CN114316870B - Injection type bar planting adhesive and preparation method thereof - Google Patents
Injection type bar planting adhesive and preparation method thereof Download PDFInfo
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Abstract
The application relates to the technical field of bar planting glue, and particularly discloses an injection type bar planting glue and a preparation method thereof. The injection type bar planting adhesive comprises two components A and B, wherein the mass ratio of the components A and B is 3:1, and the components A comprise: 50-70 parts of matrix resin; 20-40 parts of modified filler; 4-6 parts of thixotropic agent; 3-5 parts of a diluent; 2-4 parts of a coupling agent; the component B comprises the following components: 50-60 parts of a flexible curing agent; 20-30 parts of modified filler; 6-8 parts of a promoter; 1-3 parts of a diluent; 3-5 parts of thixotropic agent; 2-4 parts of a coupling agent; the matrix resin comprises the following components in percentage by mass 1-2:4-5 and bisphenol A epoxy vinyl resin. The preparation method comprises the steps of preparation of the component A, preparation of the component B and preparation of the injection type bar planting adhesive.
Description
Technical Field
The application relates to the technical field of bar planting glue, and particularly discloses an injection type bar planting glue and a preparation method thereof.
Background
With the rapid increase of the total volume of the buildings in China, some old buildings in use have performance degradation to different degrees, and the old buildings have potential safety hazards, so that the old buildings need to be maintained, reinforced and reformed so as to relieve the population, resources and environment problems. In the reconstruction of old buildings, the connection of the planted bars is recognized as an efficient connection mode. The chemical reinforcement is fixed on the steel bars or the base materials through the reinforcement-planting glue, so that the building structure has a reinforcing effect, meanwhile, the base materials cannot be damaged due to self-expansion, the original building can be reinforced and improved, and the chemical reinforcement is widely applied to projects of post-planting steel bars limited by construction.
The bar planting adhesive mainly bears compressive, tensile and bending loads, so that the bar planting adhesive needs to have excellent mechanical properties. The epoxy resin bar planting adhesive has excellent mechanical property and adhesive property, but the epoxy resin has large brittleness after being cured and is easy to generate brittle fracture when bearing high-strength load, so that the epoxy resin bar planting adhesive needs to be reinforced and toughened when in use, and after a large amount of modified components are added, the uniformity and compactness of the epoxy resin cured product are destroyed, the durability of the epoxy resin bar planting adhesive can be influenced, and the service life is reduced. The durability of the epoxy reinforced adhesive comprises the contents of wet heat aging resistance and long-term stress resistance, and GB50728-2011 technical Specification for safety identification of materials for engineering structural reinforcement materials also clearly prescribes that building structural adhesive with 30-year and 50-year durability design requirements must pass the test of the wet heat aging resistance and the long-term stress resistance, so that the preparation of the reinforced adhesive with high toughness and high wet heat resistance is a problem to be solved at present.
Disclosure of Invention
In order to improve the strength, toughness and wet heat aging resistance of the bar planting adhesive and further improve the durability of the bar planting adhesive, the application provides an injection type bar planting adhesive and a preparation method thereof, wherein the following technical scheme is adopted:
in a first aspect, the present application provides an injection-type bar planting adhesive, which adopts the following technical scheme: the injection type bar planting adhesive comprises two components, namely an A component and a B component, wherein the mass ratio of the A component to the B component is 3:1, and the A component comprises the following substances in parts by weight: 50-70 parts of matrix resin; 20-40 parts of modified filler; 4-6 parts of thixotropic agent; 3-5 parts of a diluent; 2-4 parts of a coupling agent; the component B comprises the following substances in parts by weight: 50-60 parts of a flexible curing agent; 20-30 parts of modified filler; 6-8 parts of a promoter; 1-3 parts of a diluent; 3-5 parts of thixotropic agent; 2-4 parts of a coupling agent; the matrix resin comprises the following components in percentage by mass 1-2:4-5 and bisphenol A epoxy vinyl resin.
Through the technical scheme, the matrix resin is preferably selected, the phenolic epoxy resin and the bisphenol A epoxy vinyl resin are compounded, the bisphenol A epoxy vinyl resin has high strength, good adhesiveness and low viscosity, and a large number of bisphenol A epoxy vinyl resin molecules are added into a phenolic epoxy resin system, so that the viscosity of the phenolic epoxy resin can be effectively reduced, and the workability of the phenolic epoxy resin and the bisphenol A epoxy vinyl resin is optimized; when the cross-linking curing reaction occurs, bisphenol A epoxy vinyl resin only cross-links at unsaturated double bond positions at two ends of a molecular chain, and a molecular middle chain segment, particularly an ether group, cannot be changed at all, so that the molecular chain has relatively large activity under the action of stress, can absorb the action of thermal shock and external force, and shows good heat resistance and impact resistance, the phenolic epoxy resin has relatively large number of epoxy groups in molecules, the cross-linking density of a cured product is high, the two are compounded, the structural compactness of a cured product is further improved, water vapor can be effectively blocked, the water vapor is prevented from invading into a glue layer, and the wet heat aging resistance of the bar planting glue is further improved; meanwhile, the two matrix resins optimized by the method are used in a compounding way, the reaction activity is high, the curing reaction can be carried out at low temperature, the early strength performance of the matrix resins is improved, and the construction requirement strength can be achieved in a short time.
