: 1, 2-cyclohexanediamine ═ 1: 1.5 |
| Self-made modified amine curing agent 5 | Phenol: paraformaldehyde: isophorone diamine ═ 1: 0.64: 4.52 |
| Self-made modified amine curing agent 6 | Phenol: paraformaldehyde: 1, 3-BAC ═ 1: 0.64: 3.56 |
| Self-made modified amine curing agent 7 | Phenol: paraformaldehyde: methylcyclohexanediamine ═ 1: 0.64: 3.4 |
| Self-made modified amine curing agent 8 | Phenol: paraformaldehyde: 1, 2-cyclohexanediamine ═ 1: 0.64: 3.03 |
Note: the self-made modified amine curing agent is illustrated as part of the invention, wherein the effect of the non-illustrated components is basically equivalent to the effect of the illustrated components. Wherein epoxy 128 is a commercial grade of bisphenol a type liquid epoxy and epoxy 170 is a commercial grade of bisphenol F type liquid epoxy.
Secondly, A, B components are prepared, the specific preparation methods are respectively carried out according to the preparation method of A, B components as described above, and the weight portions of the relevant examples are as follows:
table two examples ingredient parts of component a
Continuation table two
Table three examples ingredient parts of B component
Continued table III
In the above step, KH-550 is a commercial brand of 3-aminopropyltriethoxysilane, KH-560 is a commercial brand of 3- (2, 3-glycidoxy) propyltrimethoxysilane, KH-570 is a commercial brand of 3- (methacryloyloxy) propyltrimethoxysilane, KH-792 is a commercial brand of 3- (2-aminoethylamino) propyltrimethoxysilane, and DMP-30 is a commercial brand of 2, 4, 6-tris (dimethylaminomethyl) phenol.
Thirdly, mixing the components A and B according to the weight ratio of 1: 1, testing the mechanical property, and simultaneously comparing the mechanical property with the mechanical property of the epoxy dry-hanging adhesive on the market, wherein the specific data are as follows: table four examples mechanical property test data
Table four
Note: in the detection method, the harmonicity is judged by the manual stirring comparison of professional technicians, and the pot life, the compression-shear strength, the tensile-shear strength, the bending elastic modulus and the impact strength are detected at the temperature of 23 ℃ by referring to the standard JC 887-. The index of the applicable period can be determined by negotiation according to market requirements, so that no index requirement is added.
The novel fast curing modified dry-hanging adhesive related by the invention has various performances related to factors such as structural design of a self-made curing agent, selection of resin and powder, design of solid-liquid ratio, blending of a formula and the like, and can not be complained completely in space. From the performance data of the above examples, it can be seen that example 7 is the best example of this patent.
From the performance data, the novel fast curing modified dry-hang adhesive has excellent harmonious property and particularly shows obvious hand feeling advantage at low temperature because the viscosity of the acrylate monomer is extremely low, so that the two components have lower harmonious viscosity after being mixed. Meanwhile, the curing activity is high, and the gel speed is obviously higher than that of the epoxy system dry-hanging adhesive, so that the epoxy resin has certain convenience in construction. In addition, in terms of mechanical properties, the impact strength is obviously higher than that of the epoxy system dry-hanging adhesive, namely the toughness of the system is obviously better than that of the epoxy system, which is very rare in building adhesives, and other strength indexes can reach the corresponding level of the epoxy dry-hanging adhesive and further exceed the technical indexes of national standard requirements. Therefore, the novel fast-curing modified dry-hanging adhesive has obvious advantages in practical application and can completely replace epoxy dry-hanging adhesive for application.
In conclusion of all the technical indexes, the novel fast-curing modified dry-hang glue disclosed by the invention is excellent in performance of all performance indexes, is a novel dry-hang glue variety with strong applicability, and has good creativity and practical application value.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (10)
1. The fast-curing modified dry-hanging adhesive is characterized by comprising two components A and B, wherein the component A comprises the following raw materials in parts by weight: 100 parts of multifunctional acrylate monomer, 10-30 parts of thickening reinforcing agent, 0-30 parts of first thixotropic agent, 1-3 parts of first coupling agent and 50-200 parts of first powder filler; the component B comprises the following raw materials in parts by weight: 80-100 parts of self-made modified amine curing agent, 0.5-5 parts of first accelerator, 2-5 parts of second accelerator, 1-3 parts of second coupling agent, 0-30 parts of second thixotropic agent and 50-250 parts of second powder filler.
2. The fast curing modified xerogel according to claim 1 wherein the multifunctional acrylate monomer is selected from the group consisting of trimethylolpropane triacrylate, pentaerythritol tetraacrylate, methoxylated trimethylolpropane triacrylate and ethoxylated pentaerythritol tetraacrylate.
3. The fast curing modified xerogel according to claim 1 wherein the thickening and strengthening agent is selected from polyacrylate resin and solid bisphenol a epoxy resin; the first coupling agent is selected from 3- (methacryloyloxy) propyltrimethoxysilane and 3- (2, 3-glycidoxy) propyltrimethoxysilane.