In addition, the application also prefers curing agent, modified filler and functional auxiliary agent as effective components to be added into the injection type bar planting adhesive system, active groups in the curing agent molecules can react with epoxy groups in matrix resin to generate a three-dimensional network structure, so that the mechanical property of the bar planting adhesive is improved, and the fixing and reinforcing effects are exerted; the modified filler can be compounded with the matrix resin, so that the shrinkage rate of a cured product is effectively reduced, and the mechanical property and the wet heat aging resistance of the bar planting adhesive are improved; the addition of the coupling agent not only can promote the uniform dispersion of the raw material components, but also can improve the bonding performance of the bar planting adhesive and a construction interface, so that the bonding is tighter; the thixotropic agent can improve the consistency of the bar planting adhesive and improve the workability.
Further, the matrix resin also comprises 5-15 parts by weight of vinyl silicon MQ resin.
Through the technical scheme, the selection of the matrix resin is further optimized, the vinyl silicon MQ resin is added into the matrix resin system, and the vinyl silicon MQ resin contains organic silicon active groups and has excellent thermosetting performance, so that the heat resistance of the matrix resin system can be effectively improved, and the high-temperature decomposition of a cured product is reduced; the vinyl group and the organic silicon resin group can also form a good promoting effect on the curing of the matrix resin, the curing crosslinking degree of the resin is further improved, no small molecule byproducts are generated and released in the curing process, the density of the cured product of the bar planting glue is improved, the curing shrinkage rate is reduced, and the mechanical property of the bar planting glue is improved; the vinyl silicon MQ resin has excellent hydrophobic performance, and the addition of the vinyl silicon MQ resin can improve the hydrophobic effect of the surface of the bar planting adhesive and reduce the infiltration of water vapor, so that the anti-aging performance of the bar planting adhesive is improved.
Further, the flexible curing agent in the component B is epoxy resin modified diethylenetriamine.
According to the technical scheme, the selection of the curing agent is optimized, the curing performance of the diethylenetriamine is excellent, and the cured product cured by the diethylenetriamine has better chemical corrosion resistance, and the epoxy resin is adopted to modify the diethylenetriamine to generate the macromolecular curing agent, so that the heat resistance stability of the curing agent can be effectively improved, the dispersibility of the curing agent modified by the epoxy resin in an epoxy resin system is better according to a similar compatibility principle, the curing agent can be uniformly distributed in the system, the formed cured product is more uniform, and the occurrence of local brittle fracture condition is effectively reduced; the flexible long carbon chain access curing agent can further improve the shock resistance of the cured product, so that the toughness of the cured product is further improved, and the shearing stress resistance of the product is improved.
Further, the accelerator in the component B comprises an imidazole curing agent, and the imidazole curing agent comprises at least one of N-vinyl imidazole or diethyl tetramethyl imidazole.
Through the technical scheme, the composition of the accelerator is optimized, the imidazole curing agent contains tertiary amine nitrogen atoms, can initiate epoxy groups to carry out anionic chain polymerization, has the characteristic of medium-temperature rapid curing, and has high curing efficiency, and the formed cured product has higher heat distortion temperature and good heat resistance and chemical resistance. The N-vinyl imidazole and the diethyl tetramethyl imidazole which are preferred by the application are low-viscosity liquids at normal temperature, can be uniformly dispersed in an epoxy resin system, are compounded with a polyamine curing agent for use, and have obvious promotion effect on the curing strength of early-stage bar planting glue.
Further, the diluent in the component A and B is propylene carbonate.
By the technical scheme, propylene carbonate is preferably used as a diluent in the component A and B, and the addition of the propylene carbonate can effectively reduce the viscosity of the component A and B, improve the rheological property and facilitate the extrusion and mixing of the component A and B when in use; the propylene carbonate and the diethylenetriamine have good chemical compounding effect, the diethylenetriamine can preferentially perform ring-opening reaction with the propylene carbonate, and the formed amide bond is favorable for improving the bonding strength between the bar planting glue and the concrete, so that the bonding is more compact, and the invasion of external penetrating water to the bar planting glue is effectively reduced.
Further, the modified filler in the component A and the component B comprises a graphene-organic montmorillonite composite material and nano calcium carbonate, wherein the nano calcium carbonate is modified by a titanate silane coupling agent, and the mass ratio of the graphene-organic montmorillonite composite material to the modified nano calcium carbonate is (1-2): 4-6.
According to the technical scheme, the composition of the filler and the proportion of each component are further optimized, and the nano calcium carbonate is used as inorganic rigid particles, has a larger specific surface area and stronger surface activity, can improve the bonding performance of a system interface, and enables the bonding to be tighter and the structure to be more compact and waterproof; the bar planting adhesive doped with nano calcium carbonate has a very large interface, and interface atoms are disordered in arrangement, and when the bar planting adhesive is subjected to external force deformation and thermal shock, migration is easy to occur, and a large amount of plastic deformation energy and heat are absorbed, so that the effects of toughening and improving thermal stability are achieved; the titanate coupling agent modified nano calcium carbonate has good compatibility with matrix resin, high dispersibility, difficult precipitation of the filler after solidification, and the surface of the surface modified nano calcium carbonate particles is hydrophobic, so that the brittle fracture of a solidified product caused by molecular aggregation is reduced, the hydrophobic property of the bar planting adhesive is further improved, and the infiltration and invasion of water molecules are reduced, thereby improving the mechanical property and the anti-aging property of the bar planting adhesive.
Alkenyl on the surface of the organic montmorillonite lamellar can generate a crosslinking reaction with double bonds in a resin molecular chain, and meanwhile, the addition of graphene can promote the further generation of a crosslinking effect, and the crosslinking effect can also promote the migration of the resin molecular chain to the organic montmorillonite lamellar to form an intercalation composite interface, so that the effect of a micro-skeleton is achieved, the stress can be effectively dispersed, cracking cracks are promoted to be uniformly dispersed and terminated along the composite intercalation interface, and the compression resistance and stress fracture resistance of a resin system are improved.
The graphene-organic montmorillonite composite material has good thermal stability, and the flaky graphene-organic montmorillonite composite material and granular nano calcium carbonate are compounded for use, so that the compactness and continuity of a cured product can be further improved, heat transfer is effectively blocked, and the heat-resistant stability of the cured product is further improved.
Further, the preparation of the graphene-organic montmorillonite composite material comprises the following steps: (1) graphene modification: adding graphene and dicyclohexylcarbodiimide into a silane coupling agent, performing ultrasonic dispersion, heating, performing heat preservation reaction for 12 hours, cooling, centrifuging, washing, and performing vacuum drying to obtain modified graphene; (2) preparation of a dispersion: respectively adding the organic montmorillonite and the modified graphene into deionized water, and performing ultrasonic dispersion to obtain modified graphene dispersion liquid and organic montmorillonite dispersion liquid respectively; (3) preparation of composite material: and adding the modified graphene dispersion liquid into the organic montmorillonite dispersion liquid, heating, preserving heat and stirring for 12 hours to obtain a mixed liquid, centrifuging the mixed liquid, and drying in vacuum to obtain the graphene-organic montmorillonite composite material.
Through the technical scheme, the preparation method of the graphene-organic montmorillonite composite material is optimized, the graphene modified by the silane coupling agent is intercalated into the lamellar of the organic montmorillonite through hydrogen bond and crosslinking, and the prepared composite material is more tightly combined through physical and chemical double action, so that the stability of the composite material is improved; by adopting the preparation method for respectively preparing and remixing the dispersion liquid of each component, the dispersion of each component is more uniform, the possibility of agglomeration during graphene intercalation can be effectively reduced, and the prepared material is more uniform and stable.
In a second aspect, the present application provides a method for preparing an injection-type bar planting adhesive, including the following preparation steps: s1: and (3) preparation of a component A: weighing raw materials according to the proportion of the raw materials of the component A, firstly adding matrix resin and a coupling agent into a reaction container, stirring and mixing to obtain a mixture A, then adding a modified filler, a diluent and a thixotropic agent into the mixture A while stirring, and after the addition is finished, carrying out vacuum pressure maintaining and stirring, ultrasonic dispersion and defoaming to complete the preparation of the component A; s2: and (2) preparing a component B: weighing raw materials according to the proportion of the component B, firstly adding a flexible curing agent, an accelerator and a coupling agent into a reaction container, fully stirring the mixed mixture B, then adding a modified filler and a diluent into the mixture B while stirring, and after the addition is finished, carrying out vacuum pressure maintaining stirring, ultrasonic dispersion defoaming and finishing the preparation of the component B; s3: preparation of injection type bar planting glue: and injecting the component A and the component B into the double rubber pipe according to the mass ratio of 3:1, and sealing by a sealing cover to obtain the injection type bar planting adhesive.
Through above-mentioned technical scheme, the utility model has optimized the addition order of each raw materials component, add the mixture step by step, can effectively promote the even dispersion of each component, vacuum pressurize stirring, ultrasonic dispersion defoaming is favorable to improving the homogeneity and the compactness of first and second components, and when the encapsulation is after, each active ingredient is more even, has reduced the fracture condition that leads to because of mixing inhomogeneous during the use, further improves the compactness of solidification product to improve the durability of planting muscle and glue.