4. The fast curing modified xerogel according to claim 1, wherein the base amine raw material of the homemade modified amine curing agent is selected from m-xylylenediamine, isophorone diamine, 1, 3-diaminomethylcyclohexane, methylcyclohexanediamine, 4' -diaminodicyclohexylmethane, and 1, 2-cyclohexanediamine.
5. The fast curing modified xerogel according to claim 1 wherein the first accelerator is selected from the group consisting of 2, 4, 6-tris (dimethylaminomethyl) phenol, benzyldimethylamine, o-hydroxybenzyldimethylamine, and triethylamine; the second promoter is benzyl alcohol; the second coupling agent is selected from the group consisting of 3-aminopropyltriethoxysilane and 3- (2-aminoethylamino) propyltrimethoxysilane.
6. The fast-curing modified dry-hang glue of claim 1, wherein the first thixotropic agent and the second thixotropic agent are both selected from precipitated silica and fumed silica; the first powder filler and the second powder filler are selected from calcium carbonate, silicon micropowder, barium sulfate and glass beads.
7. A method for preparing the fast curing modified xerogel as claimed in any one of claims 1 to 6, comprising:
preparation of a component A:
weighing raw materials of a multifunctional acrylate monomer, a thickening reinforcing agent, a first thixotropic agent, a first coupling agent and a first powder filler according to the weight part ratio, firstly putting the multifunctional acrylate monomer and the thickening reinforcing agent into a stirrer, heating to 70-80 ℃, fully stirring until the thickening reinforcing agent is completely dissolved at the rotating speed of 50-80 r/min, then adding the first coupling agent, premixing and stirring for 5-15 min, then adding the first thixotropic agent, stirring for 5-15 min until the thickening reinforcing agent is completely uniform, then adding the first powder filler, continuously stirring for 50-60 min until the thickening reinforcing agent is completely uniform, and simultaneously cooling to 50 ℃ and discharging;
b, preparation of a component:
the method comprises the steps of firstly preparing a self-made modified amine curing agent according to a modification method, then weighing the raw materials of the self-made modified amine curing agent, a first accelerator, a second coupling agent, a second thixotropic agent and a second powder filler according to the weight part ratio, then adding the self-made modified amine curing agent, the first accelerator, the second accelerator and the second coupling agent into a stirrer, stirring for 5-15 minutes at a rotating speed of 50-80 r/min, then adding the second thixotropic agent into the stirrer, premixing and stirring for 5-15 minutes till the mixture is completely uniform, then adding the second powder filler, continuously stirring for 50-60 minutes till the mixture is completely uniform, and then discharging.
8. The preparation method of the fast curing modified dry-hang glue of claim 7, wherein the modification method of the homemade modified amine curing agent comprises addition modification or Mannich modification;
when the modification method is addition modification, the addition modification method includes:
adding a basic amine raw material into a reaction device, heating to 50-70 ℃ under stirring, adding liquid epoxy resin in batches every 20-30 minutes under continuous stirring, heating to 70-80 ℃ after adding the materials, carrying out heat preservation reaction for 1.5-2 hours, cooling to normal temperature, and discharging to obtain a self-made addition modified amine curing agent; wherein the liquid epoxy resin and the basic amine raw material are added in the following weight ratio: 1: 1.5 to 3.5;
when the modification method is a mannich modification, the mannich modification method comprises:
adding basic amine and phenol raw materials into reaction equipment, heating to 80-85 ℃ under the stirring condition, adding paraformaldehyde in batches every 20-30 minutes under continuous stirring, heating to 95-105 ℃ after adding the materials, carrying out heat preservation reaction for 3-5 hours, finally controlling the temperature to be 100-105 ℃, removing water in the system through vacuum, collecting the water through a condensation reflux mode until no water is evaporated, and cooling and discharging to obtain the self-made Mannich modified amine curing agent; wherein the adding weight ratio of phenol to paraformaldehyde and basic amine raw materials is as follows: 1: 0.64: 3.0 to 4.5.
9. The method for preparing the novel fast-curing modified xerogel according to claim 8, wherein the liquid epoxy resin is selected from bisphenol A epoxy resin and bisphenol F epoxy resin.
10. The application of the novel fast-curing modified dry-hanging adhesive as claimed in any one of claims 1 to 6, wherein when the component A and the component B are used, the weight ratio of the component A to the component B is 1: 1, mixing uniformly, and then realizing rapid reaction and solidification.
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| CN114231186B (en) | 2023-04-18 |
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Effective date of registration: 20230907 Address after: No. 6 Danjin Road, Industrial Concentration Zone, Baita Town, Jintan District, Changzhou City, Jiangsu Province, 213299 Patentee after: Jiangsu Hercules Marble Care Materials Co.,Ltd. Address before: 430040 No.26, Jinhai Industrial Park Road, Jinyinhu office, Dongxihu District, Wuhan City, Hubei Province Patentee before: WUHAN KEDA MARBLE PROTECTIVE MATERIALS Co.,Ltd. |