In summary, the present application has the following beneficial effects:
1. the preparation method optimizes the selection of matrix resin, adopts phenolic epoxy resin, bisphenol A epoxy vinyl resin and vinyl silicon MQ resin for compounding, and has high reaction activity of the compounded resin system, can be cured at low temperature and has excellent early strength performance; the curing and crosslinking degree of the compounded resin is further improved, an interpenetrating polymer network structure can be formed, and the heat resistance and impact resistance of the matrix resin are effectively improved; the compounded matrix resin has compact structure and hydrophobic surface, and can effectively prevent infiltration and invasion of water vapor, thereby improving the anti-aging performance of the cured bar planting adhesive.
2. According to the self-made flexible curing agent, the epoxy resin is used for modifying the diethylenetriamine, the flexible long-carbon-chain curing agent is connected to improve the shock resistance of a cured product, and according to a similar compatibility principle, the modified diethylenetriamine is promoted to be uniformly distributed in the bar planting adhesive system, so that the curing reaction is more uniform, the occurrence of local brittle fracture condition is effectively reduced, and the durability of the bar planting adhesive is improved.
3. The composition of the modified filler and the proportion of each component are optimized, the compatibility of the titanate coupling agent modified nano calcium carbonate and the matrix resin is good, the dispersibility is high, and the reinforcing and toughening effects of the nano material on the matrix resin are effectively exerted; the graphene-organic montmorillonite composite material can form an intercalation composite interface with matrix resin, so that the effect of a micro-skeleton is achieved, and the compression resistance and stress fracture resistance of a resin system are improved; and the flaky graphene-organic montmorillonite composite material and the granular nano calcium carbonate are compounded for use, so that the compactness and the continuity of a cured product can be further improved, and the durability of the bar planting adhesive is further improved.
4. The application optimizes the selection of the accelerator and the diluent, the imidazole curing agent has high curing efficiency as the accelerator, is used by being compounded with the polyamine curing agent, has obvious promoting effect on the curing strength of early-stage bar planting glue, and has good heat resistance of a cured product; propylene carbonate is added as a diluent to effectively reduce the viscosity of the component A and the component B, improve the rheological property, facilitate the extrusion and mixing of the component A and the component B, and simultaneously form a good chemical compounding effect with a flexible curing agent, so that the bonding capability of the bar planting adhesive and an external concrete interface is improved, the contact interface bonding is more compact, the invasion of external penetrating water to the bar planting adhesive is effectively reduced, and the water aging resistance of the bar planting adhesive is improved.
5. The preparation method of the injection type bar planting adhesive is further optimized, the addition sequence of the raw material components is optimized, the vacuum pressure maintaining stirring and ultrasonic dispersion defoaming technology is adopted, uniform mixing and densification of the components are effectively promoted, and therefore more excellent mixing and curing effects are obtained during extrusion, and the stability of a product is improved.
Detailed Description
The present application is described in further detail below in connection with examples and comparative examples.
The materials herein may be commercially available products, and the following sources are merely examples and are not representative of the specified materials.
F51 phenolic epoxy resin was purchased from sandisk chemical company, inc;
bisphenol A type epoxy vinyl resin was purchased from Guangdong Bogoso composite Co., ltd;
vinyl MQ resins were purchased from the company, guangzhou, aggregation megaindustry silicone feedstock limited;
TY-710C organic montmorillonite was purchased from Guangzhou Yifeng chemical technology Co., ltd;
4566N-vinylimidazole was purchased from Shanghai ringing chemical Co., ltd;
diethyl tetramethylimidazole, propylene carbonate, were purchased from Shanghai ethyl chemical Co., ltd;
diethylenetriamine is available from the biotechnology power supplier of the Guangzhou molecular;
ZK-211109-01 diethylene glycol methyl ether is purchased from Jinan Ze chemical industry Co., ltd;
epoxy butyl oleate Shenzhen Kaiqi chemical Co., ltd;
KD-4810 bisphenol A type liquid epoxy resin is purchased from a new material technology strong supplier;
the 201-type titanate coupling agent is purchased from Dinghai plastic chemical industry power suppliers in Dongguan city;
the nano calcium carbonate is purchased from Jingjiang city high chemical industry Co., ltd;
DN-TE9 dicyclohexylcarbodiimide was purchased from Shandong Denno chemical Co., ltd;
PT-C-001 type graphene is purchased from Shanghai Panta powder materials Co., ltd;
KH-550 type silane coupling agent is purchased from Shandong energy-accumulating chemical Co., ltd;
the thixotropic agent in the raw material is fumed silica, and the coupling agent is KH-550 type silane coupling agent.
Preparation example
Preparation example 1
5kg of diethylenetriamine, 13kg of diethylene glycol methyl ether, 6kg of bisphenol A liquid epoxy resin and 12kg of epoxy butyl oleate are respectively weighed, 5kg of diethylenetriamine is added into 8kg of diethylene glycol methyl ether, the mixture is heated to 65 ℃ while stirring, constant temperature and continuous stirring are carried out, bisphenol A liquid epoxy resin is dropwise added into the mixed liquid, the dropwise adding speed is controlled to be 20g/min for 5 hours, after the dropwise adding is finished, the reaction is continued for 1 hour, the diethylenetriamine-epoxy resin prepolymer is prepared, 5kg of diethylene glycol methyl ether is further added into the prepolymer, the temperature is controlled to be 60 ℃, the dropwise adding of epoxy butyl oleate is continued, the dropwise adding speed is controlled to be 50g/min for 4 hours, the reaction is continued for 30 minutes after the dropwise adding is finished, and the product is subjected to distillation passivation, so that the flexible curing agent can be obtained. The above steps are repeated for a plurality of times to meet the requirement of use.
Preparation example 2
Adding 10kg of nano calcium carbonate into 20L of absolute ethyl alcohol, stirring, performing ultrasonic dispersion for 30min to obtain uniform suspension, adding 1.5kg of titanate coupling agent into the suspension, performing ultrasonic mixing for 10min, raising the temperature to 60 ℃, performing constant-temperature reaction for 6h, separating the reaction solution by adopting a high-speed centrifuge, controlling the rotating speed of the centrifuge to 8000r/min, performing vacuum drying on the separated product, and grinding to obtain the modified nano calcium carbonate. Repeating the steps, and preparing for multiple times to meet the requirement of use.
Preparation example 3
Weighing 5kg KH-550 type silane coupling agent, 0.8kg graphene and 0.4kg dicyclohexyl carbodiimide respectively, adding graphene and dicyclohexyl carbodiimide into the silane coupling agent, performing ultrasonic dispersion for 1h, increasing the temperature to 75 ℃, performing heat preservation reaction for 12h, cooling, centrifuging, washing and performing vacuum drying to obtain modified graphene; repeating the steps, and preparing for multiple times to meet the requirement of use.
Preparation example 4
Respectively weighing 10kg of organic montmorillonite, 1kg of modified graphene and 18kg of deionized water, adding the organic montmorillonite into 15kg of deionized water, adding the modified graphene into 3kg of deionized water, and performing ultrasonic dispersion for 30min to respectively obtain modified graphene dispersion liquid and organic montmorillonite dispersion liquid; adding the modified graphene dispersion liquid into the organic montmorillonite dispersion liquid while stirring, carrying out heat preservation and stirring for 12h to obtain a mixed liquid, carrying out centrifugal separation on the mixed liquid, and carrying out vacuum drying on the separated product to obtain the graphene-organic montmorillonite composite material.
Preparation examples 5 to 7
Respectively weighing phenolic epoxy resin and bisphenol A epoxy vinyl resin, specifically, the mass is shown in table 1, and mixing to obtain matrix resin 1-3.
TABLE 1 preparation examples 5-7 raw material composition
Preparation examples 8 to 10
The graphene-organic montmorillonite composite material and the modified nano calcium carbonate are respectively weighed, the specific mass is shown in table 2, and the modified filler 1-3 can be obtained after mixing.
TABLE 2 preparation examples 8-10 raw material composition
Preparation examples 11 to 13
N-vinylimidazole and diethyl tetramethylimidazole were weighed separately, the specific mass is shown in Table 3, and accelerators 1-3 were mixed.
TABLE 3 preparation examples 11-13 raw material composition
Examples
Example 1
In a first aspect, the application provides an injection type bar planting adhesive, which comprises two components, namely a component A and a component B, wherein the component A comprises the following substances in parts by weight: 5kg of matrix resin 1, 2kg of modified filler 1, 0.4kg of thixotropic agent, 0.3kg of propylene carbonate, 0.2kg of coupling agent and the component B comprises the following substances by weight: 5kg of a flexible curing agent, 2kg of a modified filler, 0.6kg of an accelerator 1, 0.1kg of propylene carbonate, 0.3kg of a thixotropic agent and 0.2kg of a coupling agent.
In a second aspect, the present application provides a method for preparing an injection-type bar planting adhesive, including the following preparation steps: s1: and (3) preparation of a component A: weighing raw materials according to the proportion of the raw materials of the component A, firstly adding the matrix resin 1 and the coupling agent into a reaction container, stirring and mixing to obtain a mixture A, then adding the modified filler 1, the propylene carbonate and the thixotropic agent into the mixture A while stirring, and after the addition is finished, carrying out vacuum pressure maintaining and stirring for 30min, carrying out ultrasonic dispersion and defoaming, thus finishing the preparation of the component A; s2: and (2) preparing a component B: weighing raw materials according to the proportion of the component B, firstly adding a flexible curing agent, an accelerator 1 and a coupling agent into a reaction container, fully stirring the mixed mixture B, then adding a modified filler 1 and propylene carbonate into the mixture while stirring, and after the addition is finished, carrying out vacuum pressure maintaining stirring for 30min, carrying out ultrasonic dispersion and defoaming, thus finishing the preparation of the component B; s3: preparation of injection type bar planting glue: and respectively taking 3kg of the component A and 1kg of the component B, injecting into the double rubber tube, and sealing by a sealing cover to obtain the injection type bar planting adhesive.
Example 2
In a first aspect, the application provides an injection type bar planting adhesive, which comprises two components, namely a component A and a component B, wherein the component A comprises the following substances in parts by weight: 6kg of matrix resin 1, 3kg of modified filler 1, 0.5kg of thixotropic agent, 0.4kg of propylene carbonate, 0.3kg of coupling agent and the component B comprises the following substances by weight: 5.5kg of flexible curing agent, 2.5kg of modified filler, 0.7kg of accelerator 1, 0.2kg of propylene carbonate, 0.4kg of thixotropic agent and 0.3kg of coupling agent.
In a second aspect, the present application provides a method for preparing an injection-type bar planting adhesive, including the following preparation steps: s1: and (3) preparation of a component A: weighing raw materials according to the proportion of the raw materials of the component A, firstly adding the matrix resin 1 and the coupling agent into a reaction container, stirring and mixing to obtain a mixture A, then adding the modified filler 1, the propylene carbonate and the thixotropic agent into the mixture A while stirring, and after the addition is finished, carrying out vacuum pressure maintaining and stirring for 30min, carrying out ultrasonic dispersion and defoaming, thus finishing the preparation of the component A; s2: and (2) preparing a component B: weighing raw materials according to the proportion of the component B, firstly adding a flexible curing agent, an accelerator 1 and a coupling agent into a reaction container, fully stirring the mixed mixture B, then adding a modified filler 1 and propylene carbonate into the mixture while stirring, and after the addition is finished, carrying out vacuum pressure maintaining stirring for 30min, carrying out ultrasonic dispersion and defoaming, thus finishing the preparation of the component B; s3: preparation of injection type bar planting glue: and respectively taking 3kg of the component A and 1kg of the component B, injecting into the double rubber tube, and sealing by a sealing cover to obtain the injection type bar planting adhesive.
Example 3
In a first aspect, the application provides an injection type bar planting adhesive, which comprises two components, namely a component A and a component B, wherein the component A comprises the following substances in parts by weight: 7kg of matrix resin 1, 4kg of modified filler 1, 0.6kg of thixotropic agent, 0.5kg of propylene carbonate, 0.4kg of coupling agent and the component B comprises the following substances by weight: 6kg of a flexible curing agent, 3kg of a modified filler, 0.8kg of an accelerator 1, 0.3kg of propylene carbonate, 0.5kg of a thixotropic agent and 0.4kg of a coupling agent.
In a second aspect, the present application provides a method for preparing an injection-type bar planting adhesive, including the following preparation steps: s1: and (3) preparation of a component A: weighing raw materials according to the proportion of the raw materials of the component A, firstly adding the matrix resin 1 and the coupling agent into a reaction container, stirring and mixing to obtain a mixture A, then adding the modified filler 1, the propylene carbonate and the thixotropic agent into the mixture A while stirring, and after the addition is finished, carrying out vacuum pressure maintaining and stirring for 30min, carrying out ultrasonic dispersion and defoaming, thus finishing the preparation of the component A; s2: and (2) preparing a component B: weighing raw materials according to the proportion of the component B, firstly adding a flexible curing agent, an accelerator 1 and a coupling agent into a reaction container, fully stirring the mixed mixture B, then adding a modified filler 1 and propylene carbonate into the mixture while stirring, and after the addition is finished, carrying out vacuum pressure maintaining stirring for 30min, carrying out ultrasonic dispersion and defoaming, thus finishing the preparation of the component B; s3: preparation of injection type bar planting glue: and respectively taking 3kg of the component A and 1kg of the component B, injecting into the double rubber tube, and sealing by a sealing cover to obtain the injection type bar planting adhesive.
Examples 4 to 6
The difference from example 2 is that: the vinyl silicon MQ resin is weighed, the specific mass is shown in Table 4, the vinyl silicon MQ resin and the matrix resin are added into a reaction vessel to be stirred and mixed, and the rest preparation conditions and the preparation environment are the same as those of the example 2, so that the injection type bar planting adhesive is prepared.
TABLE 4 examples 4-6 raw material composition
Examples 7 to 8
The difference from example 5 is that: the matrix resin 2-3 is used for replacing the matrix resin 1 to prepare the injection type bar planting adhesive, and the rest preparation conditions and preparation environment are the same as those of the example 5.
Examples 9 to 10
The difference from example 7 is that: the modified filler 2-3 is used for replacing the modified filler 1 to prepare the injection type bar planting adhesive, and the rest preparation conditions and preparation environment are the same as those of the example 7.
Examples 11 to 12
The difference from example 9 is that: the accelerator 1 was replaced with the accelerator 2-3 to prepare an injection type bar planting adhesive, and the other preparation conditions and preparation environments were the same as those of example 9.
Comparative example
Comparative example 1
The difference from example 1 is that: only bisphenol a type epoxy vinyl resin was added as a matrix resin during the preparation, and the rest of the preparation process and conditions were the same as in example 1.
Comparative example 2
The difference from example 1 is that: only unmodified nano calcium carbonate was added as a modified filler during the preparation, and the rest of the preparation process and conditions were the same as in example 1.
Comparative example 3
The difference from example 1 is that: only diethylenetriamine was added as a curing agent during the preparation, and the rest of the preparation process and conditions were the same as in example 1.
Test experiment
The injectable bar planting glue prepared in examples 1-12 and comparative examples 1-3 were tested for tensile shear strength, wet heat aging resistance and long-term stress resistance.
Test method
(1) Tensile shear strength: the test was carried out with reference to GB/T7124-2008 "determination of tensile shear Strength of Adhesives (rigid Material vs rigid Material").
(2) Wet heat aging resistance test: the tensile shear test specimen was aged for 90d in a constant temperature and humidity cabinet at 50 ℃ and a relative humidity of 95%, and then cooled to room temperature for tensile shear strength test.
(3) Long-term stress resistance performance test: and in the environment with the temperature of (23+/-2) ℃ and the relative humidity of (50+/-5)%, applying the shearing stress of 4.0MPa to the tensile shear test piece by adopting a creep testing machine for continuous action 210d, and measuring the creep distance.
TABLE 5 Performance test of examples 1-12, comparative examples 1-3
Analysis of the test results in table 5:
(1) From a group of examples 1-3 and comparative example 1, and by analyzing the data in Table 5, the initial tensile shear strength and the tensile shear strength after wet heat aging of the injection type bar planting adhesive prepared in examples 1-3 are higher than those of comparative example 1, and the percentage of decrease in tensile shear strength is higher than that of comparative example 1, which indicates that after the phenolic epoxy resin and the bisphenol A type epoxy vinyl resin are compounded,
the curing crosslinking density of the two is greater than that of the single bisphenol A epoxy vinyl resin, the structure of the cured product is compact, the intrusion of water vapor into the adhesive layer can be effectively prevented, and the two resins can form an interpenetrating polymer network structure, so that the heat resistance and the impact resistance of the matrix resin are effectively improved. In the actual preparation and test process, the bar planting glue prepared in the comparative example 1 has low thixotropy, and can generate sagging phenomenon when being vertically used, which indicates that the construction performance of the bar planting glue can be improved by compounding the phenolic epoxy resin and the bisphenol A epoxy vinyl resin.
(2) By taking examples 1-3 and comparative example 2 as a group and analyzing the data in combination with Table 5, the initial tensile shear strength and the tensile shear strength after wet heat aging of the injection type bar planting glue prepared in examples 1-3 are far higher than those of comparative example 2, and the tensile shear strength reduction percentage is far higher than that of comparative example 1, which shows that the compactness and the continuity of a cured product can be effectively improved by compounding the modified nano calcium carbonate and the graphene-organic montmorillonite composite material, and the layered organic montmorillonite structure can effectively block heat transfer, so that the heat stability and the water aging resistance of the cured product are improved; unmodified nano calcium carbonate adopted in the comparative example has poor compounding effect with a matrix, is not uniformly dispersed, is easy to generate microcracks at particle aggregation positions, and leads water vapor to enter the colloid, so that the tensile shear strength is lower, and the wet heat aging resistance is also poor.
(3) By taking examples 1-3 and comparative example 3 as a group and analyzing the data in table 5, the initial tensile shear strength and the tensile shear strength after wet heat aging of the injection type bar planting adhesive prepared in examples 1-3 are higher than those of comparative example 3, because the unmodified diethylenetriamine is poor in compounding effect with a matrix in matrix resin as a curing agent, and is easy to separate out during curing, local brittle fracture is caused, and the compounding effect of the curing agent after epoxy resin modification and the matrix is high, so that the injection type bar planting adhesive has more excellent mechanical properties.
(4) Examples 4-6 and example 2 are a group, and analysis is carried out by combining the data of table 5, the initial tensile shear strength and the tensile shear strength after wet heat aging of the injection type bar planting glue prepared in examples 4-6 are higher than those of example 2, which shows that the addition of vinyl MQ resin can effectively improve the wet heat aging resistance and mechanical property of the bar planting glue, because the addition of three resins can further improve the interpenetrating crosslinking degree of a cured product, the introduction of a resin silicon active group can also improve the heat stability of a resin system, meanwhile, the hydrophobic effect of the surface of the cured product is improved, and the infiltration of water vapor is reduced, so that the water aging resistance of the bar planting glue is further improved.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (7)
1. The injection type bar planting adhesive is characterized by comprising two components A and B, wherein the mass ratio of the components A and B is 3:1, and the components A comprise the following substances in parts by weight:
50-70 parts of matrix resin;
20-40 parts of modified filler;
4-6 parts of thixotropic agent;
3-5 parts of a diluent;
2-4 parts of a coupling agent;
the component B comprises the following substances in parts by weight:
50-60 parts of a flexible curing agent;
20-30 parts of modified filler;
6-8 parts of a promoter;
1-3 parts of a diluent;
3-5 parts of thixotropic agent;
2-4 parts of a coupling agent;
the matrix resin comprises the following components in percentage by mass 1-2:4-5 of phenolic epoxy resin and bisphenol A epoxy vinyl resin;
the flexible curing agent in the component B is epoxy resin modified diethylenetriamine.
2. The injection type bar planting adhesive according to claim 1, wherein the matrix resin further comprises 5-15 parts by weight of vinyl silicone MQ resin.
3. An injectable bar planting adhesive according to claim 1 wherein the accelerator in the b component comprises an imidazole curing agent comprising at least one of N-vinylimidazole or 2-ethyl-4-methylimidazole.
4. The injectable bar planting adhesive according to claim 1, wherein the diluent in the component a and b is propylene carbonate.
5. The injection type bar planting adhesive according to claim 1, wherein the modified fillers in the component A and component B comprise graphene-organic montmorillonite composite materials and nano calcium carbonate, the nano calcium carbonate is modified nano calcium carbonate by a titanate silane coupling agent, and the mass ratio of the graphene-organic montmorillonite composite materials to the modified nano calcium carbonate is 1-2:4-6.
6. The injection type bar planting adhesive according to claim 5, wherein the preparation of the graphene-organic montmorillonite composite material comprises the following steps:
(1) Modification of graphene: adding graphene and dicyclohexylcarbodiimide into a silane coupling agent, performing ultrasonic dispersion, heating, performing heat preservation reaction for 12 hours, cooling, centrifuging, washing, and performing vacuum drying to obtain modified graphene;
(2) Preparing a dispersion liquid: respectively adding the organic montmorillonite and the modified graphene into deionized water, and performing ultrasonic dispersion to obtain modified graphene dispersion liquid and organic montmorillonite dispersion liquid respectively;
(3) Preparing a composite material: and adding the modified graphene dispersion liquid into the organic montmorillonite dispersion liquid, heating, preserving heat and stirring for 12 hours to obtain a mixed liquid, centrifuging the mixed liquid, and drying in vacuum to obtain the graphene-organic montmorillonite composite material.
7. A method for preparing the injection type bar planting adhesive as set forth in any one of claims 1 to 6, comprising the following preparation steps:
s1: and (3) preparation of a component A:
weighing raw materials according to the proportion of the raw materials of the component A, firstly adding matrix resin and a coupling agent into a reaction container, stirring and mixing to obtain a mixture A, then adding a modified filler, a diluent and a thixotropic agent into the mixture A while stirring, and after the addition is finished, carrying out vacuum pressure maintaining and stirring, ultrasonic dispersion and defoaming to complete the preparation of the component A;
s2: and (2) preparing a component B:
weighing raw materials according to the proportion of the component B, firstly adding a flexible curing agent, an accelerator and a coupling agent into a reaction container, fully stirring and mixing to obtain a mixture B, adding a modified filler and a diluent into the mixture B while stirring, and after the addition is finished, carrying out vacuum pressure maintaining and stirring, ultrasonic dispersion and defoaming to complete the preparation of the component B;
s3: preparation of injection type bar planting glue:
and injecting the component A and the component B into the double rubber pipe according to the mass ratio of 3:1, and sealing by a sealing cover to obtain the injection type bar planting adhesive.
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| CN103614104B (en) * | 2013-11-13 | 2015-04-08 | 苏州市姑苏新型建材有限公司 | Low-temperature epoxy adhesive for embedded steel bars and preparation method of adhesive |
| CN106118567A (en) * | 2016-06-24 | 2016-11-16 | 卡本复合材料（天津）有限公司 | A kind of bi-component injection epoxy anchoring adhesive and preparation method thereof |
| CN109337299B (en) * | 2018-09-11 | 2021-02-02 | 法施达(大连)实业集团有限公司 | Modified vinyl bar-planting adhesive and preparation method thereof |
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